Light-Cured Self-Etch Adhesives Undergo Hydroxyapatite-Triggered Self-Cure

PubMed Central

Liu, Y.; Bai, X.; Liu, Y.W.; Wang, Y.

2015-01-01

Light cure is a popular mode of curing for dental adhesives. However, it suffers from inadequate light delivery when the restoration site is less accessible, in which case a self-cure mechanism is desirable to salvage any compromised polymerization. We previously reported a novel self-cure system mediated by ethyl 4-(dimethylamino)-benzoate (4E) and hydroxyapatite (HAp). The present work aims to investigate if such self-cure phenomenon takes place in adhesives that underwent prior inadequate light cure and to elucidate if HAp released from the dental etching process is sufficient to trigger it. Model self-etch adhesives were formulated with various components, including bis[2-methacryloyloxy)ethyl]-phosphate (2MP) as acidic monomer and trimethylbenzoyl-diphenylphosphine oxide (TPO) as photoinitiator. In vitro evolution of degree of conversion (DC) of HAp-incorporated adhesives was monitored by infrared spectroscopy during light irradiation and dark storage. Selected adhesives were allowed to etch and extract HAp from enamel, light-cured in situ, and stored in the dark, after which Raman line mapping was used to obtain spatially resolved DC across the enamel-resin interface. Results showed that TPO+4E adhesives reached DC similar to TPO-only counterparts upon completion of light irradiation but underwent another round of initiation that boosted DC to ~100% regardless of HAp level or prior light exposure. When applied to enamel, TPO-only adhesives had ~80% DC in resin, which gradually descended to ~50% in enamel, whereas TPO+4E adhesives consistently scored ~80% DC across the enamel-resin interface. These observations suggest that polymerization of adhesives that underwent insufficient light cure is salvaged by the novel self-cure mechanism, and such salvaging effect can be triggered by HAp released from dental substrate during the etching process. PMID:26635279

Micromorphological characterization of adhesive interface of sound dentin and total-etch and self-etch adhesives.

PubMed

Drobac, Milan; Stojanac, Igor; Ramić, Bojana; Premović, Milica; Petrović, Ljubomir

2015-01-01

The ultimate goal in restorative dentistry has always been to achieve strong and permanent bond between the dental tissues and filling materials. It is not easy to achieve this task because the bonding process is different for enamel and dentin-dentin is more humid and more organic than enamel. It is moisture and organic nature of dentin that make this hard tissue very complex to achieve adhesive bond. One of the first and most widely used tools for examining the adhesive bond between hard dental tissues and composite restorative materials is scanning electron microscopy. The aim of this study was scanning electron microscopy analyzes the interfacial micro morphology of total-etch and self-etch adhesives. Micro morphological characteristics of interface between total-etch adhesive (Prime & Bond NT) in combination with the corresponding composite (Ceram X Mono) were compared with those of self-etching adhesive (AdheSE One) in, combination with the corresponding composite (Tetric EvoCeram). The specimens were observed under 1000 x magnification of scanning electron microscopy (JEOL, JSM-6460 Low Vacuum). Measurement of the thickness of the hybrid layer of the examined com posite systems was performed with the software of the device used (NIH Image Analyser). Micromorphological analysis of interface showed that the hybrid layer in sound dentin was well formed, its average thickness being 2.68 microm, with a large number of resin tags and a large amount of lateral branches for specimens with a composite system Prime & Bond NT-Ceram X Mono. However, the specimens' with composite systems Adhese One-Tetric EvoCeram did not show the presence of hybrid layer and the resin tags were poorly represented. The results of this study suggest that total-etch adhesives bond better with sound dentin than self-etch adhesive.

Self-etch and etch-and-rinse adhesive systems in clinical dentistry.

PubMed

Ozer, Fusun; Blatz, Markus B

2013-01-01

Current adhesive systems follow either an "etch-and-rinse" or "self-etch" approach, which differ in how they interact with natural tooth structures. Etch-and-rinse systems comprise phosphoric acid to pretreat the dental hard tissues before rinsing and subsequent application of an adhesive. Self-etch adhesives contain acidic monomers, which etch and prime the tooth simultaneously. Etch-and-rinse adhesives are offered as two- or three-step systems, depending on whether primer and bonding are separate or combined in a single bottle. Similarly, self-etch adhesives are available as one- or two-step systems. Both etch-and-rinse and self-etch systems form a hybrid layer as a result of resins impregnating the porous enamel or dentin. Despite current trends toward fewer and simpler clinical application steps, one-step dentin bonding systems exhibit bonding agent lower bond strengths and seem less predictable than multi-step etch-and-rinse and self-etch systems. The varying evidence available today suggests that the choice between etch-and-rinse and self-etch systems is often a matter of personal preference. In general, however, phosphoric acid creates a more pronounced and retentive etching pattern in enamel. Therefore, etch-and-rinse bonding systems are often preferred for indirect restorations and when large areas of enamel are still present. Conversely, self-etch adhesives provide superior and more predictable bond strength to dentin and are, consequently, recommended for direct composite resin restorations, especially when predominantly supported by dentin.

Effect of hydrofluoric acid surface treatments on micro-shear bond strength of CAD/CAM ceramics

PubMed Central

Mokhtarpour, Faraneh; Alaghehmand, Homayoon; Khafri, Soraya

2017-01-01

Introduction Dental ceramics are appreciated as highly esthetic restorative materials that can simulate the appearance of natural dentition better than other materials. The aim of this study was to evaluate the effect of hydrofluoric acid concentration and etching time on micro-shear bond strength (μSBS) to IPS e.max CAD and Vita Mark II of a dual cured resin cement (Panavia F2.0). Methods This study was an experimental in vitro study, performed in the dental material research center of Babol University of Medical Sciences in 2016. Two hydrofluoric acid concentrations (5% and 10%) and three different etching times (20, 60 and 120 seconds) were used to etch the specimens respectively. A silane coupling agent (Clearfil porcelain activator) and priming and bonding agent (Clearfil SE bond) were used on the etched surfaces in accordance to the manufacturer’s instructions of use. Then resin cement was applied on the prepared ceramic surfaces and light cured. μSBS between resin cement and the porcelains were measured with a universal testing machine. Mode of failure was observed with 40× magnification by means of a Stereo microscope. Data were analyzed with ANOVA and independent-samples t-test and Chi-square tests. Results In both e.max and Vita Mark II groups, μSBS were not significantly different when different etching times (one-way ANOVA) and HF acid concentrations (Independent-samples t-test) were used (p>0.05), but the highest μSBS was shown in e.max specimens etched 60 s with 5% HF and Vita Mark II specimens etched 20 s with 10% HF. μSBS of e.max was significantly higher than Vita Mark II (p=0.00). Conclusion Best surface treatment for e.max and Vita Mark II ceramics is 20 s etch using 5 % hydrofluoric acid. PMID:29238488

Hydroxyapatite induces spontaneous polymerization of model self-etch dental adhesives.

PubMed

Zhang, Ying; Wu, Ningjing; Bai, Xinyan; Xu, Changqi; Liu, Yi; Wang, Yong

2013-10-01

The objective of this study is to report for the first time the spontaneous polymerization phenomenon of self-etch dental adhesives induced by hydroxylapatite (HAp). Model self-etch adhesives were prepared by using a monomer mixture of bis[2-(methacryloyloxy)ethyl] phosphate (2MP) with 2-hydroxyethyl methacrylate (HEMA). The initiator system consisted of camphorquinone (CQ, 0.022 mmol/g) and ethyl 4-dimethylaminobenzoate (4E, 0.022-0.088 mmol/g). HAp (2-8 wt.%) was added to the neat model adhesive. In a dark environment, the polymerization was monitored in-situ using ATR/FT-IR, and the mechanical properties of the polymerized adhesives were evaluated using nanoindentation technique. Results indicated that spontaneous polymerization was not observed in the absence of HAp. However, as different amounts of HAp were incorporated into the adhesives, spontaneous polymerization was induced. Higher HAp content led to higher degree of conversion (DC), higher rate of polymerization (RP) and shorter induction period (IP). In addition, higher 4E content also elevated DC and RP and reduced IP of the adhesives. Nanoindentation result suggested that the Young's modulus of the polymerized adhesives showed similar dependence on HAp and 4E contents. In summary, interaction with HAp could induce spontaneous polymerization of the model self-etch adhesives. This result provides important information for understanding the initiation mechanism of the self-etch adhesives, and may be of clinical significance to strengthen the adhesive/dentin interface based on the finding. Copyright © 2013 Elsevier B.V. All rights reserved.

Hydroxyapatite induces spontaneous polymerization of model self-etch dental adhesives

PubMed Central

Zhang, Ying; Wu, Ningjing; Bai, Xinyan; Xu, Changqi; Liu, Yi; Wang, Yong

2013-01-01

The objective of this study is to report for the first time the spontaneous polymerization phenomenon of self-etch dental adhesives induced by hydroxylapatite (HAp). Model self-etch adhesives were prepared by using a monomer mixture of bis[2-(methacryloyloxy)ethyl] phosphate (2MP) with 2-hydroxyethyl methacrylate (HEMA). The initiator system consisted of camphorquinone (CQ, 0.022 mmol/g) and ethyl 4-dimethylaminobenzoate (4E, 0.022–0.088 mmol/g). HAp (2–8 wt.%) was added to the neat model adhesive. In a dark environment, the polymerization was monitored in-situ using ATR/FT-IR, and the mechanical properties of the polymerized adhesives were evaluated using nanoindentation technique. Results indicated that spontaneous polymerization was not observed in the absence of HAp. However, as different amounts of HAp were incorporated into the adhesives, spontaneous polymerization was induced. Higher HAp content led to higher degree of conversion (DC), higher rate of polymerization (RP) and shorter induction period (IP). In addition, higher 4E content also elevated DC and RP and reduced IP of the adhesives. Nanoindentation result suggested that the Young's modulus of the polymerized adhesives showed similar dependence on HAp and 4E contents. In summary, interaction with HAp could induce spontaneous polymerization of the model self-etch adhesives. This result provides important information for understanding the initiation mechanism of the self-etch adhesives, and may be of clinical significance to strengthen the adhesive/dentin interface based on the finding. PMID:23910263

Bond strength of etch-and-rinse and self-etch adhesive systems to enamel and dentin irradiated with a novel CO2 9.3 μm short-pulsed laser for dental restorative procedures.

PubMed

Rechmann, Peter; Bartolome, N; Kinsel, R; Vaderhobli, R; Rechmann, B M T

2017-12-01

The objective of this study was to evaluate the influence of CO 2 9.3 μm short-pulsed laser irradiation on the shear bond strength of composite resin to enamel and dentin. Two hundred enamel and 210 dentin samples were irradiated with a 9.3 µm carbon dioxide laser (Solea, Convergent Dental, Inc., Natick, MA) with energies which either enhanced caries resistance or were effective for ablation. OptiBond Solo Plus [OptiBondTE] (Kerr Corporation, Orange, CA) and Peak Universal Bond light-cured adhesive [PeakTE] (Ultradent Products, South Jordan, UT) were used. In addition, Scotchbond Universal [ScotchbondSE] (3M ESPE, St. Paul, MN) and Peak SE self-etching primer with Peak Universal Bond light-cured adhesive [PeakSE] (Ultradent Products) were tested. Clearfil APX (Kuraray, New York, NY) was bonded to the samples. After 24 h, a single plane shear bond test was performed. Using the caries preventive setting on enamel resulted in increased shear bond strength for all bonding agents except for self-etch PeakSE. The highest overall bond strength was seen with PeakTE (41.29 ± 6.04 MPa). Etch-and-rinse systems achieved higher bond strength values to ablated enamel than the self-etch systems did. PeakTE showed the highest shear bond strength with 35.22 ± 4.40 MPa. OptiBondTE reached 93.8% of its control value. The self-etch system PeakSE presented significantly lower bond strength. The shear bond strength to dentin ranged between 19.15 ± 3.49 MPa for OptiBondTE and 43.94 ± 6.47 MPa for PeakSE. Etch-and-rinse systems had consistently higher bond strength to CO 2 9.3 µm laser-ablated enamel. Using the maximum recommended energy for dentin ablation, the self-etch system PeakSE reached the highest bond strength (43.9 ± 6.5 MPa).

Characterization of the porosity of human dental enamel and shear bond strength in vitro after variable etch times: initial findings using the BET method.

PubMed

Nguyen, Trang T; Miller, Arthur; Orellana, Maria F

2011-07-01

(1) To quantitatively characterize human enamel porosity and surface area in vitro before and after etching for variable etching times; and (2) to evaluate shear bond strength after variable etching times. Specifically, our goal was to identify the presence of any correlation between enamel porosity and shear bond strength. Pore surface area, pore volume, and pore size of enamel from extracted human teeth were analyzed by Brunauer-Emmett-Teller (BET) gas adsorption before and after etching for 15, 30, and 60 seconds with 37% phosphoric acid. Orthodontic brackets were bonded with Transbond to the samples with variable etch times and were subsequently applied to a single-plane lap shear testing system. Pore volume and surface area increased after etching for 15 and 30 seconds. At 60 seconds, this increase was less pronounced. On the contrary, pore size appears to decrease after etching. No correlation was found between variable etching times and shear strength. Samples etched for 15, 30, and 60 seconds all demonstrated clinically viable shear strength values. The BET adsorption method could be a valuable tool in enhancing our understanding of enamel characteristics. Our findings indicate that distinct quantitative changes in enamel pore architecture are evident after etching. Further testing with a larger sample size would have to be carried out for more definitive conclusions to be made.

The Effect of Phosphoric Acid Pre-etching Times on Bonding Performance and Surface Free Energy with Single-step Self-etch Adhesives.

PubMed

Tsujimoto, A; Barkmeier, W W; Takamizawa, T; Latta, M A; Miyazaki, M

2016-01-01

The purpose of this study was to evaluate the effect of phosphoric acid pre-etching times on shear bond strength (SBS) and surface free energy (SFE) with single-step self-etch adhesives. The three single-step self-etch adhesives used were: 1) Scotchbond Universal Adhesive (3M ESPE), 2) Clearfil tri-S Bond (Kuraray Noritake Dental), and 3) G-Bond Plus (GC). Two no pre-etching groups, 1) untreated enamel and 2) enamel surfaces after ultrasonic cleaning with distilled water for 30 seconds to remove the smear layer, were prepared. There were four pre-etching groups: 1) enamel surfaces were pre-etched with phosphoric acid (Etchant, 3M ESPE) for 3 seconds, 2) enamel surfaces were pre-etched for 5 seconds, 3) enamel surfaces were pre-etched for 10 seconds, and 4) enamel surfaces were pre-etched for 15 seconds. Resin composite was bonded to the treated enamel surface to determine SBS. The SFEs of treated enamel surfaces were determined by measuring the contact angles of three test liquids. Scanning electron microscopy was used to examine the enamel surfaces and enamel-adhesive interface. The specimens with phosphoric acid pre-etching showed significantly higher SBS and SFEs than the specimens without phosphoric acid pre-etching regardless of the adhesive system used. SBS and SFEs did not increase for phosphoric acid pre-etching times over 3 seconds. There were no significant differences in SBS and SFEs between the specimens with and without a smear layer. The data suggest that phosphoric acid pre-etching of ground enamel improves the bonding performance of single-step self-etch adhesives, but these bonding properties do not increase for phosphoric acid pre-etching times over 3 seconds.

A macro- and nanostructure evaluation of a novel dental implant.

PubMed

Tetè, Stefano; Mastrangelo, Filiberto; Traini, Tonino; Vinci, Raffaele; Sammartino, Gilberto; Marenzi, Gaetano; Gherlone, Enrico

2008-09-01

Success in implant dentistry also comes from the implant macrodesign and nanostructure of its surface. Titanium implant surface treatments have been shown to enhance osseointegration, maximize bone healing, and bone-to-implant contact for predictable clinical results. The aim of the study, was to evaluate the geometric macrodesign and the surface nanostructure of a novel dental implant full contact covering (FCC) obtained by electrochemical procedures. FCC implants were analyzed by scanning electronic microscope, profilometer, and x-ray photoelectron spectroscopy and compared with commercial sandblasted and sandblasted, large-grit acid-etched dental implants. Sample analysis allowed to distinguish the different implant macrodesigns, the step and the profile of the coils that cover the fixture, and the surface characteristics. FCC implant showed novel macro-characteristic of crestal module, coils, and apical zone compared with sandblasted and sandblasted and acid-etched dental implants. Moreover, the FCC nanostructure surface showed roughness values statistically higher than the 2 other surfaces, with a more homogeneity in a peaks and valleys arrangement. Finally, the x-ray photoelectron spectroscopy analysis detected differences between the examined surfaces, with the presence of several contaminants according to the different treatment procedures. Research on new macrostructures and nano morphology should result in a better qualitative and quantitative osseointegration response, with a predictability of the clinical results and long-term success of the implants.

Acid-etching technique of non-decalcified bone samples for visualizing osteocyte-lacuno-canalicular network using scanning electron microscope.

PubMed

Lampi, Tiina; Dekker, Hannah; Ten Bruggenkate, Chris M; Schulten, Engelbert A J M; Mikkonen, Jopi J W; Koistinen, Arto; Kullaa, Arja M

2018-01-01

The aim of this study was to define the acid-etching technique for bone samples embedded in polymethyl metacrylate (PMMA) in order to visualize the osteocyte lacuno-canalicular network (LCN) for scanning electron microscopy (SEM). Human jaw bone tissue samples (N = 18) were collected from the study population consisting of patients having received dental implant surgery. After collection, the bone samples were fixed in 70% ethanol and non-decalcified samples embedded routinely into polymethyl metacrylate (PMMA). The PMMA embedded specimens were acid-etched in either 9 or 37% phosphoric acid (PA) and prepared for SEM for further analysis. PMMA embedded bone specimens acid-etched by 9% PA concentration accomplishes the most informative and favorable visualization of the LCN to be observed by SEM. Etching of PMMA embedded specimens is recommendable to start with 30 s or 40 s etching duration in order to find the proper etching duration for the samples examined. Visualizing osteocytes and LCN provides a tool to study bone structure that reflects changes in bone metabolism and diseases related to bone tissue. By proper etching protocol of non-decalcified and using scanning electron microscope it is possible to visualize the morphology of osteocytes and the network supporting vitality of bone tissue.

The Effect of Hydrofluoric Acid Etching Duration on the Surface Micromorphology, Roughness, and Wettability of Dental Ceramics

PubMed Central

Ramakrishnaiah, Ravikumar; Alkheraif, Abdulaziz A.; Divakar, Darshan Devang; Matinlinna, Jukka P.; Vallittu, Pekka K.

2016-01-01

The current laboratory study is evaluating the effect of hydrofluoric acid etching duration on the surface characteristics of five silica-based glass ceramics. Changes in the pore pattern, crystal structure, roughness, and wettability were compared and evaluated. Seventy-five rectangularly shaped specimens were cut from each material (IPS e-max™, Dentsply Celtra™, Vita Suprinity™, Vita mark II™, and Vita Suprinity FC™); the sectioned samples were finished, polished, and ultrasonically cleaned. Specimens were randomly assigned into study groups: control (no etching) and four experimental groups (20, 40, 80 and 160 s of etching). The etched surfaces’ microstructure including crystal structure, pore pattern, pore depth, and pore width was studied under a scanning electron microscope, and the surface roughness and wettability were analyzed using a non-contact surface profilometer and a contact angle measuring device, respectively. The results were statistically analyzed using one-way analysis of variance (ANOVA) and the post hoc Tukey’s test. The results showed a significant change in the pore number, pore pattern, crystal structure, surface roughness, and wettability with increased etching duration. Etching for a short time resulted in small pores, and etching for longer times resulted in wider, irregular grooves. A significant increase in the surface roughness and wettability was observed with an increase in the etching duration. The findings also suggested a strong association between the surface roughness and wettability. PMID:27240353

Dyract compomer: comparison of total etch vs. no etch technique.

PubMed

Kugel, G; Perry, R D; Hoang, E; Hoang, T; Ferrari, M

1998-01-01

Different dental materials and methods can influence the integrity of the marginal seal of restorations. To evaluate the microleakage of Dyract AP Light Cured Compomer, a polyacid modified resin (Caulk), using etched and unetched techniques, standardized trapezoidal Class V restorations were placed on facial or lingual surfaces of 20 human molars with the gingival margin in the cementum. Each restoration was scored at the cervical by two independent, double blinded operators, with reference to the DEJ, for dye penetration on a ranking system of: 0 = no evidence of dye penetration; 1 = dye penetration up to one-half the distance to the axial wall; 2 = dye penetration beyond one-half the distance to the axial wall but short of the axial wall; 3 = dye penetration to the axial wall or beyond. Statistical analysis (Fisher Exact Test) indicated that the etched compomer demonstrated significantly less microleakage when compared to the unetched compomer (p < 0.05).

Effect of etching time and resin bond on the flexural strength of IPS e.max Press glass ceramic.

PubMed

Xiaoping, Luo; Dongfeng, Ren; Silikas, Nick

2014-12-01

To evaluate the effect of hydrofluoric acid (HFA) etching time and resin cement bond on the flexural strength of IPS e.max(®) Press glass ceramic. Two hundred and ten bars, 25mm×3mm×2mm, were made from IPS e.max(®) Press ingots through lost-wax, hot-pressed ceramic fabrication technology and randomly divided into five groups with forty-two per group after polishing. The ceramic surfaces of different groups were etched by 9.5% hydrofluoric acid gel for 0, 20, 40, 60 and 120s respectively. Two specimens of each group were selected randomly to examine the surface roughness and 3-dimensional topography with atomic force microscope (AFM), and microstructure was analyzed by the field emission scanning electron microscope (FE-SEM). Then each group were subdivided into two subgroups (n=20). One subgroup of this material was selected to receive a thin (approximately 0.1mm) layer of resin luting agent (Variolink N) whereas the other subgroup remained unaltered. Half of subgroup's specimens were thermocycled 10,000 times before a 3-point bending test in order to determine the flexural strength. Interface between resin cement and ceramic was examined with field emission scanning electronic microscope. Roughness values increased with increasing etching time. The mean flexural strength values of group 0s, 20s, 40s, 60s and 120s were 384±33, 347±43, 330±53, 327±67 and 317±41MPa respectively. Increasing HF etching times reduced the mean flexural strength (p<0.05). However, the mean flexural strength of each group, except group 0s, increased significantly to 420±31, 435±50, 400±39 and 412±58MPa after the application of dual-curing resin cement. In the present investigation, no significant differences after thermocycling on the flexural strengths were evident. Overtime HF etching could have a wakening effect on IPS e.max(®) Press glass ceramic, but resin cement bonding to appropriately etched surface would strengthen the dental ceramic. Copyright © 2014 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of surface etching and electrodeposition of copper on nitinol

NASA Astrophysics Data System (ADS)

Ramos-Moore, E.; Rosenkranz, A.; Matamala, L. F.; Videla, A.; Durán, A.; Ramos-Grez, J.

2017-10-01

Nitinol-based materials are very promising for medical and dental applications since those materials can combine shape memory, corrosion resistance, biocompatibility and antibacterial properties. In particular, surface modifications and coating deposition can be used to tailor and to unify those properties. We report preliminary results on the study of the effect of surface etching and electrodeposition of Copper on Nitinol using optical, chemical and thermal techniques. The results show that surface etching enhances the surface roughness of Nitinol, induces the formation of Copper-based compounds at the Nitinol-Copper interface, reduces the austenitic-martensitic transformations enthalpies and reduces the Copper coating roughness. Further studies are needed in order to highlight the influence of the electrodeposited Copper on the memory shape properties of NiTi.

A comparative study of shear bond strength of orthodontic bracket after acid-etched and Er:YAG treatment on enamel surface

NASA Astrophysics Data System (ADS)

Leão, Juliana C.; Mota, Cláudia C. B. O.; Cassimiro-silva, Patricia F.; Gomes, Anderson S. L.

2016-02-01

This study aimed to evaluate the shear bond strength (SBS) of teeth prepared for orthodontic bracket bonding with 37% phosphoric acid and Er:YAG laser. Forty bovine incisors were divided into two groups. In Group I, the teeth were conditioned with 37% phosphoric acid and brackets were bonded with Transbond XT; in Group II, the teeth were irradiated with Er:YAG and bonding with Transbond XT. After SBS test, the adhesive remnant index was determined. Adhesion to dental hard tissues after Er:YAG laser etching was inferior to that obtained after acid etching but exceeded what is believed to be clinically sufficient strength, and therefore can be used in patients.

Nano-crystalline diamond-coated titanium dental implants - a histomorphometric study in adult domestic pigs.

PubMed

Metzler, Philipp; von Wilmowsky, Cornelius; Stadlinger, Bernd; Zemann, Wolfgang; Schlegel, Karl Andreas; Rosiwal, Stephan; Rupprecht, Stephan

2013-09-01

Promising biomaterial characteristics of diamond-coatings in biomedicine have been described in the literature. However, there is a lack of knowledge about implant osseointegration of this surface modification compared to the currently used sandblasted acid-etched Ti-Al6-V4 implants. The aim of this study was to investigate the osseointegration of microwave plasma-chemical-vapour deposition (MWP-CVD) diamond-coated Ti-Al6-V4 dental implants after healing periods of 2 and 5 months. Twenty-four MWP-CVD diamond-coated and 24 un-coated dental titanium-alloy implants (Ankylos(®)) were placed in the frontal skull of eight adult domestic pigs. To evaluate the effects of the nano-structured surfaces on bone formation, a histomorphometric analysis was performed after 2 and 5 months of implant healing. Histomorphometry analysed the bone-to-implant contact (BIC). No significant difference in BIC for the diamond-coated implants in comparison to reference implants could be observed for both healing periods. Scanning electron microscopy revealed an adequate interface between the bone and the diamond surface. No delamination or particle-dissociation due to shearing forces could be detected. In this study, diamond-coated dental titanium-alloy implants and sandblasted acid-etched implants showed a comparable degree of osseointegration. Copyright © 2012 European Association for Cranio-Maxillo-Facial Surgery. Published by Elsevier Ltd. All rights reserved.

An In Vitro Evaluation of Leakage of Two Etch and Rinse and Two Self-Etch Adhesives after Thermocycling

PubMed Central

Geerts, Sabine; Bolette, Amandine; Seidel, Laurence; Guéders, Audrey

2012-01-01

Our experiment evaluated the microleakage in resin composite restorations bonded to dental tissues with different adhesive systems. 40 class V cavities were prepared on the facial and lingual surfaces of each tooth with coronal margins in enamel and apical margins in cementum (root dentin). The teeth were restored with Z100 resin composite bonded with different adhesive systems: Scotchbond Multipurpose (SBMP), a 3-step Etch and Rinse adhesive, Adper Scotchbond 1 XT (SB1), a 2-step Etch and Rinse adhesive, AdheSE One (ADSE-1), a 1-step Self-Etch adhesive, and AdheSE (ADSE), a 2-step Self-Etch adhesive. Teeth were thermocycled and immersed in 50% silver nitrate solution. When both interfaces were considered, SBMP has exhibited significantly less microleakage than other adhesive systems (resp., for SB1, ADSE-1 and ADSE, P = 0.0007, P < 0.0001 and P < 0.0001). When enamel and dentin interfaces were evaluated separately, (1) for the Self-Etch adhesives, microleakage was found greater at enamel than at dentin interfaces (for ADSE, P = 0.024 and for ADSE-1, P < 0.0001); (2) for the Etch and Rinse adhesive systems, there was no significant difference between enamel and dentin interfaces; (3) SBMP was found significantly better than other adhesives both at enamel and dentin interfaces. In our experiment Etch and Rinse adhesives remain better than Self-Etch adhesives at enamel interface. In addition, there was no statistical difference between 1-step (ADSE-1) and 2-step (ADSE) Self-Etch adhesives. PMID:22675358

Enamel Bond Strength of New Universal Adhesive Bonding Agents.

PubMed

McLean, D E; Meyers, E J; Guillory, V L; Vandewalle, K S

2015-01-01

Universal bonding agents have been introduced for use as self-etch or etch-and-rinse adhesives depending on the dental substrate and clinician's preference. The purpose of this study was to evaluate the shear bond strength (SBS) of composite to enamel using universal adhesives compared to a self-etch adhesive when applied in self-etch and etch-and-rinse modes over time. Extracted human third molars were used to create 120 enamel specimens. The specimens were ground flat and randomly divided into three groups: two universal adhesives and one self-etch adhesive. Each group was then subdivided, with half the specimens bonded in self-etch mode and half in etch-and-rinse mode. The adhesives were applied as per manufacturers' instructions, and composite was bonded using a standardized mold and cured incrementally. The groups were further divided into two subgroups with 10 specimens each. One subgroup was stored for 24 hours and the second for six months in 37°C distilled water and tested in shear. Failure mode was also determined for each specimen. A three-way analysis of variance (ANOVA) found a significant difference between groups based on bonding agent (p<0.001) and surface treatment (p<0.001) but not on time (p=0.943), with no significant interaction (p>0.05). Clearfil SE in etch-and-rinse and self-etch modes had more mixed fractures than either universal adhesive in either mode. Etching enamel significantly increased the SBS of composite to enamel. Clearfil SE had significantly greater bond strength to enamel than either universal adhesive, which were not significantly different from each other.

Early diagnosis of teeth erosion using polarized laser speckle imaging

NASA Astrophysics Data System (ADS)

Nader, Christelle Abou; Pellen, Fabrice; Loutfi, Hadi; Mansour, Rassoul; Jeune, Bernard Le; Brun, Guy Le; Abboud, Marie

2016-07-01

Dental erosion starts with a chemical attack on dental tissue causing tooth demineralization, altering the tooth structure and making it more sensitive to mechanical erosion. Medical diagnosis of dental erosion is commonly achieved through a visual inspection by the dentist during dental checkups and is therefore highly dependent on the operator's experience. The detection of this disease at preliminary stages is important since, once the damage is done, cares become more complicated. We investigate the difference in light-scattering properties between healthy and eroded teeth. A change in light-scattering properties is observed and a transition from volume to surface backscattering is detected by means of polarized laser speckle imaging as teeth undergo acid etching, suggesting an increase in enamel surface roughness.

Bonding performance of universal adhesives to er,cr:YSGG laser-irradiated enamel.

PubMed

Ayar, Muhammet Kerim; Erdemir, Fatih

2017-04-01

Universal adhesives have been recently introduced for use as self-etch or etch-and-rinse adhesives depending on the dental substrate and clinical condition. However, their bonding effectiveness to laser-irradiated enamel is still not well-known. Thus, the aim of this study was to compare the shear bond strength (SBS) of universal adhesives (Single Bond Universal; Nova Compo-B Plus) applied to Er,Cr:YSGG laser-irradiated enamel with SBS of the same adhesives applied in self-etch and acid-etching modes, respectively. Crown segments of sixty bovine incisors were embedded into standardized acrylic blocks. Flattened enamel surfaces were prepared. Specimens were divided into six groups according to universal adhesives and application modes randomly (n = 10), as follows: Single Bond Universal/acid-etching mode; Nova Compo-B Plus/acid-etching mode; Single Bond Universal/self-etching mode; Nova Compo-B Plus/self-etching mode; and Single Bond Universal/Er,Cr:YSGG Laser-etching mode; Nova Compo-B Plus/Er,Cr:YSGG Laser-etching mode. After surface treatments, universal adhesives were applied onto surfaces. SBS was determined after storage in water for 24 h using a universal testing machine with a crosshead speed of 0.5 mm min -1 . Failure modes were evaluated using a stereomicroscope. Data was analyzed using two-way of analyses of variances (ANOVA) (p = 0.05). Two-way ANOVA revealed that adhesive had no effect on SBS (p = 0.88), but application mode significantly influenced SBS (p = 0.00). Acid-etching significantly increased SBS, whereas there are no significant differences between self-etch mode and laser-etching for both adhesives. The bond strength of universal adhesives may depend on application mode. Acid etching may significantly increase bond strength, while laser etching may provide similar bond strength when compared to self-etch mode. © 2016 Wiley Periodicals, Inc.

Effect of bracket bonding with Er: YAG laser on nanomechanical properties of enamel.

PubMed

Alavi, Shiva; Birang, Reza; Hajizadeh, Fatemeh; Banimostafaee, Hamed

2014-01-01

The aim of this study was to compare the effects of conventional acid etching and laser etching on the nano-mechanical properties of the dental enamel using nano-indentation test. In this experimental in vitro study, buccal surfaces of 10 premolars were divided into three regions. One of the regions was etched with 37% phosphoric acid and another etched with Er:YAG laser, the third region was not etched. The brackets were bonded to both of etched regions. After thermocycling for 500 cycles, the brackets were removed and the teeth were decoronated from the bracket bonding area. Seven nano-indentations were applied at 1-31 μm depth from the enamel surface in each region. Mean values of the hardness and elastic modulus were analyzed with repeated measures analysis of variance and Tukey HSD tests, using the SPSS software (SPSS Inc., version16.0, Chicago, Il, USA). P < 0.05 was considered as significant. The hardness up to 21 μm in depth and elastic modulus up to 6 μm in depth from the enamel surface for laser-etched enamel had significantly higher values than control enamel and the hardness up to 11 μm in depth and elastic modulus up to 6 μm in depth for acid-etched enamel had significantly lower values than the control enamel. The mechanical properties of the enamel were decreased after bracket bonding with conventional acid etching and increased after bonding with Er:YAG laser.

Addition of Grape Seed Extract Renders Phosphoric Acid a Collagen-stabilizing Etchant.

PubMed

Liu, Y; Dusevich, V; Wang, Y

2014-08-01

Previous studies found that grape seed extract (GSE), which is rich in proanthocyanidins, could protect demineralized dentin collagen from collagenolytic activities following clinically relevant treatment. Because of proanthocyanidin's adverse interference to resin polymerization, it was believed that GSE should be applied and then rinsed off in a separate step, which in effect increases the complexity of the bonding procedure. The present study aimed to investigate the feasibility of combining GSE treatment with phosphoric acid etching to address the issue. It is also the first attempt to formulate collagen-cross-linking dental etchants. Based on Fourier-transformed infrared spectroscopy and digestion assay, it was established that in the presence of 20% to 5% phosphoric acid, 30 sec of GSE treatment rendered demineralized dentin collagen inert to bacterial collagenase digestion. Based on this positive result, the simultaneous dentin etching and collagen protecting of GSE-containing phosphoric acid was evaluated on the premise of a 30-second etching time. According to micro-Raman spectroscopy, the formulation containing 20% phosphoric acid was found to lead to overetching. Based on scanning and transmission electronic microscopy, this same formulation exhibited unsynchronized phosphoric acid and GSE penetration. Therefore, addition of GSE did render phosphoric acid a collagen-stabilizing etchant, but the preferable phosphoric acid concentration should be <20%. © International & American Associations for Dental Research.

Cell Adhesion and in Vivo Osseointegration of Sandblasted/Acid Etched/Anodized Dental Implants

PubMed Central

Kim, Mu-Hyon; Park, Kyeongsoon; Choi, Kyung-Hee; Kim, Soo-Hong; Kim, Se Eun; Jeong, Chang-Mo; Huh, Jung-Bo

2015-01-01

The authors describe a new type of titanium (Ti) implant as a Modi-anodized (ANO) Ti implant, the surface of which was treated by sandblasting, acid etching (SLA), and anodized techniques. The aim of the present study was to evaluate the adhesion of MG-63 cells to Modi-ANO surface treated Ti in vitro and to investigate its osseointegration characteristics in vivo. Four different types of Ti implants were examined, that is, machined Ti (control), SLA, anodized, and Modi-ANO Ti. In the cell adhesion study, Modi-ANO Ti showed higher initial MG-63 cell adhesion and induced greater filopodia growth than other groups. In vivo study in a beagle model revealed the bone-to-implant contact (BIC) of Modi-ANO Ti (74.20% ± 10.89%) was much greater than those of machined (33.58% ± 8.63%), SLA (58.47% ± 12.89), or ANO Ti (59.62% ± 18.30%). In conclusion, this study demonstrates that Modi-ANO Ti implants produced by sandblasting, acid etching, and anodizing improve cell adhesion and bone ongrowth as compared with machined, SLA, or ANO Ti implants. These findings suggest that the application of Modi-ANO surface treatment could improve the osseointegration of dental implant. PMID:25955650

Influence of Different Etching Modes on Bond Strength to Enamel using Universal Adhesive Systems.

PubMed

Diniz, Ana Cs; Bandeca, Matheus C; Pinheiro, Larissa M; Dos Santosh Almeida, Lauber J; Torres, Carlos Rg; Borges, Alvaro H; Pinto, Shelon Cs; Tonetto, Mateus R; De Jesus Tavarez, Rudys R; Firoozmand, Leily M

2016-10-01

The adhesive systems and the techniques currently used are designed to provide a more effective adhesion with reduction of the protocol application. The objective of this study was to evaluate the bond strength of universal adhesive systems on enamel in different etching modes (self-etch and total etch). The mesial and distal halves of 52 bovine incisors, healthy, freshly extracted, were used and divided into seven experimental groups (n = 13). The enamel was treated in accordance with the following experimental conditions: FUE-Universal System - Futurabond U (VOCO) with etching; FUWE - Futurabond U (VOCO) without etching; SB-Total Etch System - Single Bond 2 (3M); SBUE-Universal System - Single Bond Universal (3M ESPE) with etching; SBUWE - Single Bond Universal (3M ESPE) without etching; CLE-Self-etch System - Clearfil SE Bond (Kuraray) was applied with etching; CLWE - Clearfil SE Bond (Kuraray) without etching. The specimens were made using the composite spectrum TPH (Dentsply) and stored in distilled water (37 ± 1°C) for 1 month. The microshear test was performed using the universal testing machine EMIC DL 2000 with the crosshead speed of 0.5 mm/minute. The bond strength values were analyzed using statistical tests (Kruskal-Wallis test and Mann-Whitney test) with Bonferroni correction. There was no statistically significant difference between groups (p < 0.05), where FUE (36.83 ± 4.9 MPa) showed the highest bond strength values and SBUWE (18.40 ± 2.2 MPa) showed the lowest bond strength values. The analysis of adhesive interface revealed that most failures occurred between the interface composite resin and adhesive. The universal adhesive system used in dental enamel varies according to the trademark, and the previous enamel etching for universal systems and the self-etch both induced greater bond strength values. Selective enamel etching prior to the application of a universal adhesive system is a relevant strategy for better performance bonding.

The Effect of Primer Application Modifications on the Bond Strength of 4th Generation Adhesive Bonding Agents

DTIC Science & Technology

2012-03-30

dentin. Methods: The coronal enamel of 120 extracted human third molars was removed with a low-speed saw. The teeth were mounted in PVC pipe with dental...LITERATURE REVIEW A. Background 1. Acid Etching in Dentistry. Buonocore demonstrated in 1955 that the preparation of dental enamel with an...The influence of deviations from the manufacturer’s instructions for the use of six adhesive systems on the bond strengths to enamel and dentin

Evaluation of erbium:YAG and holmium:YAG laser radiation and dental hard tissue

NASA Astrophysics Data System (ADS)

Attrill, David Cameron

Lasers have become increasingly established in medicine as effective alternatives or adjuncts to conventional techniques. In dentistry, several clinical laser systems have been developed and marketed, but their applications have been limited to soft tissue surgery. To date, no laser has been capable of effectively cutting or modifying the highly mineralised dental tissues of enamel and dentine. The aim of this study was to evaluate two new laser systems for use in dentistry through a series of in vitro experiments. Both generic erbium and holmium lasers have theoretically superior operating characteristics over currently established lasers for applications with dental hard tissues. The two lasers investigated in this study were pulsed Er:YAG (lambda=2.94) a.m. and Cr-Tm-Ho:YAG (lambda=2.1mu.m). Both operated with a macropulse duration of approximately 200lambdas, at pulse repetition rates of 2-8Hz and mean pulse energies up to 230mJ. Radiation was focused using CaF[2] lenses (f=50-120mm). The lasers could be operated with or without the addition of a surface water film at the interaction site. Tissue removal efficiency was expressed as a latent heat of ablation (LHA, kJ/cm[3]) using a modification of the technique described by Charlton et al. (1990). The mean LHA's for the Er:YAG laser were 6.24kJ/cm[3] and 22.99kJ/cm[3] with dentine and enamel respectively without water, and 10.07kJ/cm[3] and 18.73kJ/cm[3] for dentine and enamel with water. The Cr-Tm-Ho:YAG laser was unable to effectively remove enamel at the fluences and pulse energies available; the mean LHA's for the Cr-Tm- Ho:YAG laser with dentine were 82.79kJ/cm3 and 57.57kJ/cm3 with and without water respectively. The Cr-Tm-Ho;YAG was approximately 8-9 times less efficient for tissue removal than the Er:YAG system. Er:YAG tissue removal with water was characterised by clean "surgical" cuts, comparable in histological appearance to those obtained using conventional instrumentation. Some thermal disruption and evidence of molten enamel in particular were apparent when the Er:YAG laser was used without water. The Cr-Tm-Ho;YAG laser produced extensive charring and carbonisation of tissues. It was concluded that this laser was unsuitable for clinical applications directed at the removal or modification of enamel and dentine, particularly as the Er:YAG laser offers superior qualities. Further research with the Cr-Tm-Ho:YAG laser was discontinued. A comparison of the mean shear bond strengths of a composite (ZlOO, 3M Dental Products) bonded to enamel was made using either a conventional acid etch technique or one of a range of experimental Er:YAG laser etching configurations. The mean values for acid etching (16.6 MPa) were in all cases significantly greater (p<0.01, Bonferroni) than those obtained with laser etching. The optimal laser etching parameters were a fluence of 24J/cm[2] (1/e[2] calculation) with water resulting in a mean bond strength of 11.5 MPa. This figure represents approximately 70% of the mean obtained with acid etching, and was significantly greater (p<0.01, Bonferroni) than the mean recorded for non etched negative control surfaces (4.4 MPa). Histological evaluation of the etched surfaces demonstrated clear differences in the etching patterns observed between laser and acid etching. Some surface cracking was noted in most laser etched surfaces, but the extent of this was minimised when the laser was applied in conjunction with a surface water film. Pulpal temperature increments following Er:YAG laser irradiation were significantly lower in teeth prepared with water than without (paired t-test, p<0.01). The largest increment in samples prepared with water was 3.9°C, compared to 24.7°C without water. The principal determinant of the temperature increment in either group was the total delivered energy, up to 140J. Linear regression modelling predicts that continuous irradiation up to 160J with water would not result in iatrogenic pulpal damage. In conclusion, the Er:YAG laser was shown to be an effective tool for cutting and modifying dental hard tissues. It almost certainly offers the best combination of safety, efficiency and speed of any laser system designed for preparing cavities. The laser must be used in conjunction with a water coolant on the tissues to minimise the possibility of iatrogenic damage, improve the quality of the laser cuts and in some circumstances increase cutting efficiency. The Er:YAG laser has shown much promise in these in vitro experiments and its progression to clinical use is supported. The Cr-Tm-Ho:YAG laser is significantly less efficient and in vitro results are unfavourable in comparison with the Er:YAG laser. Its clinical use is not supported.

Aggressiveness of contemporary self-etching adhesives. Part II: etching effects on unground enamel.

PubMed

Pashley, D H; Tay, F R

2001-09-01

The aggressiveness of three self-etching adhesives on unground enamel was investigated. Ultrastructural features and microtensile bond strength were examined, first using these adhesives as both the etching and resin-infiltration components, and then examining their etching efficacy alone through substitution of the proprietary resins with the same control resins. For SEM examination, buccal, mid-coronal, unground enamel from human extracted bicuspids were etched with either Clearfil Mega Bond (Kuraray), Non-Rinse Conditioner (NRC; Dentsply DeTrey) or Prompt L-Pop (ESPE). Those in the control group were etched with 32% phosphoric acid (Bisco) for 15s. They were all rinsed off prior to examination of the etching efficacy. For TEM examination, the self-etching adhesives were used as recommended. Unground enamel treated with NRC were further bonded using Prime&Bond NT (Dentsply), while those in the etched, control group were bonded using All-Bond 2 (Bisco). Completely demineralized, resin replicas were embedded in epoxy resin for examination of the extent of resin infiltration. For microtensile bond strength evaluation, specimens were first etched and bonded using the self-etching adhesives. A second group of specimens were etched with the self-etching adhesives, rinsed but bonded using a control adhesive. Following restoration with Z100 (3M Dental Products), they were sectioned into beams of uniform cross-sectional areas and stressed to failure. Etching patterns of aprismatic enamel, as revealed by SEM, and the subsurface hybrid layer morphology, as revealed by TEM, varied according to the aggressiveness of the self-etching adhesives. Clearfil Mega Bond exhibited the mildest etching patterns, while Prompt L-Pop produced an etching effect that approached that of the total-etch control group. Microtensile bond strength of the three experimental groups were all significantly lower than the control group, but not different from one another. When the self-etching adhesives were replaced with the control adhesive after etching, bond strengths of NRC/Prime&Bond NT and Prompt L-Pop were not significantly different from that of the control group, but were significantly higher than that of Clearfil Mega Bond. Both etching efficacy and strength of the resins are important contributing factors in bonding of self-etching adhesives to unground enamel.

Application of 252Cf plasma desorption mass spectrometry in dental research

NASA Astrophysics Data System (ADS)

Fritsch, Hans-Walter; Schmidt, Lothar; Köhl, Peter; Jungclas, Hartmut; Duschner, Heins

1993-07-01

Topically applied fluorides introduced in dental hygiene products elevate the concentration levels of fluoride in oral fluids and thus also affect chemical reactions of enamel de- and remineralisation. The chemical reactions on the surface of tooth enamel still are a subject of controversy. Here 252Cf-plasma desorption mass spectrometry and argon ion etching are used to analyse the molecular structure of the upper layes of enamel. The mass spectrum of untreated enamel is characterised by a series of cluster ions containing phosphate. It is evident that under certain conditions the molecular structure of the surface enamel is completely transformed by treatment with fluorides. The result of the degradation and precipitation processes is reflected by a total replacement of the phosphate by fluoride in the measured cluster ion distribution. Stepwise etching of the upper layers by Ar+ ions reveals the transition from a nearly pure CaF2 structure to the unchanged composition of the enamel mineral.

The influence of temporary cements on dental adhesive systems for luting cementation.

PubMed

Ribeiro, José C V; Coelho, Paulo G; Janal, Malvin N; Silva, Nelson R F A; Monteiro, André J; Fernandes, Carlos A O

2011-03-01

This study tested the hypothesis that bond strength of total- and self-etching adhesive systems to dentine is not affected by the presence of remnants from either eugenol-containing (EC) or eugenol-free (EF) temporary cements after standardized cleaning procedures. Thirty non-carious human third molars were polished flat to expose dentine surfaces. Provisional acrylic plates were fabricated and cemented either with EC, EF or no temporary cements. All specimens were incubated for 7 days in water at 37°C. The restorations were then taken out and the remnants of temporary cements were mechanically removed with a dental instrument. The dentine surfaces were cleaned with pumice and treated with either total-etching (TE) or self-etching (SE) dental adhesive systems. Atomic force microscopy was used to examine the presence of remnants of temporary cements before and after dentine cleaning procedures. Composite resin build-ups were fabricated and cemented to the bonded dentine surfaces with a resin luting cement. The specimens were then sectioned to obtain 0.9mm(2) beams for microtensile bond strength testing. Fractographic analysis was performed by optical and scanning electron microscopy. ANOVA showed lower mean microtensile bond strength in groups of specimens treated with EC temporary cement than in groups treated with either no cement or an EF cement (p<0.05). Mean microtensile bond strength was lower in groups employing the SE rather than the TE adhesive system (p<0.001). SE samples were also more likely to fail during initial processing of the samples. There was no evidence of interaction between cement and adhesive system effects on tensile strength. Fractographic analysis indicated different primary failure modes for SE and TE bonding systems, at the dentine-adhesive interface and at the resin cement-resin composite interface, respectively. The use of eugenol-containing temporary cements prior to indirect bonding restorations reduce, to a statistically similar extent, the bond strength of both total- and self-etching adhesive systems to dentine. Copyright © 2011 Elsevier Ltd. All rights reserved.

The Effects of Acid Etching on the Nanomorphological Surface Characteristics and Activation Energy of Titanium Medical Materials.

PubMed

Hung, Kuo-Yung; Lin, Yi-Chih; Feng, Hui-Ping

2017-10-11

The purpose of this study was to characterize the etching mechanism, namely, the etching rate and the activation energy, of a titanium dental implant in concentrated acid and to construct the relation between the activation energy and the nanoscale surface topographies. A commercially-pure titanium (CP Ti) and Ti-6Al-4V ELI surface were tested by shot blasting (pressure, grain size, blasting distance, blasting angle, and time) and acid etching to study its topographical, weight loss, surface roughness, and activation energy. An Arrhenius equation was applied to derive the activation energy for the dissolution of CP Ti/Ti-6Al-4V ELI in sulfuric acid (H₂SO₄) and hydrochloric acid (HCl) at different temperatures. In addition, white-light interferometry was applied to measure the surface nanomorphology of the implant to obtain 2D or 3D roughness parameters (Sa, Sq, and St). The nanopore size that formed after etching was approximately 100-500 nm. The surface roughness of CP Ti and Ti-6Al-4V ELI decreased as the activation energy decreased but weight loss increased. Ti-6Al-4V ELI has a higher level of activation energy than Ti in HCl, which results in lower surface roughness after acid etching. This study also indicates that etching using a concentrated hydrochloric acid provided superior surface modification effects in titanium compared with H₂SO₄.

Effect of bracket bonding with Er: YAG laser on nanomechanical properties of enamel

PubMed Central

Alavi, Shiva; Birang, Reza; Hajizadeh, Fatemeh; Banimostafaee, Hamed

2014-01-01

Background: The aim of this study was to compare the effects of conventional acid etching and laser etching on the nano-mechanical properties of the dental enamel using nano-indentation test. Materials and Methods: In this experimental in vitro study, buccal surfaces of 10 premolars were divided into three regions. One of the regions was etched with 37% phosphoric acid and another etched with Er:YAG laser, the third region was not etched. The brackets were bonded to both of etched regions. After thermocycling for 500 cycles, the brackets were removed and the teeth were decoronated from the bracket bonding area. Seven nano-indentations were applied at 1-31 μm depth from the enamel surface in each region. Mean values of the hardness and elastic modulus were analyzed with repeated measures analysis of variance and Tukey HSD tests, using the SPSS software (SPSS Inc., version16.0, Chicago, Il, USA). P < 0.05 was considered as significant. Results: The hardness up to 21 μm in depth and elastic modulus up to 6 μm in depth from the enamel surface for laser-etched enamel had significantly higher values than control enamel and the hardness up to 11 μm in depth and elastic modulus up to 6 μm in depth for acid-etched enamel had significantly lower values than the control enamel. Conclusion: The mechanical properties of the enamel were decreased after bracket bonding with conventional acid etching and increased after bonding with Er:YAG laser. PMID:24688560

Adhesion of Dental Materials to Tooth Structure

NASA Astrophysics Data System (ADS)

Mitra, Sumita B.

2000-03-01

The understanding and proper application of the principles of adhesion has brought forth a new paradigm in the realm of esthetic dentistry. Modern restorative tooth procedures can now conserve the remaining tooth-structure and also provide for the strengthening of the tooth. Adhesive restorative techniques call for the application and curing of the dental adhesive at the interface between the tooth tissue and the filling material. Hence the success of the restoration depends largely on the integrity of this interface. The mechanism of adhesion of the bonding materials to the dental hard tissue will be discussed in this paper. There are four main steps that occur during the application of the dental adhesive to the oral hard tissues: 1) The first step is the creation of a microstructure in the tooth enamel or dentin by means of an acidic material. This can be through the application of a separate etchant or can be accomplished in situ by the adhesive/primer. This agent has to be effective in removing or modifying the proteinaceous “smear” layer, which would otherwise act as a weak boundary layer on the surface to be bonded. 2) The primer/adhesive must then be able to wet and penetrate the microstructure created in the tooth. Since the surface energies of etched enamel and that of etched dentin are different finding one material to prime both types of dental tissues can be quite challenging. 3) The ionomer types of materials, particularly those that are carboxylate ion-containing, can chemically bond with the calcium ions of the hydroxyapatite mineral. 4) Polymerization in situ allows for micromechanical interlocking of the adhesive. The importance of having the right mechanical properties of the cured adhesive layer and its role in absorbing and dissipating stresses encountered by a restored tooth will also be discussed.

In vitro dentin barrier cytotoxicity testing of some dental restorative materials.

PubMed

Jiang, R D; Lin, H; Zheng, G; Zhang, X M; Du, Q; Yang, M

2017-03-01

To investigate the cytotoxicity of four dental restorative materials in three-dimensional (3D) L929 cell cultures using a dentin barrier test. The cytotoxicities of light-cured glass ionomer cement (Vitrebond), total-etching adhesive (GLUMA Bond5), and two self-etching adhesives (GLUMA Self Etch and Single Bond Universal) were evaluated. The permeabilities of human dentin disks with thicknesses of 300, 500, and 1000μm were standardized using a hydraulic device. Test materials and controls were applied to the occlusal side of human dentin disks. The 3D-cell scaffolds were placed beneath the dentin disks. After a 24-h contact with the dentin barrier test device, cell viabilities were measured by performing MTT assays. Statistical analysis was performed using the Mann-Whitney U test. The mean (SD) permeabilities of the 300-μm, 500-μm, and 1000-μm dentin disks were 0.626 (0.214), 0.219 (0.0387) and 0.089 (0.028) μlmin -1 cm -2 cm H 2 O -1 . Vitrebond was severely cytotoxic, reducing the cell viability to 10% (300-μm disk), 17% (500μm), and 18% (1000μm). GLUMA Bond5 reduced the cell viability to 40% (300μm), 83% (500μm), and 86% (1000μm), showing moderate cytotoxicity (300-μm) and non-cytotoxicity (500-μm and 1000-μm). Single Bond Universal and GLUMA Self Etch did not significantly reduce cell viability, regardless of the dentin thicknesses, which characterized them as non-cytotoxic. Cytotoxicity varied with the materials tested and the thicknesses of the dentin disks. The tested cytotoxicity of materials applied on 300-, 500-, and 1000-μm dentin disks indicates that the clinical use of the test materials (excepting self-etching adhesives) in deep cavities poses a potential risk of damage to the pulp tissues to an extent, depending on the thickness of the remaining dentin. Copyright © 2017 Elsevier Ltd. All rights reserved.

Effects of the micro-nano surface topography of titanium alloy on the biological responses of osteoblast.

PubMed

Yin, Chengcheng; Zhang, Yanjing; Cai, Qing; Li, Baosheng; Yang, Hua; Wang, Heling; Qi, Hua; Zhou, Yanmin; Meng, Weiyan

2017-03-01

In clinical applications, osseointegration is essential for the long-term stability of dental implants. Inspired by the hierarchical structure of natural bone, we applied the electrochemical etching (EC) technique to form a micro-nano structure on a titanium alloy (Ti6Al4V) substrate, called EC surface. Sand blasting and acid etching (SLA) and machined (M) methods were employed to generate micro and smooth textures, respectively, as the control groups. The surface topographies of the three substrates were characterized using scanning electron microscopy (SEM). Then, human osteoblast-like cells (MG63) were cultured on substrates, and adhesion, proliferation, morphology, alkaline phosphatase activity (ALP), and gene expression levels of Runt-related transcription factor 2 (RUNX2), osteocalcin (OCN), osteopontin (OPN), and type I collagen (COLIA 1) were analyzed. MG63 cells cultured on the EC Ti alloy substrates displayed better cell adhesion, significant proliferation, and a higher production level of ALP, gene expressions of RUNX2, OCN, OPN and COLIA 1 (p < 0.01 or p < 0.05) compared with those of SLA and M substrates. These results indicate that the micro-nano structure fabricated by electrochemical etching method is beneficial for the biological functions of MG63 cells and may be a promising candidate in dental implants. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part A: 105A: 757-769, 2017. © 2016 Wiley Periodicals, Inc.

[Observation of topography and analysis of surface contamination of titanium implant after roughness treatment].

PubMed

Cao, Hongdan; Yang, Xiaodong; Wu, Dayi; Zhang, Xingdong

2007-04-01

The roughness treatment of dental implant surface could improve the bone bonding and increase the success rate of implant, but the difference of diverse treatments is still unknown. In this study using scanning electron microscopy (SEM), energy disperse spectrometer (EDS) and the test of contact angle, we studied the microstructure, surface contamination and surface energy, and hence conducted a comparative analysis of the following surface roughness treatments: Polished Treatment (PT), Sandblasting with Alumina(SA), Sandblasting with Aluminia and Acid-etched (SAA), Sandblasting with Titanium Acid-etched (STA), Electro-erosion Treatment(ET). The result of SEM showed that the surface displayed irregularities after roughness treatments and that the surface properties of different roughness treatments had some distinctions. SAA and SA had some sharp edges and protrutions; the STA showed a regular pattern like honeycomb, but the ET sample treated by electric erosion exhibited the deeper pores of different sizes and the pores with a perforated secondary structure. The EDS indicated that the surface was contaminated after the treatment with foreign materials; the SA surface had some embedded contaminations even after acid etching. The measurement of water contact angle indicated that the morphology correlated with the surface treatments. These findings suggest that the distinction of surface structure and composition caused by different treatments may result in the disparity in biological behavior of dental implant.

Influence of the height of the external hexagon and surface treatment on fatigue life of commercially pure titanium dental implants.

PubMed

Gil, Francisco Javier; Aparicio, Conrado; Manero, Jose M; Padros, Alejandro

2009-01-01

This study evaluated the effect of external hexagon height and commonly applied surface treatments on the fatigue life of titanium dental implants. Electropolished commercially pure titanium dental implants (seven implants per group) with three different external hexagon heights (0.6, 1.2, and 1.8 mm) and implants with the highest external hexagon height (1.8 mm) and different surface treatments (electropolishing, grit blasting with aluminium oxide, and acid etching with sulfuric acid) were tested to evaluate their mechanical fatigue life. To do so, 10-Hz triangular flexural load cycles were applied at 37 degrees C in artificial saliva, and the number of load cycles until implant fracture was determined. Tolerances of the hexagon/abutment fit and implant surface roughness were analyzed by scanning electron microscopy and light interferometry. Transmission electron microscopy and electron diffraction analyses of titanium hydrides were performed. First, the fatigue life of implants with the highest hexagon (8,683 +/- 978 load cycles) was more than double that of the implants with the shortest hexagons (3,654 +/- 789 load cycles) (P < .02). Second, the grit-blasted implants had the longest fatigue life of the tested materials (21,393 +/- 2,356 load cycles), which was significantly greater than that of the other surfaces (P < .001). The compressive surface residual stresses induced when blasting titanium are responsible for this superior mechanical response. Third, precipitation of titanium hydrides in grain boundaries of titanium caused by hydrogen adsorption from the acid solution deteriorates the fatigue life of acid-etched titanium dental implants. These implants had the shortest fatigue life (P < .05). The fatigue life of threaded root-form dental implants varies with the height of the external hexagon and/or the surface treatment of the implant. An external hexagon height of 1.8 mm and/or a blasting treatment appear to significantly increase fatigue life of dental implants.

Laboratory evaluation of the effect of unfilled resin after the use of self-etch and total-etch dentin adhesives on the Shear Bond Strength of composite to dentin.

PubMed

Nasseri, Ehsan Baradaran; Majidinia, Sara; Sharbaf, Davood Aghasizadeh

2017-05-01

Based on the frequent application of composite resins as tooth-colored fillings, this method is considered a viable alternative to dental amalgam. However, this method has the low bond strength of the composite to dentin. To solve this issue, various dental adhesive systems with different characteristics have been developed by dentistry experts. To assess the effect of an additional layer of unfilled resin in self-etch and total-etch dentin adhesives on the shear bond strength (SBS) of composite to dentin. Moreover, we assessed the effects of sample storage in artificial saliva on the SBS of composite to dentin. Methods: This experimental study was conducted on 160 freshly extracted human first or second premolar teeth, which were randomly divided into 16 groups. The teeth were prepared from Mashhad University of Medical Sciences, Mashhad, Iran (2008-2009). Scotchbond Multi-purpose (SBMP), single bond (SB), Clearfil SE Bond, and Clearfil S3 Bond were applied to dentin surface with or without the placement of hydrophobic resin (Margin Bond) in accordance with the instructions of the manufacturers. To expose the coronal dentin, the teeth were abraded with 600 grit SiC paper. Immediately after restoration, half of the samples were tested in terms of SBS, while the other samples were evaluated in terms of SBS after three months of storage in artificial saliva. SBS rates of dental composites evaluated by universal testing machine and samples were studied by optical stereomicroscopy to verify the failure type. Data analysis was performed in SPSS V.16 using Kolmogorov-Smirnov test, independent-samples t-test, ANOVA, and Duncan's logistic regression test. In this study, a significant reduction was observed in the SBS rates of SB and S3 bond adhesive systems after storage with and without hydrophobic resin (p>0.000). Without storage in normal saline, a significant increase was observed in the SBS rate of the SE bond (p=0.013). In addition, SBS rate of SBMP significantly increased after storage with hydrophobic resin (p=0.001). Finally, the highest and lowest rates of SBS were observed in the SE and S3 bonds in all the experimental groups, respectively. The effects of using a hydrophobic resin layer on shear bond strength values seem to be effective. The mild self-etch adhesive exhibited the best resin-dentine bond strength after aging.

Laboratory evaluation of the effect of unfilled resin after the use of self-etch and total-etch dentin adhesives on the Shear Bond Strength of composite to dentin

PubMed Central

Nasseri, Ehsan Baradaran; Majidinia, Sara; Sharbaf, Davood Aghasizadeh

2017-01-01

Background Based on the frequent application of composite resins as tooth-colored fillings, this method is considered a viable alternative to dental amalgam. However, this method has the low bond strength of the composite to dentin. To solve this issue, various dental adhesive systems with different characteristics have been developed by dentistry experts. Aim To assess the effect of an additional layer of unfilled resin in self-etch and total-etch dentin adhesives on the shear bond strength (SBS) of composite to dentin. Moreover, we assessed the effects of sample storage in artificial saliva on the SBS of composite to dentin. Methods Methods: This experimental study was conducted on 160 freshly extracted human first or second premolar teeth, which were randomly divided into 16 groups. The teeth were prepared from Mashhad University of Medical Sciences, Mashhad, Iran (2008–2009). Scotchbond Multi-purpose (SBMP), single bond (SB), Clearfil SE Bond, and Clearfil S3 Bond were applied to dentin surface with or without the placement of hydrophobic resin (Margin Bond) in accordance with the instructions of the manufacturers. To expose the coronal dentin, the teeth were abraded with 600 grit SiC paper. Immediately after restoration, half of the samples were tested in terms of SBS, while the other samples were evaluated in terms of SBS after three months of storage in artificial saliva. SBS rates of dental composites evaluated by universal testing machine and samples were studied by optical stereomicroscopy to verify the failure type. Data analysis was performed in SPSS V.16 using Kolmogorov-Smirnov test, independent-samples t-test, ANOVA, and Duncan’s logistic regression test. Results In this study, a significant reduction was observed in the SBS rates of SB and S3 bond adhesive systems after storage with and without hydrophobic resin (p>0.000). Without storage in normal saline, a significant increase was observed in the SBS rate of the SE bond (p=0.013). In addition, SBS rate of SBMP significantly increased after storage with hydrophobic resin (p=0.001). Finally, the highest and lowest rates of SBS were observed in the SE and S3 bonds in all the experimental groups, respectively. Conclusion The effects of using a hydrophobic resin layer on shear bond strength values seem to be effective. The mild self-etch adhesive exhibited the best resin-dentine bond strength after aging PMID:28713512

Influence of caries infiltrant contamination on shear bond strength of different adhesives to dentin.

PubMed

Jia, Liuhe; Stawarczyk, Bogna; Schmidlin, Patrick R; Attin, Thomas; Wiegand, Annette

2013-03-01

To analyze whether the contamination with a caries infiltrant system impairs the adhesive performance of etch-and-rinse and self-etching adhesives on dentin. Dentin contamination with the caries infiltrant system (Icon, DMG) was simulated by applying either hydrochloric acid (15 % HCl, Icon Etch, 15 s), the resin infiltrant (Icon infiltrant, 4 min), or both prior to the application of the respective adhesives (each group n = 10). In the control groups, the etch-and-rinse adhesive (Optibond FL, Kerr) and the self-etching adhesive (iBOND Self Etch, Hereaus) were applied without former contamination with the infiltrant system. Additionally, the adhesive performance of the resin infiltrant alone was tested. Shear bond strength of a nano-hybrid composite was analyzed after thermocycling (5,000×, 5-55°C) of the specimens and analyzed by ANOVA/Scheffé post hoc tests (p < 0.05) and Weibull statistics. Failure mode was inspected under a stereomicroscope at × 25 magnification. Contamination with the resin infiltrant alone did not impair shear bond strength, while contamination with hydrochloric acid or with hydrochloric acid and the resin infiltrant reduced shear bond strength (MPa) of the adhesives (Optibond FL: 20.5 ± 3.6, iBOND Self Etch: 17.9 ± 2.6) significantly. Hydrochloric acid contamination increased the number of adhesive failures. The adhesive performance of the caries infiltrant system alone was insufficient. The contamination with the caries infiltrant system impaired the shear bond strength of conventional dental adhesives. Contamination of the caries infiltrant system on dentin should be avoided due to the detrimental effect of hydrochloric acid etching.

The Effects of Acid Etching on the Nanomorphological Surface Characteristics and Activation Energy of Titanium Medical Materials

PubMed Central

Hung, Kuo-Yung; Lin, Yi-Chih; Feng, Hui-Ping

2017-01-01

The purpose of this study was to characterize the etching mechanism, namely, the etching rate and the activation energy, of a titanium dental implant in concentrated acid and to construct the relation between the activation energy and the nanoscale surface topographies. A commercially-pure titanium (CP Ti) and Ti-6Al-4V ELI surface were tested by shot blasting (pressure, grain size, blasting distance, blasting angle, and time) and acid etching to study its topographical, weight loss, surface roughness, and activation energy. An Arrhenius equation was applied to derive the activation energy for the dissolution of CP Ti/Ti-6Al-4V ELI in sulfuric acid (H2SO4) and hydrochloric acid (HCl) at different temperatures. In addition, white-light interferometry was applied to measure the surface nanomorphology of the implant to obtain 2D or 3D roughness parameters (Sa, Sq, and St). The nanopore size that formed after etching was approximately 100–500 nm. The surface roughness of CP Ti and Ti-6Al-4V ELI decreased as the activation energy decreased but weight loss increased. Ti-6Al-4V ELI has a higher level of activation energy than Ti in HCl, which results in lower surface roughness after acid etching. This study also indicates that etching using a concentrated hydrochloric acid provided superior surface modification effects in titanium compared with H2SO4. PMID:29019926

Effect of Phosphoric Acid Pre-etching on Fatigue Limits of Self-etching Adhesives.

PubMed

Takamizawa, T; Barkmeier, W W; Tsujimoto, A; Scheidel, D D; Erickson, R L; Latta, M A; Miyazaki, M

2015-01-01

The purpose of this study was to use shear bond strength (SBS) and shear fatigue limit (SFL) testing to determine the effect of phosphoric acid pre-etching of enamel and dentin prior to application of self-etch adhesives for bonding resin composite to these substrates. Three self-etch adhesives--1) G- ænial Bond (GC Corporation, Tokyo, Japan); 2) OptiBond XTR (Kerr Corp, Orange, CA, USA); and 3) Scotchbond Universal (3M ESPE Dental Products, St Paul, MN, USA)--were used to bond Z100 Restorative resin composite to enamel and dentin surfaces. A stainless-steel metal ring with an inner diameter of 2.4 mm was used to bond the resin composite to flat-ground (4000 grit) tooth surfaces for determination of both SBS and SFL. Fifteen specimens each were used to determine initial SBS to human enamel/dentin, with and without pre-etching with a 35% phosphoric acid (Ultra-Etch, Ultradent Products Inc, South Jordan, UT, USA) for 15 seconds prior to the application of the adhesives. A staircase method of fatigue testing (25 specimens for each test) was then used to determine the SFL of resin composite bonded to enamel/dentin using a frequency of 10 Hz for 50,000 cycles or until failure occurred. A two-way analysis of variance and Tukey post hoc test were used for analysis of SBS data, and a modified t-test with Bonferroni correction was used for the SFL data. Scanning electron microscopy was used to examine the area of the bonded restorative/tooth interface. For all three adhesive systems, phosphoric acid pre-etching of enamel demonstrated significantly higher (p<0.05) SBS and SFL with pre-etching than it did without pre-etching. The SBS and SFL of dentin bonds decreased with phosphoric acid pre-etching. The SBS and SFL of bonds using phosphoric acid prior to application of self-etching adhesives clearly demonstrated different tendencies between enamel and dentin. The effect of using phosphoric acid, prior to the application of the self-etching adhesives, on SBS and SFL was dependent on the adhesive material and tooth substrate and should be carefully considered in clinical situations.

Bone Response to Two Dental Implants with Different Sandblasted/Acid-Etched Implant Surfaces: A Histological and Histomorphometrical Study in Rabbits

PubMed Central

Piattelli, Adriano; Quaranta, Alesandro

2017-01-01

Background Scientific evidence in the field of implant dentistry of the past 20 years established that titanium rough surfaces have shown improved osseointegration rates. In a majority of dental implants, the surface microroughness was obtained by grit blasting and/or acid etching. The aim of the study was to evaluate in vivo two different highly hydrophilic surfaces at different experimental times. Methods Calcium-modified (CA) and SLActive surfaces were evaluated and a total of 18 implants for each type of surface were positioned into the rabbit articular femoral knee-joint in a split model experiment, and they were evaluated histologically and histomorphometrically at 15, 30, and 60 days of healing. Results Bone-implant contact (BIC) at the two-implant surfaces was significantly different in favor of the CA surface at 15 days (p = 0.027), while SLActive displayed not significantly higher values at 30 (p = 0.51) and 60 days (p = 0.061). Conclusion Both implant surfaces show an intimate interaction with newly formed bone. PMID:29445746

Comparison of bond strength and surface morphology of dental enamel for acid and Nd-YAG laser etching

NASA Astrophysics Data System (ADS)

Parmeswearan, Diagaradjane; Ganesan, Singaravelu; Ratna, P.; Koteeswaran, D.

1999-05-01

Recently, laser pretreatment of dental enamel has emerged as a new technique in the field of orthodontics. However, the changes in the morphology of the enamel surface is very much dependent on the wavelength of laser, emission mode of the laser, energy density, exposure time and the nature of the substance absorbing the energy. Based on these, we made a comparative in vitro study on laser etching with acid etching with reference to their bond strength. Studies were conducted on 90 freshly extracted, non carious, human maxillary or mandibular anteriors and premolars. Out of 90, 60 were randomly selected for laser irradiation. The other 30 were used for conventional acid pretreatment. The group of 60 were subjected to Nd-YAG laser exposure (1060 nm, 10 Hz) at differetn fluences. The remaining 30 were acid pretreated with 30% orthophosphoric acid. Suitable Begg's brackets were selected and bound to the pretreated surface and the bond strength were tested using Instron testing machine. The bond strength achieved through acid pretreatment is found to be appreciably greater than the laser pretreated tooth. Though the bond strength achieved through the acid pretreated tooth is found to be significantly greater than the laser pretreated specimens, the laser pretreatement is found to be successful enough to produce a clinically acceptable bond strength of > 0.60 Kb/mm. Examination of the laser pre-treated tooth under SEM showed globule formation which may produce the mechanical interface required for the retention of the resin material.

Permeability of Dental Adhesives – A SEM Assessment

PubMed Central

Malacarne-Zanon, Juliana; de Andrade e Silva, Safira M.; Wang, Linda; de Goes, Mario F.; Martins, Adriano Luis; Narvaes-Romani, Eliene O.; Anido-Anido, Andrea; Carrilho, Marcela R. O.

2010-01-01

Objectives: To morphologically evaluate the permeability of different commercial dental adhesives using scanning electron microscopy. Methods: Seven adhesive systems were evaluated: one three-step system (Scotchbond Multi-Purpose - MP); one two-step self-etching primer system (Clearfil SE Bond – SE); three two-step etch-and-rinse systems (Single Bond 2 – SB; Excite – EX; One-Step – OS); and two single-step self-etching adhesives (Adper Prompt – AP; One-Up Bond F – OU). The mixture of primer and bond agents of the Clearfil SE Bond system (SE-PB) was also tested. The adhesives were poured into a brass mold (5.8 mm x 0.8 mm) and light-cured for 80 s at 650 mW/cm2. After a 24 h desiccation process, the specimens were immersed in a 50% ammoniac silver nitrate solution for tracer permeation. Afterwards, they were sectioned in ultra-fine slices, carbon-coated, and analyzed under backscattered electrons in a scanning electron microscopy. Results: MP and SE showed slight and superficial tracer permeation. In EX, SB, and OS, permeation extended beyond the inner superficies of the specimens. SE-PB did not mix well, and most of the tracer was precipitated into the primer agent. In AP and OU, “water-trees” were observed all over the specimens. Conclusions: Different materials showed distinct permeability in aqueous solution. The extent of tracer permeation varied according to the composition of each material and it was more evident in the more hydrophilic and solvated ones. PMID:20922163

Influence of different repair procedures on bond strength of adhesive filling materials to etched enamel in vitro.

PubMed

Hannig, Christian; Hahn, Petra; Thiele, Patrick-Philipp; Attin, Thomas

2003-01-01

Contamination of etched enamel with repair bond agents during repair of dental restorations may interfere with the bonding of composite to enamel. This study examined the bond strength of adhesive filling materials to etched bovine enamel after pre-treatment with the repair systems Monobond S, Silibond and Co-Jet. The materials Tetric Ceram, Dyract and Definite and their corresponding bonding agents (Syntac Single Comp, Prime & Bond NT, Etch and Prime) were tested in combination with the repair systems. One hundred and thirty-five enamel specimens were etched (37% phosphoric acid, 60 seconds) and equally distributed among three groups (A-C). In Group A, the repair materials were applied on etched enamel followed by applying the composite materials without using their respective bonding material. In Group B, the composite materials were placed on etched enamel after applying the repair materials and bonding agents. In control Group C, the composite materials and bonding agents were applied on etched enamel without using the repair systems. In each sub-group, every composite material was applied on 15 specimens. Samples were stored in artificial saliva for 14 days and thermocycled 1,000 times (5 degrees C/55 degrees C). The shear bond strength of the samples were then determined in a universal testing machine (ISO 10477). Applying Monobond or Silibond followed by the use of its respective bonding agents resulted in a bond strength that was not statistically different from the controls for all filling materials (Group C). The three composites that used Monobond and Silibond without applying the corresponding bonding agent resulted in bond strengths that were significantly lower than the controls. Utilizing the Co-Jet-System drastically reduced the bond strength of composites on etched enamel. Contamination of etched enamel with the repairing bonding agents Monobond and Silibond does not interfere with bond strength if the application of Monobond and Silibond is followed by using its corresponding bonding system of the composites tested.

The improvement of adhesive properties of PEEK through different pre-treatments

NASA Astrophysics Data System (ADS)

Hallmann, Lubica; Mehl, Albert; Sereno, Nuno; Hämmerle, Christoph H. F.

2012-07-01

The purpose of this in vitro study was the evaluation of the bond strength of the adhesives/composite resin to Poly Ether Ether Ketone (PEEK) based dental polymer after using different surface conditioning methods. PEEK blanks were cut into discs. All disc specimens were polished with 800 grit SiC paper and divided into 6 main groups. Main groups were divided into 2 subgroups. The main groups of 32 specimens each were treated as follow: (1) control specimens (no treatment), (2) piranha solution etching, (3) abraded with 50 μm alumina particles and chemical etching, (4) abraded with 110 μm alumina particles and chemical etching, (5) abraded with 30 μm silica-coated alumina particles and chemical etching, (6) abraded with 110 μm silica-coated alumina particles and chemical etching. Plexiglas tubes filled with a composite resin (RelyX Unicem) were bonded to the specimens. The adhesives used were Heliobond and Clearfil Ceramic Primer. Each specimen was stored in distilled water (37 °C) for 3 days. Tensile bond strength was measured in a universal testing machine and failure methods were evaluated. Abraded surface with 50 μm alumina particles followed by etching with piranha solution lead to the highest bond strength of 21.4 MPa when Heliobond like adhesive was used. Tribochemical silica coated/etched PEEK surfaces did not have an effect on the bond strength. Non-treated PEEK surface was not able to establish a bond with composite resin. The proper choice of adhesive/composite resin system leads to a strong bond. ConclusionAirborne particle abrasion in combination with piranha solution etching improves the adhesive properties of PEEK.

Influence of Conditioning Time of Universal Adhesives on Adhesive Properties and Enamel-Etching Pattern.

PubMed

Cardenas, A M; Siqueira, F; Rocha, J; Szesz, A L; Anwar, M; El-Askary, F; Reis, A; Loguercio, A

2016-01-01

To evaluate the effect of application protocol in resin-enamel microshear bond strength (μSBS), in situ degree of conversion, and etching pattern of three universal adhesive systems. Sixty-three extracted third molars were sectioned in four parts (buccal, lingual, and proximals) and divided into nine groups, according to the combination of the main factors-Adhesive (Clearfil Universal, Kuraray Noritake Dental Inc, Tokyo, Japan; Futurabond U, VOCO, Cuxhaven, Germany; and Scotchbond Universal Adhesive, 3M ESPE, St Paul, MN, USA)-and enamel treatment/application time (etch-and-rinse mode [ER], self-etch [SE] application for 20 seconds [SE20], and SE application for 40 seconds [SE40]). Specimens were stored in water (37°C/24 h) and tested at 1.0 mm/min (μSBS). The degree of conversion of the adhesives at the resin-enamel interfaces was evaluated using micro-Raman spectroscopy. The enamel-etching pattern was evaluated under a scanning electron microscope. Data were analyzed with two-way analysis of variance and Tukey test (α=0.05). In general, the application of the universal adhesives in the SE40 produced μSBS and degree of conversion that were higher than in the SE20 (p<0.01) and similar to the ER mode. The deepest enamel-etching pattern was obtained in the ER mode, followed by the SE40. The active and prolonged application of universal adhesives in the SE mode may be a viable alternative to increase the degree of conversion, etching pattern, and resin-enamel bond strength.

Ultrastructure of the surface of dental enamel with molar incisor hypomineralization (MIH) with and without acid etching.

PubMed

Bozal, Carola B; Kaplan, Andrea; Ortolani, Andrea; Cortese, Silvina G; Biondi, Ana M

2015-01-01

The aim of the present work was to analyze the ultrastructure and mineral composition of the surface of the enamel on a molar with MIH, with and without acid etching. A permanent tooth without clinical MIH lesions (control) and a tooth with clinical diagnosis of mild and moderate MIH, with indication for extraction, were processed with and without acid etching (H3PO4 37%, 20") for observation with scanning electron microscope (SEM) ZEISS (Supra 40) and mineral composition analysis with an EDS detector (Oxford Instruments). The control enamel showed normal prismatic surface and etching pattern. The clinically healthy enamel on the tooth with MIH revealed partial loss of prismatic pattern. The mild lesion was porous with occasional cracks. The moderate lesion was more porous, with larger cracks and many scales. The mineral composition of the affected surfaces had lower Ca and P content and higher O and C. On the tooth with MIH, even on normal looking enamel, the demineralization does not correspond to an etching pattern, and exhibits exposure of crystals with rods with rounded ends and less demineralization in the inter-prismatic spaces. Acid etching increased the presence of cracks and deep pores in the adamantine structure of the enamel with lesion. In moderate lesions, the mineral composition had higher content of Ca, P and Cl. Enamel with MIH, even on clinically intact adamantine surfaces, shows severe alterations in the ultrastructure and changes in ionic composition, which affect the acid etching pattern and may interfere with adhesion.

Finite element analysis (FEA) of dental implant fixture for mechanical stability and rapid osseointegration

NASA Astrophysics Data System (ADS)

Tabassum, Shafia; Murtaza, Ahmar; Ali, Hasan; Uddin, Zia Mohy; Zehra, Syedah Sadaf

2017-10-01

For rapid osseointegration of dental implant fixtures, various surface treatments including plasma spraying, hydroxyapatite coating, acid-etching, and surface grooving are used. However undesirable effects such as chemical modifications, loss of mechanical properties, prolonged processing times and post production treatment steps are often associated with these techniques. The osseointegration rate of the dental implants can be promoted by increasing the surface area of the dental implant, thus increasing the bone cells - implant material contact and allow bone tissues to grow rapidly. Additive Manufacturing (AM) techniques can be used to fabricate dental implant fixtures with desirable surface area in a single step manufacturing process. AM allows the use of Computer Aided Designing (CAD) for customised rapid prototyping of components with precise control over geometry. In this study, the dental implant fixture that replaces the tooth root was designed on commercially available software COMSOL. Nickel - titanium alloy was selected as build materials for dental implant. The geometry of the dental fixture was varied by changing the interspacing distance (thread pitch) and number of threads to increase the total surface area. Three different microstructures were introduced on the surface of dental implant. The designed models were used to examine the effect of changing geometries on the total surface area. Finite Element Analysis (FEA) was performed to investigate the effect of changing geometries on the mechanical properties of the dental implant fixtures using stress analysis.

In-vitro transdentinal diffusion of monomers from adhesives.

PubMed

Putzeys, Eveline; Duca, Radu Corneliu; Coppens, Lieve; Vanoirbeek, Jeroen; Godderis, Lode; Van Meerbeek, Bart; Van Landuyt, Kirsten L

2018-06-01

Biocompatibility of adhesives is important since adhesives may be applied on dentin near the pulp. Accurate knowledge of the quantity of monomers reaching the pulp is important to determine potential side effects. The aim of this study was to assess the transdentinal diffusion of residual monomers from dental adhesive systems using an in-vitro pulp chamber model. Dentin disks with a thickness of 300 µm were produced from human third molars. These disks were fixed between two open-ended glass tubes, representing an in-vitro pulp chamber. The etch-and-rinse adhesive OptiBond FL and the self-etch adhesive Clearfil SE Bond were applied to the dentin side of the disks, while on in the pulpal side, the glass tube was filled with 600 µL water. The transdentinal diffusion of different monomers was quantified using ultra-performance liquid chromatography-tandem mass spectrometry. The monomers HEMA, CQ, BisGMA, GPDM, 10-MDP and UDMA eluted from the dental materials and were able to diffuse through the dentin disks to a certain extent. Compounds with a lower molecular weight (uncured group: HEMA 7850 nmol and CQ 78.2 nmol) were more likely to elute and diffuse compared to monomers with a higher molecular weight (uncured group: BisGMA 0.42 nmol). When the adhesives were left uncured, diffusion was up to 10 times higher compared to the cured conditions. This in-vitro research resulted in the quantification of various monomers able to diffuse through dentin and therefore contributes to a more detailed understanding about the potential exposure of the dental pulp to monomers from dental adhesives. Biocompatibility of adhesives is important since adhesives may be applied on dentin near the pulp, where tubular density and diameter are greatest. Copyright © 2018. Published by Elsevier Ltd.

Analysis of eroded bovine teeth through laser speckle imaging

NASA Astrophysics Data System (ADS)

Koshoji, Nelson H.; Bussadori, Sandra K.; Bortoletto, Carolina C.; Oliveira, Marcelo T.; Prates, Renato A.; Deana, Alessandro M.

2015-02-01

Dental erosion is a non-carious lesion that causes progressive tooth wear of structure through chemical processes that do not involve bacterial action. Its origin is related to eating habits or systemic diseases involving tooth contact with substances that pose a very low pH. This work demonstrates a new methodology to quantify the erosion by coherent light scattering of tooth surface. This technique shows a correlation between acid etch duration and laser speckle contrast map (LASCA). The experimental groups presented a relative contrast between eroded and sound tissue of 17.8(45)%, 23.4 (68)% 39.2 (40)% and 44.3 (30)%, for 10 min, 20 min, 30 min and 40 min of acid etching, respectively.

Measurement of the efficacy of calcium silicate for the protection and repair of dental enamel.

PubMed

Parker, Alexander S; Patel, Anisha N; Al Botros, Rehab; Snowden, Michael E; McKelvey, Kim; Unwin, Patrick R; Ashcroft, Alexander T; Carvell, Mel; Joiner, Andrew; Peruffo, Massimo

2014-06-01

To investigate the formation of hydroxyapatite (HAP) from calcium silicate and the deposition of calcium silicate onto sound and acid eroded enamel surfaces in order to investigate its repair and protective properties. Calcium silicate was mixed with phosphate buffer for seven days and the resulting solids analysed for crystalline phases by Raman spectroscopy. Deposition studies were conducted on bovine enamel surfaces. Acid etched regions were produced on the enamel surfaces using scanning electrochemical cell microscopy (SECCM) with acid filled pipettes and varying contact times. Following treatment with calcium silicate, the deposition was visualised with FE-SEM and etch pit volumes were measured by AFM. A second set of bovine enamel specimens were pre-treated with calcium silicate and fluoride, before acid exposure with the SECCM. The volumes of the resultant acid etched pits were measured using AFM and the intrinsic rate constant for calcium loss was calculated. Raman spectroscopy confirmed that HAP was formed from calcium silicate. Deposition studies demonstrated greater delivery of calcium silicate to acid eroded than sound enamel and that the volume of acid etched enamel pits was significantly reduced following one treatment (p<0.05). In the protection study, the intrinsic rate constant for calcium loss from enamel was 0.092 ± 0.008 cm/s. This was significantly reduced, 0.056 ± 0.005 cm/s, for the calcium silicate treatments (p<0.0001). Calcium silicate can transform into HAP and can be deposited on acid eroded and sound enamel surfaces. Calcium silicate can provide significant protection of sound enamel from acid challenges. Calcium silicate is a material that has potential for a new approach to the repair of demineralised enamel and the protection of enamel from acid attacks, leading to significant dental hard tissue benefits. © 2014 Elsevier Ltd. All rights reserved.

Bonding strategies for MIH-affected enamel and dentin.

PubMed

Krämer, Norbert; Bui Khac, Ngoc-Han Nana; Lücker, Susanne; Stachniss, Vitus; Frankenberger, Roland

2018-02-01

Aim of the present study was to evaluate resin composite adhesion to dental hard tissues affected by molar incisor hypomineralisation (MIH). 94 freshly extracted human molars and incisors (53 suffering MIH) were used. 68 teeth (35 with MIH) were used for μ-TBS tests in enamel and dentin, 26 (18 with MIH) for qualitative evaluation. Specimens were bonded with Clearfil SE Bond, Scotchbond Universal, and OptiBond FL. For MIH affected enamel, additional OptiBond FL groups with NaOCl and NaOCl+Icon were investigated. Beside fractographic analysis, also qualitative evaluations were performed using SEM at different magnifications as well as histological sectioning. Highest μ-TBS values were recorded with dentin specimens (ANOVA, mod. LSD, p<0.05). Results were independent of adhesive and dentin substrate (p>0.05). Pre-test failures did not occur in dentin specimens. Sound enamel specimens exhibited significantly higher μ-TBS values than MIH enamel (p<0.05). The two-step self-etch adhesive (Clearfil SE Bond) and the two-step etch-and-rinse adhesive (Scotchbond Universal) showed the lowest values in affected enamel specimens (p<0.05) with most pre-test failures (p<0.05). OptiBond FL on affected enamel showed better results than Clearfil SE Bond (p<0.05). An additional pre-treatment of affected enamel with NaOCl or NaOCl and Icon did not enhance enamel bonding (p>0.05), however, it caused less pre-test failures (p<0.05). Micromorphological analyses revealed that conventional phosphoric acid etching produces a much less pronounced etching pattern in affected enamel and a porous structure as weak link for the resin-enamel bond was identified. Bonding to porous hypomineralized MIH enamel is the limiting factor in adhesion to MIH teeth. MIH-affected dentin may be bonded conventionally. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

[Nutrition, diet and dental health--de- and remineralisation of teeth].

PubMed

Imfeld, Thomas

2008-02-01

There is little if any evidence that nutrition during the time of tooth formation has any clinically significant effect on caries susceptibility of erupted teeth in man. Caries, erosion and demastication are not nutritional diseases. They are, however, diet-related diseases because erupted teeth are subject to local chemical and mechanical effects of the diet contacting the teeth. Caries is the result of a chronic undermining demineralisation of the teeth by organic acids that are produced by the bacteria of the dental biofilm while fermenting carbohydrates from the human diet. Dental erosion is the result of a chronic localised loss of dental hard tissue etched away from the surface by acids derived from the diet or from gastric reflux. The physicochemical grounds of de- and remineralisation of teeth are explained using detailed diagrams. Initial caries lesions without cavitation of the surface can remineralise (heal) under conditions of low cariogenic diet and good oral hygiene. However, once the surface has broken and cavitation occurred, there is no alternative to restorative dental therapy because remineralisation is no more possible.

Impact of Dental Implant Surface Modifications on Osseointegration

PubMed Central

Smeets, Ralf; Stadlinger, Bernd; Schwarz, Frank; Beck-Broichsitter, Benedicta; Jung, Ole; Precht, Clarissa; Kloss, Frank; Gröbe, Alexander; Heiland, Max

2016-01-01

Objective. The aim of this paper is to review different surface modifications of dental implants and their effect on osseointegration. Common marketed as well as experimental surface modifications are discussed. Discussion. The major challenge for contemporary dental implantologists is to provide oral rehabilitation to patients with healthy bone conditions asking for rapid loading protocols or to patients with quantitatively or qualitatively compromised bone. These charging conditions require advances in implant surface design. The elucidation of bone healing physiology has driven investigators to engineer implant surfaces that closely mimic natural bone characteristics. This paper provides a comprehensive overview of surface modifications that beneficially alter the topography, hydrophilicity, and outer coating of dental implants in order to enhance osseointegration in healthy as well as in compromised bone. In the first part, this paper discusses dental implants that have been successfully used for a number of years focusing on sandblasting, acid-etching, and hydrophilic surface textures. Hereafter, new techniques like Discrete Crystalline Deposition, laser ablation, and surface coatings with proteins, drugs, or growth factors are presented. Conclusion. Major advancements have been made in developing novel surfaces of dental implants. These innovations set the stage for rehabilitating patients with high success and predictable survival rates even in challenging conditions. PMID:27478833

Surface Modifications and Their Effects on Titanium Dental Implants

PubMed Central

Jemat, A.; Ghazali, M. J.; Razali, M.; Otsuka, Y.

2015-01-01

This review covers several basic methodologies of surface treatment and their effects on titanium (Ti) implants. The importance of each treatment and its effects will be discussed in detail in order to compare their effectiveness in promoting osseointegration. Published literature for the last 18 years was selected with the use of keywords like titanium dental implant, surface roughness, coating, and osseointegration. Significant surface roughness played an important role in providing effective surface for bone implant contact, cell proliferation, and removal torque, despite having good mechanical properties. Overall, published studies indicated that an acid etched surface-modified and a coating application on commercial pure titanium implant was most preferable in producing the good surface roughness. Thus, a combination of a good surface roughness and mechanical properties of titanium could lead to successful dental implants. PMID:26436097

Atomic force microscopy analysis of different surface treatments of Ti dental implant surfaces

NASA Astrophysics Data System (ADS)

Bathomarco, Ti R. V.; Solorzano, G.; Elias, C. N.; Prioli, R.

2004-06-01

The surface of commercial unalloyed titanium, used in dental implants, was analyzed by atomic force microscopy. The morphology, roughness, and surface area of the samples, submitted to mechanically-induced erosion, chemical etching and a combination of both, were compared. The results show that surface treatments strongly influence the dental implant physical and chemical properties. An analysis of the length dependence of the implant surface roughness shows that, for scan sizes larger than 50 μm, the average surface roughness is independent of the scanning length and that the surface treatments lead to average surface roughness in the range of 0.37 up to 0.48 μm. It is shown that the implant surface energy is sensitive to the titanium surface area. As the area increases there is a decrease in the surface contact angle.

Biocompatability of compomer restorative systems on nonexposed dental pulps of primate teeth.

PubMed

Tarim, B; Hafez, A A; Suzuki, S H; Suzuki, S; Cox, C F

1997-01-01

This study evaluated the histologic response of total-etched and nonetched compomer restored cavity preparations. One hundred fifteen class 5 cavity preparations were placed in the teeth of four healthy adult monkeys at 7, 27, and 90 days. A 37% H3PO4 was applied for 10 seconds and rinsed in total-etched preparations. No statistical differences were seen in inflammatory reactions among total-etched or nonetched compomers at 7, 27, and 90 days. There were no statistical differences in inflammatory cell responses among all compomer systems in regard to time intervals. Pulpal responses of compomers were greater than IRM at each time period. Pulp responses were associated with stained bacteria in 32 of 89 compomer teeth. No necrotic pulps were seen in any teeth. Statistical data show a positive correlation (P < 0.05) between bacterial presence and pulpal inflammation. IRM pulps showed no inflammation or bacterial staining. Compomers are biologically compatible with pulp tissues when bacteria are excluded.

Effects of various etching protocols on the flexural properties and surface topography of fiber-reinforced composite dental posts.

PubMed

Aksornmuang, Juthatip; Chuenarrom, Chanya; Chittithaworn, Natjira

2017-09-26

The purpose of this study was to evaluate the flexural properties and surface topography of fiber posts surface-treated with various etching protocols. Seventy each of three types of fiber posts: RelyX Fiber Post, Tenax Fiber Trans, and D.T. Light-Post Illusion X-Ro, were randomly divided into 7 groups: no surface treatment, surface treated with hydrofluoric acid (HF) 4.5% for 60 s, HF 4.5% for 120 s, HF 9.6% for 15 s, HF 9.6% for 60 s, HF 9.6% for 120 s, and treated with H 2 O 2 24% for 10 min. The specimens were then subjected to a three-point bending test. Surface topographies of the posts were observed using a SEM. The results indicate that fiber post surface pretreatments had no adverse effects on the flexural properties. However, the fiber posts treated with high HF concentrations or long etching times seemed to have more surface irregularities.

Comparison of bioactive glass coated and hydroxyapatite coated titanium dental implants in the human jaw bone.

PubMed

Mistry, S; Kundu, D; Datta, S; Basu, D

2011-03-01

Current trends in clinical dental implant therapy include modification of titanium surfaces for the purpose of improving osseointegration by different additive (bioactive coatings) and subtractive processes (acid etching, grit-blasting). The aim of this study was to evaluate and compare the behaviour of hydroxyapatite and the newly developed bioactive glass coated implants (62 implants) in osseous tissue following implantation in 31 patients. Bioactive glass and hydroxyapatite was suitably coated on titanium alloy. Hydroxyapatite coating was applied on the implant surface by air microplasma spray technique and bioactive glass coating was applied by vitreous enamelling technique. The outcome was assessed up to 12 months after prosthetic loading using different clinical and radiological parameters. Hydroxyapatite and bioactive glass coating materials were non-toxic and biocompatible. Overall results showed that bioactive glass coated implants were as equally successful as hydroxyapatite in achieving osseointegration and supporting final restorations. The newly developed bioactive glass is a good alternative coating material for dental implants. © 2011 Australian Dental Association.

Relationship between mechanical properties of one-step self-etch adhesives and water sorption.

PubMed

Hosaka, Keiichi; Nakajima, Masatoshi; Takahashi, Masahiro; Itoh, Shima; Ikeda, Masaomi; Tagami, Junji; Pashley, David H

2010-04-01

The purpose of this study was to evaluate the relationship between changes in the modulus of elasticity and ultimate tensile strength of one-step self-etch adhesives, and their degree of water sorption. Five one-step self-etch adhesives, Xeno IV (Dentsply Caulk), G Bond (GC Corp.), Clearfil S3 Bond (Kuraray Medical Inc.), Bond Force (Tokuyama Dental Corp.), and One-Up Bond F Plus (Tokuyama Dental Corp.) were used. Ten dumbelled-shaped polymers of each adhesive were used to obtain the modulus of elasticity by the three-point flexural bending test and the ultimate tensile strength by microtensile testing. The modulus of elasticity and the ultimate tensile strength were measured in both dry and wet conditions before/after immersion in water for 24h. Water sorption was measured, using a modification of the ISO-4049 standard. Each result of the modulus of elasticity and ultimate tensile strength was statistically analyzed using a two-way ANOVA and the result of water sorption was statistically analyzed using a one-way ANOVA. Regression analyses were used to determine the correlations between the modulus of elasticity and the ultimate tensile strength in dry or wet states, and also the percent decrease in these properties before/after immersion of water vs. water sorption. In the dry state, the moduli of elasticity of the five adhesive polymers varied from 948 to 1530 MPa, while the ultimate tensile strengths varied from 24.4 to 61.5 MPa. The wet specimens gave much lower moduli of elasticity (from 584 to 1073 MPa) and ultimate tensile strengths (from 16.5 to 35.0 MPa). Water sorption varied from 32.1 to 105.8 g mm(-3). The moduli of elasticity and ultimate tensile strengths of the adhesives fell significantly after water-storage. Water sorption depended on the constituents of the adhesive systems. The percent decreases in the ultimate tensile strengths of the adhesives were related to water sorption, while the percent reductions in the moduli of elasticity of the adhesives were not related to water sorption. Copyright (c) 2009 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Repair bond strength of resin composite to bilayer dental ceramics

PubMed Central

2018-01-01

PURPOSE The purpose of this study was to investigate the effect of various surface treatments (ST) on the shear bond strength of resin composite to three bilayer dental ceramics made by CAD/CAM and two veneering ceramics. MATERIALS AND METHODS Three different bilayer dental ceramics and two different veneering ceramics were used (Group A: IPS e.max CAD+IPS e.max Ceram; Group B: IPS e.max ZirCAD+IPS e.max Ceram, Group C: Vita Suprinity+Vita VM11; Group D: IPS e.max Ceram; Group E: Vita VM11). All groups were divided into eight subgroups according to the ST. Then, all test specimens were repaired with a nano hybrid resin composite. Half of the test specimens were subjected to thermocycling procedure and the other half was stored in distilled water at 37℃. Shear bond strength tests for all test specimens were carried out with a universal testing machine. RESULTS There were statistically significant differences among the tested surface treatments within the all tested fracture types (P<.005). HF etching showed higher bond strength values in Groups A, C, D, and E than the other tested ST. However, bonding durability of all the surface-treated groups were similar after thermocycling (P>.00125). CONCLUSION This study revealed that HF etching for glass ceramics and sandblasting for zirconia ceramics were adequate for repair of all ceramic restorations. The effect of ceramic type exposed on the fracture area was not significant on the repair bond strength of resin composites to different ceramic types. PMID:29713430

Effect of moisture on dental enamel in the interaction of two orthodontic bonding systems.

PubMed

Bertoz, André Pinheiro de Magalhães; de Oliveira, Derly Tescaro Narcizo; Gimenez, Carla Maria Melleiro; Briso, André Luiz Fraga; Bertoz, Francisco Antonio; Santos, Eduardo César Almada

2013-01-01

The purpose of this study was to assess by means of scanning electron microscopy (SEM) the remaining adhesive interface after debonding orthodontic attachments bonded to bovine teeth with the use of hydrophilic and hydrophobic primers under different dental substrate moisture conditions. Twenty mandibular incisors were divided into four groups (n = 5). In Group I, bracket bonding was performed with Transbond MIP hydrophilic primer and Transbond XT adhesive paste applied to moist substrate, and in Group II a bonding system comprising Transbond XT hydrophobic primer and adhesive paste was applied to moist substrate. Brackets were bonded to the specimens in Groups III and IV using the same adhesive systems, but on dry dental enamel. The images were qualitatively assessed by SEM. The absence of moisture in etched enamel enabled better interaction between bonding materials and the adamantine structure. The hydrophobic primer achieved the worst micromechanical interlocking results when applied to a moist dental structure, whereas the hydrophilic system proved versatile, yielding acceptable results in moist conditions and excellent interaction in the absence of contamination. The authors assert that the best condition for the application of primers to dental enamel occurs in the absence of moisture.

Effect of a non-thermal, atmospheric-pressure, plasma brush on conversion of model self-etch adhesive formulations compared to conventional photo-polymerization

PubMed Central

Chen, Mingsheng; Zhang, Ying; Yao, Xiaomei; Li, Hao; Yu, Qingsong; Wang, Yong

2012-01-01

Objective To determine the effectiveness and efficiency of non-thermal, atmospheric plasmas for inducing polymerization of model dental self-etch adhesives. Methods The monomer mixtures used were bis-[2-(methacryloyloxy)ethyl] phosphate (2MP) and 2-hydroxyethyl methacrylate (HEMA), with mass ratios of 70/30, 50/50 and 30/70. Water was added to the above formulations: 10–30 wt%. These monomer/water mixtures were treated steadily for 40 s under a non-thermal atmospheric plasma brush working at temperatures from 32° to 35°C. For comparison, photo-initiators were added to the above formulations for photo-polymerization studies, which were light-cured for 40 s. The degree of conversion (DC) of both the plasma- and light-cured samples was measured using FTIR spectroscopy with an attenuated total reflectance attachment. Results The non-thermal plasma brush was effective in inducing polymerization of the model self-etch adhesives. The presence of water did not negatively affect the DC of plasma-cured samples. Indeed, DC values slightly increased, with increasing water content in adhesives: from 58.3% to 68.7% when the water content increased from 10% to 30% in the adhesives with a 50/50 (2MP/HEMA) mass ratio. Conversion values of the plasma-cured groups were higher than those of light-cured samples with the same mass ratio and water content. Spectral differences between the plasma- and light-cured groups indicate subtle structural distinctions in the resultant polymer networks. Significance This research if the first to demonstrate that the non-thermal plasma brush induces polymerization of model adhesives under clinical settings by direct/indirect energy transfer. This device shows promise for polymerization of dental composite restorations having enhanced properties and performance. PMID:23018084

Enhanced transport of materials into enamel nanopores via electrokinetic flow.

PubMed

Gan, H Y; Sousa, F B; Carlo, H L; Maciel, P P; Macena, M S; Han, J

2015-04-01

The ability to infiltrate various molecules and resins into dental enamel is highly desirable in dentistry, yet transporting materials into dental enamel is limited by the nanometric scale of their pores. Materials that cannot be infiltrated into enamel by diffusion/capillarity are often considered molecules with sizes above a critical threshold, which are often considered to be larger than the pores of enamel. We challenge this notion by reporting the use of electrokinetic flow to transport solutions with molecules with sizes above a critical threshold-namely, an aqueous solution with a high refractive index (Thoulet's solution) and a curable fluid resin infiltrant (without acid etching)-deep into the normal enamel layer. Volume infiltration by Thoulet's solution is increased by 5- to 6-fold, and resin infiltration depths as large as 600 to 2,000 µm were achieved, in contrast to ~10 µm resulting from diffusion/capillarity. Incubation with demineralization solution for 192 h resulted in significant demineralization at noninfiltrated histologic points but not at resin infiltrated. These results open new avenues for the transport of materials in dental enamel. © International & American Associations for Dental Research 2015.

Morphological and chemical characteristics of different titanium surfaces treated by bicarbonate and glycine powder air abrasive systems.

PubMed

Menini, Maria; Piccardo, Paolo; Baldi, Domenico; Dellepiane, Elena; Pera, Paolo

2015-02-01

This in vitro study investigated possible morphological and chemical changes induced by glycine or sodium bicarbonate powder air polishing on machined and acid-etched titanium surfaces. The glycine powder (granulometry <65 μm) and sodium bicarbonate powder (granulometry <150 μm) were applied on 2 machined healing abutments and on 2 acid-etched healing abutments. The samples were characterized by scanning electron microscopy coupled with energy dispersive x-ray spectroscopy. The analyses were performed at different steps: (1) as received, right after opening the abutment packaging; (2) after 20 minutes air exposure; (3) after aging in artificial saliva; (4) after glycine or sodium bicarbonate powder air polishing for 5 seconds; (5) after repetition of steps 3 and 4 with longer time of polishing (20 seconds). Air polishing using glycine and sodium bicarbonate powder seemed to be safe for professional oral hygiene of titanium dental implants, although acid-etched abutments and abutments treated with bicarbonate harbored more salts. This might indicate a greater plaque accumulation in a clinical situation. However, this result has to be investigated in vivo to understand its clinical relevance.

Retrospective clinical study of an implant with a sandblasted, large-grit, acid-etched surface and internal connection: analysis of short-term success rate and marginal bone loss.

PubMed

Lee, Jae-Wang; An, Jun Hyeong; Park, Sang-Hoon; Chong, Jong-Hyon; Kim, Gwang-Seok; Han, JeongJoon; Jung, Seunggon; Kook, Min-Suk; Oh, Hee-Kyun; Ryu, Sun-Youl; Park, Hong-Ju

2016-12-01

The purpose of this retrospective study was to evaluate the clinical utility of an implant with a sandblasted, large-grit, acid-etched (SLA) surface and internal connection. Six patients who received dental implants in the Department of Oral and Maxillofacial Surgery, Chonnam National University Dental Hospital, were analyzed by factors influencing the success rate and marginal bone loss. Factors included patient's age, sex, implant installation site, whether bone graft was done, type of bone graft materials, approaching method if sinus lift was done, and the size of the fixture. In addition, the marginal bone loss was analyzed by using a radiograph. All implants were successful, and the cumulative survival rate was 100 %. Average marginal bone loss of 6 months after the installation was 0.52 mm and 20 months after the functional loading was 1.06 mm. Total marginal bone resorption was 1.58 mm on average. There was no statistically significant difference in mesial and distal marginal bone loss. The short-term clinical success rate of the implant with an SLA surface and internal connection was satisfactory. Moreover, the marginal bone loss was also consistent with the implant success criteria.

The impact of hydrofluoric acid etching followed by unfilled resin on the biaxial strength of a glass-ceramic.

PubMed

Posritong, Sumana; Borges, Alexandre Luiz Souto; Chu, Tien-Min Gabriel; Eckert, George J; Bottino, Marco A; Bottino, Marco C

2013-11-01

To evaluate the null hypotheses that hydrofluoric (HF) acid etching time would neither decrease the biaxial flexural strength of a glass-based veneering ceramic nor enhance it after silane and unfilled resin (UR) applications. Disc-shaped IPS e.max ZirPress specimens were allocated into 12 groups: G1-control (no-etching), G2-30 s, G3-60 s, G4-90 s, G5-120 s, G6-60 s+60 s. Groups (G7-G12) were treated in the same fashion as G1-G6, but followed by silane and UR applications. Surface morphology and roughness (Ra and Rq) of the ceramics were assessed by means of scanning electron microscopy (SEM) and profilometry, respectively. Flexural strength was determined by biaxial testing. Data were analyzed by two-way ANOVA and the Sidak test (α=0.05). Weibull statistics were estimated and finite element analysis (FEA) was carried out to verify the stress concentration end areas of fracture. The interaction (etching time vs. surface treatment) was significant for Ra (p=0.008) and Rq (0.0075). Resin-treated groups presented significantly lower Ra and Rq than non-treated groups, except for the 60s group (p<0.005). SEM revealed that etching affected the ceramic microstructure and that the UR was able to penetrate into the irregularities. A significant effect of etching time (p=0.029) on flexural strength was seen. G7-G12 presented higher strength than G1-G6 (p<0.0001). None of experimental groups failed to show 95% confidence intervals of σ0 and m overlapped. FEA showed lower stress concentration after resin treatment. HF acid etching time did not show a damaging effect on the ceramic flexural strength. Moreover, the flexural strength could be enhanced after UR treatment. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of Storage Time on Bond Strength and Nanoleakage Expression of Universal Adhesives Bonded to Dentin and Etched Enamel.

PubMed

Makishi, P; André, C B; Ayres, Apa; Martins, A L; Giannini, M

2016-01-01

To investigate bond strength and nanoleakage expression of universal adhesives (UA) bonded to dentin and etched enamel. Extracted human third molars were sectioned and ground to obtain flat surfaces of dentin (n = 36) and enamel (n = 48). Dentin and etched enamel surfaces were bonded with one of two UAs, All-Bond Universal (ABU) or Scotchbond Universal (SBU); or a two-step self-etching adhesive, Clearfil SE Bond (CSEB). A hydrophobic bonding resin, Adper Scotchbond Multi-Purpose Bond (ASMP Bond) was applied only on etched enamel. Following each bonding procedure, resin composite blocks were built up incrementally. The specimens were sectioned and subjected to microtensile bond strength (MTBS) testing after 24 hours or one year water storage, or immersed into ammoniacal silver nitrate solution after aging with 10,000 thermocycles and observed using scanning electron microscopy. The percentage distribution of silver particles at the adhesive/tooth interface was calculated using digital image-analysis software. The MTBS (CSEB = SBU > ABU, for dentin; and CSEB > ABU = SBU = ASMP Bond, for etched enamel) differed significantly between the adhesives after 24 hours. After one year, MTBS values were reduced significantly within the same adhesive for both substrates (analysis of variance, Bonferroni post hoc, p<0.05), and no significant differences were found among the adhesives for etched enamel. Silver particles could be detected within the adhesive/dentin interface of all specimens tested. Kruskal-Wallis mean ranks for nanoleakage in ABU, SBU, and CSEB were 16.9, 18.5 and 11, respectively (p>0.05). In the short term, MTBS values were material and dental-substrate dependent. After aging, a decrease in bonding effectiveness was observed in all materials, with nanoleakage at the adhesive/dentin interface. The bonding of the UAs was equal or inferior to that of the conventional restorative systems when applied to either substrate and after either storage period.

Do matrix metalloproteinase inhibitors improve the bond durability of universal dental adhesives?

PubMed

Tekçe, Neslihan; Tuncer, Safa; Demirci, Mustafa; Balci, Sibel

2016-11-01

The aim of this study was to evaluate the effects of matrix metalloproteinases (MMPs) inhibitors on the microtensile bond strength (μTBS) and the adhesive-dentin interface of two universal dentin bonding agents, Single Bond Universal and All Bond Universal, after 12 months of water storage. Seventy extracted, caries-free, human third molars were used in this study. Of these, 50 were used for μTBS testing and 20 were used for scanning electron microscopy. The two bonding agents were applied to flat dentin surfaces in five different ways: self-etch mode, etch-and-rinse mode with 37% phosphoric acid, etch-and-rinse mode with phosphoric acid containing 1% benzalkonium chloride, etch-and-rinse mode with phosphoric acid and 2% chlorhexidine, and etch-and-rinse mode with 0.5 M ethylenediaminetetraacetic acid (EDTA) (n = 5 for each bonding agent in each group; N = 50). Half the specimens were subjected to μTBS tests at 24 h, while half were subjected to the tests after 12 months of water storage. For each bonding agent, inhibition, storage, and their interaction effects were tested by two-way analysis of variance and Bonferroni tests. For Single Bond Universal, the benzalkonium chloride (p = 0.024) and chlorhexidine groups (p = 0.033) exhibited significantly higher μTBS values at 24 h compared with the self-etch group. For All Bond Universal, all groups displayed similar bond strengths at 24 h (p > 0.05). After 12 months of water storage, the μTBS values decreased significantly in the benzalkonium chloride group for Single Bond Universal (p = 0.001) and the self-etch (p = 0.029), chlorhexidine (p = 0.046), and EDTA (p = 0.032) groups for All Bond Universal. These results suggest that the immediate dentin bond strength increases when universal bonding systems are applied in the etch-and-rinse mode, although the durability decreases. The use of chlorhexidine and EDTA can increase the bond durability of mild adhesives such as Single Bond Universal. SCANNING 38:535-544, 2016. © 2016 Wiley Periodicals, Inc. © Wiley Periodicals, Inc.

Shear bond strength of different types of adhesive systems to dentin and enamel of deciduous teeth in vitro.

PubMed

Kensche, A; Dähne, F; Wagenschwanz, C; Richter, G; Viergutz, G; Hannig, C

2016-05-01

The present study aimed to evaluate the suitability of self-etch adhesives for restoration of deciduous teeth compared with etch and rinse approaches. One hundred twenty primary teeth were divided into five groups, each being assigned to an adhesive system. Self-etch adhesives XenoV (XV) and Clearfil S(3) Bond (CB), Prime&Bond NT with (PBE)/without preliminary etching (PBN), and Optibond FL (OBFL) as an etch and rinse system were included. Enamel and dentin specimens were prepared (n = 36/group), adhesives applied, and compomer cylinders polymerized. After 24-h storage in 37 °C distilled water and thermo-cycling (1440 cycles, 5/55 °C, 27 s), shear bond tests and fracture mode classification based on SEM investigation were performed. Statistical analysis involved ANOVA and Scheffé procedure with Bonferroni-Holm correction (p ≤ 0.005). High shear bond strengths to primary enamel were determined for PBE (mean [M] = 22.48 ± 7.7 MPa) > OBFL (M = 19.06 ± 5.62 MPa) > CB (M = 17.6 ± 6.55 MPa), and XV (M = 16.85 ± 5.38 MPa) and PBN (M = 8.26 ± 4.46 MPa) formed significantly less reliable enamel-resin interfaces (p ≤ 0.005). PBE generated the highest bond strength on primary dentin (M = 21.97 ± 8.02 MPa); significantly lower values were measured for XV (M = 13.44 ± 5.43 MPa) and OBFL (M = 12.92 ± 4.31 MPa) (p ≤ 0.005). Adhesives requiring preliminary etching ensure optimal bond strength to primary enamel. If separate etching is to be avoided, selected self-etch adhesives obtain acceptable shear bond values on primary enamel and dentin. The treatment of pediatric patients presents a great challenge in dental practice, and optimization of treatment processes is important.

Bonding efficacy of new self-etching, self-adhesive dual-curing resin cements to dental enamel.

PubMed

Benetti, Paula; Fernandes, Virgílio Vilas; Torres, Carlos Rocha; Pagani, Clovis

2011-06-01

This study evaluated the efficacy of the union between two new self-etching self-adhesive resin cements and enamel using the microtensile bond strength test. Buccal enamel of 80 bovine teeth was submitted to finishing and polishing with metallographic paper to a refinement of #600, in order to obtain a 5-mm2 flat area. Blocks (2 x 4 x 4 mm) of laboratory composite resin were cemented to enamel according to different protocols: (1) untreated enamel + RelyX Unicem cement (RX group); (2) untreated enamel + Bifix SE cement (BF group); (3) enamel acid etching and application of resin adhesive Single Bond + RelyX Unicem (RXA group); (4) enamel acid etching and application of resin adhesive Solobond M + Bifix SE (BFA group). After 7 days of storage in distillated water at 37°C, the blocks were sectioned for obtaining microbar specimens with an adhesive area of 1 mm2 (n = 120). Specimens were submitted to the microtensile bond strength test at a crosshead speed of 0.5 mm/min. The results (in MPa) were analyzed statistically by ANOVA and Tukey's test. Enamel pre-treatment with phosphoric acid and resin adhesive (27.9 and 30.3 for RXA and BFA groups) significantly improved (p ≤ 0.05) the adhesion of both cements to enamel compared to the union achieved with as-polished enamel (9.9 and 6.0 for RX and BF). Enamel pre-treatment with acid etching and the application of resin adhesive significantly improved the bond efficacy of both luting agents compared to the union achieved with as-polished enamel.

Comparative evaluation of surface topography of tooth prepared using erbium, chromium: Yttrium, scandium, gallium, garnet laser and bur and its clinical implications.

PubMed

Verma, Mahesh; Kumari, Pooja; Gupta, Rekha; Gill, Shubhra; Gupta, Ankur

2015-01-01

Erbium, chromium: Yttrium, scandium, gallium, garnet (Er, Cr: YSGG) laser has been successfully used in the ablation of dental hard and soft tissues. It has been reported that this system is also useful for preparing tooth surfaces and etching, but no consensus exist in the literature regarding the advantage of lasers over conventional tooth preparation technique. Labial surfaces of 25 extracted human maxillary central incisors were divided into two halves. Right half was prepared with diamond bur and left half with Er, Cr; YSGG laser and a reduction of 0.3-0.5 mm was carried out. Topography of prepared surfaces of five teeth were examined under scanning electron microscope (SEM). The remaining samples were divided into 4 groups of 10 specimens each based on the surface treatment received: One group was acid etched and other was nonetched. Composite resin cylinders were bonded on prepared surfaces and shear bond strength was assessed using a universal testing machine. The SEM observation revealed that the laser prepared surfaces were clean, highly irregular and devoid of a smear layer. Bur prepared surfaces were relatively smooth but covered with smear layer. Highest bond strength was shown by laser prepared acid etched group, followed by bur prepared the acid etched group. The bur prepared nonacid etched group showed least bond strength. Er, Cr: YSGG laser can be used for preparing tooth and bond strength value achieved by laser preparation alone without surface treatment procedure lies in the range of clinical acceptability.

Cytotoxicity of Etch-and-Rinse, Self-Etch, and Universal Dental Adhesive Systems in Fibroblast Cell Line 3T3

PubMed Central

Bernardo, Cintia Fernanda de Freitas; de Souza, Francielly Fernanda de Freitas A.; Michél, Milton Domingos; Ribeiro, Camila Nunes de Morais; Germano, Sandro; Maluf, Daniela Florencio

2017-01-01

The aim of this study was to evaluate in fibroblast cultures the direct cytotoxic effects of etch-and-rinse, self-etch, and universal adhesive systems. The sterile glass cover slips (n = 3) were then immersed in culture medium to obtain the eluates for the experimental groups: (1) Adper™ Single Bond 2; (2) Ambar; (3) Adper™ Scotchbond™ Multi-Purpose; (4) Scotchbond™ Universal; (5) Ambar Universal; and (6) OptiBond All-In-One. As a negative control, sterile glass cover slips were immersed in culture medium only. After 24 h, the eluate obtained was applied on fibroblast culture. Cell viability and cell morphology were evaluated by MTT assay and SEM, respectively. Data were analyzed by Kruskal–Wallis and Mann–Whitney tests (α = 0.05). All adhesive systems except universal reduced cell viability in 3T3 cells to between 26.04% and 56.57%, and Scotchbond Universal and Ambar Universal reduced cell viability to 2.13% and 3.57%, respectively, when compared to the negative control. Cytoplasmic membrane shrinkage and cell-free areas with residual membrane fragments from dead cells were observed. In conclusion, improvements in universal adhesive system formulations and their mechanisms of action are not accompanied by increased toxicity compared with those in other systems, warranting commitment to the use of these dentin-pulp complexes. PMID:29109829

Self-cleaning and antibiofouling enamel surface by slippery liquid-infused technique

NASA Astrophysics Data System (ADS)

Yin, Jiali; Mei, May Lei; Li, Quanli; Xia, Rong; Zhang, Zhihong; Chu, Chun Hung

2016-05-01

We aimed to create a slippery liquid-infused enamel surface with antibiofouling property to prevent dental biofilm/plaque formation. First, a micro/nanoporous enamel surface was obtained by 37% phosphoric acid etching. The surface was then functionalized by hydrophobic low-surface energy heptadecafluoro-1,1,2,2-tetra- hydrodecyltrichlorosilane. Subsequent infusion of fluorocarbon lubricants (Fluorinert FC-70) into the polyfluoroalkyl-silanized rough surface resulted in an enamel surface with slippery liquid-infused porous surface (SLIPS). The results of water contact angle measurement, diffuse-reflectance Fourier transform infrared spectroscopy, and atomic force microscope confirmed that the SLIPS was successfully constructed on the enamel surface. The antibiofouling property of the SLIPS was evaluated by the adsorption of salivary protein of mucin and Streptococcus mutans in vitro, as well as dental biofilm formation using a rabbit model in vivo. The results showed that the SLIPS on the enamel surface significantly inhibited mucin adhesion and S. mutans biofilm formation in vitro, and inhibited dental plaque formation in vivo.

Evaluation of dental adhesive systems incorporating an antibacterial monomer eugenyl methacrylate (EgMA) for endodontic restorations.

PubMed

Almaroof, A; Niazi, S A; Rojo, L; Mannocci, F; Deb, S

2017-05-01

The purpose of this study was to incorporate EgMA, an antibacterial monomer into two commercial dental adhesive systems for their application in endodontic restoration with the aim to disinfect the root canal space before curing and to inhibit bacterial growth on their surfaces after being cured. EgMA monomer was added at 20%wt. into the formulation of the single-component self-etch, Clearfil Universal Bond™ (CUB) and into the catalyst and the adhesive components of the total-etch Adper Scotchbond-multipurpose™ (SBMP) adhesive systems. The degree of conversion (DC) was calculated from FTIR spectra, glass transition temperature (Tg) determined by DSC, water sorption and solubility were measured gravimetrically, and surface free energy (SFE) via contact angle measurements. The bonding performance to coronal and middle root canal dentin was assessed through push-out bond strength after filling the canals with a composite core material and the surface integrity was observed using SEM and confocal laser scanning microscopy (CLSM). The standard agar diffusion test (ADT) was used to identify the sensitivity of three endodontically pathogenic bacteria, Enterococcus faecalis, Streptococcus mutans and Propionibacterium acnes to uncured EgMA modified adhesives. Multispecies biofilm model from these strains was grown on the disc surface of cured adhesives and investigated using quantitative microbial culture and CLSM with live/dead staining. MTT assay was also used to determine the cytotoxicity of these adhesives. The incorporation of EgMA lowered polymerization exotherm and enhanced the hydrophobic character of these adhesives, without changing the DC and Tg in comparison to the controls (without EgMA). The total push-out bond strengths of the EgMA-containing adhesives were not significantly different from those of the controls (p>0.05). The modification of self-etch adhesive system enhanced the bond strength in the middle region of the roots canal. SEM of debonded specimens and CLSM examination showed the integrity of the resin-dentin interfaces. For all three bacteria tested, the sizes of the inhibition zones produced by uncured EgMA modified adhesives were significantly greater (p<0.05) than those of the controls. The results of biofilm inhibition tests showed less CFU for total bacteria on bonding agents with EgMA compared to the control materials (p<0.05). The modification at 20% monomer concentration had no adverse effects on cytocompatibility of both adhesives tested. The inclusion of EgMA endows dental adhesives with effective antibacterial effects without influencing their curing properties, bonding ability to root canal dentin, and cytotoxicity against human gingival fibroblasts, indicating the usefulness of their application in endodontic restorations. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

The importance of size-exclusion characteristics of type I collagen in bonding to dentin matrices

PubMed Central

M, Takahashi; M, Nakajima; J, Tagami; DLS, Scheffel; RM, Carvalho; A, Mazzoni; M, Carrilho; A, Tezvergil-Mutluay; L, Breschi; L, Tjäderhane; SS, Jang; FR, Tay; KA, Agee; DH, Pashley

2013-01-01

The mineral phase of dentin is located primarily within collagen fibrils. During development, bone or dentin collagen fibrils are formed first and then water within the fibril is replaced with apatite crystallites. Mineralized collagen contains very little water. During dentin bonding, acid-etching of mineralized dentin solubilizes the mineral crystallites and replaces them with water. During the infiltration phase of dentin bonding, adhesive comonomers are supposed to replace all of the collagen water with adhesive monomers that are then polymerized into copolymers. The authors of a recently published review suggested that dental monomers were too large to enter and displace water from collagen fibrils. If that were true, the endogenous proteases bound to dentin collagen could be responsible for unimpeded collagen degradation that is responsible for the poor durability of resin-dentin bonds. The current work studied the size-exclusion characteristics of dentin collagen, using a gel-filtration-like column chromatography technique, using dentin powder instead of Sephadex. The elution volumes of test molecules, including adhesive monomers, revealed that adhesive monomers smaller than about 1000 Da can freely diffuse into collagen water, while molecules of 10,000 Da begin to be excluded, and bovine serum albumin (66,000 Da) was fully excluded. These results validate the concept that dental monomers can permeate between collagen molecules during infiltration by etch-and-rinse adhesives. PMID:23928333

Stereo imaging and cytocompatibility of a model dental implant surface formed by direct laser fabrication.

PubMed

Mangano, Carlo; Raspanti, Mario; Traini, Tonino; Piattelli, Adriano; Sammons, Rachel

2009-03-01

Direct laser fabrication (DLF) allows solids with complex geometry to be produced by sintering metal powder particles in a focused laser beam. In this study, 10 Ti6Al4V alloy model dental root implants were obtained by DLF, and surface characterization was carried out using stereo scanning electron microscopy to produce 3D reconstructions. The surfaces were extremely irregular, with approximately 100 microm deep, narrow intercommunicating crevices, shallow depressions and deep, rounded pits of widely variable shape and size, showing ample scope for interlocking with the host bone. Roughness parameters were as follows: R(t), 360.8 microm; R(z), 358.4 microm; R(a), 67.4 microm; and R(q), 78.0 microm. Disc specimens produced by DLF with an identically prepared surface were used for biocompatibility studies with rat calvarial osteoblasts: After 9 days, cells had attached and spread on the DLF surface, spanning across the crevices, and voids. Cell density was similar to that on a commercial rough microtextured surface but lower than on commercial smooth machined and smooth-textured grit-blasted, acid-etched surfaces. Human fibrin clot extension on the DLF surface was slightly improved by inorganic acid etching to increase the microroughness. With further refinements, DLF could be an economical means of manufacturing implants from titanium alloys. (c) 2008 Wiley Periodicals, Inc.

Influence of pH, bleaching agents, and acid etching on surface wear of bovine enamel

PubMed Central

Soares, Ana Flávia; Bombonatti, Juliana Fraga Soares; Alencar, Marina Studart; Consolmagno, Elaine Cristina; Honório, Heitor Marques; Mondelli, Rafael Francisco Lia

2016-01-01

ABSTRACT Development of new materials for tooth bleaching justifies the need for studies to evaluate the changes in the enamel surface caused by different bleaching protocols. Objective The aim of this study was to evaluate the bovine dental enamel wear in function of different bleaching gel protocols, acid etching and pH variation. Material and Methods Sixty fragments of bovine teeth were cut, obtaining a control and test areas. In the test area, one half received etching followed by a bleaching gel application, and the other half, only the bleaching gel. The fragments were randomly divided into six groups (n=10), each one received one bleaching session with five hydrogen peroxide gel applications of 8 min, activated with hybrid light, diode laser/blue LED (HL) or diode laser/violet LED (VHL) (experimental): Control (C); 35% Total Blanc Office (TBO35HL); 35% Lase Peroxide Sensy (LPS35HL); 25% Lase Peroxide Sensy II (LPS25HL); 15% Lase Peroxide Lite (LPL15HL); and 10% hydrogen peroxide (experimental) (EXP10VHL). pH values were determined by a pHmeter at the initial and final time periods. Specimens were stored, subjected to simulated brushing cycles, and the superficial wear was determined (μm). ANOVA and Tukey´s tests were applied (α=0.05). Results The pH showed a slight decrease, except for Group LPL15HL. Group LPS25HL showed the highest degree of wear, with and without etching. Conclusion There was a decrease from the initial to the final pH. Different bleaching gels were able to increase the surface wear values after simulated brushing. Acid etching before bleaching increased surface wear values in all groups. PMID:27008254

Influence of pH, bleaching agents, and acid etching on surface wear of bovine enamel.

PubMed

Soares, Ana Flávia; Bombonatti, Juliana Fraga Soares; Alencar, Marina Studart; Consolmagno, Elaine Cristina; Honório, Heitor Marques; Mondelli, Rafael Francisco Lia

2016-01-01

Development of new materials for tooth bleaching justifies the need for studies to evaluate the changes in the enamel surface caused by different bleaching protocols. The aim of this study was to evaluate the bovine dental enamel wear in function of different bleaching gel protocols, acid etching and pH variation. Sixty fragments of bovine teeth were cut, obtaining a control and test areas. In the test area, one half received etching followed by a bleaching gel application, and the other half, only the bleaching gel. The fragments were randomly divided into six groups (n=10), each one received one bleaching session with five hydrogen peroxide gel applications of 8 min, activated with hybrid light, diode laser/blue LED (HL) or diode laser/violet LED (VHL) (experimental): Control (C); 35% Total Blanc Office (TBO35HL); 35% Lase Peroxide Sensy (LPS35HL); 25% Lase Peroxide Sensy II (LPS25HL); 15% Lase Peroxide Lite (LPL15HL); and 10% hydrogen peroxide (experimental) (EXP10VHL). pH values were determined by a pHmeter at the initial and final time periods. Specimens were stored, subjected to simulated brushing cycles, and the superficial wear was determined (μm). ANOVA and Tukey´s tests were applied (α=0.05). The pH showed a slight decrease, except for Group LPL15HL. Group LPS25HL showed the highest degree of wear, with and without etching. There was a decrease from the initial to the final pH. Different bleaching gels were able to increase the surface wear values after simulated brushing. Acid etching before bleaching increased surface wear values in all groups.

Smear layer-deproteinizing improves bonding of one-step self-etch adhesives to dentin.

PubMed

Thanatvarakorn, Ornnicha; Prasansuttiporn, Taweesak; Thittaweerat, Suppason; Foxton, Richard M; Ichinose, Shizuko; Tagami, Junji; Hosaka, Keiichi; Nakajima, Masatoshi

2018-03-01

Smear layer deproteinizing was proved to reduce the organic phase of smear layer covered on dentin surface. It was shown to eliminate hybridized smear layer and nanoleakage expression in resin-dentin bonding interface of two-step self-etch adhesive. This study aimed to investigate those effects on various one-step self-etch adhesives. Four different one-step self-etch adhesives were used in this study; SE One (SE), Scotchbond™ Universal (SU), BeautiBond Multi (BB), and Bond Force (BF). Flat human dentin surfaces with standardized smear layer were prepared. Smear layer deproteinizing was carried out by the application of 50ppm hypochlorous acid (HOCl) on dentin surface for 15s followed by Accel ® (p-toluenesulfinic acid salt) for 5s prior to adhesive application. No surface pretreatment was used as control. Microtensile bond strength (μTBS) and nanoleakage under TEM observation were investigated. The data were analyzed by two-way ANOVA and Tukey's post-hoc test and t-test at the significant level of 0.05. Smear layer deproteinizing significantly improved μTBS of SE, SU, and BB (p<0.001). Hybridized smear layer observed in control groups of SE, BB, and BF, and reticular nanoleakage presented throughout the hybridized complex in control groups of BB and BF were eliminated upon the smear layer deproteinizing. Smear layer deproteinizing by HOCl and Accel ® application could enhance the quality of dentin for bonding to one-step self-etch adhesives, resulting in the improving μTBS, eliminating hybridized smear layer and preventing reticular nanoleakage formation in resin-dentin bonding interface. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

A new universal simplified adhesive: 6-month clinical evaluation.

PubMed

Mena-Serrano, Alexandra; Kose, Carlos; De Paula, Eloisa Andrade; Tay, Lidia Yileng; Reis, Alessandra; Loguercio, Alessandro D; Perdigão, Jorge

2013-02-01

Multimode adhesives, which can be used as etch-and-rinse or as self-etch adhesives, have been recently introduced without clinical data to back their use. To evaluate the 6-month clinical performance of Scotchbond Universal Adhesive (SU; 3M ESPE, St. Paul, MN, USA) in noncarious cervical lesions (NCCLs) using two evaluation criteria. Thirty-nine patients participated in this study. Two hundred restorations were assigned to four groups: SU-TEm: etch-and-rinse + moist dentin; SU-TEd: etch-and-rinse + dry dentin; SU-SEet: selective enamel etching; and SU-SE: self-etch. The composite resin Filtek Supreme Ultra (3M ESPE) was placed incrementally. The restorations were evaluated at baseline and after 6 months using both the World Dental Federation (FDI) and the United States Public Health Service (USPHS) criteria. Statistical analyses were performed with Friedman repeated measures analysis of variance by rank and McNemar test for significance in each pair (α = 0.05). Only four restorations (SU-SE: 3 and SU-TEm: 1) were lost after 6 months (p > 0.05 for either criteria). Marginal discoloration occurred in one restoration in the SU-SE group (p > 0.05 for either criteria). Only 2/200 restorations were scored as bravo for marginal adaptation using the USPHS criteria (one for SU-SE and one for SU-SEet, p > 0.05). However, when using the FDI criteria, the percentage of bravo scores for marginal adaptation at 6 months were 32%, 36%, 42%, and 46% for groups SU-TEm, SU-TEd, SU-SEet, and SU-SE, respectively (p > 0.05). The clinical behavior of the multimode adhesive does not depend on the bonding strategy at 6 months. The FDI evaluation criteria are more sensitive than the USPHS criteria. At 6 months, the clinical behavior of the new multimode adhesive Scotchbond Universal was found to be reliable when used in noncarious cervical lesions and may not depend on the bonding strategy employed. © 2012 Wiley Periodicals, Inc.

Matrix metalloproteinase inhibitor modulates esterase-catalyzed degradation of resin-dentin interfaces.

PubMed

Serkies, Kyle B; Garcha, Reena; Tam, Laura E; De Souza, Grace M; Finer, Yoav

2016-12-01

Assess the modulating effect of matrix metalloproteinase (MMP) inhibition on simulated human salivary enzyme (SHSE)-catalyzed degradation of interfacial fracture-toughness (FT) of self-etched and total-etched resin-dentin interfaces. Miniature short-rod FT specimens (N=10/group) containing a resin composite bonded to human dentin, using a self-etch (Easy Bond, EB) or a total-etch (Scotchbond, SB) adhesives, were prepared with and without application of an MMP inhibitor (galardin). Specimens were non-incubated or incubated in phosphate buffered saline (PBS) or SHSE for 7, 30, 90, or 180-days. FT data were obtained using a universal testing machine. Incubation media were analyzed by high performance liquid chromatography (HPLC) for the presence of a 2,2-bis-[4-2(2-hydroxy-3-methacryloxypropoxy)phenyl]-propane (bisGMA)-derived degradation product, bis-hydroxy-propoxy-phenyl-propane (bisHPPP). Fractographic analysis was performed by scanning electron microscopy and image processing software (ImageJ). Statistical analysis was performed by ANOVA and Tukey's (p<0.05). More bisHPPP was detected in SHSE vs. PBS for both adhesive systems (p<0.05). EB specimens yielded no difference in FT and failed preferentially in the resin after >30-days (p<0.05). SB specimens yielded lower FT values after 180-days with SHSE ±galardin vs. 0-days/no-galardin (p<0.05) and failed preferentially in the hybrid-layer after >30-days (p<0.05). Galardin mildly modulated the change in fracture mode for both systems. Esterase-catalyzed degradation of total-etch interfaces is modulated by MMP-inhibition, however, self-etch interfaces possess greater biostability under simulated intra-oral conditions, regardless of MMP inhibition. This could be related to different chemical compositions and/or mode of adhesion. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Association of dental enamel lead levels with risk factors for environmental exposure.

PubMed

Olympio, Kelly Polido Kaneshiro; Naozuka, Juliana; Oliveira, Pedro Vitoriano; Cardoso, Maria Regina Alves; Bechara, Etelvino José Henriques; Günther, Wanda Maria Risso

2010-10-01

To analyze household risk factors associated with high lead levels in surface dental enamel. A cross-sectional study was conducted with 160 Brazilian adolescents aged 1418 years living in poor neighborhoods in the city of Bauru, southeastern Brazil, from August to December 2008. Body lead concentrations were assessed in surface dental enamel acid-etch microbiopsies. Dental enamel lead levels were measured by graphite furnace atomic absorption spectrometry and phosphorus levels were measured by inductively coupled plasma optical emission spectrometry. The parents answered a questionnaire about their children's potential early (05 years old) exposure to well-known lead sources. Logistic regression was used to identify associations between dental enamel lead levels and each environmental risk factor studied. Social and familial covariables were included in the models. The results suggest that the adolescents studied were exposed to lead sources during their first years of life. Risk factors associated with high dental enamel lead levels were living in or close to a contaminated area (OR = 4.49; 95% CI: 1.69;11.97); and member of the household worked in the manufacturing of paints, paint pigments, ceramics or batteries (OR = 3.43; 95% CI: 1.31;9.00). Home-based use of lead-glazed ceramics, low-quality pirated toys, anticorrosive paint on gates and/or sale of used car batteries (OR = 1.31; 95% CI: 0.56;3.03) and smoking (OR = 1.66; 95% CI: 0.52;5.28) were not found to be associated with high dental enamel lead levels. Surface dental enamel can be used as a marker of past environmental exposure to lead and lead concentrations detected are associated to well-known sources of lead contamination.

Evaluation of microshear bond strength of resin composites to enamel of dental adhesive systems associated with Er,Cr:YSGG laser

NASA Astrophysics Data System (ADS)

Cassimiro-Silva, Patricia F.; Zezell, Denise M.; Monteiro, Gabriela Q. d. M.; Benetti, Carolina; de Paula Eduardo, Carlos; Gomes, Anderson S. L.

2016-02-01

The aim of this in vitro study was to evaluate the microshear bond strength (μSBS) of resin composite to enamel etching by Er,Cr:YSGG laser with the use of two differents adhesives systems. Fifty freshly extracted human molars halves were embedded in acrylic resin before preparation for the study, making a total of up to 100 available samples. The specimens were randomly assigned into six groups (η=10) according to substrate pre-treatment and adhesive system on the enamel. A two-step self-etching primer system (Clearfil SE Bond) and a universal adhesive used as an etch-andrinse adhesive (Adper Single Bond Universal) were applied to the nonirradiated enamel surface according to manufacturer's instructions, as control groups (Control CF and Control SB, respectively). For the other groups, enamel surfaces were previously irradiated with the Er,Cr:YSGG laser with 0.5 W, 75 mJ and 66 J/cm2 (CF 5 Hz and SB 5 Hz) and 1.25 W, 50 mJ and 44 J/cm2 (CF 15 Hz and SB 15 Hz). Irradiation was performed under air (50%) and water (50%) cooling. An independent t-test was performed to compare the adhesive systems. Mean μSBS ± sd (MPa) for each group was 16.857 +/- 2.61, 17.87 +/- 5.83, 12.23 +/- 2.02, 9.88 +/- 2.26, 15.94 +/- 1.98, 17.62 +/- 2.10, respectively. The control groups and the 50 mJ laser groups showed no statistically significant differences, regardless of the adhesive system used. The results obtained lead us to affirm that the bonding interaction of adhesives to enamel depends not only on the morphological aspects of the dental surface, but also on the characteristics of the adhesive employed and the parameters of the laser.

Morphological effects of MMPs inhibitors on the dentin bonding

PubMed Central

Li, He; Li, Tianbo; Li, Xiuying; Zhang, Zhimin; Li, Penglian; Li, Zhenling

2015-01-01

Matrix metalloproteinases (MMPs) have been studied extensively, and MMP inhibitors have been used as dental pretreatment agents prior to dentin bonding because they reduce collagen fiber degradation and improve bonding strength. However, morphologic characteristics of the collagen network after etching and of the post-adhesive dentin hybrid layers (DHL) after MMP inhibitors pretreatment have not been evaluated. Thus, we investigated demineralized dentin pretreated with chlorhexidine (CHX) and minocycline (MI) in an etch- and -rinse adhesive system with field emission scanning electron microscopy (FESEM) and immuno-gold labeling markers to observe the collagen network and DHL. FESEM revealed after CHX and MI, a demineralized dentin surface and improved collagen network formation, reduced collagen degradation, and distinct gold-labeling signals. Applying adhesive after either MMP inhibitor created a better dentin interface as evidenced by immuno-gold staining, better adhesive penetration, and higher DHL quality. With microtensile bond strength tests (µTBS) we estimated bonding strength using µTBS data. Immediate µTBS was enhanced with MMP inhibitor application to the bonding surface, and the CHX group was significantly different than non-treated etched surfaces, but no significant change was detected in the MI group. Surface micromorphology of the fractured dentin resin restoration showed that the CHX group had a better resin and dentin tube combination. Both MMP inhibitors created uniform resin coverage. Thus, morphologic results and µTBS data suggest that CHX and MI can inhibit MMP activity, improve immediate bonding strength, and enhance dentin bonding stability with an etch- and -rinse adhesive system. PMID:26379873

Abstracts of Research Project Reports by National Naval Dental Center First-, Second-, and Third-Year Residents - June 1980.

DTIC Science & Technology

1980-08-30

resin ( Silar ). Extracted teeth were thermocycled at 60 and 450 C and incu- bated in a strong solution of tea. In a double-blind study, three dentists...Concise, the other with Silar . Each tooth had a control preparation and an experimental preparation. Both preparations were filled according to the...significantly I.ss than Silar . Although the initial resuits indicate that stannous fluoride applied to acid-etched enamel does not increase the

High-speed scanning ablation of dental hard tissues with a λ=9.3-μm CO2 laser: heat accumulation and peripheral thermal damage

NASA Astrophysics Data System (ADS)

Nguyen, Daniel; Staninec, Michal; Lee, Chulsung; Fried, Daniel

2010-02-01

A mechanically scanned CO2 laser operated at high laser pulse repetition rates can be used to rapidly and precisely remove dental decay. This study aims to determine whether these laser systems can safely ablate enamel and dentin without excessive heat accumulation and peripheral thermal damage. Peripheral thermal damage can adversely impact the mechanical strength of the irradiated tissue, particularly for dentin, and reduce the adhesion characteristics of the modified surfaces. Samples were derived from noncarious extracted molars. Pulpal temperatures were recorded using microthermocouples situated at the pulp chamber roof of samples (n=12), which were occlusally ablated using a rapid-scanning, water-cooled 300 Hz CO2 laser over a two minute time course. The mechanical strength of facially ablated dentin (n=10) was determined via four-point bend test and compared to control samples (n=10) prepared with 320 grit wet sand paper to simulate conventional preparations. Composite-to-enamel bond strength was measured via single-plane shear test for ablated/non-etched (n=10) and ablated/acid-etched (n=8) samples and compared to control samples (n=9) prepared by 320 grit wet sanding. Thermocouple measurements indicated that the temperature remained below ambient temperature at 19.0°C (s.d.=0.9) if water-cooling was used. There was no discoloration of either dentin and enamel, the treated surfaces were uniformly ablated and there were no cracks observable on the laser treated surfaces. Fourpoint bend tests yielded mean mechanical strengths of 18.2 N (s.d.=4.6) for ablated dentin and 18.1 N (s.d.=2.7) for control (p>0.05). Shear tests yielded mean bond strengths of 31.2 MPa (s.d.=2.5, p<0.01) for ablated/acid-etched samples, 5.2 MPa (s.d.=2.4, p<0.001) for ablated/non-etched samples, and 37.0 MPa (s.d.=3.6) for control. The results indicate that a rapid-scanning 300 Hz CO2 laser can effectively ablate dentin and enamel without excessive heat accumulation and with minimal thermal damage. It is not clear whether the small (16%) but statistically significant reduction in the shear bond strength to enamel is clinically significant since the mean shear bond strength exceeded 30 MPa.

The management of defective resin composite restorations: current trends in dental school teaching in Japan.

PubMed

Lynch, C D; Hayashi, M; Seow, L L; Blum, I R; Wilson, N H F

2013-01-01

The aim of this article is to investigate the contemporary teaching of the management of defective direct resin composite restorations in dental schools in Japan. A questionnaire relating to the teaching of the management of defective resin composite restorations was developed and e-mailed to 29 dental schools in Japan in 2010. Completed responses were received from 19 of the 29 invited schools (response rate = 66%). Eighteen schools (95%) report that they included the teaching of repair of direct defective resin composite restorations in their dental school programs. Thirteen schools reported that they included both clinical and didactic instruction on the repair of direct resin composite restorations. Fourteen schools did not teach any mechanical roughening of the exposed resin composite restoration surface before undertaking a repair. The most commonly reported treatment was acid etching with phosphoric acid (12 schools). The most commonly taught material for completing repairs was a flowable resin composite (16 schools). The teaching of repair of defective resin composite restorations is well established within many Japanese dental schools, to a greater extent than in some other regions of the world. The impact of this teaching on subsequent clinical practices in Japan should be investigated. Furthermore, it is concluded that there is a need for much stronger leadership in operative and conservative dentistry, ideally at the global level, to resolve differences in key aspects of operative procedures such as repairs.

SEM analysis of enamel surface treated by Er:YAG laser: influence of irradiation distance.

PubMed

Souza-Gabriel, A E; Chinelatti, M A; Borsatto, M C; Pécora, J D; Palma-Dibb, R G; Corona, S A M

2008-07-01

Depending on the distance of laser tip to dental surface a specific morphological pattern should be expected. However, there have been limited reports that correlate the Er:YAG irradiation distance with dental morphology. To assess the influence of Er:YAG laser irradiation distance on enamel morphology, by means of scanning electron microscopy (SEM). Sixty human third molars were employed to obtain discs (approximately =1 mm thick) that were randomly assigned to six groups (n=10). Five groups received Er:YAG laser irradiation (80 mJ/2 Hz) for 20 s, according to the irradiation distance: 11, 12, 14, 16, or 17 mm and the control group was treated with 37% phosphoric acid for 15 s. The laser-irradiated discs were bisected. One hemi-disc was separated for superficial analysis without subsequent acid etching, and the other one, received the phosphoric acid for 15 s. Samples were prepared for SEM. Laser irradiation at 11 and 12 mm provided an evident ablation of enamel, with evident fissures and some fused areas. At 14, 16 and 17 mm the superficial topography was flatter than in the other distances. The subsequent acid etching on the lased-surface partially removed the disorganized tissue. Er:YAG laser in defocused mode promoted slight morphological alterations and seems more suitable for enamel conditioning than focused irradiation. The application of phosphoric acid on lased-enamel surface, regardless of the irradiation distance, decreased the superficial irregularities.

Polydopamine-induced tooth remineralization.

PubMed

Zhou, Yun-Zhi; Cao, Ying; Liu, Wei; Chu, Chun Hung; Li, Quan-Li

2012-12-01

Inspired by mussel bioadhesion in nature, dopamine is extensively used for biomaterial surface modification. In this study, we coated dopamine on demineralized enamel and dentin surfaces to evaluate the effect of polydopamine coating on dental remineralization. Dental slices containing enamel and dentin were first etched with 37% phosphoric acid for 2 min, followed by immersion in a 2 mg/mL freshly prepared solution of dopamine (10 mM Tris buffer, pH 8.5) for approximately 24 h at room temperature in the dark to obtain polydopamine coating. Then, the dental slices with and without polydopamine coating were immersed in the supersaturated solution of calcium and phosphate at 37 °C for 2 and 7 days. The supersaturated solution of calcium and phosphate was refreshed each day. The precipitates were characterized by SEM, XRD, FTIR, microhardness, and nanoscratch analyses. No significant difference was observed in the remineralization of enamel whether it was coated with polydopamine or not. However, a significant difference was found in dentin remineralization between dentin with and without polydopamine coating. Polydopamine coating remarkably promoted demineralized dentin remineralization, and all dentin tubules were occluded by densely packed hydroxyapatite crystals. Thus, coating polydopamine on dental tissue surface may be a simple universal technique to induce enamel and dentin remineralization simultaneously.

Scaling of titanium implants entrains inflammation-induced osteolysis

PubMed Central

Eger, Michal; Sterer, Nir; Liron, Tamar; Kohavi, David; Gabet, Yankel

2017-01-01

With millions of new dental and orthopedic implants inserted annually, periprosthetic osteolysis becomes a major concern. In dentistry, peri-implantitis management includes cleaning using ultrasonic scaling. We examined whether ultrasonic scaling releases titanium particles and induces inflammation and osteolysis. Titanium discs with machined, sandblasted/acid-etched and sandblasted surfaces were subjected to ultrasonic scaling and we physically and chemically characterized the released particles. These particles induced a severe inflammatory response in macrophages and stimulated osteoclastogenesis. The number of released particles and their chemical composition and nanotopography had a significant effect on the inflammatory response. Sandblasted surfaces released the highest number of particles with the greatest nanoroughness properties. Particles from sandblasted/acid-etched discs induced a milder inflammatory response than those from sandblasted discs but a stronger inflammatory response than those from machined discs. Titanium particles were then embedded in fibrin membranes placed on mouse calvariae for 5 weeks. Using micro-CT, we observed that particles from sandblasted discs induced more osteolysis than those from sandblasted/acid-etched discs. In summary, ultrasonic scaling of titanium implants releases particles in a surface type-dependent manner and may aggravate peri-implantitis. Future studies should assess whether surface roughening affects the extent of released wear particles and aseptic loosening of orthopedic implants. PMID:28059080

Nanoporous hydroxyapatite/sodium titanate bilayer on titanium implants for improved osteointegration.

PubMed

Carradò, A; Perrin-Schmitt, F; Le, Q V; Giraudel, M; Fischer, C; Koenig, G; Jacomine, L; Behr, L; Chalom, A; Fiette, L; Morlet, A; Pourroy, G

2017-03-01

The aim of this study was to improve the strength and quality of the titanium-hydroxyapatite interface in order to prevent long-term failure of the implanted devices originating from coating delamination and to test it in an in-vivo model. Ti disks and dental commercial implants were etched in Kroll solution. Thermochemical treatments of the acid-etched titanium were combined with sol-gel hydroxyapatite (HA) coating processes to obtain a nanoporous hydroxyapatite/sodium titanate bilayer. The sodium titanate layer was created by incorporating sodium ions onto the Ti surface during a NaOH alkaline treatment and stabilized using a heat treatment. HA layer was added by dip-coating in a sol-gel solution. The bioactivity was assessed in vitro with murine MC3T3-E1 and human SaOs-2 cells. Functional and histopathological evaluations of the coated Ti implants were performed at 22, 34 and 60days of implantation in a dog lower mandible model. Nanoporous hydroxyapatite/sodium titanate bilayer on titanium implants was sensitive neither to crack propagation nor to layer delamination. The in vitro results on murine MC3T3-E1 and human SaOs-2 cells confirm the advantage of this coating regarding the capacity of cell growth and differentiation. Signs of progressive bone incorporation, such as cancellous bone formed in contact with the implant over the existing compact bone, were notable as early as day 22. Overall, osteoconduction and osteointegration mean scores were higher for test implants compared to the controls at 22 and 34 days. Nanoporous hydroxyapatite/sodium titanate bilayer improves the in-vivo osteoconduction and osteointegration. It prevents the delamination during the screwing and it could increase HA-coated dental implant stability without adhesive failures. The combination of thermochemical treatments with dip coating is a low-cost strategy. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Polymer Nanocarriers for Dentin Adhesion

PubMed Central

Osorio, R.; Osorio, E.; Medina-Castillo, A.L.; Toledano, M.

2014-01-01

To obtain more durable adhesion to dentin, and to protect collagen fibrils of the dentin matrix from degradation, calcium- and phosphate-releasing particles have been incorporated into the dental adhesive procedure. The aim of the present study was to incorporate zinc-loaded polymeric nanocarriers into a dental adhesive system to facilitate inhibition of matrix metalloproteinases (MMPs)-mediated collagen degradation and to provide calcium ions for mineral deposition within the resin-dentin bonded interface. PolymP-nActive nanoparticles (nanoMyP) were zinc-loaded through 30-minute ZnCl2 immersion and tested for bioactivity by means of 7 days’ immersion in simulated body fluid solution (the Kokubo test). Zinc-loading and calcium phosphate depositions were examined by scanning and transmission electron microscopy, elemental analysis, and x-ray diffraction. Nanoparticles in ethanol solution infiltrated into phosphoric-acid-etched human dentin and Single Bond (3M/ESPE) were applied to determine whether the nanoparticles interfered with bonding. Debonded sticks were analyzed by scanning electron microscopy. A metalloproteinase collagen degradation assay was also performed in resin-infiltrated dentin with and without nanoparticles, measuring C-terminal telopeptide of type I collagen (ICTP) concentration in supernatants, after 4 wk of immersion in artificial saliva. Numerical data were analyzed by analysis of variance (ANOVA) and Student-Newman-Keuls multiple comparisons tests (p < .05). Nanoparticles were effectively zinc-loaded and were shown to have a chelating effect, retaining calcium regardless of zinc incorporation. Nanoparticles failed to infiltrate demineralized intertubular dentin and remained on top of the hybrid layer, without altering bond strength. Calcium and phosphorus were found covering nanoparticles at the hybrid layer, after 24 h. Nanoparticle application in etched dentin also reduced MMP-mediated collagen degradation. Tested nanoparticles may be incorporated into dental adhesive systems to provide the appropriate environment in which dentin MMP collagen degradation is inhibited and mineral growth can occur. PMID:25227634

Optimization of the etch-and-rinse technique: New perspectives to improve resin-dentin bonding and hybrid layer integrity by reducing residual water using dimethyl sulfoxide pretreatments.

PubMed

Stape, Thiago Henrique Scarabello; Tjäderhane, Leo; Abuna, Gabriel; Sinhoreti, Mário Alexandre Coelho; Martins, Luís Roberto Marcondes; Tezvergil-Mutluay, Arzu

2018-04-13

To determine whether bonding effectiveness and hybrid layer integrity on acid-etched dehydrated dentin would be comparable to the conventional wet-bonding technique through new dentin biomodification approaches using dimethyl sulfoxide (DMSO). Etched dentin surfaces from extracted sound molars were randomly bonded in wet or dry conditions (30s air drying) with DMSO/ethanol or DMSO/H 2 O as pretreatments using a simplified (Scotchbond Universal Adhesive, 3M ESPE: SU) and a multi-step (Adper Scotchbond Multi-Purpose, 3M ESPE: SBMP) etch-and-rinse adhesives. Untreated dentin surfaces served as control. Bonded teeth (n=8) were stored in distilled water for 24h and sectioned into resin-dentin beams (0.8mm 2 ) for microtensile bond strength test and quantitative interfacial nanoleakage analysis (n=8) under SEM. Additional teeth (n=2) were prepared for micropermeability assessment by CFLSM under simulated pulpar pressure (20cm H 2 O) using 5mM fluorescein as a tracer. Microtensile data was analyzed by 3-way ANOVA followed by Tukey Test and nanoleakage by Kruskal-Wallis and Dunn-Bonferroni multiple comparison test (α=0.05). While dry-bonding of SBMP produced significantly lower bond strengths than wet-bonding (p<0.05), DMSO/H 2 O and DMSO/ethanol produced significantly higher bond strengths for SBMP irrespective of dentin condition (p<0.05). SU presented significantly higher nanoleakage levels (p<0.05) and micropermeability than SBMP. Improvement in hybrid layer integrity occurred for SBMP and SU for both pretreatments, albeit most pronouncedly for DMSO/ethanol regardless of dentin moisture. DMSO pretreatments may be used as a new suitable strategy to improve bonding of water-based adhesives to demineralized air-dried dentin beyond conventional wet-bonding. Less porous resin-dentin interfaces with higher bond strengths on air-dried etched dentin were achieved; nonetheless, overall efficiency varied according to DMSO's co-solvent and adhesive type. DMSO pretreatments permit etched dentin to be air-dried before hybridization facilitating residual water removal and thus improving bonding effectiveness. This challenges the current paradigm of wet-bonding requirement for the etch-and-rinse approach creating new possibilities to enhance the clinical longevity of resin-dentin interfaces. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

Influence of Nd:YAG laser on the bond strength of self-etching and conventional adhesive systems to dental hard tissues.

PubMed

Marimoto, A K; Cunha, L A; Yui, K C K; Huhtala, M F R L; Barcellos, D C; Prakki, A; Gonçalves, S E P

2013-01-01

The aim of this study was to investigate the influence of Nd:YAG laser on the shear bond strength to enamel and dentin of total and self-etch adhesives when the laser was applied over the adhesives, before they were photopolymerized, in an attempt to create a new bonding layer by dentin-adhesive melting. One-hundred twenty bovine incisors were ground to obtain flat surfaces. Specimens were divided into two substrate groups (n=60): substrate E (enamel) and substrate D (dentin). Each substrate group was subdivided into four groups (n=15), according to the surface treatment accomplished: X (Xeno III self-etching adhesive, control), XL (Xeno III + laser Nd:YAG irradiation at 140 mJ/10 Hz for 60 seconds + photopolymerization, experimental), S (acid etching + Single Bond conventional adhesive, Control), and SL (acid etching + Single Bond + laser Nd:YAG at 140 mJ/10 Hz for 60 seconds + photopolymerization, experimental). The bonding area was delimited with 3-mm-diameter adhesive tape for the bonding procedures. Cylinders of composite were fabricated on the bonding area using a Teflon matrix. The teeth were stored in water at 37°C/48 h and submitted to shear testing at a crosshead speed of 0.5 mm/min in a universal testing machine. Results were analyzed with three-way analysis of variance (ANOVA; substrate, adhesive, and treatment) and Tukey tests (α=0.05). ANOVA revealed significant differences for the substrate, adhesive system, and type of treatment: lased or unlased (p<0.05). The mean shear bond strength values (MPa) for the enamel groups were X=20.2 ± 5.61, XL=23.6 ± 4.92, S=20.8 ± 4.55, SL=22.1 ± 5.14 and for the dentin groups were X=14.1 ± 7.51, XL=22.2 ± 6.45, S=11.2 ± 5.77, SL=15.9 ± 3.61. For dentin, Xeno III self-etch adhesive showed significantly higher shear bond strength compared with Single Bond total-etch adhesive; Nd:YAG laser irradiation showed significantly higher shear bond strength compared with control (unlased). Nd:YAG laser application prior to photopolymerization of adhesive systems significantly increased the bond strength to dentin.

Influence of phosphoproteins' biomimetic analogs on remineralization of mineral-depleted resin-dentin interfaces created with ion-releasing resin-based systems.

PubMed

Sauro, Salvatore; Osorio, Raquel; Watson, Timothy F; Toledano, Manuel

2015-07-01

The study aimed at evaluating the remineralization of acid-etched dentin pre-treated with primers containing biomimetic analogs and bonded using an ion-releasing light-curable resin-based material. An experimental etch-and-rinse adhesive system filled with Ca(2+), PO4(3-)-releasing Ca-Silicate micro-fillers was created along with two experimental primers containing biomimetic analogs such as sodium trimetaphosphate (TMP) and/or polyaspartic acid (PLA). Dentin specimens etched with 37% H3PO4 were pre-treated with two different aqueous primers containing the polyanionic biomimetic analogs or deionized water and subsequently bonded using the experimental resin-based materials. The specimens were sectioned and analyzed by AFM/nanoindentation to evaluate changes in the modulus of elasticity (Ei) across the resin-dentin interface at different AS storage periods (up to 90 days). Raman cluster analysis was also performed to evaluate the chemical changes along the interface. The phosphate uptake by the acid-etched dentin was evaluated using the ATR-FTIR. Additional resin-dentin specimens were tested for microtensile bond strength. SEM examination was performed after de-bonding, while confocal laser microscopy was used to evaluate the interfaces ultramorphology and micropermeability. Both biomimetic primers induced phosphate uptake by acid-etched dentin. Specimens created with the ion-releasing resin in combination with the pre-treatment primers containing either PLA and TMA showed the greatest recovery of the Ei of the hybrid layer, with no decrease in μTBS (p>0.05) after 3-month AS storage. The ion-releasing resin applied after use of the biomimetic primers showed the greatest reduction in micropermeability due to mineral precipitation; these results were confirmed using SEM. The use of the ion-releasing resin-based system applied to acid-etched dentin pre-treated with biomimetic primers containing analogs of phosphoproteins such as poly-l-aspartic acid and/or sodium trimetaphosphate provides a suitable bonding approach for biomimetic remineralization of resin-dentin interfaces. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

10-year survival rate and the incidence of peri-implant disease of 374 titanium dental implants with a SLA surface: a prospective cohort study in 177 fully and partially edentulous patients.

PubMed

van Velzen, Frank J J; Ofec, Ronen; Schulten, Engelbert A J M; Ten Bruggenkate, Christiaan M

2015-10-01

This prospective cohort study evaluates the 10-year survival and incidence of peri-implant disease at implant and patient level of sandblasted, large grid, and acid-etched titanium dental implants (Straumann, soft tissue level, SLA surface) in fully and partially edentulous patients. Patients who had dental implant surgery in the period between November 1997 and June 2001, with a follow-up of at least 10 years, were investigated for clinical and radiological examination. Among the 506 inserted dental implants in 250 patients, 10-year data regarding the outcome of implants were available for 374 dental implants in 177 patients. In the current study, peri-implantitis was defined as advanced bone loss (≧1.5 mm. postloading) in combination with bleeding on probing. At 10-year follow-up, only one implant was lost (0.3%) 2 months after implant surgery due to insufficient osseointegration. The average bone loss at 10 year postloading was 0.52 mm. Advanced bone loss at 10-year follow-up was present in 35 dental implants (9.8%). Seven percent of the observed dental implants showed bleeding on probing in combination with advanced bone loss and 4.2% when setting the threshold for advanced bone loss at 2.0 mm. Advanced bone loss without bleeding on probing was present in 2.8% of all implants. In this prospective study, the 10-year survival rate at implant and patient level was 99.7% and 99.4%, respectively. Peri-implantitis was present in 7% of the observed dental implants according to the above-mentioned definition of peri-implantitis. This study shows that SLA implants offer predictable long-term results as support in the treatment of fully and partially edentulous patients. © 2014 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

PEEK surface treatment effects on tensile bond strength to veneering resins.

PubMed

Stawarczyk, Bogna; Jordan, Peter; Schmidlin, Patrick R; Roos, Malgorzata; Eichberger, Marlis; Gernet, Wolfgang; Keul, Christine

2014-11-01

Polyetheretherketone (PEEK) can be used as a framework material for fixed dental prostheses. However, information about the durable bond to veneering resins is still scarce. The purpose of this study was to investigate the effect of chemical treatments of PEEK on tensile bond strength (TBS) to veneering resins with special emphasis on surface free energy (SFE) and surface roughness (SR). Seven-hundred fifty PEEK specimens were fabricated and divided into the following 3 pretreatment groups (n=250/group): etching with sulfuric acid for 60 seconds, etching with piranha acid for 30 seconds, and an unetched control. After pretreatment, SFE was determined by using contact angle measurements and SR with a profilometer (n=10/group). The topography of pretreated PEEK surfaces was examined with scanning electron microscopy. Remaining specimens (n=240 per group) were conditioned with visio.link or Signum PEEK Bond, or were left untreated as the control group. Half of each group was veneered with Sinfony or VITA VM LC (n=40/group), and TBS was measured after storage in distilled water at 37°C for either 24 hours or 60 days. Data were analyzed by 4-way and 1-way ANOVA followed by the Scheffé post hoc test and chi-square test (α=.05). PEEK specimens etched with sulfuric acid resulted in higher SFE and SR than specimens without pretreatment or etching with piranha acid. Etching with sulfuric acid or piranha acid led to no general recommendations with respect to TBS. Conditioning with visio.link or Signum PEEK Bond significantly increased the TBS (P<.001). PEEK veneered with Sinfony showed significantly higher TBS values than those veneered with VITA VM LC (P<.001). Sufficient TBS for bonding to veneering resin can only be achieved when additional adhesive materials were applied. Copyright © 2014 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

High-speed scanning ablation of dental hard tissues with a λ = 9.3 μm CO2 laser: adhesion, mechanical strength, heat accumulation, and peripheral thermal damage

PubMed Central

Nguyen, Daniel; Chang, Kwang; Hedayatollahnajafi, Saba; Staninec, Michal; Chan, Kenneth; Lee, Robert; Fried, Daniel

2011-01-01

CO2 lasers can be operated at high laser pulse repetition rates for the rapid and precise removal of dental decay. Excessive heat accumulation and peripheral thermal damage is a concern when using high pulse repetition rates. Peripheral thermal damage can adversely impact the mechanical strength of the irradiated tissue, particularly for dentin, and reduce the adhesion characteristics of the modified surfaces. The interpulpal temperature rise was recorded using microthermocouples situated at the roof of the pulp chamber on teeth that were occlusally ablated using a rapidly-scanned CO2 laser operating at 9.3 μm with a pulse duration of 10 to 15 μs and repetition rate of 300 Hz over a 2 min time course. The adhesion strength of laser treated enamel and dentin surfaces was measured for various laser scanning parameters with and without post-ablation acid etching using the single-plane shear test. The mechanical strength of laser-ablated dentin surfaces were determined via the four-point bend test and compared to control samples prepared with 320 grit wet sand paper to simulate conventional preparations. Thermocouple measurements indicated that the temperature remained below ambient temperature if water-cooling was used. There was no discoloration of either dentin or enamel laser treated surfaces, the surfaces were uniformly ablated, and there were no cracks visible. Four-point bend tests yielded mean mechanical strengths of 18.2 N (s.d. = 4.6) for ablated dentin and 18.1 N (s.d. = 2.7) for control (p > 0.05). Shear tests yielded mean bond strengths approaching 30 MPa for both enamel and dentin under certain irradiation conditions. These values were slightly lower than nonirradiated acid-etched control samples. Additional studies are needed to determine if the slightly lower bond strength than the acid-etched control samples is clinically significant. These measurements demonstrate that enamel and dentin surfaces can be rapidly ablated by CO2 lasers with minimal peripheral thermal and mechanical damage and without excessive heat accumulation. PMID:21806256

Alteration of dentin-enamel mechanical properties due to dental whitening treatments.

PubMed

Zimmerman, B; Datko, L; Cupelli, M; Alapati, S; Dean, D; Kennedy, M

2010-05-01

The mechanical properties of dentin and enamel affect the reliability and wear properties of a tooth. This study investigated the influence of clinical dental treatments and procedures, such as whitening treatments or etching prior to restorative procedures. Both autoclaved and non-autoclaved teeth were studied in order to allow for both comparison with published values and improved clinical relevance. Nanoindentation analysis with the Oliver-Pharr model provided elastic modulus and hardness across the dentin-enamel junction (DEJ). Large increases were observed in the elastic modulus of enamel in teeth that had been autoclaved (52.0 GPa versus 113.4 GPa), while smaller increases were observed in the dentin (17.9 GPa versus 27.9 GPa). Likewise, there was an increase in the hardness of enamel (2.0 GPa versus 4.3 GPa) and dentin (0.5 GPa versus 0.7 GPa) with autoclaving. These changes suggested that the range of elastic modulus and hardness values previously reported in the literature may be partially due to the sterilization procedures. Treatment of the exterior of non-autoclaved teeth with Crest Whitestrips, Opalescence or UltraEtch caused changes in the mechanical properties of both the enamel and dentin. Those treated with Crest Whitestrips showed a reduction in the elastic modulus of enamel (55.3 GPa to 32.7 GPa) and increase in the elastic modulus of dentin (17.2 GPa to 24.3 GPa). Opalescence treatments did not significantly affect the enamel properties, but did result in a decrease in the modulus of dentin (18.5 GPa to 15.1 GPa). Additionally, as expected, UltraEtch treatment decreased the modulus and hardness of enamel (48.7 GPa to 38.0 GPa and 1.9 GPa to 1.5 GPa, respectively) and dentin (21.4 GPa to 15.0 GPa and 1.9 GPa to 1.5 GPa, respectively). Changes in the mechanical properties were linked to altered protein concentration within the tooth, as evidenced by fluorescence microscopy and Fourier transform infrared spectroscopy. Published by Elsevier Ltd.

High-speed scanning ablation of dental hard tissues with a λ = 9.3 μm CO2 laser: adhesion, mechanical strength, heat accumulation, and peripheral thermal damage

NASA Astrophysics Data System (ADS)

Nguyen, Daniel; Chang, Kwang; Hedayatollahnajafi, Saba; Staninec, Michal; Chan, Kenneth; Lee, Robert; Fried, Daniel

2011-07-01

CO2 lasers can be operated at high laser pulse repetition rates for the rapid and precise removal of dental decay. Excessive heat accumulation and peripheral thermal damage is a concern when using high pulse repetition rates. Peripheral thermal damage can adversely impact the mechanical strength of the irradiated tissue, particularly for dentin, and reduce the adhesion characteristics of the modified surfaces. The interpulpal temperature rise was recorded using microthermocouples situated at the roof of the pulp chamber on teeth that were occlusally ablated using a rapidly-scanned CO2 laser operating at 9.3 μm with a pulse duration of 10 to 15 μs and repetition rate of 300 Hz over a 2 min time course. The adhesion strength of laser treated enamel and dentin surfaces was measured for various laser scanning parameters with and without post-ablation acid etching using the single-plane shear test. The mechanical strength of laser-ablated dentin surfaces were determined via the four-point bend test and compared to control samples prepared with 320 grit wet sand paper to simulate conventional preparations. Thermocouple measurements indicated that the temperature remained below ambient temperature if water-cooling was used. There was no discoloration of either dentin or enamel laser treated surfaces, the surfaces were uniformly ablated, and there were no cracks visible. Four-point bend tests yielded mean mechanical strengths of 18.2 N (s.d. = 4.6) for ablated dentin and 18.1 N (s.d. = 2.7) for control (p > 0.05). Shear tests yielded mean bond strengths approaching 30 MPa for both enamel and dentin under certain irradiation conditions. These values were slightly lower than nonirradiated acid-etched control samples. Additional studies are needed to determine if the slightly lower bond strength than the acid-etched control samples is clinically significant. These measurements demonstrate that enamel and dentin surfaces can be rapidly ablated by CO2 lasers with minimal peripheral thermal and mechanical damage and without excessive heat accumulation.

Early healing of nanothickness bioceramic coatings on dental implants. An experimental study in dogs.

PubMed

Coelho, Paulo G; Cardaropoli, Giuseppe; Suzuki, Marcelo; Lemons, Jack E

2009-02-01

Thick bioceramic coatings like plasma sprayed hydroxyapatite have been shown to increase the overall tissue response and biomechanical fixation of dental implants. However, the presence and potential fracture of a bone-coating-metallic substrate interface at long times after implantation led these implants to fall from favor in clinical practice. The purpose of this study was to evaluate the biomechanical fixation and biological response of Ca- and P-based, 20-50 nm thickness bioceramic deposition on a previously alumina-blasted/acid-etched Ti-6Al-4V implant surface in a dog model. Cylindrical alumina-blasted/acid-etched (AB/AE) (Control, n = 16), and Nanothickness bioceramic coated AB/AE(Nano, n = 16) implant surfaces were surgically placed in dogs proximal tibia and remained for 2 and 4 weeks in vivo. Following euthanization, the implants-in-bone were mounted in epoxy and pullout at a 0.5 mm/min rate. Following mechanical testing, the specimens were decalcified and processed (Hematoxylin and Eosin) for standard transmitted light microscopy evaluation. Percent bone-to-implant contact (BIC) to the pulled out implant surface was determined through computer software. Statistical analyses were performed by one-way ANOVA at 95% level of significance and Tukey's post-hoc multiple comparisons. No significant differences in pullout force were observed (p > 0.88): 2W Control (212.08 +/- 42.96 N), 2W Nano (224.35 +/- 42.97 N), 4W Control (207.07 +/- 42.97 N), and 4W Nano (190.15 +/- 45.94 N). No significant differences in %BIC were observed (p > 0.94): 2W Control (72.66 +/- 8.51), 2W Nano (69.44 +/- 8.51), 4W Control (70.44 +/- 8.51), and 4W Nano (69.11 +/- 9.09). It is shown that 20-50 nm thickness bioceramic depositions onto previously alumina-blasted/acid-etched substrates did not improve the biomechanical fixation and the BIC at early implantation times, and studies concerning shorter and longer implantation times are recommended for confirmation or before a conclusion can be made. Copyright 2008 Wiley Periodicals, Inc.

High-speed scanning ablation of dental hard tissues with a λ = 9.3 μm CO2 laser: adhesion, mechanical strength, heat accumulation, and peripheral thermal damage.

PubMed

Nguyen, Daniel; Chang, Kwang; Hedayatollahnajafi, Saba; Staninec, Michal; Chan, Kenneth; Lee, Robert; Fried, Daniel

2011-07-01

CO(2) lasers can be operated at high laser pulse repetition rates for the rapid and precise removal of dental decay. Excessive heat accumulation and peripheral thermal damage is a concern when using high pulse repetition rates. Peripheral thermal damage can adversely impact the mechanical strength of the irradiated tissue, particularly for dentin, and reduce the adhesion characteristics of the modified surfaces. The interpulpal temperature rise was recorded using microthermocouples situated at the roof of the pulp chamber on teeth that were occlusally ablated using a rapidly-scanned CO(2) laser operating at 9.3 μm with a pulse duration of 10 to 15 μs and repetition rate of 300 Hz over a 2 min time course. The adhesion strength of laser treated enamel and dentin surfaces was measured for various laser scanning parameters with and without post-ablation acid etching using the single-plane shear test. The mechanical strength of laser-ablated dentin surfaces were determined via the four-point bend test and compared to control samples prepared with 320 grit wet sand paper to simulate conventional preparations. Thermocouple measurements indicated that the temperature remained below ambient temperature if water-cooling was used. There was no discoloration of either dentin or enamel laser treated surfaces, the surfaces were uniformly ablated, and there were no cracks visible. Four-point bend tests yielded mean mechanical strengths of 18.2 N (s.d. = 4.6) for ablated dentin and 18.1 N (s.d. = 2.7) for control (p > 0.05). Shear tests yielded mean bond strengths approaching 30 MPa for both enamel and dentin under certain irradiation conditions. These values were slightly lower than nonirradiated acid-etched control samples. Additional studies are needed to determine if the slightly lower bond strength than the acid-etched control samples is clinically significant. These measurements demonstrate that enamel and dentin surfaces can be rapidly ablated by CO(2) lasers with minimal peripheral thermal and mechanical damage and without excessive heat accumulation.

Adhesive sealing of dentin surfaces in vitro: A review

PubMed Central

Abu-Nawareg, Manar M; Zidan, Ahmed Z; Zhou, Jianfeng; Agee, Kelli; Chiba, Ayaka; Tagami, Jungi; Pashley, David H

2016-01-01

Purpose The purpose of this review is to describe the evolution of the use of dental adhesives to form a tight seal of freshly prepared dentin to protect the pulp from bacterial products, during the time between crown preparation and final cementum of full crowns. The evolution of these “immediate dentin sealants” follows the evolution of dental adhesives, in general. That is, they began with multiple-step, etch-and-rinse adhesives, and then switched to the use of simplified adhesives. Methods Literature was reviewed for evidence that bacteria or bacterial products diffusing across dentin can irritate pulpal tissues before and after smear layer removal. Smear layers can be solubilized by plaque organisms within 7–10 days if they are directly exposed to oral fluids. It is likely that smear layers covered by temporary restorations may last more than one month. As long as smear layers remain in place, they can partially seal dentin. Thus, many in vitro studies evaluating the sealing ability of adhesive resins use smear layer-covered dentin as a reference condition. Surprisingly, many adhesives do not seal dentin as well as do smear layers. Results Both in vitro and in vivo studies show that resin-covered dentin allows dentinal fluid to cross polymerized resins. The use of simplified single bottle adhesives to seal dentin was a step backwards. Currently, most authorities use either 3-step adhesives such as Scotchbond Multi-Purposea or OptiBond FLb or two-step self-etching primer adhesives, such as Clearfil SEc, Unifil Bondd or AdheSEe, respectfully. PMID:26846037

Non-thermal Atmospheric Plasma Treatment for Deactivation of Oral Bacteria and Improvement of Dental Composite Restoration

NASA Astrophysics Data System (ADS)

Yu, Qing Song; Li, H.; Ritts, A. C.; Yang, B.; Chen, M.; Hong, L.; Xu, C.; Yao, X.; Wang, Y.

This paper reviews our recent research results of using non-thermal ­atmospheric plasmas for oral bacterial deactivation and for composite restoration improvement. Oral bacteria of Streptococcus mutans (S. mutans) and Lactobacillus acidophilus (L. acidophilus) with an initial bacterial population density between 1.0 × 108 and 5.0 × 108 cfu/ml were seeded on various media and their survivability with plasma exposure was examined. The plasma exposure time for a 99.9999% cell reduction was less than 15 s for S. mutans and within 5 min for L. acidophilus. To evaluate the dentin/composite interfacial bonding, extracted unerupted human third molars were used by removing the crowns and etching the exposed dentin surfaces with 35% phosphoric acid gel. After dental composite application and light curing, the teeth were then sectioned into micro-bars as the specimens for microtensile test. Student Newman Keuls (SNK) tests showed that the bonding strength of the composite restoration to peripheral dentin was significantly increased (by 64%) after 30 s plasma treatment of the dentin surfaces. These findings indicated that non-thermal atmospheric plasma technology is very promising for dental clinical applications.

Dental biothermophotonics: How photothermal methods are winning the race with X-rays for dental caries diagnostic needs of clinical dentistry

NASA Astrophysics Data System (ADS)

Mandelis, A.; Jeon, R.; Matvienko, A.; Abrams, S. H.; Amaechi, B. T.

2008-01-01

Recent trends in biothermophotonics of teeth are presented. The presentation is centered on the development of clinical-level frequency-domain photothermal radiometry and modulated luminescence to address issues associated with the early diagnosis of demineralization caries in human teeth. Biothermophotonic principles and applications to the detection of the carious state in human teeth as embodied by laser photothermal radiometry are presented and further supported by modulated luminescence. The emphasis is on recent developments with regard to abilities of these techniques to diagnose interproximal lesions between teeth, etching with phosphoric acid and with an artificial demineralization gel in order to simulate early demineralization, as well as demineralization and remineralization of dental crown enamel and root dentin. These are lesions which normally go undetected by X-ray radiographs. Comparisons with X rays, Micro-Computed Tomography (μ-CT) and Transverse Micro-Radiography (TMR) are discussed. A theoretical model involving coupled diffuse photon density and thermal-wave fields is developed and applied to frequency scans from demineralized artificial lesions to produce quantitative values for optical and thermophysical parameters of teeth as well as the thickness of the induced lesion.

Effect of Induced Periimplantitis on Dental Implants With and Without Ultrathin Hydroxyapatite Coating.

PubMed

Madi, Marwa; Zakaria, Osama; Ichinose, Shizuko; Kasugai, Shohei

2016-02-01

The aim of this study was to compare the effect of ligature-induced periimplantitis on dental implants with and without hydroxyapatite (HA) coat. Thirty-two dental implants (3.3 mm wide, 13 mm long) with 4 surface treatments (8 implant/group) (M: machined, SA: sandblasted acid etched, S: sputter HA coat and P: plasma-sprayed HA coat) were inserted into canine mandibles. After 12 weeks, oral hygiene procedures were stopped and silk ligatures were placed around the implant abutments to allow plaque accumulation for the following 16 weeks. Implants with the surrounding tissues were retrieved and prepared for histological examination. Bone-to-implant contact (BIC) and implant surfaces were examined using scanning electron microscopy and energy dispersive x-ray spectroscopy. Histological observation revealed marginal bone loss and large inflammatory cell infiltrates in the periimplant soft tissue. Sputter HA implants showed the largest BIC (98.1%) and machined implant showed the smallest values (70.4%). After 28 weeks, thin sputter HA coat was almost completely dissolved, whereas plasma-sprayed HA coat showed complete thickness preservation. Thin sputter HA-coated implants showed more bone implant contact and less marginal bone loss than thick HA-coated implants under periimplantitis condition.

Effect of handpiece maintenance method on bond strength.

PubMed

Roberts, Howard W; Vandewalle, Kraig S; Charlton, David G; Leonard, Daniel L

2005-01-01

This study evaluated the effect of dental handpiece lubricant on the shear bond strength of three bonding agents to dentin. A lubrication-free handpiece (one that does not require the user to lubricate it) and a handpiece requiring routine lubrication were used in the study. In addition, two different handpiece lubrication methods (automated versus manual application) were also investigated. One hundred and eighty extracted human teeth were ground to expose flat dentin surfaces that were then finished with wet silicon carbide paper. The teeth were randomly divided into 18 groups (n=10). The dentin surface of each specimen was exposed for 30 seconds to water spray from either a lubrication-free handpiece or a lubricated handpiece. Prior to exposure, various lubrication regimens were used on the handpieces that required lubrication. The dentin surfaces were then treated with total-etch, two-step; a self-etch, two-step or a self-etch, one-step bonding agent. Resin composite cylinders were bonded to dentin, the specimens were then thermocycled and tested to failure in shear at seven days. Mean bond strength data were analyzed using Dunnett's multiple comparison test at an 0.05 level of significance. Results indicated that within each of the bonding agents, there were no significant differences in bond strength between the control group and the treatment groups regardless of the type of handpiece or use of routine lubrication.

Shear strengths of a gallium alloy bonded to human enamel following nine different surface treatments.

PubMed

Claire, J; Williams, P T

2001-03-01

Gallium and indium-containing alloys have demonstrated an ability to wet and bond to many types of materials including enamel. The purpose of this study was to evaluate and compare the bond strengths of a gallium-and-indium-containing alloy and a dental amalgam to human enamel surfaces. A flat enamel bonding surface was created by slicing recently extracted human molars with a 180-grit diamond wheel. Cylinders of amalgam or a gallium-indium alloy were bonded to the as-cut surfaces or to as-cut surfaces that had been pumiced, air-abraded or acid-etched for various times. Before testing, samples were stored under different conditions (100% humidity, immersed in water, thermocycled). The shear-bond strength was determined using a crosshead speed of 0.1 mm x min(-1). Sample size was 10. Data was subjected to ANOVA and a post-hoc Tukey's test. The bond strength of amalgam to enamel was zero. The bond strength of the gallium-indium alloy ranged between 6.5 MPa (10s etch with 10% phosphoric acid) and 4.2 MPa (pumiced enamel). Acid-etching significantly increased the bond strength (P>0.0001) The bond strength was not significantly affected by the type of mechanical surface preparation, storage conditions, thermocycling, etching times or acid concentrations. Bonding, particularly chemical bonding, suggests a greater potential for better wetting and therefore better sealing of a cavity. Since microleakage of restorations is one of the principal causes of restoration failure, materials that can bond may in turn posses enhanced resistance to microleakage and ultimately, resistance to restoration failure. The gallium-indium alloy evaluated in this study may be such an alloy.

Titanium hydride and hydrogen concentration in acid-etched commercially pure titanium and titanium alloy implants: a comparative analysis of five implant systems.

PubMed

Szmukler-Moncler, S; Bischof, M; Nedir, R; Ermrich, M

2010-09-01

Acid etching is a popular method to texture the surface of dental implants. During etching, the titanium oxide protective layer is dissolved and small native hydrogen ions diffuse into the unprotected implant surface. They enrich the implant surface with hydrogen and precipitate into titanium hydride (TiH). The aim of this study was to measure the concentration of TiH at the implant surface and the total concentration of Hydrogen at five commercially available implant systems, made of either commercially pure (cp) titanium or titanium alloy. X-Ray diffraction (XRD) was conducted on each implant system to determine the compounds present at the implant surface. Following a TiH(2)/Ti calibration curve, the concentration of TiH was determined. Concentration of hydrogen in the implants was measured by the inert gas fusion thermal conductivity/infrared detection method. XRD data showed that TiH was present on all cp titanium implants but not on the alloyed implants. TiH concentration varied between 5% and 37%. Hydrogen concentration varied between 43 and 108 ppm, no difference in uptake was found between the cp titanium and alloyed implants. Low solubility of hydrogen in alpha-titanium is responsible for precipitation into TiH. Stronger etching conditions led to higher concentration of TiH2-x. High solubility of hydrogen in the beta-phase of the alloy is preventing hydrogen from precipitating into TiH. All implants, even those lacking TiH at the surface, were enriched with hydrogen. In all implants, hydrogen concentration was within the normative limit of 130 ppm.

A new universal simplified adhesive: 18-month clinical evaluation.

PubMed

Perdigão, J; Kose, C; Mena-Serrano, A P; De Paula, E A; Tay, L Y; Reis, A; Loguercio, A D

2014-01-01

To evaluate the 18-month clinical performance of a multimode adhesive (Scotchbond Universal Adhesive, SU, 3M ESPE, St Paul, MN, USA) in noncarious cervical lesions (NCCLs) using two evaluation criteria. Thirty-nine patients participated in this study. Two-hundred restorations were assigned to four groups: ERm, etch-and-rinse + moist dentin; ERd, etch-and-rinse + dry dentin; Set, selective enamel etching; and SE, self-etch. The composite resin, Filtek Supreme Ultra (3M ESPE), was placed incrementally. The restorations were evaluated at baseline, and at 18 months, using both the World Dental Federation (FDI) and the United States Public Health Service (USPHS) criteria. Statistical analyses were performed using Friedman repeated-measures analysis of variance by rank and McNemar test for significance in each pair (α=0.05). Five restorations (SE: 3; Set: 1; and ERm: 1) were lost after 18 months (p>0.05 for either criteria). Marginal staining occurred in four and 10% of the restorations evaluated (p>0.05), respectively, for USPHS and FDI criteria. Nine restorations were scored as bravo for marginal adaptation using the USPHS criteria and 38%, 40%, 36%, and 44% for groups ERm, ERd, Set, and SE, respectively, when the FDI criteria were applied (p>0.05). However, when semiquantitative scores (or SQUACE) for marginal adaptation were used, SE resulted in a significantly greater number of restorations, with more than 30% of the total length of the interface showing marginal discrepancy (28%) in comparison with the other groups (8%, 6%, and 8%, respectively, for ERm, ERd, and Set). The clinical retention of the multimode adhesive at 18 months does not depend on the bonding strategy. The only differences between strategies were found for the parameter marginal adaptation, for which the FDI criteria were more sensitive than the USPHS criteria.

Dentin bond optimization using the dimethyl sulfoxide-wet bonding strategy: A 2-year in vitro study.

PubMed

Stape, Thiago Henrique Scarabello; Tjäderhane, Leo; Tezvergil-Mutluay, Arzu; Yanikian, Cristiane Rumi Fujiwara; Szesz, Anna Luiza; Loguercio, Alessandro Dourado; Martins, Luís Roberto Marcondes

2016-12-01

This study evaluated a new approach, named dimethyl sulfoxide (DMSO)-wet bonding, to produce more desirable long-term prospects for the ultrafine interactions between synthetic polymeric biomaterials and the inherently hydrated dentin substrate. Sound third molars were randomly restored with/without DMSO pretreatment using a total-etch (Scocthbond Multipurpose: SBMP) and a self-etch (Clearfil SE Bond: CF) adhesive systems. Restored teeth (n=10)/group were sectioned into sticks and submitted to different analyses: micro-Raman determined the degree of conversion inside the hybrid layer (DC); resin-dentin microtensile bond strength and fracture pattern analysis at 24h, 1year and 2 years of aging; and nanoleakage evaluation at 24h and 2 years. DMSO-wet bonding produced significantly higher 24h bond strengths for SBMP that were sustained over the two-year period, with significantly less adhesive failures. Similarly, DMSO-treated CF samples presented significantly higher bond strength than untreated samples at two years. Both adhesives had significant less adhesive failures at 2 years with DMSO. DMSO had no effect on DC of SBMP, but significantly increased the DC of CF. DMSO-treated SBMP samples presented reduced silver uptake compared to untreated samples after aging. Biomodification of the dentin substrate by the proposed strategy using DMSO is a suitable approach to produce more durable hybrid layers with superior ability to withstand hydrolytic degradation over time. Although the active role of DMSO on dentin bond improvement may vary according to monomer composition, its use seems to be effective on both self-etch and etch-and-rinse bonding mechanisms. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Titanium Surface Roughing Treatments contribute to Higher Interaction with Salivary Proteins MG2 and Lactoferrin.

PubMed

Cavalcanti, Yuri Wanderley; Soare, Rodrigo Villamarim; Leite Assis, Marina Araújo; Zenóbio, Elton Gonçalves; Girundi, Francisco Mauro da Silva

2015-02-01

Some surface treatments performed on titanium can alter the composition of salivary pellicle formed on this abiotic surface. Such treatments modify the titanium's surface properties and can promote higher adsorption of proteins, which allow better integration of titanium to the biotic system. This study aimed to evaluate the interactions between salivary proteins and titanium disks with different surface treatments. Machined titanium disks (n = 48) were divided into four experimental groups (n = 12), according to their surface treatments: surface polishing (SP); acid etching (A); spot-blasting plus acid etching (SB-A); spot-blasting followed by acid etching and nano-functionalization (SB-A-NF). Titanium surfaces were characterized by surface roughness and scanning electron microscopy (SEM). Specimens were incubated with human saliva extracted from submandibular and sublingual glands. Total salivary protein adsorbed to titanium was quantified and samples were submitted to western blotting for mucin glycoprotein 2 (MG2) and lactoferrin identification. Surface roughness was statistically higher for SB-A and SB-A-NF groups. Scanning electron microscopy images confirmed that titanium surface treatments increased surface roughness with higher number of porous and scratches for SB-A and SB-A-NF groups. Total protein adsorption was significantly higher for SB-A and SB-A-NF groups (p < 0.05), which also presented higher interactions with MG2 and lactoferrin proteins. The roughing of titanium surface by spot-blasting plus acid etching treatments contribute to higher interaction with salivary proteins, such as MG2 and lactoferrin. Titanium surface roughing increases the interactions of the substratum with salivary proteins, which can influence the integration of dental implants and their components to the oral environment. However, those treatments should be used carefully intraorally, avoiding increase biofilm formation.

Interfacial adhesion of dental ceramic-resin systems

NASA Astrophysics Data System (ADS)

Della Bona, Alvaro

The clinical success of resin bonding procedures for indirect ceramic restorations and ceramic repairs depends on the quality and durability of the bond between the ceramic and the resin. The quality of this bond will depend upon the bonding mechanisms that are controlled in part by the surface treatment that promotes micromechanical and/or chemical bonding to the substrate. The objective of this study is to correlate interfacial toughness (K A) with fracture surface morphological parameters of the dental ceramic-resin systems as a function of ceramic surface treatment. The analytical procedures focused on characterizing the microstructure and fracture properties of EmpressRTM ceramics (a leucite-based core ceramic, two lithia disilicate-based core ceramics, and a glass veneer) and determining the ceramic-resin adhesion zone bond strength characteristics. Microstructure and composition are controlling factors in the development of micromechanical retention produced by etching. Silane treated ceramics negated the effect of surface roughening produced by etching, inducing lower surface energy of the ceramic and, reduced bonding effectiveness. There was a positive correlation between WA, tensile bond strength (a), and KA, i.e., higher mean WA value, and higher mean sigma and KA values. This study suggests that (1) the sigma and KA values for ceramic bonded to resin are affected by the ceramic microstructure and the ceramic surface treatments; (2) the definition of the adhesion zone is essential to classify the modes of failure, which should be an integral component of all failure analyses; (3) the microtensile test may be preferable to conventional shear or flexural tests as an indicator of composite-ceramic bond quality; and (4) careful microscopic analysis of fracture surfaces and an x-ray dot map can produce a more consistent and complete description of the fracture process and interpretation of the modes of failure. The mode of failure and fractographic analyses provide important a more comprehensive assessment of mechanisms that control the survival times of dental adhesive systems. Thus, the quality of the bond should not be assessed based on bond strength data alone.

Adhesive Bonding to Computer-aided Design/ Computer-aided Manufacturing Esthetic Dental Materials: An Overview.

PubMed

Awad, Mohamed Moustafa; Alqahtani, H; Al-Mudahi, A; Murayshed, M S; Alrahlah, A; Bhandi, Shilpa H

2017-07-01

To review the adhesive bonding to different computer-aided design/computer-aided manufacturing (CAD/CAM) esthetic restorative materials. The use of CAD/CAM esthetic restorative materials has gained popularity in recent years. Several CAD/ CAM esthetic restorative materials are commercially available. Adhesive bonding is a major determinant of success of CAD/ CAM restorations. Review result: An account of the currently available bonding strategies are discussed with their rationale in various CAD/ CAM materials. Different surface treatment methods as well as adhesion promoters can be used to achieve reliable bonding of CAD/CAM restorative materials. Selection of bonding strategy to such material is determined based on its composition. Further evidence is required to evaluate the effect of new surface treatment methods, such as nonthermal atmospheric plasma and self-etching ceramic primer on bonding to different dental ceramics. An understanding of the currently available bonding strategies to CA/CAM materials can help the clinician to select the most indicated system for each category of materials.

Effect of etching and airborne particle abrasion on the microstructure of different dental ceramics.

PubMed

Borges, Gilberto Antonio; Sophr, Ana Maria; de Goes, Mario Fernando; Sobrinho, Lourenço Correr; Chan, Daniel C N

2003-05-01

The ceramic composition and microstructure surface of all-ceramic restorations are important components of an effective bonding substrate. Both hydrofluoric acid etching and airborne aluminum oxide particle abrasion produce irregular surfaces necessary for micromechanical bonding. Although surface treatments of feldspathic and leucite porcelains have been studied previously, the high alumina-containing and lithium disilicate ceramics have not been fully investigated. The purpose of this study was to assess the surface topography of 6 different ceramics after treatment with either hydrofluoric acid etching or airborne aluminum oxide particle abrasion. Five copings each of IPS Empress, IPS Empress 2 (0.8 mm thick), Cergogold (0.7 mm thick), In-Ceram Alumina, In-Ceram Zirconia, and Procera (0.8 mm thick) were fabricated following the manufacturer's instructions. Each coping was longitudinally sectioned into 4 equal parts by a diamond disk. The resulting sections were then randomly divided into 3 groups depending on subsequent surface treatments: Group 1, specimens without additional surface treatments, as received from the laboratory (control); Group 2, specimens treated by use of airborne particle abrasion with 50-microm aluminum oxide; and Group 3, specimens treated with 10% hydrofluoric acid etching (20 seconds for IPS Empress 2; 60 seconds for IPS Empress and Cergogold; and 2 minutes for In-Ceram Alumina, In-Ceram Zirconia, and Procera). Airborne particle abrasion changed the morphologic surface of IPS Empress, IPS Empress 2, and Cergogold ceramics. The surface topography of these ceramics exhibited shallow irregularities not evident in the control group. For Procera, the 50-microm aluminum oxide airborne particle abrasion produced a flattened surface. Airborne particle abrasion of In-Ceram Alumina and In-Ceram Zirconia did not change the morphologic characteristics and the same shallows pits found in the control group remained. For IPS Empress 2, 10% hydrofluoric acid etching produced elongated crystals scattered with shallow irregularities. For IPS Empress and Cergogold, the morphologic characteristic was honeycomb-like on the ceramic surface. The surface treatment of In-Ceram Alumina, In-Ceram Zirconia, and Procera did not change their superficial structure. Hydrofluoric acid etching and airborne particle abrasion with 50-microm aluminum oxide increased the irregularities on the surface of IPS Empress, IPS Empress 2, and Cergogold ceramics. Similar treatment of In-Ceram Alumina, In-Ceram Zirconia, and Procera did not change their morphologic microstructure.

Direct and transdentinal (indirect) antibacterial activity of commercially available dental gel formulations against Streptococcus mutans.

PubMed

Tüzüner, Tamer; Ulusoy, Ayça Tuba; Baygin, Ozgul; Yahyaoglu, Gorkem; Yalcin, Ilkay; Buruk, Kurtulus; Nicholson, John

2013-01-01

To evaluate the direct and transdentinal (indirect) agar diffusion antibacterial activity of different commercially available antibacterial dental gel formulations against Streptococcus mutans. The commercially available dental gel formulations were Corsodyl® (COG, 1% chlorhexidine), Cervitec® (CEG, 0.2% chlorhexidine + 0.2% sodium fluoride), Forever Bright® (FOB, aloe vera), Gengigel® (GEG, 0.2% hyaluronic acid), 35% phosphoric acid gel and distilled water (control). Direct agar diffusion was performed by isolating three wells from brain-heart infusion agar plates using sterile glass pipettes attached to a vacuum pump and adding 0.1 ml of the gels to each well. Transdentinal (indirect) agar diffusion was performed by applying gel to 0.2- and 0.5-mm-thick human dentin discs previously etched with phosphoric acid and rinsed with distilled water. Zones formed around the wells and the dentin discs were measured and analyzed using Kruskal-Wallis and Mann-Whitney U tests with Bonferroni correction (p < 0.01). Direct agar diffusion tests showed significant differences among all gel formulations (p < 0.01) except for COG and CEG (p > 0.01). COG and CEG exhibited higher antibacterial effects compared to FOB and GEG (p < 0.01) in both direct and transdentinal (indirect) testing procedures. GEG did not show any antimicrobial activity in transdentinal (indirect) testing. Commercially available dental gels inhibited S. mutans, which may indicate their potential as cavity disinfectants. Copyright © 2013 S. Karger AG, Basel.

Evaluating tooth restorations: micro-computed tomography in practical training for students in dentistry

NASA Astrophysics Data System (ADS)

Deyhle, Hans; Schmidli, Fredy; Krastl, Gabriel; Müller, Bert

2010-09-01

Direct composite fillings belong to widespread tooth restoration techniques in dental medicine. The procedure consists of successive steps, which include etching of the prepared tooth surface, bonding and placement of composite in incrementally built up layers. Durability and lifespan of the composite inlays strongly depend on the accurate completion of the individual steps to be also realized by students in dental medicine. Improper handling or nonconformity in the bonding procedure often lead to air enclosures (bubbles) as well as to significant gaps between the composite layers or at the margins of the restoration. Traditionally one analyzes the quality of the restoration cutting the tooth in an arbitrarily selected plane and inspecting this plane by conventional optical microscopy. Although the precision of this established method is satisfactory, it is restricted to the selected two-dimensional plane. Rather simple micro computed tomography (μCT) systems, such as SkyScan 1174™, allows for the non-destructive three-dimensional imaging of restored teeth ex vivo and virtually cutting the tomographic data in any desired direction, offering a powerful tool for inspection of the restored tooth with micrometer resolution before cutting and thus also to select a two-dimensional plane with potential defects. In order to study the influence of the individual steps on the resulted tooth restoration, direct composite fillings were placed in mod cavities of extracted teeth. After etching, an adhesive was applied in half of the specimens. From the tomographic datasets, it becomes clear that gaps occur more frequently when bonding is omitted. The visualization of air enclosures offers to determine the probability to find a micrometer-sized defect using an arbitrarily selected cutting plane for inspection.

Microleakage of class V resin composite restorations after bur, air-abrasion or Er:YAG laser preparation.

PubMed

Corona, S A; Borsatto, M; Dibb, R G; Ramos, R P; Brugnera, A; Pécora, J D

2001-01-01

This in vitro study compared the microleakage of Class V resin composite restorations placed in cavities prepared with a high-speed dental bur, air-abrasion or Er:YAG laser. Twenty sound extracted human third molars were selected and randomly assigned to four equal Groups (n=10): Group I, cavities were cut by dental drill at high-speed; Group II, aluminum oxide air-abrasion was used for cavity preparation, and in Groups III and IV, cavities were prepared by Er:YAG laser. Following cavity preparation, Groups I and II were acid-etched, Group III was treated only by Er:YAG laser and Group IV was conditioned by Er:YAG laser followed by acid-etching. Cavities were restored (Single Bond + Z-100) and the teeth stored for seven days in distilled water. Then, the restorations were polished and the specimens thermocycled, immersed in a 0.2% Rhodamine solution, sectioned and analyzed for leakage at the occlusal (enamel) and cervical (dentin/cementum) interfaces using an optical microscope connected to a video camera. The images were digitized and software was utilized for microleakage assessment. Upon analyzing the results, statistically significant differences (p<0.01) between the occlusal and cervical regions for all groups was observed, and, as a rule, there was better marginal sealing at the enamel margins. The highest degree of infiltration was observed for cavities prepared and treated exclusively by Er:YAG (Group III). The other experimental groups showed statistical similarities in the amount of marginal leakage at the enamel margins. However, at the cervical margins, there was a significant difference (p<0.05) between Group I and the remaining groups. None of the techniques completely eliminated marginal microleakage at the dentin/ cementum margins.

Effect of changes to the manufacturer application techniques 
on the shear bond strength of simplified dental adhesives.

PubMed

Chasqueira, Ana Filipa; Arantes-Oliveira, Sofia; Portugal, Jaime

2013-09-13

The aim of this work was to assess the shear bond strength (SBS) between a composite resin and dentin, promoted by two dental adhesive systems (one-step self-etching adhesive Easy Bond [3M ESPE], and two-step etch-and-rinse adhesive Scotchbond 1XT [3M ESPE]) with different application protocols (per manufacturer's instruction (control group); with one to four additional adhesive layers; or with an extra hydrophobic adhesive layer). Proximal enamel was removed from ninety caries-free human molars to obtain two dentin discs per tooth, which were randomly assigned to twelve experimental groups (n=15). After adhesion protocol, the composite resin (Filtek Z250 [3M ESPE]) was applied. Specimens were mounted in the Watanabe test device and shear bond test was performed in a universal testing machine with a crosshead speed of 5 mm/min. Data were analyzed with ANOVA followed by Student-Newman-Keuls tests (P<0.05). The highest SBS mean value was attained with the Easy Bond three layers group (41.23±2.71 MPa) and the lowest with Scotchbond 1XT per manufacturer's instructions (27.15±2.99 MPa). Easy Bond yielded higher SBS values than Scotchbond 1XT. There were no statistically significant differences (P>0.05) between the application protocols tested, except for the three and four layers groups, that presented higher SBS results compared to manufacturer's instruction groups (P<0.05). No statistically significant differences were detected between the three and four layers groups (P≥0.05). It is recommendable to apply three adhesive layers when using Easy Bond and Scotchbond 1XT adhesives, since it improves SBS values without consuming much time.

Effect of Ceramic Surface Treatments After Machine Grinding on the Biaxial Flexural Strength of Different CAD/CAM Dental Ceramics.

PubMed

Bagheri, Hossein; Hooshmand, Tabassom; Aghajani, Farzaneh

2015-09-01

This study aimed to evaluate the effect of different ceramic surface treatments after machining grinding on the biaxial flexural strength (BFS) of machinable dental ceramics with different crystalline phases. Disk-shape specimens (10mm in diameter and 1.3mm in thickness) of machinable ceramic cores (two silica-based and one zirconia-based ceramics) were prepared. Each type of the ceramic surfaces was then randomly treated (n=15) with different treatments as follows: 1) machined finish as control, 2) machined finish and sandblasting with alumina, and 3) machined finish and hydrofluoric acid etching for the leucite and lithium disilicate-based ceramics, and for the zirconia; 1) machined finish and post-sintered as control, 2) machined finish, post-sintered, and sandblasting, and 3) machined finish, post-sintered, and Nd;YAG laser irradiation. The BFS were measured in a universal testing machine. Data based were analyzed by ANOVA and Tukey's multiple comparisons post-hoc test (α=0.05). The mean BFS of machined finish only surfaces for leucite ceramic was significantly higher than that of sandblasted (P=0.001) and acid etched surfaces (P=0.005). A significantly lower BFS was found after sandblasting for lithium disilicate compared with that of other groups (P<0.05). Sandblasting significantly increased the BFS for the zirconia (P<0.05), but the BFS was significantly decreased after laser irradiation (P<0.05). The BFS of the machinable ceramics was affected by the type of ceramic material and surface treatment method. Sandblasting with alumina was detrimental to the strength of only silica-based ceramics. Nd:YAG laser irradiation may lead to substantial strength degradation of zirconia.

[Influence of long-term water storage on the physical and chemical properties of four different dental cements].

PubMed

Xu, Xiaodong; Meng, Xiangfeng

2014-11-01

To evaluate and compare the physical and chemical properties of four different dental cements under long-term water storage. A glass-ionomer cement (A:Fuji I), a resin reinforced glass-ionomer (B: Fuji Plus), a self-adhesive resin cement (C:G-Cem), and an etch & rinse resin cement (D: Duolink) were taken as samples. According to ISO 4049, water sorption and solubility of four resin cements under different storage times (1 week, 1, 3, 6 and 12 months) were calculated (n = 5), meanwhile their surface Knoop micro hardness values were measured. Surface cracks were detected on sample B and C after 12 months. Sample A was fragmentized after 6 months. Sample B showed significantly lower surface hardness after 12 months than it did after the first 24 hours of water storage (P < 0.05). Sample D showed significantly lower water sorption than other cements did at all exam time point. The highest water sorption values were observed in Sample D after 1 month [(40.8±2.5) µg/mm(3)], in Sample B after 3 months [(551.3±22.5) µg/mm(3)], in Sample C after 12 months [(147.5±8.3) µg/mm(3)]. The highest solubility values were detected in Sample B after 3 months [(105.3±10.5) µg/mm(3)], in Sample C after 12 months [(79.3 ± 6.2) µg/mm(3)], and in Sample D after 12 months [(23.9 ± 6.9) µg/mm(3)]. Among the four types of cements, the etch & rinse resin cement showed the best stability of physical and chemical properties under long-term water storage.

Effect of Ceramic Surface Treatments After Machine Grinding on the Biaxial Flexural Strength of Different CAD/CAM Dental Ceramics

PubMed Central

Bagheri, Hossein; Aghajani, Farzaneh

2015-01-01

Objectives: This study aimed to evaluate the effect of different ceramic surface treatments after machining grinding on the biaxial flexural strength (BFS) of machinable dental ceramics with different crystalline phases. Materials and Methods: Disk-shape specimens (10mm in diameter and 1.3mm in thickness) of machinable ceramic cores (two silica-based and one zirconia-based ceramics) were prepared. Each type of the ceramic surfaces was then randomly treated (n=15) with different treatments as follows: 1) machined finish as control, 2) machined finish and sandblasting with alumina, and 3) machined finish and hydrofluoric acid etching for the leucite and lithium disilicate-based ceramics, and for the zirconia; 1) machined finish and post-sintered as control, 2) machined finish, post-sintered, and sandblasting, and 3) machined finish, post-sintered, and Nd;YAG laser irradiation. The BFS were measured in a universal testing machine. Data based were analyzed by ANOVA and Tukey’s multiple comparisons post-hoc test (α=0.05). Results: The mean BFS of machined finish only surfaces for leucite ceramic was significantly higher than that of sandblasted (P=0.001) and acid etched surfaces (P=0.005). A significantly lower BFS was found after sandblasting for lithium disilicate compared with that of other groups (P<0.05). Sandblasting significantly increased the BFS for the zirconia (P<0.05), but the BFS was significantly decreased after laser irradiation (P<0.05). Conclusions: The BFS of the machinable ceramics was affected by the type of ceramic material and surface treatment method. Sandblasting with alumina was detrimental to the strength of only silica-based ceramics. Nd:YAG laser irradiation may lead to substantial strength degradation of zirconia. PMID:27148372

Acids with an equivalent taste lead to different erosion of human dental enamel.

PubMed

Beyer, Markus; Reichert, Jörg; Bossert, Jörg; Sigusch, Bernd W; Watts, David C; Jandt, Klaus D

2011-10-01

The consumption of acidic soft drinks may lead to demineralization and softening of human dental enamel, known as dental erosion. The aims of this in vitro study were to determine: (i) if different acids with a similar sensorial acidic taste lead to different hardness loss of enamel and (ii) if the fruit acids tartaric, malic, lactic or ascorbic acid lead to less hardness loss of enamel than citric or phosphoric acid when their concentration in solution is based on an equivalent sensorial acidic taste. Enamel samples of non-erupted human third molars were treated with acidic solutions of tartaric (TA), malic (MA), lactic (LA), ascorbic (AA), phosphoric (PA) and citric (CA) acids with a concentration that gave an equivalent sensorial acidic taste. The acidic solutions were characterized by pH value and titratable acidity. Atomic force microscopy (AFM) based nanoindentation was used to study the nano mechanical properties and scanning electron microscopy (SEM) was used to study the morphology of the treated enamel samples and the untreated control areas, respectively. The investigated acids fell into two groups. The nano hardnesses of MA, TA and CA treated enamel samples (group I) were statistically significantly greater (p<0.05) than the nano hardnesses of PA, AA and LA treated enamel samples (group II). Within each group the nano hardness was not statistically significantly different (p>0.05). The SEM micrographs showed different etch prism morphologies depending on the acid used. In vitro, the acids investigated led to different erosion effects on human dental enamel, despite their equivalent sensorial acidic taste. This has not been reported previously. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Control of dental-derived induced pluripotent stem cells through modified surfaces for dental application.

PubMed

Choi, Hyunmin; Park, Kyu-Hyung; Lee, Ah-Reum; Mun, Chin Hee; Shin, Yong Dae; Park, Yong-Beom; Park, Young-Bum

2017-07-01

The aim of this study is to investigate the behaviour of iPSc derived from dental stem cells in terms of initial adhesion, differentiation potential on differently surface-treated titanium disc. iPSc derived from human gingival fibroblasts (hGFs) were established using 4-reprogramming factors transduction with Sendai virus. The hGF-iPSc established in this study exhibited the morphology and growth properties similar to human embryonic stem (ES) cells and expressed pluripotency makers. Alkaline Phosphatase (AP) staining, Embryoid Body (EB) formation and in vitro differentiation and karyotyping further confirmed pluripotency of hGF-iPSc. Then, hGF-iPSc were cultured on machined- and Sandblasted and acid etched (SLA)-treated titanium discs with osteogenic induction medium and their morphological as well as quantitative changes according to different surface types were investigated using Alizrin Red S staining, Scanning electron microscopy (SEM), Flow cytometry and RT-PCR. Time-dependent and surface-dependent morphological changes as well as quantitative change in osteogenic differentiation of hGF-iPSc were identified and osteogenic gene expression of hGF-iPSc cultured on SLA-treated titanium disc found to be greater than machined titanium disc, suggesting the fate of hGF-iPSc may be determined by the characteristics of surface to which hGF-iPSc first adhere. iPSc derived from dental stem cell can be one of the most promising and practical cell sources for personalized regenerative dentistry and their morphological change as well as quantitative change in osteogenic differentiation according to different surface types may be further utilized for future clinical application incorporated with dental implant.

[Nanoleakage at the resin-dental interface of four self-etching adhesives].

PubMed

Liao, Zhi-qing; Ouyang, Yong; Yang, Jian-zhen

2011-09-01

To evaluate the nanoleakage and ultramorphology of four self-etching adhesives. Sixteen freshly extracted, caries-free human third molars were selected. A flat dentin surface was exposed by removing occlusal enamel. All teeth were randomly divided into four groups acorrding to four different self-etch adhesive: Adper Prompt (A), iBond (B), Xeno III (C) and SE Bond (D). The dentin were bonded with dentin adhesive system according to manufacturer's directions. Composite layers were built up incrementally. The specimens were sectioned longitudinally across the resin-dentin interface into 4.0 mm×0.9 mm sticks and then traced with ammoniacal silver solution. Epoxy resin-embedded sections were prepared for transmission electron microscope (TEM) to observe nanoleakage. The images were qualitatively compared by NIH software, and data was analyzed by SPSS. Different thickness of hybrid layer and adhesives layer were observed for each adhesive. The hybrid layer of A, C was thicker than that of B, D, and adhesive layer of D was thicker than the others. The extent of nanoleakage varied among different adhesives: A (45.02 ± 9.49), B (43.97 ± 8.55), C (27.02 ± 10.86), D (12.94 ± 2.07). D presented significantly less silver deposition than any of the others did (P < 0.05). The thickness of hybrid layer and adhesive layer vary among the four adhesives. The shape and extent of nanoleakage of each adhesive are also different. Two-step system shows less nanoleakage than one-step systems do.

Imunohistological aspects of the tissue around dental implants

NASA Astrophysics Data System (ADS)

Nimigean, Victor; Nimigean, Vanda R.; Sǎlǎvǎstru, Dan I.; Moraru, Simona; BuÅ£incu, Lavinia; Ivaşcu, Roxana V.; Poll, Alexandru

2016-03-01

Objectives: study of soft and hard tissues around implants. Material and methods: For the immunohistochemical and histological study of the implant/soft tissue interface, we examined pieces of peri-implant mucosa harvested from 35 patients. The implant/bone interface was assessed using histologic and histomorphometric examination of hard tissues around unloaded, early loaded or delayed loaded dental implants with pre-established design, with a sandblasted and acid-etched surface, placed both in extraction sockets, or after bone healing following tooth removal. This study was performed on 9 common race dogs. Results: The histological study of the implant/soft tissue interface showed regenerative modifications and moderate chronic subepithelial inflammatory reactions. Immunohistochemical evaluation of the soft tissue biopsies revealed the presence of specific immunocompetent cells and proteins of the matrix metalloproteinase (MMP) expression. Bone-implants contacts were more obvious in the apical half of the implants and at the edges of the threads, than between them. A mature, lamelliform bone containing lacunae with osteocytes and lack of connective tissue were noticed around implants that were late placed and loaded. The new-formed bone was also abundant in the crestal zone, not only in the apical part of the implants. Conclusions: A thorough understanding of the microstructure of dental implant/soft and hard tissue interface will improve the longevity of osseointegrated implants.

Corrosion of dental aluminium bronze in neutral saline and saline lactic acid.

PubMed

Tibballs, J E; Erimescu, Raluca

2006-09-01

To compare the corrosion behaviours of two aluminium bronze, dental casting alloys during a standard immersion test and for immersion in neutral saline. Cast specimens of aluminium bronzes with 1.4 wt% Fe (G) and 4 wt% Fe (N) were subject to progressively longer periods (up to in total 7 days) immersed in 0.1 M saline, 0.1 M lactic acid solutions and examined by scanning electron microscopy with EDX analysis. Immersion in 0.1M neutral saline was for 7 days. In the acidic solution, exposed interdendritic volumes in alloy N corroded completely away in 7 days with dissolution of Ni-enriched precipitate species as well as the copper-rich matrix. Alloy G begins to corrode more slowly but by a similar mechanism. The number density of an Fe-enriched species is insufficient to maintain a continuous galvanic potential to the copper matrix, and dissolution becomes imperceptible. In neutral saline solution, galvanic action alone caused pit-etching, without the dissolution of either precipitate species. The upper limit for the total dissolution of metallic ions in the standard immersion test can be set at 200 microg cm(-2). Aluminium bronze dental alloys can be expected to release both copper and nickel ions into an acidic oral environment.

Effect of dimethyl sulfoxide wet-bonding technique on hybrid layer quality and dentin bond strength.

PubMed

Stape, Thiago Henrique Scarabello; Tjäderhane, Leo; Marques, Marcelo Rocha; Aguiar, Flávio Henrique Baggio; Martins, Luís Roberto Marcondes

2015-06-01

This study examined the effect of a dimethyl sulfoxide (DMSO) wet bonding technique on the resin infiltration depths at the bonded interface and dentin bond strength of different adhesive systems. Flat dentin surfaces of 48 human third molars were treated with 50% DMSO (experimental groups) or with distilled water (controls) before bonding using an etch-and-rinse (SBMP: Scotchbond Multi-Purpose, 3M ESPE) or a self-etch (Clearfil: Clearfil SE Bond, Kuraray) adhesive system. The restored crown segments (n=12/group) were stored in distilled water (24h) and sectioned for interfacial analysis of exposed collagen using Masson's Trichrome staining and for microtensile bond strength testing. The extent of exposed collagen was measured using light microscopy and a histometric analysis software. Failure modes were examined by SEM. Data was analyzed by two-way ANOVA followed by Tukey Test (α=0.05). The interaction of bonding protocol and adhesive system had significant effects on the extension of exposed collagen matrix (p<0.0001) and bond strength (p=0.0091). DMSO-wet bonding significantly reduced the extent of exposed collagen matrix for SBMP and Clearfil (p<0.05). Significant increase in dentin bond strength was observed on DMSO-treated specimens bonded with SBMP (p<0.05), while no differences were observed for Clearfil (p>0.05). DMSO-wet bonding was effective to improve the quality of resin-dentin bonds of the tested etch-and-rinse adhesives by reducing the extent of exposed collagen matrix at the base of the resin-dentin biopolymer. The improved penetration of adhesive monomers is reflected as an increase in the immediate bond strength when the DMSO-wet bonding technique is used with a water-based etch-and-rinse adhesive. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Resin-dentin bonds to EDTA-treated vs. acid-etched dentin using ethanol wet-bonding. Part II: Effects of mechanical cycling load on microtensile bond strengths.

PubMed

Sauro, Salvatore; Toledano, Manuel; Aguilera, Fatima Sánchez; Mannocci, Francesco; Pashley, David H; Tay, Franklin R; Watson, Timothy F; Osorio, Raquel

2011-06-01

To compare microtensile bond strengths (MTBS) subsequent to load cycling of resin bonded acid-etched or EDTA-treated dentin using a modified ethanol wet-bonding technique. Flat dentin surfaces were obtained from extracted human molars and conditioned using 37% H(3)PO(4) (PA) (15s) or 0.1M EDTA (60s). Five experimental adhesives and one commercial bonding agent were applied to the dentin and light-cured. Solvated experimental resins (50% ethanol/50% comonomers) were used as primers and their respective neat resins were used as the adhesives. The resin-bonded teeth were stored in distilled water (24h) or submitted to 5000 loading cycles of 90N. The bonded teeth were then sectioned in beams for MTBS. Modes of failure were examined by scanning electron microscopy. The most hydrophobic resin 1 gave the lowest bond strength values to both acid and EDTA-treated dentin. The hydrophobic resin 2 applied to EDTA-treated dentin showed lower bond strengths after cycling load but this did not occur when it was bonded to PA-etched dentin. Resins 3 and 4, which contained hydrophilic monomers, gave higher bond strengths to both EDTA-treated or acid-etched dentin and showed no significant difference after load cycling. The most hydrophilic resin 5 showed no significant difference in bond strengths after cycling loading when bonded to EDTA or phosphoric acid treated dentin but exhibited low bond strengths. The presence of different functional monomers influences the MTBS of the adhesive systems when submitted to cyclic loads. Adhesives containing hydrophilic comonomers are not affected by cycling load challenge especially when applied on EDTA-treated dentin followed by ethanol wet bonding. Copyright © 2011 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Influence of degradation conditions on dentin bonding durability of three universal adhesives.

PubMed

Sai, Keiichi; Shimamura, Yutaka; Takamizawa, Toshiki; Tsujimoto, Akimasa; Imai, Arisa; Endo, Hajime; Barkmeier, Wayne W; Latta, Mark A; Miyazaki, Masashi

2016-11-01

This study aims to determine dentin bonding durability of universal adhesives using shear bond strength (SBS) tests under various degradation conditions. G-Premio Bond (GP, GC), Scotchbond Universal (SU, 3M ESPE) and All Bond Universal (AB, Bisco) were compared with conventional two-step self-etch adhesive Clearfil SE Bond (SE, Kuraray Noritake Dental). Bonded specimens were divided into three groups of ten, and SBSs with bovine dentin were determined after the following treatments: 1) Storage in distilled water at 37°C for 24h followed by 3000, 10,000, 20,000 or 30,000 thermal cycles (TC group), 2) Storage in distilled water at 37°C for 3 months, 6 months or 1year (water storage, WS group) and 3) Storage in distilled water at 37°C for 24h (control). SE bonded specimens showed significantly higher SBSs than universal adhesives, regardless of TC or storage periods, although AB specimens showed significantly increased SBSs after 30,000 thermal cycles. In comparisons of universal adhesives under control and degradation conditions, SBS was only reduced in SU after 1year of WS. Following exposure of various adhesive systems to degradation conditions of thermal cycling and long term storage, SBS values of adhesive systems varied primarily with degradation period. Although universal adhesives have lower SBSs than the two-step self-etch adhesive SE, the present data indicate that the dentin bonding durability of universal adhesives in self-etch mode is sufficient for clinical use. Copyright © 2016 Elsevier Ltd. All rights reserved.

Laser ablation of hard tissue: correlation between the laser beam parameters and the post-ablative tissue characteristics

NASA Astrophysics Data System (ADS)

Serafetinides, Alexandros A.; Makropoulou, Mersini I.; Khabbaz, Maruan

2003-11-01

Hard dental tissue laser applications, such as preventive treatment, laser diagnosis of caries, laser etching of enamel, laser decay removal and cavity preparation, and more recently use of the laser light to enlarge the root canal during the endodontic therapy, have been investigated for in vitro and in vivo applications. Post-ablative surface characteristics, e.g. degree of charring, cracks and other surface deformation, can be evaluated using scanning electron microscopy. The experimental data are discussed in relevance with the laser beam characteristics, e.g. pulse duration, beam profile, and the beam delivery systems employed. Techniques based on the laser illumination of the dental tissues and the subsequent evaluation of the scattered fluorescent light will be a valuable tool in early diagnosis of tooth diseases, as carious dentin or enamel. The laser induced autofluorescence signal of healthy dentin is much stronger than that of the carious dentin. However, a better understanding of the transmission patterns of laser light in teeth, for both diagnosis and therapy is needed, before the laser procedures can be used in a clinical environment.

Chemical interaction of glycero-phosphate dimethacrylate (GPDM) with hydroxyapatite and dentin.

PubMed

Yoshihara, Kumiko; Nagaoka, Noriyuki; Hayakawa, Satoshi; Okihara, Takumi; Yoshida, Yasuhiro; Van Meerbeek, Bart

2018-04-28

Although the functional monomer glycero-phosphate dimethacrylate (GPDM) has since long been used in several dental adhesives and more recently in self-adhesive composite cements and restoratives, its mechanism of chemical adhesion to hydroxyapatite (HAp) is still unknown. We therefore investigated the chemical interaction of GPDM with HAp using diverse chemical analyzers and ultra-structurally characterized the interface of a GPDM-based primer formulation with dentin. HAp particles were added to a GPDM solution for various periods, upon which they were thoroughly washed with ethanol and water prior to being air-dried. As control, 10-methacryloyloxydecyl dihydrogen phosphate (MDP) was used. The molecular interaction of GPDM with HAp was analyzed using X-ray diffraction (XRD) and solid-state nuclear magnetic resonance (NMR) spectroscopy. Crystal formation upon application of GPDM onto dentin was analyzed using thin-film XRD (TF-XRD). Its hydrophobicity was measured using contact-angle measurement. The interaction of GPDM with dentin was characterized using transmission electron microscopy (TEM). XRD revealed the deposition of dicalcium phosphate dihydrate (DCPD: CaHPO 4 ·2H 2 O) on HAp after 24h. NMR confirmed the adsorption of GPDM onto HAp. However, GPDM was easily removed after washing with water, unlike MDP that remained adhered to HAp. Dentin treated with GPDM appeared more hydrophilic compared to dentin treated with MDP. TEM disclosed exposed collagen in the hybrid layer produced by the GPDM-based primer formulation. Although GPDM adsorbed to HAp, it did not form a stable calcium salt. The bond between GPDM and HAp was weak, unlike the strong bond formed by MDP to HAp. Due to its high hydrophilicity, GPDM might be an adequate monomer for an etch-and-rinse adhesive, but appears less appropriate for a 'mild' self-etch adhesive that besides micro-retention ionically interacts with HAp, or for a self-adhesive restorative material. Copyright © 2018 The Academy of Dental Materials. Published by Elsevier Inc. All rights reserved.

Hierarchical micro-nano structured Ti6Al4V surface topography via two-step etching process for enhanced hydrophilicity and osteoblastic responses.

PubMed

Moon, Byeong-Seok; Kim, Sungwon; Kim, Hyoun-Ee; Jang, Tae-Sik

2017-04-01

Hierarchical micro-nano (HMN) surface structuring of dental implants is a fascinating strategy for achieving fast and mechanically stable fixation due to the synergetic effect of micro- and nano-scale surface roughness with surrounding tissues. However, the introduction of a well-defined nanostructure on a microstructure having complex surface geometry is still challenging. As a means of fabricating HMN surface on Ti6Al4V-ELI, target-ion induced plasma sputtering (TIPS) was used onto a sand-blasted, large-grit and acid-etched substrate. The HMN surface topography was simply controlled by adjusting the tantalum (Ta) target power of the TIPS technique, which is directly related to the Ta ion flux and the surface chemical composition of the substrate. Characterization using scanning electron microscopy (SEM), transmission electron microscopy (TEM), and laser scanning microscopy (LSM) verified that well-defined nano-patterned surface structures with a depth of ~300 to 400nm and a width of ~60 to 70nm were uniformly distributed and followed the complex micron-sized surface geometry. In vitro cellular responses of pre-osteoblast cells (MC3T3-E1) were assessed by attachment and proliferation of cells on flat, nano-roughened, micro-roughened, and an HMN surface structure of Ti6Al4V-ELI. Moreover, an in vivo dog mandible defect model study was used to investigate the biological effect of the HMN surface structure compared with the micro-roughened surface. The results showed that the surface nanostructure significantly increased the cellular activities of flat and micro-roughened Ti, and the bone-to-implant contact area and new bone volume were significantly improved on the HMN surface structured Ti. These results support the idea that an HMN surface structure on Ti6Al4V-ELI alloy has great potential for enhancing the biological performance of dental implants. Copyright © 2016 Elsevier B.V. All rights reserved.

Inhibition of demineralization around the enamel-dentin/restoration interface after dentin pretreatment with TiF4 and self-etching adhesive systems.

PubMed

Bridi, Enrico Coser; do Amaral, Flávia Lucisano Botelho; França, Fabiana Mantovani Gomes; Turssi, Cecilia Pedroso; Basting, Roberta Tarkany

2016-05-01

The objective of this study was to evaluate the inhibition of demineralization around enamel-dentin/restoration interface after dentin pretreatment with 2.5% titanium tetrafluoride (TiF4). Forty dental class V cavities at the cementoenamel junction were distributed into four groups (n = 10), according to the presence or absence of TiF4 and to the adhesive system (Clearfil SE Bond/CL and Adper EasyOne/AD), and restored with a resin composite. A dynamic pH cycling model was used to induce the development of artificial caries lesions. After sectioning the dental blocks, Knoop microhardness tests were performed at different depths (20, 40, and 60 μm from the occlusal margin of the restoration) and at different distances (100, 200, and 300 μm from the adhesive interface). Repeated measures three-way analysis of variance (ANOVA) and Tukey's test were used (α = 0.05). For enamel, there were no differences in the microhardness values for CL, AD, and TiF4-AD at depths, regardless of the distances. Considering each depth, there were no significant differences among treatments. For dentin, ANOVA showed no significant interaction among the independent variables treatment*distance*depth (p = 0.994), no significant interaction between treatment*depth (p = 0.722), no significant interaction between treatment*distance (p = 0.265), no significant interaction between depth*distance (p = 0.365), and no significant effect on treatment (p = 0.151), depth (p = 0.067), or distance (p = 0.251). Dentin pretreatment of the cavity walls with TiF4 before self-etching adhesive systems was not effective in inhibiting demineralization around the enamel-dentin/restoration interfaces. The mechanism of incorporating fluoride in enamel and dentin of the cavity walls to inhibit demineralization around restorations seems ineffective when using TiF4 as a dentin pretreatment.

Circummandibular Wires for Treatment of Dentoalveolar Fractures Adjacent to Edentulous Areas: A Report of Two Cases.

PubMed

Maloney, Karl

2015-09-01

In general, dentoalveolar fractures are a common injury seen in emergency departments, dental offices, and oral and maxillofacial surgery practices. These injuries can be the result of direct trauma or indirect trauma. Direct trauma more often causes trauma to the maxillary dentition due to the exposure of the maxillary anterior teeth. Indirect trauma is usually the result of forced occlusion secondary to a blow to the chin or from a whiplash injury. Falls are the most common mechanism of injury seen in the pediatric group. In adolescents, many of these fractures are sustained during sporting activities. However, the use of mouth guards and other protective equipment has decreased this number. Most adult injuries are caused by motor vehicle accidents, contact sports, falls, bicycles, interpersonal violence, medical/dental mishaps, and industrial accidents. Early intervention to reduce and stabilize the fracture is required to establish a bony union and ensure correct function. Most dentoalveolar fractures have bilateral stable adjacent dentition and are treated with a closed technique utilizing an acid-etch/resin splint followed by splint removal at 4 weeks. Other inferior stabilization treatments used are arch bars and other wiring techniques. It is widely accepted that semirigid stabilization techniques, such as an acid-etch/resin splint or wiring procedures, are adequate to treat dentoalveolar fractures. This is in contrast to the treatment of mandible fractures where AO principles of rigid fixation are often followed. Fractures that are unable to be reduced sometimes necessitate an open reduction followed by internal fixation, sometimes using a secondary splint for mobile teeth. In those rare cases when there are not stable adjacent teeth bilaterally other modalities must be considered. In the present report, two cases are presented where circummandibular wires were used to treat fractured mandibular dentoalveolar segments adjacent to edentulous areas.

Immediate performance of self-etching versus system adhesives with multiple light-activated restoratives.

PubMed

Irie, M; Suzuki, K; Watts, D C

2004-11-01

The purpose of this study was to evaluate the performance of both single and double applications of (Adper Prompt L-Pop) self-etching dental adhesive, when used with three classes of light-activated restorative materials, in comparison to the performance of each restorative system adhesive. Evaluation parameters to be considered for the adhesive systems were (a) immediate marginal adaptation (or gap formation) in tooth cavities, (b) free setting shrinkage-strain determined by the immediate marginal gap-width in a non-bonding Teflon cavity, and (c) their immediate shear bond-strengths to enamel and to dentin. The maximum marginal gap-width and the opposing-width (if any) in the tooth cavities and in the Teflon cavities were measured immediately (3 min) after light-activation. The shear bond-strengths to enamel and to dentin were also measured at 3 min. For light-activated restorative materials during early setting (<3 min), application of Adper Prompt L-Pop exhibited generally superior marginal adaptation to most system adhesives. But there was no additional benefit from double application. The marginal-gaps in tooth cavities and the marginal-gaps in Teflon cavities were highly correlated (r = 0.86-0.89, p < 0.02-0.01). For enamel and dentin shear bond-strengths, there were no significant differences between single and double applications, for all materials tested except Toughwell and Z 250 with enamel. Single application of a self-etch adhesive was a feasible and beneficial alternative to system adhesives for several classes of restorative. Marginal gap-widths in tooth cavities correlated more strongly with free shrinkage-strain magnitudes than with bond-strengths to tooth structure.

The effect of dimethyl sulfoxide (DMSO) on dentin bonding and nanoleakage of etch-and-rinse adhesives.

PubMed

Tjäderhane, Leo; Mehtälä, Pekka; Scaffa, Polliana; Vidal, Cristina; Pääkkönen, Virve; Breschi, Lorenzo; Hebling, Josimeri; Tay, Franklin R; Nascimento, Fabio D; Pashley, David H; Carrilho, Marcela R

2013-10-01

The objective was to examine the effect of a solvent dimethyl sulfoxide (DMSO) on resin-dentin bond durability, as well as potential functional mechanisms behind the effect. Microtensile bond strength (μTBS) was evaluated in extracted human teeth in two separate experiments. Dentin specimens were acid-etched and assigned to pre-treatment with 0.5mM (0.004%) DMSO as additional primer for 30s and to controls with water pre-treatment. Two-step etch-and-rinse adhesive (Scotchbond 1XT, 3M ESPE) was applied and resin composite build-ups were created. Specimens were immediately tested for μTBS or stored in artificial saliva for 6 and 12 months prior to testing. Additional immediate and 6-month specimens were examined for interfacial nanoleakage analysis under SEM. Matrix metalloproteinase (MMP) inhibition by DMSO was examined with gelatin zymography. Demineralized dentin disks were incubated in 100% DMSO to observe the optical clearing effect. The use of 0.5mM DMSO had no effect on immediate bond strength or nanoleakage. In controls, μTBS decreased significantly after storage, but increased significantly in DMSO-treated group. The control group had significantly lower μTBS than DMSO-group after 6 and 12 months. DMSO also eliminated the increase in nanoleakage seen in controls. 5% and higher DMSO concentrations significantly inhibited the gelatinases. DMSO induced optical clearing effect demonstrating collagen dissociation. DMSO as a solvent may be useful in improving the preservation of long-term dentin-adhesive bond strength. The effect may relate to dentinal enzyme inhibition or improved wetting of collagen by adhesives. The collagen dissociation required much higher DMSO concentrations than the 0.5mM DMSO used for bonding. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Immediate occlusal loading of double acid-etched surface titanium implants in 41 consecutive full-arch cases in the mandible and maxilla: 6- to 74-month results.

PubMed

Ibañez, Juan C; Tahhan, Marcelo J; Zamar, Juan A; Menendez, Alicia B; Juaneda, Agustina M; Zamar, Nicolas J; Monqaut, Jose L

2005-11-01

The high success rate of dental implants has changed the quality of life for many patients. Immediate loading finds its application in some clinical cases and certainly adds another modality of treatment for the implant patient. Starting with a few implants immediately loaded with a bar overdenture in the mandible, the concept of immediate loading evolved to loading multiple implants in both the maxilla and mandible. In this investigation, 41 consecutive patients who needed full-arch restorations were treated with 343 double acid-etched surface implants between May 1998 and March 2004. The sample included smokers and bruxers. Twenty-three mandibular and 26 maxillary cases were treated, loading the implants within 48 hours, by using resin provisional prostheses, metal-reinforced provisional prostheses, or definitive prostheses (metal-acrylic or metal-ceramic). All implants were followed for 12 to 74 months. Follow-up consisted of clinical as well as radiographic examination. Furthermore, resonance frequency analysis was done in most of the implants during the last 2 years. The success rate obtained was 99.42% (only two mandibular implants that are still surviving were considered failures). The bone level was measured every year. The average radiographic bone level change was 0.56 mm at 12, 0.76 mm at 24, 0.84 mm at 36, 0.82 mm at 48, 0.83 mm at 60, and 0.94 mm at 72 months. A high success rate can be achieved when double acid-etched surface implants are immediately loaded with fixed full-arch restorations in the maxilla and mandible.

Microtensile bond strength analysis of different adhesive systems and dentin prepared with high-speed and Er:YAG laser: a comparative study.

PubMed

Oliveira, Denise Cerqueira; Manhães, Lussara Azevedo; Marques, Márcia Martins; Matos, Adriana Bona

2005-04-01

The aim of this study was to evaluate the bond strength of two adhesive systems (Single Bond and Clearfil SE Bond) subjected or not to a thermocycling procedure and applied to cavities prepared either with high-speed diamond bur or Er:YAG laser. One of the possible applications of dental lasers includes increasing the quality of bond strength. This in vitro study was carried out using a microtensile test on 16 bovine teeth, divided into eight groups. Cavities were prepared on superficial dentin of the medium portion of the buccal surface. After application of adhesive systems, composite restorations were performed at 5-mm height. After 24 h, four groups of teeth were immersed in water, and the other four were thermocycled. Bonded specimens were sectioned into serial 1x1-mm beams, which were subjected to a microtensile test. Final values of bond strength were measured, expressed in MPa, and statistically analyzed. Results were as follows: G1 (26.281 +/- 5.454 MPa); G2 (10.965 +/- 3.714 MPa); G3 (18.549 +/- 6.113 MPa); G4 (14.295 +/- 3.806 MPa); G5 (18.225 +/- 5.701 MPa); G6 (5.588 +/- 2.211 MPa); G7 (18.256 +/- 3.819 MPa); and G8 (15.423 +/- 4.714 MPa). Self-etching adhesive system (SE) produced more stable bond strength results than the system that indicates total etching (SB). For dentin prepared at high speed, the total etching adhesive system was more indicated, whereas Er:YAG laser-preparation dentin was not influenced by the adhesive system. The thermocycling procedure could negatively affect microtensile bond strength of both adhesive systems, being more deleterious to SB than to SE.

Effect of a new desensitizing material on human dentin permeability.

PubMed

Rusin, Richard P; Agee, Kelli; Suchko, Michael; Pashley, David H

2010-06-01

Resin-modified glass ionomers (RMGI) have demonstrated clinical success providing immediate and long-term relief from root sensitivity. RMGIs have been recently introduced as paste-liquid systems for convenience of clinical usage. The objective of this study was to measure the ability of a new paste-liquid RMGI to reduce fluid flow through human dentin, compared to an established single-bottle nanofilled total etch resin adhesive indicated for root desensitization. Dentin permeability was measured on human crown sections on etched dentin, presenting a model for the exposed tubules typical of root sensitivity, and permitting measurement of the maximum permeability. In the first two groups, the etched dentin was coated with either the RMGI or adhesive, and permeability measured on the coated dentin. In a third group, a smear layer was created on the dentin with sandpaper, then the specimens were coated with the RMGI; permeability was measured on the smeared and coated dentin. Specimens from each group were sectioned and examined via scanning electron microscopy (SEM). Both the resin adhesive and the new paste-liquid RMGI protective material significantly reduced fluid flow through dentin, and exhibited excellent seal on dentin with either open tubules or smear-layer occluded tubules. The RMGI infiltrated the smear layer with resin during placement, penetrated dentin tubules, and formed resin tags. The RMGI was equivalent to the adhesive in its ability to reduce fluid flow and seal dentin. It is therefore concluded that the new RMGI and the adhesive show the potential to offer excellent sensitivity relief on exposed root dentin. Copyright (c) 2010 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

The application of ozone in dentistry: a systematic review of literature.

PubMed

Azarpazhooh, Amir; Limeback, Hardy

2008-02-01

(1) To systematically review the clinical application and remineralization potentials of ozone in dentistry; (2) To summarize the available in vitro applications of ozone in dentistry. Ovid MEDLINE, CINAHL, etc. (up to April 2007). In vitro or in vivo English language publications, original studies, and reviews were included. Conference papers, abstracts, and posters were excluded. In vitro: Good evidence of ozone biocompatibility with human oral epithelial cells, gingival fibroblast, and periodontal cells; Conflicting evidence of antimicrobial efficacy of ozone but some evidence that ozone is effective in removing the microorganisms from dental unit water lines, the oral cavity, and dentures; Conflicting evidence for the application of ozone in endodontics; Insufficient evidence for the application of ozone in oral surgery and implantology; Good evidence of the prophylactic application of ozone in restorative dentistry prior to etching and the placement of dental sealants and restorations. In vivo: Despite the promising in vitro evidence, the clinical application of ozone in dentistry (so far in management of dental and root caries) has not achieved a strong level of efficacy and cost-effectiveness. While laboratory studies suggest a promising potential of ozone in dentistry, this has not been fully realised in clinical studies to date. More well designed and conducted double-blind randomised clinical trials with adequate sample size, limited or no loss to follow up, and carefully standardised methods of measurement and analyses are needed to evaluate the possible use of ozone as a treatment modality in dentistry.

[Comperative study of implant surface characteristics].

PubMed

Katona, Bernadett; Daróczi, Lajos; Jenei, Attila; Bakó, József; Hegedus, Csaba

2013-12-01

The osseointegration between the implant and its' bone environment is very important. The implants shall meet the following requirements: biocompatibility, rigidity, resistance against corrosion and technical producibility. In our present study surface morphology and material characteristics of different implants (Denti Bone Level, Denti Zirconium C, Bionika CorticaL, Straumann SLA, Straumann SLA Active, Dentsply Ankylos and Biotech Kontact implant) were investigated with scanning electron microscopy and energy-dispersive X-ray spectroscopy. The possible surface alterations caused by the manufacturing technology were also investigated. During grit-blasting the implants' surface is blasted with hard ceramic particles (titanium oxide, alumina, calcium phosphate). Properties of blasting material are critical because the osseointegration of dental implants should not be hampered. The physical and chemical features of blasting particles could importantly affect the produced surfaces of implants. Titanium surfaces with micro pits are created after immersion in mixtures of strong acids. On surfaces after dual acid-etching procedures the crosslinking between fibrin and osteogenetic cells could be enhanced therefore bone formation could be directly facilitated on the surface of the implant. Nowadays there are a number of surface modification techniques available. These can be used as a single method or in combination with each other. The effect of the two most commonly used surface modifications (acid-etching and grit-blasting) on different implants are demonstrated in our investigation.

Evaluation of microtensile bond strength of different fissure sealants to bovine enamel.

PubMed

Sen Tunc, E; Bayrak, S; Tuloglu, N; Ertas, E

2012-03-01

The aim of this study was to evaluate the microtensile bond strength (μTBS) of a new fissure sealant and compare it with conventional sealants which are applied to enamel alone, and also with self-etch and etch-and-rinse adhesives. Enamel specimens were prepared and randomly distributed into three groups according to fissure sealant (Aegis, Helioseal F, Helioseal Clear). Each group was then subdivided according to adhesive system (Clearfil S3, Single Bond, no adhesive). A universal testing machine was used to measure μTBS, and data were analysed using one-way ANOVA and Tukey's tests. μTBS values for all Aegis subgroups were significantly lower than for comparable Helioseal F and Helioseal Clear subgroups (p < 0.05). No differences were observed in μTBS of Helioseal F and Helioseal Clear (p > 0.05). In the Helioseal Clear group, μTBS values for Single Bond were significantly higher than for Clearfil S3 (p < 0.05). However, no significant differences were found between the μTBS values of the adhesive subgroups in the Aegis or Helioseal F groups (p > 0.05). Sealant μTBS values may be affected by material content. The addition of an adhesive may improve μTBS values of sealant to enamel. © 2012 Australian Dental Association.

Characterization of a human tooth with carious lesions using conventional and synchrotron radiation-based micro computed tomography

NASA Astrophysics Data System (ADS)

Dziadowiec, Iwona; Beckmann, Felix; Schulz, Georg; Deyhle, Hans; Müller, Bert

2014-09-01

In a dental office, every day X rays of teeth within the oral cavity are obtained. Caries induces a mineral loss and, therefore, becomes visible by reduced X-ray absorption. The detailed spatial distribution of the mineral loss, however, is inaccessible in conventional dental radiology, since the dose for such studies is intolerable. As a consequence, such measurements can only be performed after tooth extraction. We have taken advantage of synchrotron radiation-based micro computed tomography to characterize a human tooth with a rather small, natural caries lesion and an artificially induced lesion provoked by acidic etching. Both halves of the tooth were separately visualized from 2400 radiographs recorded at the beam line P07 / PETRA III (HASYLAB at DESY, Hamburg, Germany) with an asymmetric rotation axis at photon energy of 45 keV. Because of the setup, one finds an energy shift in the horizontal plane, to be corrected. After the appropriate three-dimensional registration of the data with the ones of the same crown using the better accessible phoenix nanotom® m of General Electric, Wunstorf, Germany, one can determine the joint histogram, which enable to calibrate the system with the conventional X-ray source.

Direct Midline Diastema Closure with Composite Layering Technique: A One-Year Follow-Up.

PubMed

Korkut, Bora; Yanikoglu, Funda; Tagtekin, Dilek

2016-01-01

Objective. Maxillary anterior spacing is a common aesthetic complaint of patients. Midline diastema has a multifactorial etiology such as labial frenulum, microdontia, mesiodens, peg-shaped lateral incisors, agenesis, cysts, habits such as finger sucking, tongue thrusting, or lip sucking, dental malformations, genetics, proclinations, dental-skeletal discrepancies, and imperfect coalescence of interdental septum. Appropriate technique and material for effective treatment are based on time, physical, psychological, and economical limitations. Direct composite resins in diastema cases allow dentist and patient complete control of these limitations and formation of natural smile. Clinical Considerations. In this case report a maxillary midline diastema was closed with direct composite resin restorations in one appointment without any preparation. One bottle total etch adhesive was used and translucent/opaque composite resin shades were layered on mesial surfaces of the teeth that were isolated with rubber dam and Teflon bands. Finishing and polishing procedures were achieved by using polishing discs. Patient was informed for recalls for every 6 months. Conclusions. At one-year recall no sensitivities, discolorations, or fractures were detected on teeth and restorations. Direct composite resins seemed to be highly aesthetic and durable restorations that can satisfy patients as under the conditions of case presented.

New Coating Technique of Ceramic Implants with Different Glass Solder Matrices for Improved Osseointegration-Mechanical Investigations.

PubMed

Mick, Enrico; Markhoff, Jana; Mitrovic, Aurica; Jonitz, Anika; Bader, Rainer

2013-09-11

Ceramics are a very popular material in dental implant technology due to their tribological properties, their biocompatibility and their esthetic appearance. However, their natural surface structure lacks the ability of proper osseointegration, which constitutes a crucial process for the stability and, thus, the functionality of a bone implant. We investigated the application of a glass solder matrix in three configurations-consisting mainly of SiO₂, Al₂O₃, K₂O and Na₂O to TZP-A ceramic specimens. The corresponding adhesive strength and surface roughness of the coatings on ceramic specimens have been analyzed. Thereby, high adhesive strength (70.3 ± 7.9 MPa) was found for the three different coatings. The obtained roughness (R z ) amounted to 18.24 ± 2.48 µm in average, with significant differences between the glass solder configurations. Furthermore, one configuration was also tested after additional etching which did not lead to significant increase of surface roughness (19.37 ± 1.04 µm) or adhesive strength (57.2 ± 5.8 MPa). In conclusion, coating with glass solder matrix seems to be a promising surface modification technique that may enable direct insertion of ceramic implants in dental and orthopaedic surgery.

Reality of Dental Implant Surface Modification: A Short Literature Review

PubMed Central

Yeo, In-Sung

2014-01-01

Screw-shaped endosseous implants that have a turned surface of commercially pure titanium have a disadvantage of requiring a long time for osseointegration while those implants have shown long-term clinical success in single and multiple restorations. Titanium implant surfaces have been modified in various ways to improve biocompatibility and accelerate osseointegration, which results in a shorter edentulous period for a patient. This article reviewed some important modified titanium surfaces, exploring the in vitro, in vivo and clinical results that numerous comparison studies reported. Several methods are widely used to modify the topography or chemistry of titanium surface, including blasting, acid etching, anodic oxidation, fluoride treatment, and calcium phosphate coating. Such modified surfaces demonstrate faster and stronger osseointegration than the turned commercially pure titanium surface. However, there have been many studies finding no significant differences in in vivo bone responses among the modified surfaces. Considering those in vivo results, physical properties like roughening by sandblasting and acid etching may be major contributors to favorable bone response in biological environments over chemical properties obtained from various modifications including fluoride treatment and calcium phosphate application. Recently, hydrophilic properties added to the roughened surfaces or some osteogenic peptides coated on the surfaces have shown higher biocompatibility and have induced faster osseointegration, compared to the existing modified surfaces. However, the long-term clinical studies about those innovative surfaces are still lacking. PMID:25400716

In vitro and in vivo evaluation of SLA titanium surfaces with further alkali or hydrogen peroxide and heat treatment.

PubMed

Zhang, E W; Wang, Y B; Shuai, K G; Gao, F; Bai, Y J; Cheng, Y; Xiong, X L; Zheng, Y F; Wei, S C

2011-04-01

The present study aimed to evaluate the bioactivity of titanium surfaces sandblasted with large-grit corundum and acid etched (SLA) plus further alkali or hydrogen peroxide and heat treatment for dental implant application. Pure titanium disks were mechanically polished as control surface (Ti-control) and then sandblasted with large-grit corundum and acid etched (SLA). Further chemical modifications were conducted using alkali and heat treatment (ASLA) and hydrogen peroxide and heat treatment (HSLA) alternatively. The surface properties were characterized by scanning electron microscopy (SEM), x-ray photoelectron spectroscopy (XPS), and contact angle and roughness measurements. Further evaluation of surface bioactivity was conducted by MC3T3-E1 cell attachment, proliferation, morphology, alkaline phosphatase (ALP) activity and calcium deposition on the sample surfaces. After insertion in the beagle's mandibula for a specific period, cylindrical implant samples underwent micro-CT examination and then histological examination. It was found that ASLA and HSLA surfaces significantly increased the surface wettability and MC3T3-E1 cell attachment percentage, ALP activity and the quality of calcium deposition in comparison with simple SLA and Ti-control surfaces. Animal studies showed good osseointegration of ASLA and HSLA surfaces with host bone. In conclusion, ASLA and HSLA surfaces enhanced the bioactivity of the traditional SLA surface by integrating the advantages of surface topography, composition and wettability.

Loading capacity of zirconia implant supported hybrid ceramic crowns.

PubMed

Rohr, Nadja; Coldea, Andrea; Zitzmann, Nicola U; Fischer, Jens

2015-12-01

Recently a polymer infiltrated hybrid ceramic was developed, which is characterized by a low elastic modulus and therefore may be considered as potential material for implant supported single crowns. The purpose of the study was to evaluate the loading capacity of hybrid ceramic single crowns on one-piece zirconia implants with respect to the cement type. Fracture load tests were performed on standardized molar crowns milled from hybrid ceramic or feldspar ceramic, cemented to zirconia implants with either machined or etched intaglio surface using four different resin composite cements. Flexure strength, elastic modulus, indirect tensile strength and compressive strength of the cements were measured. Statistical analysis was performed using two-way ANOVA (p=0.05). The hybrid ceramic exhibited statistically significant higher fracture load values than the feldspar ceramic. Fracture load values and compressive strength values of the respective cements were correlated. Highest fracture load values were achieved with an adhesive cement (1253±148N). Etching of the intaglio surface did not improve the fracture load. Loading capacity of hybrid ceramic single crowns on one-piece zirconia implants is superior to that of feldspar ceramic. To achieve maximal loading capacity for permanent cementation of full-ceramic restorations on zirconia implants, self-adhesive or adhesive cements with a high compressive strength should be used. Copyright © 2015 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Erosive effects of common beverages on extracted premolar teeth.

PubMed

Seow, W K; Thong, K M

2005-09-01

Dental erosion is highly prevalent today, and acidic drinks are thought to be an important cause. The aim of the present investigation was to determine the erosive potential of a range of common beverages on extracted human teeth. The beverages were tested for their individual pHs using a pH meter. The clinical effects of the most erosive beverages were determined by the degree of etching and Vickers microhardness of enamel. The results showed that many common beverages have pHs sufficiently low to cause enamel erosion. Lime juice concentrate (pH 2.1) had the lowest pH, followed by Coca-cola and Pepsi (both with pH 2.3) and Lucozade (pH 2.5). The erosive potential of these beverages was demonstrated by the deep etching of the enamel after five minutes. The Vickers Hardness of enamel was reduced by about 50 per cent in the case of lime juice (p < 0.001) and 24 per cent in the case of Coca-cola (p < 0.004). Addition of saliva to 50 per cent (v/v) of Coca-cola completely reversed the erosive effects on the enamel. Although only a few of the beverages with the lowest pHs were tested, the present study showed that the most acidic drinks had the greatest erosive effects on enamel. While saliva was protective against erosion, relatively large volumes were required to neutralize the acidity.

[Effects of different surface conditioning agents on the bond strength of resin-opaque porcelain composite].

PubMed

Liu, Wenjia; Fu, Jing; Liao, Shuang; Su, Naichuan; Wang, Hang; Liao, Yunmao

2014-04-01

The objective of this research is to evaluate the effects of different silane coupling agents on the bond strength between Ceramco3 opaque porcelain and indirect composite resin. Five groups of Co-Cr metal alloy substrates were fabricated according to manufacturer's instruction. The surface of metal alloy with a layer of dental opaque porcelain was heated by fire. After the surface of opaque porcelain was etched, five different surface treatments, i.e. RelyX Ceramic Primer (RCP), Porcelain Bond Activator and SE Bond Primer (mixed with a proportion of 1:1) (PBA), Shofu Porcelain Primer (SPP), SE bond primer (SEP), and no primer treatment (as a control group), were used to combine P60 and opaque porcelain along with resin cement. Shear bond strength of specimens was tested in a universal testing machine. The failure modes of specimens in all groups were observed and classified into four types. Selected specimens were subjected to scanning electron microscope and energy disperse spectroscopy to reveal the relief of the fracture surface and to confirm the failure mode of different types. The experimental results showed that the values of the tested items in all the tested groups were higher than that in the control group. Group PBA exhibited the highest value [(37.52 +/- 2.14) MPa] and this suggested a fact that all of the specimens in group PBA revealed combined failures (failure occurred in metal-porcelain combined surface and within opaque porcelain). Group SPP and RCP showed higher values than SEP (P < 0.05) and most specimens of SPP and RCP performed combined failures (failure occurred in bond surface and within opaque porcelain or composite resin) while all the specimens in group SEP and control group revealed adhesive failures. Conclusions could be drawn that silane coupling agents could reinforce the bond strength of dental composite resin to metal-opaque porcelain substrate. The bond strength between dental composite resin and dental opaque porcelain could meet the clinical requirements.

Paucity of Nanolayering in Resin-Dentin Interfaces of MDP-based Adhesives.

PubMed

Tian, F; Zhou, L; Zhang, Z; Niu, L; Zhang, L; Chen, C; Zhou, J; Yang, H; Wang, X; Fu, B; Huang, C; Pashley, D H; Tay, F R

2016-04-01

Self-assembled nanolayering structures have been reported in resin-dentin interfaces created by adhesives that contain 10-methacryloyloxydecyl dihydrogen phosphate (10-MDP). These structures have been hypothesized to contribute to bond durability. The objective of the present study was to determine the extent of nanolayering in resin-dentin interfaces after application of commercialized 10-MDP-containing self-etch and universal adhesives to human dentin. Seven commercialized adhesives were examined: Adhese Universal (Ivoclar-Vivadent), All-Bond Universal (Bisco, Inc.), Clearfil SE Bond 2, Clearfil S3 Bond Plus, Clearfil Universal Bond (all from Kuraray Noritake Dental Inc.), G-Premio Bond (GC Corp.), and Scotchbond Universal (3M ESPE). Each adhesive was applied in the self-etch mode on midcoronal dentin according to the respective manufacturer's instructions. Bonded specimens (n = 6) were covered with flowable resin composite, processed for transmission electron microscopy, and examined at 30 random sites without staining. Thin-film glancing angle X-ray diffraction (XRD) was used to detect the characteristic peaks exhibited by nanolayering (n = 4). The control consisted of 15%wt, 10%wt, and 5%wt 10-MDP (DM Healthcare Products, Inc.) dissolved in a mixed solvent (ethanol and water weight ratio 9:8, with photoinitiators). Experimental primers were applied to dentin for 20 s, covered with hydrophobic resin layer, and examined in the same manner. Profuse nanolayering with highly ordered periodicity (~3.7 nm wide) was observed adjacent to partially dissolved apatite crystallites in dentin treated with the 15% 10-MDP primer. Three peaks in the 2θ range of 2.40° (3.68 nm), 4.78° (1.85 nm), and 7.18° (1.23 nm) were identified from thin-film XRD. Reduction in the extent of nanolayering was observed in the 10% and 5% 10-MDP experimental primer-dentin interface along with lower intensity XRD peaks. Nanolayering and characteristic XRD peaks were rarely observed in specimens prepared from the commercialized adhesives. The sparsity of nanolayering in resin-dentin interfaces created by commercialized adhesives challenges its clinical effectiveness as a mechanism for improving bond longevity in dentin bonding. © International & American Associations for Dental Research 2015.

Efficacy of standard (SLA) and modified sandblasted and acid-etched (SLActive) dental implants in promoting immediate and/or early occlusal loading protocols: a systematic review of prospective studies.

PubMed

Chambrone, Leandro; Shibli, Jamil Awad; Mercúrio, Carlos Eduardo; Cardoso, Bruna; Preshaw, Philip M

2015-04-01

To assess the survival percentage, clinical and radiographic outcomes of sandblasted and acid-etched (SLA) dental implants and its modified surface (SLActive) in protocols involving immediate and early occlusal loading. MEDLINE, EMBASE and the Cochrane Oral Health Group's Trials Register CENTRAL were searched in duplicate up to, and including, June 2013 to include randomised controlled trials (RCTs) and prospective observational studies of at least 6-month duration published in all languages. Studies limited to patients treated with SLA and/or SLActive implants involving a treatment protocol describing immediate and early loading of these implants were eligible for inclusion. Data on clinical and/or radiographic outcomes following implant placement were considered for inclusion. Of the 447 potentially eligible publications identified by the search strategy, seven RCTs comprising a total of 853 implants (8% titanium plasma-sprayed, 41.5% SLA and 50.5% SLActive) and 12 prospective observational studies including 1394 SLA and 145 SLActive implants were included in this review. According to the Cochrane Collaboration's tool for assessing risk of bias, one of the studies was considered to be at a low risk of bias, whereas the remaining studies were considered to be at an unclear risk. Regarding the observational studies, all of them presented a medium methodological quality based on the Modified Newcastle-Ottawa scale. There were no significant differences reported in the studies in relation to implant loss or clinical parameters between the immediate/early loading and delayed loading protocols. Overall, 95% of SLA and 97% of SLActive implants still survive at the end of follow-up. Despite of the positive findings achieved by the included studies, few RCTs were available for analysis for SLActive implants. Study heterogeneity, scarcity of data and the lack of pooled estimates represent a limitation between studies' comparisons and should be considered when interpreting the present findings. © 2014 John Wiley & Sons A/S. Published by John Wiley & Sons Ltd.

Introducing etch kernels for efficient pattern sampling and etch bias prediction

NASA Astrophysics Data System (ADS)

Weisbuch, François; Lutich, Andrey; Schatz, Jirka

2018-01-01

Successful patterning requires good control of the photolithography and etch processes. While compact litho models, mainly based on rigorous physics, can predict very well the contours printed in photoresist, pure empirical etch models are less accurate and more unstable. Compact etch models are based on geometrical kernels to compute the litho-etch biases that measure the distance between litho and etch contours. The definition of the kernels, as well as the choice of calibration patterns, is critical to get a robust etch model. This work proposes to define a set of independent and anisotropic etch kernels-"internal, external, curvature, Gaussian, z_profile"-designed to represent the finest details of the resist geometry to characterize precisely the etch bias at any point along a resist contour. By evaluating the etch kernels on various structures, it is possible to map their etch signatures in a multidimensional space and analyze them to find an optimal sampling of structures. The etch kernels evaluated on these structures were combined with experimental etch bias derived from scanning electron microscope contours to train artificial neural networks to predict etch bias. The method applied to contact and line/space layers shows an improvement in etch model prediction accuracy over standard etch model. This work emphasizes the importance of the etch kernel definition to characterize and predict complex etch effects.

A quantitative method to measure biofilm removal efficiency from complex biomaterial surfaces using SEM and image analysis

NASA Astrophysics Data System (ADS)

Vyas, N.; Sammons, R. L.; Addison, O.; Dehghani, H.; Walmsley, A. D.

2016-09-01

Biofilm accumulation on biomaterial surfaces is a major health concern and significant research efforts are directed towards producing biofilm resistant surfaces and developing biofilm removal techniques. To accurately evaluate biofilm growth and disruption on surfaces, accurate methods which give quantitative information on biofilm area are needed, as current methods are indirect and inaccurate. We demonstrate the use of machine learning algorithms to segment biofilm from scanning electron microscopy images. A case study showing disruption of biofilm from rough dental implant surfaces using cavitation bubbles from an ultrasonic scaler is used to validate the imaging and analysis protocol developed. Streptococcus mutans biofilm was disrupted from sandblasted, acid etched (SLA) Ti discs and polished Ti discs. Significant biofilm removal occurred due to cavitation from ultrasonic scaling (p < 0.001). The mean sensitivity and specificity values for segmentation of the SLA surface images were 0.80 ± 0.18 and 0.62 ± 0.20 respectively and 0.74 ± 0.13 and 0.86 ± 0.09 respectively for polished surfaces. Cavitation has potential to be used as a novel way to clean dental implants. This imaging and analysis method will be of value to other researchers and manufacturers wishing to study biofilm growth and removal.

Effects of different black mediators on the shear strength of orthodontic bracket to the enamel treated with Nd-Yag laser

NASA Astrophysics Data System (ADS)

Huang, Shun-Te; Lin, I.-Shueng; Tsai, Chi-Cheng

1995-04-01

The Nd:YAG laser has ablation, crack, and crater effects on the dental enamel through black mediators which are very similar to the acid etching effects of phosphoric acid. This study was designed for searching how the different black mediators influence the shear strengths of the brackets bound to the enamel surfaces which were treated with the Nd:YAG laser. 90 bovine enamels divided into 5 groups were painted with 5 kinds of black mediators including Chinese ink, oil ink, black ball pen, water ink and black transfer paper. The enamel surfaces painted with black mediators were then radiated by Nd:YAG laser (ADL; American Dental Laser 300dl, power: 20 pps, 87.5 mj). Orthodontic brackets were bonded to the radiated surfaces. Then the shear strengths of the brackets to the enamels were measured by Instron. The results showed that the Chinese ink group and oil ink group has the strongest shear strength, ball pen group and water ink group showed the second strength, and the transfer paper group has the lowest shear strength. In addition, scanning electronic microscope also was used to observe the topographic changes of the enamel surfaces induced by the laser ablation.

Osseointegration mechanisms: a proteomic approach.

PubMed

Araújo-Gomes, N; Romero-Gavilán, F; García-Arnáez, I; Martínez-Ramos, C; Sánchez-Pérez, A M; Azkargorta, M; Elortza, F; de Llano, J J Martín; Gurruchaga, M; Goñi, I; Suay, J

2018-05-01

The prime objectives in the development of biomaterials for dental applications are to improve the quality of osseointegration and to short the time needed to achieve it. Design of implants nowadays involves changes in the surface characteristics to obtain a good cellular response. Incorporating osteoinductive elements is one way to achieve the best regeneration possible post-implantation. This study examined the osteointegrative potential of two distinct biomaterials: sandblasted acid-etched titanium and a silica sol-gel hybrid coating, 70% MTMOS-30% TEOS. In vitro, in vivo, and proteomic characterisations of the two materials were conducted. Enhanced expression levels of ALP and IL-6 in the MC3T3-E1 cells cultured with coated discs, suggest that growing cells on such surfaces may increase mineralisation levels. 70M30T-coated implants showed improved bone growth in vivo compared to uncoated titanium. Complete osseointegration was achieved on both. However, coated implants displayed osteoinductive properties, while uncoated implants demonstrated osteoconductive characteristics. Coagulation-related proteins attached predominantly to SAE-Ti surface. Surface properties of the material might drive the regenerative process of the affected tissue. Analysis of the proteins on the coated dental implant showed that few proteins specifically attached to its surface, possibly indicating that its osteoinductive properties depend on the silicon delivery from the implant.

Thermal effects associated with the Nd/YAG dental laser.

PubMed

von Fraunhofer, J A; Allen, D J

1993-01-01

The heat produced at the dentinal pulpal wall opposite the irradiation site was measured during etching of dental enamel with an Nd:YAG laser in preparation for direct bonding of orthodontic appliances. Forty extracted human teeth were randomly divided into four groups of 10 teeth. Within each group, the buccal surfaces of 5 teeth and the lingual surfaces of the other 5 teeth were laser treated for 12 sec. Irradiation was performed with a commercial Nd:YAG laser at the power settings of 80mJ, 1W, 2W and 3W. Prior to irradiation, an occlusal access preparation was made into the pulp in order to facilitate the placement of a thermocouple for measurement of temperature changes at the dentinal pulpal wall opposite the irradiation site. The thermocouple was held against the dentinal pulpal wall and the resulting temperature changes were recorded. Heating effects at the dentinal pulpal wall on both buccal and lingual surfaces showed an increase in heat as a function of the increase in power output from the laser unit (p < 0.01). The temperatures measured at power levels 1-3W appeared to be of sufficient magnitude to cause at least localized pulpal inflammation and possible irreversible damage to the pulp tissue immediately opposite the site of laser irradiation.

A study on the compatibility between one-bottle dentin adhesives and composite resins using micro-shear bond strength.

PubMed

Song, Minju; Shin, Yooseok; Park, Jeong-Won; Roh, Byoung-Duck

2015-02-01

This study was performed to determine whether the combined use of one-bottle self-etch adhesives and composite resins from same manufacturers have better bond strengths than combinations of adhesive and resins from different manufacturers. 25 experimental micro-shear bond test groups were made from combinations of five dentin adhesives and five composite resins with extracted human molars stored in saline for 24 hr. Testing was performed using the wire-loop method and a universal testing machine. Bond strength data was statistically analyzed using two way analysis of variance (ANOVA) and Tukey's post hoc test. Two way ANOVA revealed significant differences for the factors of dentin adhesives and composite resins, and significant interaction effect (p < 0.001). All combinations with Xeno V (Dentsply De Trey) and Clearfil S(3) Bond (Kuraray Dental) adhesives showed no significant differences in micro-shear bond strength, but other adhesives showed significant differences depending on the composite resin (p < 0.05). Contrary to the other adhesives, Xeno V and BondForce (Tokuyama Dental) had higher bond strengths with the same manufacturer's composite resin than other manufacturer's composite resin. Not all combinations of adhesive and composite resin by same manufacturers failed to show significantly higher bond strengths than mixed manufacturer combinations.

Experimental etch-and-rinse adhesives doped with bioactive calcium silicate-based micro-fillers to generate therapeutic resin-dentin interfaces.

PubMed

Profeta, A C; Mannocci, F; Foxton, R; Watson, T F; Feitosa, V P; De Carlo, B; Mongiorgi, R; Valdré, G; Sauro, S

2013-07-01

This study aimed at evaluating the therapeutic bioactive effects on the bond strength of three experimental bonding agents containing modified Portland cement-based micro-fillers applied to acid-etched dentin and submitted to aging in simulated body fluid solution (SBS). Confocal laser (CLSM) and scanning electron microscopy (SEM) were also performed. A type-I ordinary Portland cement was tailored using different compounds such as sodium-calcium-aluminum-magnesium silicate hydroxide (HOPC), aluminum-magnesium-carbonate hydroxide hydrates (HCPMM) and titanium oxide (HPCTO) to create three bioactive micro-fillers. A resin blend mainly constituted by Bis-GMA, PMDM and HEMA was used as control (RES-Ctr) or mixed with each micro-filler to create three experimental bonding agents: (i) Res-HOPC, (ii) Res-HCPMM and (iii) Res-HPCTO. The bonding agents were applied onto 37% H3PO4-etched dentin and light-cured for 30s. After build-ups, they were prepared for micro-tensile bond strength (μTBS) and tested after 24h or 6 months of SBS storage. SEM analysis was performed after de-bonding, while CLSM was used to evaluate the ultra-morphology/nanoleakage and the mineral deposition at the resin-dentin interface. High μTBS values were achieved in all groups after 24h. Only Res-HOPC and Res-HCPMM showed stable μTBS after SBS storage (6 months). All the resin-dentin interfaces created using the bonding agents containing the bioactive micro-fillers tested in this study showed an evident reduction of nanoleakage and mineral deposition after SBS storage. Resin bonding systems containing specifically tailored Portland cement micro-fillers may promote a therapeutic mineral deposition within the hybrid layer and increase the durability of the resin-dentin bond. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of various surface treatment methods on the bond strength of the heat-pressed ceramic samples.

PubMed

Saraçoğlu, A; Cura, C; Cötert, H S

2004-08-01

This in vitro study was conducted to evaluate the interaction between the shear bond strength and the surface treatment method for a commercial dental ceramic. Ninety bonded ceramic units were manufactured for this study. Each unit was made by luting two cylinder-shaped ceramic samples to each other with a resin-composite luting agent. The units were then divided into nine groups, containing 10 units in each group. Samples from each group were treated with one of the following: etching with 4.9% hydrofluoric acid for 10, 20 and 40 s, 9.5% hydrofluoric acid for 10, 20 and 40 s, 40% orthophosphoric acid for 40 s, air abrasion with alumina in 50-microm particles, and grinding with a high-speed diamond bur. The treated samples were then silanated and luted with a resin-composite luting agent. The luted units were then loaded to failure. Two samples from each group were neither silanated nor luted after the surface treatment procedure, and morphological changes obtained by various surface treatment regimens were investigated by scanning electron microscopy. A statistically significant difference was observed among the mean shear bond strengths of the groups prepared with different surface treatment techniques (P = 0.00). Hydrofluoric acid appeared to be the most suitable chemical medium to produce a reliable ceramic bond. Etching time and concentration of the acidic medium were also observed as important prognostic variates. Orthophosphoric acid treatment was observed to be the least effective surface treatment method on the heat-pressed ceramic samples. Physical applications such as bur grinding and air blasting maintained stronger bonds than the orthophosphoric acid, while producing weaker bonds than surfaces treated with hydrofluoric acid in all concentrations and etching periods. The effect of the silane priming agent was not considered in this study. Copyright 2004 Blackwell Publishing Ltd.

Comparative histomorphometry and resonance frequency analysis of implants with moderately rough surfaces in a loaded animal model.

PubMed

Al-Nawas, B; Groetz, K A; Goetz, H; Duschner, H; Wagner, W

2008-01-01

Test of favourable conditions for osseointegration with respect to optimum bone-implant contact (BIC) in a loaded animal model. The varied parameters were surface roughness and surface topography of commercially available dental implants. Thirty-two implants of six types of macro and microstructure were included in the study (total 196). The different types were: minimally rough control: Branemark machined Mk III; oxidized surface: TiUnite MkIII and MkIV; ZL Ticer; blasted and etched surface: Straumann SLA; rough control: titanium plasma sprayed (TPS). Sixteen beagle dogs were implanted with the whole set of the above implants. After a healing period of 8 weeks, implants were loaded for 3 months. For the evaluation of the BIC areas, adequately sectioned biopsies were visualized by subsurface scans with confocal laser scanning microscopy (CLSM). The primary statistical analysis testing BIC of the moderately rough implants (mean 56.1+/-13.0%) vs. the minimally rough and the rough controls (mean 53.9+/-11.2%) does not reveal a significant difference (P=0.57). Mean values of 50-70% BIC were found for all implant types. Moderately rough oxidized implants show a median BIC, which is 8% higher than their minimally rough turned counterpart. The intraindividual difference between the TPS and the blasted and etched counterparts revealed no significant difference. The turned and the oxidized implants show median values of the resonance frequency [implant stability quotients (ISQ)] over 60; the nonself-tapping blasted and etched and TPS implants show median values below 60. In conclusion, the benefit of rough surfaces relative to minimally rough ones in this loaded animal model was confirmed histologically. The comparison of different surface treatment modalities revealed no significant differences between the modern moderately rough surfaces. Resonance frequency analysis seems to be influenced in a major part by the transducer used, thus prohibiting the comparison of different implant systems.

Shear bond strength of metal brackets to feldspathic porcelain treated by Nd:YAG laser and hydrofluoric acid.

PubMed

Hosseini, Mohammad Hashem; Sobouti, Farhad; Etemadi, Ardavan; Chiniforush, Nasim; Shariati, Mahsa

2015-02-01

Adult orthodontic treatment requires bonding orthodontic attachment to dental restorations. Ceramics are commonly used as esthetic restorative materials for the crowns and bridges. The present study evaluated the shear bond strength of metal orthodontic brackets to the feldspathic porcelain surfaces following conditioning by different powers of neodymium-doped yttrium aluminum garnet (Nd:YAG) laser and hydrofluoric acid as a conventional method. Seventy-two glazed porcelain samples were prepared and randomly attributed to six equal groups of 12. In the conventional hydrofluoric (HF) group, the specimens were etched by 9.6% hydrofluoric acid for 4 min. In laser groups, samples were conditioned by 0.75-, 1-, 1.25-, 1.5-, and 2-W Nd:YAG laser for 10 s. Metal brackets were bonded to porcelain samples and after being stored in distilled water for 24 h, they were subjected to thermocycling for 500 cycles. The debonding was carried out by a Zwick testing machine. The data were statistically analyzed by ANOVA and Tamhane multiple comparisons tests. The mean ± SD of the shear bond strength in the laser group 0.75, 1, 1.25, 1.5, and 2 W and HF group was 2.2 ± 0.9, 4.2 ± 1.1, 4.9 ± 2.4, 7 ± 1.7, 9.6 ± 2.7, and 9.4 ± 2.5, respectively. Together with the increased power of laser, the mean shear bond strength was increased continuously and no significant differences were found between the HF group and the laser groups with power of 1.5 or 2 W. Also, there was no significant difference between all test groups in ARI scores. There was no significant difference between bond strength of laser groups with power of 1.5 and 2 W and HF-etched group. So, Nd:YAG laser with appropriate parameters can be used as an alternative method for porcelain etching.

The effects of ethanol on the size-exclusion characteristics of type I dentin collagen to adhesive resin monomers.

PubMed

Chiba, A; Zhou, J; Nakajima, M; Tan, J; Tagami, J; Scheffel, D L S; Hebling, J; Agee, K A; Breschi, L; Grégoire, G; Jang, S S; Tay, F R; Pashley, D H

2016-03-01

During dentin bonding with etch-and-rinse adhesive systems, phosphoric acid etching of mineralized dentin solubilizes the mineral crystallites and replaces them with bound and unbound water. During the infiltration phase of dentin bonding, solvated adhesive resin comonomers are supposed to replace all of the unbound collagen water and polymerize into copolymers. A recently published review suggested that dental monomers are too large to enter and displace water from tightly-packed collagen molecules. Conversely, recent work from the authors' laboratory demonstrated that HEMA and TEGDMA freely equilibrate with water-saturated dentin matrices. However, because adhesive blends are solvated in organic solvents, those solvents may remove enough free water to allow collagen molecules to come close enough to exclude adhesive monomer permeation. The present study analyzed the size-exclusion characteristics of dentin collagen, using a gel permeation-like column chromatography technique, filled with dentin powder instead of Sephadex beads as the stationary phase. The elution volumes of different sized test molecules, including adhesive resin monomers, studied in both water-saturated dentin, and again in ethanol-dehydrated dentin powder, showed that adhesive resin monomers can freely diffuse into both hydrated and dehydrated collagen molecules. Under these in vitro conditions, all free and some of the loosely-bound water seems to have been removed by ethanol. These results validate the concept that adhesive resin monomers can permeate tightly-bound water in ethanol-saturated collagen molecules during infiltration by etch-and-rinse adhesives. It has been reported that collagen molecules in dentin matrices are packed too close together to allow permeation of adhesive monomers between them. Resin infiltration, in this view, would be limited to extrafibrillar spaces. Our work suggests that monomers equilibrate with collagen water in both water and ethanol-saturated dentin matrices. Copyright © 2016 Acta Materialia Inc. Published by Elsevier Ltd. All rights reserved.

Comparison of enamel bond fatigue durability between universal adhesives and two-step self-etch adhesives: Effect of phosphoric acid pre-etching.

PubMed

Suda, Shunichi; Tsujimoto, Akimasa; Barkmeier, Wayne W; Nojiri, Kie; Nagura, Yuko; Takamizawa, Toshiki; Latta, Mark A; Miyazaki, Masashi

2018-03-30

The effect of phosphoric acid pre-etching on enamel bond fatigue durability of universal adhesives and two-step self-etch adhesives was investigated. Four universal adhesives and three two-step self-etch adhesives were used. The initial shear bond strengths and shear fatigue strengths to enamel with and without phosphoric acid pre-etching using the adhesives were determined. SEM observations were also conducted. Phosphoric acid pre-etching of enamel was found to increase the bond fatigue durability of universal adhesives, but its effect on two-step self-etch adhesives was material-dependent. In addition, some universal adhesives with phosphoric acid pre-etching showed similar bond fatigue durability to the two-step self-etch adhesives, although the bond fatigue durability of universal adhesives in self-etch mode was lower than that of the two-step self-etch adhesives. Phosphoric acid pre-etching enhances enamel bond fatigue durability of universal adhesives, but the effect of phosphoric acid pre-etching on the bond fatigue durability of two-step self-etch adhesives was material-dependent.

Dry etching of metallization

NASA Technical Reports Server (NTRS)

Bollinger, D.

1983-01-01

The production dry etch processes are reviewed from the perspective of microelectronic fabrication applications. The major dry etch processes used in the fabrication of microelectronic devices can be divided into two categories - plasma processes in which samples are directly exposed to an electrical discharge, and ion beam processes in which samples are etched by a beam of ions extracted from a discharge. The plasma etch processes can be distinguished by the degree to which ion bombardment contributes to the etch process. This, in turn is related to capability for anisotropic etching. Reactive Ion Etching (RIE) and Ion Beam Etching are of most interest for etching of thin film metals. RIE is generally considered the best process for large volume, anisotropic aluminum etching.

A study of GaN-based LED structure etching using inductively coupled plasma

NASA Astrophysics Data System (ADS)

Wang, Pei; Cao, Bin; Gan, Zhiyin; Liu, Sheng

2011-02-01

GaN as a wide band gap semiconductor has been employed to fabricate optoelectronic devices such as light-emitting diodes (LEDs) and laser diodes (LDs). Recently several different dry etching techniques for GaN-based materials have been developed. ICP etching is attractive because of its superior plasma uniformity and strong controllability. Most previous reports emphasized on the ICP etching characteristics of single GaN film. In this study dry etching of GaN-based LED structure was performed by inductively coupled plasmas (ICP) etching with Cl2 as the base gas and BCl3 as the additive gas. The effects of the key process parameters such as etching gases flow rate, ICP power, RF power and chamber pressure on the etching properties of GaN-based LED structure including etching rate, selectivity, etched surface morphology and sidewall was investigated. Etch depths were measured using a depth profilometer and used to calculate the etch rates. The etch profiles were observed with a scanning electron microscope (SEM).

Study of Thermal Electrical Modified Etching for Glass and Its Application in Structure Etching

PubMed Central

Zhan, Zhan; Li, Wei; Yu, Lingke; Wang, Lingyun; Sun, Daoheng

2017-01-01

In this work, an accelerating etching method for glass named thermal electrical modified etching (TEM etching) is investigated. Based on the identification of the effect in anodic bonding, a novel method for glass structure micromachining is proposed using TEM etching. To validate the method, TEM-etched glasses are prepared and their morphology is tested, revealing the feasibility of the new method for micro/nano structure micromachining. Furthermore, two kinds of edge effect in the TEM and etching processes are analyzed. Additionally, a parameter study of TEM etching involving transferred charge, applied pressure, and etching roughness is conducted to evaluate this method. The study shows that TEM etching is a promising manufacture method for glass with low process temperature, three-dimensional self-control ability, and low equipment requirement. PMID:28772521

Combinatorial localized dissolution analysis: Application to acid-induced dissolution of dental enamel and the effect of surface treatments.

PubMed

Parker, Alexander S; Al Botros, Rehab; Kinnear, Sophie L; Snowden, Michael E; McKelvey, Kim; Ashcroft, Alexander T; Carvell, Mel; Joiner, Andrew; Peruffo, Massimo; Philpotts, Carol; Unwin, Patrick R

2016-08-15

A combination of scanning electrochemical cell microscopy (SECCM) and atomic force microscopy (AFM) is used to quantitatively study the acid-induced dissolution of dental enamel. A micron-scale liquid meniscus formed at the end of a dual barrelled pipette, which constitutes the SECCM probe, is brought into contact with the enamel surface for a defined period. Dissolution occurs at the interface of the meniscus and the enamel surface, under conditions of well-defined mass transport, creating etch pits that are then analysed via AFM. This technique is applied to bovine dental enamel, and the effect of various treatments of the enamel surface on acid dissolution (1mM HNO3) is studied. The treatments investigated are zinc ions, fluoride ions and the two combined. A finite element method (FEM) simulation of SECCM mass transport and interfacial reactivity, allows the intrinsic rate constant for acid-induced dissolution to be quantitatively determined. The dissolution of enamel, in terms of Ca(2+) flux ( [Formula: see text] ), is first order with respect to the interfacial proton concentration and given by the following rate law: [Formula: see text] , with k0=0.099±0.008cms(-1). Treating the enamel with either fluoride or zinc ions slows the dissolution rate, although in this model system the partly protective barrier only extends around 10-20nm into the enamel surface, so that after a period of a few seconds dissolution of modified surfaces tends towards that of native enamel. A combination of both treatments exhibits the greatest protection to the enamel surface, but the effect is again transient. Copyright © 2016 Elsevier Inc. All rights reserved.

Ion release, fluoride charge of and adhesion of an orthodontic cement paste containing microcapsules.

PubMed

Burbank, Brant D; Slater, Michael; Kava, Alyssa; Doyle, James; McHale, William A; Latta, Mark A; Gross, Stephen M

2016-02-01

Dental materials capable of releasing calcium, phosphate and fluoride are of great interest for remineralization. Microencapsulated aqueous solutions of these ions in orthodontic cement demonstrate slow, sustained release by passive diffusion through a permeable membrane without the need for dissolution or etching of fillers. The potential to charge a dental material formulated with microencapsulated water with fluoride by toothbrushing with over the counter toothpaste and the effect of microcapsules on cement adhesion to enamel was determined. Orthodontic cements that contained microcapsules with water and controls without microcapsules were brushed with over-the-counter toothpaste and fluoride release was measured. Adhesion measurements were performed loading orthodontic brackets to failure. Cements that contained microencapsulated solutions of 5.0M Ca(NO3)2, 0.8M NaF, 6.0MK2HPO4 or a mixture of all three were prepared. Ion release profiles were measured as a function of time. A greater fluoride charge and re-release from toothbrushing was demonstrated compared to a control with no microcapsules. Adhesion of an orthodontic cement that contained microencapsulated remineralizing agents was 8.5±2.5MPa compared to the control without microcapsules which was of 8.3±1.7MPa. Sustained release of fluoride, calcium and phosphate ions from cement formulated with microencapsulated remineralizing agents was demonstrated. Orthodontic cements with microcapsules show a release of bioavailable fluoride, calcium, and phosphate ions near the tooth surface while having the ability to charge with fluoride and not effect the adhesion of the material to enamel. Incorporation of microcapsules in dental materials is promising for promoting remineralization. Copyright © 2015 Elsevier Ltd. All rights reserved.

Two-year Randomized Clinical Trial of Self-etching Adhesives and Selective Enamel Etching.

PubMed

Pena, C E; Rodrigues, J A; Ely, C; Giannini, M; Reis, A F

2016-01-01

The aim of this randomized, controlled prospective clinical trial was to evaluate the clinical effectiveness of restoring noncarious cervical lesions with two self-etching adhesive systems applied with or without selective enamel etching. A one-step self-etching adhesive (Xeno V(+)) and a two-step self-etching system (Clearfil SE Bond) were used. The effectiveness of phosphoric acid selective etching of enamel margins was also evaluated. Fifty-six cavities were restored with each adhesive system and divided into two subgroups (n=28; etch and non-etch). All 112 cavities were restored with the nanohybrid composite Esthet.X HD. The clinical effectiveness of restorations was recorded in terms of retention, marginal integrity, marginal staining, caries recurrence, and postoperative sensitivity after 3, 6, 12, 18, and 24 months (modified United States Public Health Service). The Friedman test detected significant differences only after 18 months for marginal staining in the groups Clearfil SE non-etch (p=0.009) and Xeno V(+) etch (p=0.004). One restoration was lost during the trial (Xeno V(+) etch; p>0.05). Although an increase in marginal staining was recorded for groups Clearfil SE non-etch and Xeno V(+) etch, the clinical effectiveness of restorations was considered acceptable for the single-step and two-step self-etching systems with or without selective enamel etching in this 24-month clinical trial.

Influence of Pre-etching Times on Fatigue Strength of Self-etch Adhesives to Enamel.

PubMed

Takamizawa, Toshiki; Barkmeier, Wayne W; Tsujimoto, Akimasa; Endo, Hajime; Tsuchiya, Kenji; Erickson, Robert L; Latta, Mark A; Miyazaki, Masashi

To use shear bond strength (SBS) and shear fatigue strength (SFS) testing to determine the influence of phosphoric acid pre-etching times prior to application of self-etch adhesives on enamel bonding. Two single-step self-etch universal adhesives (Prime&Bond Elect and Scotchbond Universal), a conventional single-step self-etch adhesive (G-ӕnial Bond), and a conventional two-step self-etch adhesive (OptiBond XTR) were used. The SBS and SFS were obtained with phosphoric acid pre-etching for 3, 10, or 15 s prior to application of the adhesives, and without pre-etching (0 s) as a control. A staircase method was used to determine the SFS with 10 Hz frequency for 50,000 cycles or until failure occurred. The mean demineralization depth for each treated enamel surface was also measured using a profilometer. For all the adhesives, the groups with pre-etching showed significantly higher SBS and SFS than groups without pre-etching. However, there was no significant difference in SBS and SFS among groups with > 3 s of preetching. In addition, although the groups with pre-etching showed significantly deeper demineralization depths than groups without pre-etching, there was no significant difference in depth among groups with > 3 s of pre-etching. Three seconds of phosphoric acid pre-etching prior to application of self-etch adhesive can enhance enamel bonding effectiveness.

Influence of different pre-etching times on fatigue strength of self-etch adhesives to dentin.

PubMed

Takamizawa, Toshiki; Barkmeier, Wayne W; Tsujimoto, Akimasa; Suzuki, Takayuki; Scheidel, Donal D; Erickson, Robert L; Latta, Mark A; Miyazaki, Masashi

2016-04-01

The purpose of this study was to use shear bond strength (SBS) and shear fatigue strength (SFS) testing to determine the influence on dentin bonding of phosphoric acid pre-etching times before the application of self-etch adhesives. Two single-step self-etch universal adhesives [Prime & Bond Elect (EL) and Scotchbond Universal (SU)], a conventional single-step self-etch adhesive [G-aenial Bond (GB)], and a two-step self-etch adhesive [OptiBond XTR (OX)] were used. The SBS and SFS values were obtained with phosphoric acid pre-etching times of 3, 10, or 15 s before application of the adhesives, and for a control without pre-etching. For groups with 3 s of pre-etching, SU and EL showed higher SBS values than control groups. No significant difference was observed for GB among the 3 s, 10 s, and control groups, but the 15 s pre-etching group showed significantly lower SBS and SFS values than the control group. No significant difference was found for OX among the pre-etching groups. Reducing phosphoric acid pre-etching time can minimize the adverse effect on dentin bonding durability for the conventional self-etch adhesives. Furthermore, a short phosphoric acid pre-etching time enhances the dentin bonding performance of universal adhesives. © 2016 Eur J Oral Sci.

Direct comparison of the performance of commonly used e-beam resists during nano-scale plasma etching of Si, SiO2, and Cr

NASA Astrophysics Data System (ADS)

Goodyear, Andy; Boettcher, Monika; Stolberg, Ines; Cooke, Mike

2015-03-01

Electron beam writing remains one of the reference pattern generation techniques, and plasma etching continues to underpin pattern transfer. We report a systematic study of the plasma etch resistance of several e-beam resists, both negative and positive as well as classical and Chemically Amplified Resists: HSQ[1,2] (Dow Corning), PMMA[3] (Allresist GmbH), AR-P6200 (Allresist GmbH), ZEP520 (Zeon Corporation), CAN028 (TOK), CAP164 (TOK), and an additional pCAR (non-disclosed provider). Their behaviour under plasma exposure to various nano-scale plasma etch chemistries was examined (SF6/C4F8 ICP silicon etch, CHF3/Ar RIE SiO2 etch, Cl2/O2 RIE and ICP chrome etch, and HBr ICP silicon etch). Samples of each resist type were etched simultaneously to provide a direct comparison of their etch resistance. Resist thicknesses (and hence resist erosion rates) were measured by spectroscopic ellipsometer in order to provide the highest accuracy for the resist comparison. Etch selectivities (substrate:mask etch rate ratio) are given, with recommendations for the optimum resist choice for each type of etch chemistry. Silicon etch profiles are also presented, along with the exposure and etch conditions to obtain the most vertical nano-scale pattern transfer. We identify one resist that gave an unusually high selectivity for chlorinated and brominated etches which could enable pattern transfer below 10nm without an additional hard mask. In this case the resist itself acts as a hard mask. We also highlight the differing effects of fluorine and bromine-based Silicon etch chemistries on resist profile evolution and hence etch fidelity.

Deep inductively coupled plasma etching of ELO-GaN grown with high fill factor

NASA Astrophysics Data System (ADS)

Gao, Haiyong; Lee, Jaesoong; Ni, Xianfeng; Leach, Jacob; Özgür, Ümit; Morkoç, Hadis

2011-02-01

The epitaxial lateral overgrowth (ELO) gallium nitride (GaN) was grown with high fill factor using metal organic chemical vapor deposition (MOCVD). The inductively coupled plasma (ICP) etching of ELO-GaN based on Cl2/Ar/SiCl4 gas mixture was performed. Surface properties of ELO-GaN subjected to ICP etching have been investigated and optimized etching condition in ELO-GaN with ICP etching is presented. Radiofrequency (RF) power and the flow rate of Cl2 gas were modified during the experiments. The window region, wing region and the edge region of ELO-GaN pattern present different etching characteristics. Different etching conditions were studied to get the minimized plasma-induced damage, relatively high etching rates, and excellent surface profiles. Etch depths of the etched ELO-GaN with smooth surface up to about 19 μm were achieved. The most suitable three-step etching condition is discussed with the assessment based on the morphology observation of the etched surface of ELO-GaN patterns.

Temperature-Dependent Nanofabrication on Silicon by Friction-Induced Selective Etching.

PubMed

Jin, Chenning; Yu, Bingjun; Xiao, Chen; Chen, Lei; Qian, Linmao

2016-12-01

Friction-induced selective etching provides a convenient and practical way for fabricating protrusive nanostructures. A further understanding of this method is very important for establishing a controllable nanofabrication process. In this study, the effect of etching temperature on the formation of protrusive hillocks and surface properties of the etched silicon surface was investigated. It is found that the height of the hillock produced by selective etching increases with the etching temperature before the collapse of the hillock. The temperature-dependent selective etching rate can be fitted well by the Arrhenius equation. The etching at higher temperature can cause rougher silicon surface with a little lower elastic modulus and hardness. The contact angle of the etched silicon surface decreases with the etching temperature. It is also noted that no obvious contamination can be detected on silicon surface after etching at different temperatures. As a result, the optimized condition for the selective etching was addressed. The present study provides a new insight into the control and application of friction-induced selective nanofabrication.

Metallographic examination of TD-nickel base alloys. [thermal and chemical etching technique evaluation

NASA Technical Reports Server (NTRS)

Kane, R. D.; Petrovic, J. J.; Ebert, L. J.

1975-01-01

Techniques are evaluated for chemical, electrochemical, and thermal etching of thoria dispersed (TD) nickel alloys. An electrochemical etch is described which yielded good results only for large grain sizes of TD-nickel. Two types of thermal etches are assessed for TD-nickel: an oxidation etch and vacuum annealing of a polished specimen to produce an etch. It is shown that the first etch was somewhat dependent on sample orientation with respect to the processing direction, the second technique was not sensitive to specimen orientation or grain size, and neither method appear to alter the innate grain structure when the materials were fully annealed prior to etching. An electrochemical etch is described which was used to observe the microstructures in TD-NiCr, and a thermal-oxidation etch is shown to produce better detail of grain boundaries and to have excellent etching behavior over the entire range of grain sizes of the sample.

Investigation of Nitride Morphology After Self-Aligned Contact Etch

NASA Technical Reports Server (NTRS)

Hwang, Helen H.; Keil, J.; Helmer, B. A.; Chien, T.; Gopaladasu, P.; Kim, J.; Shon, J.; Biegel, Bryan (Technical Monitor)

2001-01-01

Self-Aligned Contact (SAC) etch has emerged as a key enabling technology for the fabrication of very large-scale memory devices. However, this is also a very challenging technology to implement from an etch viewpoint. The issues that arise range from poor oxide etch selectivity to nitride to problems with post etch nitride surface morphology. Unfortunately, the mechanisms that drive nitride loss and surface behavior remain poorly understood. Using a simple langmuir site balance model, SAC nitride etch simulations have been performed and compared to actual etched results. This approach permits the study of various etch mechanisms that may play a role in determining nitride loss and surface morphology. Particle trajectories and fluxes are computed using Monte-Carlo techniques and initial data obtained from double Langmuir probe measurements. Etched surface advancement is implemented using a shock tracking algorithm. Sticking coefficients and etch yields are adjusted to obtain the best agreement between actual etched results and simulated profiles.

Dry etching of chrome for photomasks for 100-nm technology using chemically amplified resist

NASA Astrophysics Data System (ADS)

Mueller, Mark; Komarov, Serguie; Baik, Ki-Ho

2002-07-01

Photo mask etching for the 100nm technology node places new requirements on dry etching processes. As the minimum-size features on the mask, such as assist bars and optical proximity correction (OPC) patterns, shrink down to 100nm, it is necessary to produce etch CD biases of below 20nm in order to reproduce minimum resist features into chrome with good pattern fidelity. In addition, vertical profiles are necessary. In previous generations of photomask technology, footing and sidewall profile slope were tolerated, since this dry etch profile was an improvement from wet etching. However, as feature sizes shrink, it is extremely important to select etch processes which do not generate a foot, because this will affect etch linearity and also limit the smallest etched feature size. Chemically amplified resist (CAR) from TOK is patterned with a 50keV MEBES eXara e-beam writer, allowing for patterning of small features with vertical resist profiles. This resist is developed for raster scan 50 kV e-beam systems. It has high contrast, good coating characteristics, good dry etch selectivity, and high environmental stability. Chrome etch process development has been performed using Design of Experiments to optimize parameters such as sidewall profile, etch CD bias, etch CD linearity for varying sizes of line/space patterns, etch CD linearity for varying sizes of isolated lines and spaces, loading effects, and application to contact etching.

Modeling the characteristic etch morphologies along specific crystallographic orientations by anisotropic chemical etching

NASA Astrophysics Data System (ADS)

Li, Kun-Dar; Miao, Jin-Ru

2018-02-01

To improve the advanced manufacturing technology for functional materials, a sophisticated control of chemical etching process is highly demanded, especially in the fields of environment and energy related applications. In this study, a phase-field-based model is utilized to investigate the etch morphologies influenced by the crystallographic characters during anisotropic chemical etching. Three types of etching modes are inspected theoretically, including the isotropic, <100> and <111> preferred oriented etchings. Owing to the specific etching behavior along the crystallographic directions, different characteristic surface structures are presented in the simulations, such as the pimple-like, pyramidal hillock and ridge-like morphologies. In addition, the processing parameters affecting the surface morphological formation and evolution are also examined systematically. According to the numerical results, the growth mechanism of surface morphology in a chemical etching is revealed distinctly. While the etching dynamics plays a dominant role on the surface formation, the characteristic surface morphologies corresponding to the preferred etching direction become more apparent. As the atomic diffusion turned into a determinative factor, a smoothened surface would appear, even under the anisotropic etching conditions. These simulation results provide fundamental information to enhance the development and application of anisotropic chemical etching techniques.

Phase Analysis of Laser Direct Etching and Water Assisted Laser Combined Etching of SiC Ceramics

NASA Astrophysics Data System (ADS)

Yuan, Genfu; Cong, Qidong; Zhang, Chen; Xie, Bingbing

2017-12-01

In this study, to discover the etching mechanism of SiC ceramics under laser direct etching and water-jet assisted laser combined etching, the phenomena of substance change on the etched surface were investigated. Also, the rules of substance transfer in etching are discussed. The elemental content change and the phase change of the etching products on the etched surface were analyzed by energy dispersive spectroscopy (EDS) and X-ray diffraction (XRD), respectively. These studies showed a high amount of carbon black on the etched surface, because of the decomposition of SiC ceramics under the high-power-density laser irradiation. SiC decomposed to Si under the laser irradiation, and the subsequent chemical reaction of Si and O2 easily produced SiO2. The SiO2 on the etched surface melted and vaporized, whereas most of SiO2 was removed through splashing, changing the chemical composition of the etched surface. Following the water jet introduction, an increased amount of O existed on the combined etching surface, because the chemical reaction of SiC and H2O easily produced SiO2 under the high-power-density laser irradiation.

Introduction of pre-etch deposition techniques in EUV patterning

NASA Astrophysics Data System (ADS)

Xiang, Xun; Beique, Genevieve; Sun, Lei; Labonte, Andre; Labelle, Catherine; Nagabhirava, Bhaskar; Friddle, Phil; Schmitz, Stefan; Goss, Michael; Metzler, Dominik; Arnold, John

2018-04-01

The thin nature of EUV (Extreme Ultraviolet) resist has posed significant challenges for etch processes. In particular, EUV patterning combined with conventional etch approaches suffers from loss of pattern fidelity in the form of line breaks. A typical conventional etch approach prevents the etch process from having sufficient resist margin to control the trench CD (Critical Dimension), minimize the LWR (Line Width Roughness), LER (Line Edge Roughness) and reduce the T2T (Tip-to-Tip). Pre-etch deposition increases the resist budget by adding additional material to the resist layer, thus enabling the etch process to explore a wider set of process parameters to achieve better pattern fidelity. Preliminary tests with pre-etch deposition resulted in blocked isolated trenches. In order to mitigate these effects, a cyclic deposition and etch technique is proposed. With optimization of deposition and etch cycle time as well as total number of cycles, it is possible to open the underlying layers with a beneficial over etch and simultaneously keep the isolated trenches open. This study compares the impact of no pre-etch deposition, one time deposition and cyclic deposition/etch techniques on 4 aspects: resist budget, isolated trench open, LWR/LER and T2T.

Shrinkage vectors of a flowable composite in artificial cavity models with different boundary conditions: Ceramic and Teflon.

PubMed

Kaisarly, Dalia; El Gezawi, Moataz; Xu, Xiaohui; Rösch, Peter; Kunzelmann, Karl-Heinz

2018-01-01

Polymerization shrinkage of dental resin composites leads to stress build-up at the tooth-restoration interface that predisposes the restoration to debonding. In contrast to the heterogeneity of enamel and dentin, this study investigated the effect of boundary conditions in artificial cavity models such as ceramic and Teflon. Ceramic serves as a homogenous substrate that provides optimal bonding conditions, which we presented in the form of etched and silanized ceramic in addition to an etched, silanized and bonded ceramic cavity. In contrast, the Teflon cavity presented a non-adhesive boundary condition that provided an exaggerated condition of poor bonding as in the case of contamination during the application procedure or a poor bonding substrate such as sclerotic or deep dentin. The greatest 3D shrinkage vectors and movement in the axial direction were observed in the ceramic cavity with the bonding agent followed by the silanized ceramic cavity, and smallest shrinkage vectors and axial movements were observed in the Teflon cavity. The shrinkage vectors in the ceramic cavities exhibited downward movement toward the cavity bottom with great downward shrinkage of the free surface. The shrinkage vectors in the Teflon cavity pointed towards the center of the restoration with lateral movement greater at one side denoting the site of first detachment from the cavity walls. These results proved that the boundary conditions, in terms of bonding substrates, significantly influenced the shrinkage direction. Copyright © 2017 Elsevier Ltd. All rights reserved.

Influence of an oxygen-inhibited layer on enamel bonding of dental adhesive systems: surface free-energy perspectives.

PubMed

Ueta, Hirofumi; Tsujimoto, Akimasa; Barkmeier, Wayne W; Oouchi, Hajime; Sai, Keiichi; Takamizawa, Toshiki; Latta, Mark A; Miyazaki, Masashi

2016-02-01

The influence of an oxygen-inhibited layer (OIL) on the shear bond strength (SBS) to enamel and surface free-energy (SFE) of adhesive systems was investigated. The adhesive systems tested were Scotchbond Multipurpose (SM), Clearfil SE Bond (CS), and Scotchbond Universal (SU). Resin composite was bonded to bovine enamel surfaces to determine the SBS, with and without an OIL, of adhesives. The SFE of cured adhesives with and without an OIL were determined by measuring the contact angles of three test liquids. There were no significant differences in the mean SBS of SM and CS specimens with or without an OIL; however, the mean SBS of SU specimens with an OIL was significantly higher than that of SU specimens without an OIL. For all three systems, the mean total SFE (γS), polarity force (γSp), and hydrogen bonding force (γSh) values of cured adhesives with an OIL were significantly higher than those of cured adhesives without an OIL. The results of this study indicate that the presence of an OIL promotes higher SBS of a single-step self-etch adhesive system, but not of a three-step or a two-step self-etch primer system. The SFE values of cured adhesives with an OIL were significantly higher than those without an OIL. The SFE characteristics of the OIL of adhesives differed depending on the type of adhesive. © 2015 Eur J Oral Sci.

Influence of water storage on fatigue strength of self-etch adhesives.

PubMed

Takamizawa, Toshiki; Barkmeier, Wayne W; Tsujimoto, Akimasa; Scheidel, Donal D; Watanabe, Hidehiko; Erickson, Robert L; Latta, Mark A; Miyazaki, Masashi

2015-12-01

The purpose of this study was to determine enamel and dentin bond durability after long-term water storage using self-etch adhesives. Two single step self-etch adhesives (SU, Scotchbond Universal and GB, G-ӕnial Bond) and a two-step self-etch adhesive (OX, OptiBond XTR) were used. The shear bond strength (SBS) and shear fatigue strength (FS) of the enamel and dentin were obtained with and without phosphoric acid pre-etching prior to application of the adhesives. The specimens were stored in distilled water at 37 °C for 24 h, 6 months, and one year. A staircase method was used to determine the FS using a frequency of 10 Hz for 50,000 cycles or until failure occurred. The SBS and FS of enamel bonds were significantly higher with pre-etching, when compared to no pre-etching for the same water storage period. The FS of dentin bonds with pre-etching tended to decrease relative to no pre-etching at the same storage period. For the one year storage period, SU and GB with pre-etching showed significantly lower FS values than the groups without pre-etching. The influence of water storage on FS of the self-etch adhesives was dependent on the adhesive material, storage period and phosphoric acid pre-etching of the bonding site. Phosphoric acid pre-etching of enamel improves the effectiveness of self-etch adhesive systems. Inadvertent contact of phosphoric acid on dentin appears to reduce the ability of self-etch adhesives to effectively bond resin composite materials. Copyright © 2015 Elsevier Ltd. All rights reserved.

Depth of Etch Comparison Between Self-limiting and Traditional Etchant Systems

DTIC Science & Technology

2016-06-18

two different etchants (Ultradent’s Opal Etch 35%, a self-limiting phosphoric acid, or 34% Tooth Conditioning Gel by Dentsply) at varied time... Opal versus Dentsply and there was also a significant difference between etch time. There is no significant difference between the interaction of...etch material and etch time. Conclusion: The depth of etch of Opal etchant was consistently less than Dentsply etchant but continued to etch and

Effect of Reduced Phosphoric Acid Pre-etching Times 
on Enamel Surface Characteristics and Shear Fatigue Strength Using Universal Adhesives.

PubMed

Tsujimoto, Akimasa; Fischer, Nicholas; Barkmeier, Wayne; Baruth, Andrew; Takamizawa, Toshiki; Latta, Mark; Miyazaki, Masashi

2017-01-01

To examine the effect of reduced phosphoric acid pre-etching times on enamel fatigue bond strength of universal adhesives and surface characteristics by using atomic force microscopy (AFM). Three universal adhesives were used in this study (Clearfil Universal Bond [C], G-Premio Bond [GP], Scotchbond Universal Adhesive [SU]). Four pre-etching groups were employed: enamel pre-etched with phosphoric acid and immediately rinsed with an air-water spray, and enamel pre-etched with phosphoric acid for 5, 10, or 15 s. Ground enamel was used as the control group. For the initial bond strength test, 15 specimens per etching group for each adhesive were used. For the shear fatigue test, 20 specimens per etching group for each adhesive were loaded using a sine wave at a frequency of 20 Hz for 50,000 cycles or until failure occurred. Initial shear bond strengths and fatigue shear strengths of composite adhesively bonded to ground and pre-etched enamel were determined. AFM observations of ground and pre-etched enamel were also conducted, and surface roughness as well as surface area were evaluated. The initial shear bond strengths and fatigue shear strengths of the universal adhesives in the pre-etched groups were significantly higher than those of the control group, and were not influenced by the pre-etching time. Significantly higher surface roughness and surface area of enamel surfaces in pre-etched groups were observed compared with those in the control group. While the surface area was not significantly influenced by etching time, surface roughness of the enamel surfaces in the pre-etched groups significantly increased with pre-etching time. The results of this in vitro study suggest that reduced phosphoric acid pre-etching times do not impair the fatigue bond strength of universal adhesives. Although fatigue bond strength and surface area were not influenced by phosphoric-acid etching times, surface roughness increased with increasing etching time.

Chemical Etching of Zinc Oxide for Thin-Film Silicon Solar Cells

PubMed Central

Hüpkes, Jürgen; Owen, Jorj I; Pust, Sascha E; Bunte, Eerke

2012-01-01

Abstract Chemical etching is widely applied to texture the surface of sputter-deposited zinc oxide for light scattering in thin-film silicon solar cells. Based on experimental findings from the literature and our own results we propose a model that explains the etching behavior of ZnO depending on the structural material properties and etching agent. All grain boundaries are prone to be etched to a certain threshold, that is defined by the deposition conditions and etching solution. Additionally, several approaches to modify the etching behavior through special preparation and etching steps are provided. PMID:22162035

Anisotropic diamond etching through thermochemical reaction between Ni and diamond in high-temperature water vapour.

PubMed

Nagai, Masatsugu; Nakanishi, Kazuhiro; Takahashi, Hiraku; Kato, Hiromitsu; Makino, Toshiharu; Yamasaki, Satoshi; Matsumoto, Tsubasa; Inokuma, Takao; Tokuda, Norio

2018-04-27

Diamond possesses excellent physical and electronic properties, and thus various applications that use diamond are under development. Additionally, the control of diamond geometry by etching technique is essential for such applications. However, conventional wet processes used for etching other materials are ineffective for diamond. Moreover, plasma processes currently employed for diamond etching are not selective, and plasma-induced damage to diamond deteriorates the device-performances. Here, we report a non-plasma etching process for single crystal diamond using thermochemical reaction between Ni and diamond in high-temperature water vapour. Diamond under Ni films was selectively etched, with no etching at other locations. A diamond-etching rate of approximately 8.7 μm/min (1000 °C) was successfully achieved. To the best of our knowledge, this rate is considerably greater than those reported so far for other diamond-etching processes, including plasma processes. The anisotropy observed for this diamond etching was considerably similar to that observed for Si etching using KOH.

Bi/In thermal resist for both Si anisotropic wet etching and Si/SiO2 plasma etching

NASA Astrophysics Data System (ADS)

Chapman, Glenn H.; Tu, Yuqiang; Peng, Jun

2004-01-01

Bi/In thermal resist is a bilayer structure of Bi over In films which can be exposed by laser with a wide range of wavelengths and can be developed by diluted RCA2 solutions. Current research shows bimetallic resist can work as etch masking layer for both dry plasma etching and wet anisotropic etching. It can act as both patterning and masking layers for Si and SiO2 with plasma "dry" etch using CF4/CHF3. The etching condition is CF4 flow rate 50 sccm, pressure 150 mTorr, and RF power 100 - 600W. The profile of etched structures can be tuned by adding CHF3 and other gases such as Ar, and by changing the CF4/CHF3 ratio. Depending on the fluorocarbon plasma etching recipe the etch rate of laser exposed Bi/In can be as low as 0.1 nm/min, 500 times lower than organic photoresists. O2 plasma ashing has little etching effect on exposed Bi/In. Bi/In also creates etch masking layers for alkaline-based (KOH, TMAH and EDP) "wet" anisotropic bulk Si etch without the need of SiO2 masking steps. The laser exposed Bi/In etches two times more slowly than SiO2. Experiment result shows that single metal Indium film exhibits thermal resist characteristics but at twice the exposure levels. It can be developed in diluted RCA2 solution and used as an etch mask layer for Si anisotropic etch. X-ray diffraction analysis shows that laser exposure causes both Bi and In single film to oxidize. In film may become amorphous when exposed to high laser power.

Pattern sampling for etch model calibration

NASA Astrophysics Data System (ADS)

Weisbuch, François; Lutich, Andrey; Schatz, Jirka

2017-06-01

Successful patterning requires good control of the photolithography and etch processes. While compact litho models, mainly based on rigorous physics, can predict very well the contours printed in photoresist, pure empirical etch models are less accurate and more unstable. Compact etch models are based on geometrical kernels to compute the litho-etch biases that measure the distance between litho and etch contours. The definition of the kernels as well as the choice of calibration patterns is critical to get a robust etch model. This work proposes to define a set of independent and anisotropic etch kernels -"internal, external, curvature, Gaussian, z_profile" - designed to capture the finest details of the resist contours and represent precisely any etch bias. By evaluating the etch kernels on various structures it is possible to map their etch signatures in a multi-dimensional space and analyze them to find an optimal sampling of structures to train an etch model. The method was specifically applied to a contact layer containing many different geometries and was used to successfully select appropriate calibration structures. The proposed kernels evaluated on these structures were combined to train an etch model significantly better than the standard one. We also illustrate the usage of the specific kernel "z_profile" which adds a third dimension to the description of the resist profile.

Copper-assisted, anti-reflection etching of silicon surfaces

DOEpatents

Toor, Fatima; Branz, Howard

2014-08-26

A method (300) for etching a silicon surface (116) to reduce reflectivity. The method (300) includes electroless deposition of copper nanoparticles about 20 nanometers in size on the silicon surface (116), with a particle-to-particle spacing of 3 to 8 nanometers. The method (300) includes positioning (310) the substrate (112) with a silicon surface (116) into a vessel (122). The vessel (122) is filled (340) with a volume of an etching solution (124) so as to cover the silicon surface (116). The etching solution (124) includes an oxidant-etchant solution (146), e.g., an aqueous solution of hydrofluoric acid and hydrogen peroxide. The silicon surface (116) is etched (350) by agitating the etching solution (124) with, for example, ultrasonic agitation, and the etching may include heating (360) the etching solution (124) and directing light (365) onto the silicon surface (116). During the etching, copper nanoparticles enhance or drive the etching process.

A review on plasma-etch-process induced damage of HgCdTe

NASA Astrophysics Data System (ADS)

Liu, Lingfeng; Chen, Yiyu; Ye, Zhenhua; Ding, Ruijun

2018-05-01

Dry etching techniques with minimal etch induced damage are required to develop highly anisotropic etch for pixel delineation of HgCdTe infrared focal plane arrays (IRFPAs). High density plasma process has become the main etching technique for HgCdTe in the past twenty years, In this paper, high density plasma electron cyclotron resonance (ECR) and inductively coupled plasma (ICP) etching of HgCdTe are summarized. Common plasma-etch-process induced type conversion and related mechanisms are reviewed particularly.

Comparative evaluation of the three different surface treatments - conventional, laser and Nano technology methods in enhancing the surface characteristics of commercially pure titanium discs and their effects on cell adhesion: An in vitro study.

PubMed

Vignesh; Nayar, Sanjna; Bhuminathan; Mahadevan; Santhosh, S

2015-04-01

The surface area of the titanium dental implant materials can be increased by surface treatments without altering their shape and form, thereby increasing the biologic properties of the biomaterial. A good biomaterial helps in early cell adhesion and cell signaling. In this study, the commercially pure titanium surfaces were prepared to enable machined surfaces to form a control material and to be compared with sandblasted and acid-etched surfaces, laser treated surfaces and titanium dioxide (20 nm) Nano-particle coated surfaces. The surface elements were characterized. The biocompatibility was evaluated by cell culture in vitro using L929 fibroblasts. The results suggested that the titanium dioxide Nano-particle coated surfaces had good osteoconductivity and can be used as a potential method for coating the biomaterial.

Effects of Chemical Cross-linkers on Caries-affected Dentin Bonding

PubMed Central

Macedo, G.V.; Yamauchi, M.; Bedran-Russo, A.K.

2009-01-01

The achievement of a strong and stable bond between composite resin and dentin remains a challenge in restorative dentistry. Over the past two decades, dental materials have been substantially improved, with better handling and bonding characteristics. However, little attention has been paid to the contribution of collagen structure/stability to bond strength. We hypothesized that the induction of cross-linking in dentin collagen improves dentin collagen stability and bond strength. This study investigated the effects of glutaraldehyde- and grape seed extract-induced cross-linking on the dentin bond strengths of sound and caries-affected dentin, and on the stability of dentin collagen. Our results demonstrated that the application of chemical cross-linking agents to etched dentin prior to bonding procedures significantly enhanced the dentin bond strengths of caries-affected and sound dentin. Glutaraldehyde and grape seed extract significantly increased dentin collagen stability in sound and caries-affected dentin, likely via distinct mechanisms. PMID:19892915

Antibacterial activity and dentin bonding ability of combined use of Clearfil SE Protect and sodium hypochlorite.

PubMed

Muratovska, Ilijana; Kitagawa, Haruaki; Hirose, Nanako; Kitagawa, Ranna; Imazato, Satoshi

2018-02-08

The aim of this study was to evaluate the antibacterial activity and dentin bonding ability of a commercial self-etch adhesive Clearfil SE Protect (Kuraray Noritake Dental, Tokyo, Japan) in combination with sodium hypochlorite (NaOCl). Agar disc diffusion tests and measurement of minimum inhibitory/bactericidal concentrations (MIC/MBC) against Streptococcus mutans were performed to evaluate antibacterial effects. The mixture solution of 5.25% NaOCl and the primer of Clearfil SE Protect demonstrated less antibacterial activity than primer only. In microtensile bond strength tests using non-carious human molars, pretreatment with 5.25% NaOCl aqueous solution had no influence on the bond strength of Clearfil SE Protect. These results indicate that pretreatment with NaOCl does not influence the bonding ability of Clearfil SE Protect, while their combined use does not enhance cavity disinfecting effects.

Oriented and Ordered Biomimetic Remineralization of the Surface of Demineralized Dental Enamel Using HAP@ACP Nanoparticles Guided by Glycine

PubMed Central

Wang, Haorong; Xiao, Zuohui; Yang, Jie; Lu, Danyang; Kishen, Anil; Li, Yanqiu; Chen, Zhen; Que, Kehua; Zhang, Qian; Deng, Xuliang; Yang, Xiaoping; Cai, Qing; Chen, Ning; Cong, Changhong; Guan, Binbin; Li, Ting; Zhang, Xu

2017-01-01

Achieving oriented and ordered remineralization on the surface of demineralized dental enamel, thereby restoring the satisfactory mechanical properties approaching those of sound enamel, is still a challenge for dentists. To mimic the natural biomineralization approach for enamel remineralization, the biological process of enamel development proteins, such as amelogenin, was simulated in this study. In this work, carboxymethyl chitosan (CMC) conjugated with alendronate (ALN) was applied to stabilize amorphous calcium phosphate (ACP) to form CMC/ACP nanoparticles. Sodium hypochlorite (NaClO) functioned as the protease which decompose amelogenin in vivo to degrade the CMC-ALN matrix and generate HAP@ACP core-shell nanoparticles. Finally, when guided by 10 mM glycine (Gly), HAP@ACP nanoparticles can arrange orderly and subsequently transform from an amorphous phase to well-ordered rod-like apatite crystals to achieve oriented and ordered biomimetic remineralization on acid-etched enamel surfaces. This biomimetic remineralization process is achieved through the oriented attachment (OA) of nanoparticles based on non-classical crystallization theory. These results indicate that finding and developing analogues of natural proteins such as amelogenin involved in the biomineralization by natural macromolecular polymers and imitating the process of biomineralization would be an effective strategy for enamel remineralization. Furthermore, this method represents a promising method for the management of early caries in minimal invasive dentistry (MID). PMID:28079165

Oriented and Ordered Biomimetic Remineralization of the Surface of Demineralized Dental Enamel Using HAP@ACP Nanoparticles Guided by Glycine

NASA Astrophysics Data System (ADS)

Wang, Haorong; Xiao, Zuohui; Yang, Jie; Lu, Danyang; Kishen, Anil; Li, Yanqiu; Chen, Zhen; Que, Kehua; Zhang, Qian; Deng, Xuliang; Yang, Xiaoping; Cai, Qing; Chen, Ning; Cong, Changhong; Guan, Binbin; Li, Ting; Zhang, Xu

2017-01-01

Achieving oriented and ordered remineralization on the surface of demineralized dental enamel, thereby restoring the satisfactory mechanical properties approaching those of sound enamel, is still a challenge for dentists. To mimic the natural biomineralization approach for enamel remineralization, the biological process of enamel development proteins, such as amelogenin, was simulated in this study. In this work, carboxymethyl chitosan (CMC) conjugated with alendronate (ALN) was applied to stabilize amorphous calcium phosphate (ACP) to form CMC/ACP nanoparticles. Sodium hypochlorite (NaClO) functioned as the protease which decompose amelogenin in vivo to degrade the CMC-ALN matrix and generate HAP@ACP core-shell nanoparticles. Finally, when guided by 10 mM glycine (Gly), HAP@ACP nanoparticles can arrange orderly and subsequently transform from an amorphous phase to well-ordered rod-like apatite crystals to achieve oriented and ordered biomimetic remineralization on acid-etched enamel surfaces. This biomimetic remineralization process is achieved through the oriented attachment (OA) of nanoparticles based on non-classical crystallization theory. These results indicate that finding and developing analogues of natural proteins such as amelogenin involved in the biomineralization by natural macromolecular polymers and imitating the process of biomineralization would be an effective strategy for enamel remineralization. Furthermore, this method represents a promising method for the management of early caries in minimal invasive dentistry (MID).

Thermodynamics of nuclear track chemical etching

NASA Astrophysics Data System (ADS)

Rana, Mukhtar Ahmed

2018-05-01

This is a brief paper with new and useful scientific information on nuclear track chemical etching. Nuclear track etching is described here by using basic concepts of thermodynamics. Enthalpy, entropy and free energy parameters are considered for the nuclear track etching. The free energy of etching is determined using etching experiments of fission fragment tracks in CR-39. Relationship between the free energy and the etching temperature is explored and is found to be approximately linear. The above relationship is discussed. A simple enthalpy-entropy model of chemical etching is presented. Experimental and computational results presented here are of fundamental interest in nuclear track detection methodology.

High rate dry etching of InGaZnO by BCl3/O2 plasma

NASA Astrophysics Data System (ADS)

Park, Wanjae; Whang, Ki-Woong; Gwang Yoon, Young; Hwan Kim, Jeong; Rha, Sang-Ho; Seong Hwang, Cheol

2011-08-01

This paper reports the results of the high-rate dry etching of indium gallium zinc oxide (IGZO) at room temperature using BCl3/O2 plasma. We achieved an etch rate of 250 nm/min. We inferred from the x-ray photoelectron spectroscopy analysis that BOx or BOClx radicals generated from BCl3/O2 plasma cause the etching of the IGZO material. O2 initiates the etching of IGZO, and Ar removes nonvolatile byproducts from the surface during the etching process. Consequently, a smooth etched surface results when these gases are added to the etch gas.

Chemical method for producing smooth surfaces on silicon wafers

DOEpatents

Yu, Conrad

2003-01-01

An improved method for producing optically smooth surfaces in silicon wafers during wet chemical etching involves a pre-treatment rinse of the wafers before etching and a post-etching rinse. The pre-treatment with an organic solvent provides a well-wetted surface that ensures uniform mass transfer during etching, which results in optically smooth surfaces. The post-etching treatment with an acetic acid solution stops the etching instantly, preventing any uneven etching that leads to surface roughness. This method can be used to etch silicon surfaces to a depth of 200 .mu.m or more, while the finished surfaces have a surface roughness of only 15-50 .ANG. (RMS).

Fabrication of ultra-high aspect ratio (>160:1) silicon nanostructures by using Au metal assisted chemical etching

NASA Astrophysics Data System (ADS)

Li, Hailiang; Ye, Tianchun; Shi, Lina; Xie, Changqing

2017-12-01

We present a facile and effective approach for fabricating high aspect ratio, dense and vertical silicon nanopillar arrays, using a combination of metal etching following electron-beam lithography and Au metal assisted chemical etching (MacEtch). Ti/Au nanostructures used as catalysts in MacEtch are formed by single layer resist-based electron-beam exposure followed by ion beam etching. The effects of MacEtch process parameters, including half period, etching time, the concentrations of H2O2 and HF, etching temperature and drying method are systematically investigated. Especially, we demonstrate an enhancement of etching quality by employing cold MacEtch process, and an enhancement in preventing the collapse of high aspect ratio nanostructures by employing low surface tension rinse liquid and natural evaporation in the drying stage. Using an optimized MacEtch process, vertical silicon nanopillar arrays with a period of 250 nm and aspect ratio up to 160:1 are realized. Our results should be instructive for exploring the achievable aspect ratio limit in silicon nanostructures and may find potential applications in photovoltaic devices, thermoelectric devices and x-ray diffractive optics.

Damage-Free Smooth-Sidewall InGaAs Nanopillar Array by Metal-Assisted Chemical Etching.

PubMed

Kong, Lingyu; Song, Yi; Kim, Jeong Dong; Yu, Lan; Wasserman, Daniel; Chim, Wai Kin; Chiam, Sing Yang; Li, Xiuling

2017-10-24

Producing densely packed high aspect ratio In 0.53 Ga 0.47 As nanostructures without surface damage is critical for beyond Si-CMOS nanoelectronic and optoelectronic devices. However, conventional dry etching methods are known to produce irreversible damage to III-V compound semiconductors because of the inherent high-energy ion-driven process. In this work, we demonstrate the realization of ordered, uniform, array-based In 0.53 Ga 0.47 As pillars with diameters as small as 200 nm using the damage-free metal-assisted chemical etching (MacEtch) technology combined with the post-MacEtch digital etching smoothing. The etching mechanism of In x Ga 1-x As is explored through the characterization of pillar morphology and porosity as a function of etching condition and indium composition. The etching behavior of In 0.53 Ga 0.47 As, in contrast to higher bandgap semiconductors (e.g., Si or GaAs), can be interpreted by a Schottky barrier height model that dictates the etching mechanism constantly in the mass transport limited regime because of the low barrier height. A broader impact of this work relates to the complete elimination of surface roughness or porosity related defects, which can be prevalent byproducts of MacEtch, by post-MacEtch digital etching. Side-by-side comparison of the midgap interface state density and flat-band capacitance hysteresis of both the unprocessed planar and MacEtched pillar In 0.53 Ga 0.47 As metal-oxide-semiconductor capacitors further confirms that the surface of the resultant pillars is as smooth and defect-free as before etching. MacEtch combined with digital etching offers a simple, room-temperature, and low-cost method for the formation of high-quality In 0.53 Ga 0.47 As nanostructures that will potentially enable large-volume production of In 0.53 Ga 0.47 As-based devices including three-dimensional transistors and high-efficiency infrared photodetectors.

Comparative analysis of barium titanate thin films dry etching using inductively coupled plasmas by different fluorine-based mixture gas

PubMed Central

2014-01-01

In this work, the inductively coupled plasma etching technique was applied to etch the barium titanate thin film. A comparative study of etch characteristics of the barium titanate thin film has been investigated in fluorine-based (CF4/O2, C4F8/O2 and SF6/O2) plasmas. The etch rates were measured using focused ion beam in order to ensure the accuracy of measurement. The surface morphology of etched barium titanate thin film was characterized by atomic force microscope. The chemical state of the etched surfaces was investigated by X-ray photoelectron spectroscopy. According to the experimental result, we monitored that a higher barium titanate thin film etch rate was achieved with SF6/O2 due to minimum amount of necessary ion energy and its higher volatility of etching byproducts as compared with CF4/O2 and C4F8/O2. Low-volatile C-F compound etching byproducts from C4F8/O2 were observed on the etched surface and resulted in the reduction of etch rate. As a result, the barium titanate films can be effectively etched by the plasma with the composition of SF6/O2, which has an etch rate of over than 46.7 nm/min at RF power/inductively coupled plasma (ICP) power of 150/1,000 W under gas pressure of 7.5 mTorr with a better surface morphology. PMID:25278821

The K 2S 2O 8-KOH photoetching system for GaN

NASA Astrophysics Data System (ADS)

Weyher, J. L.; Tichelaar, F. D.; van Dorp, D. H.; Kelly, J. J.; Khachapuridze, A.

2010-09-01

A recently developed photoetching system for n-type GaN, a KOH solution containing the strong oxidizing agent potassium peroxydisulphate (K 2S 2O 8), was studied in detail. By careful selection of the etching parameters, such as the ratio of components and the hydrodynamics, two distinct modes were defined: defect-selective etching (denoted by KSO-D) and polishing (KSO-P). Both photoetching methods can be used under open-circuit (electroless) conditions. Well-defined dislocation-related etch whiskers are formed during KSO-D etching. All types of dislocations are revealed, and this was confirmed by cross-sectional TEM examination of the etched samples. Extended electrically active defects are also clearly revealed. The known relationship between etch rate and carrier concentration for photoetching of GaN in KOH solutions was confirmed for KSO-D etch using Raman measurements. It is shown that during KSO-P etching diffusion is the rate-limiting step, i.e. this etch is suitable for polishing of GaN. Some constraints of the KSO etching system for GaN are discussed and peculiar etch features, so far not understood, are described.

Ultradeep electron cyclotron resonance plasma etching of GaN

DOE PAGES

Harrison, Sara E.; Voss, Lars F.; Torres, Andrea M.; ...

2017-07-25

Here, ultradeep (≥5 μm) electron cyclotron resonance plasma etching of GaN micropillars was investigated. Parametric studies on the influence of the applied radio-frequency power, chlorine content in a Cl 2/Ar etch plasma, and operating pressure on the etch depth, GaN-to-SiO 2 selectivity, and surface morphology were performed. Etch depths of >10 μm were achieved over a wide range of parameters. Etch rates and sidewall roughness were found to be most sensitive to variations in RF power and % Cl 2 in the etch plasma. Selectivities of >20:1 GaN:SiO 2 were achieved under several chemically driven etch conditions where a maximummore » selectivity of ~39:1 was obtained using a 100% Cl 2 plasma. The etch profile and (0001) surface morphology were significantly influenced by operating pressure and the chlorine content in the plasma. Optimized etch conditions yielded >10 μm tall micropillars with nanometer-scale sidewall roughness, high GaN:SiO 2 selectivity, and nearly vertical etch profiles. These results provide a promising route for the fabrication of ultradeep GaN microstructures for use in electronic and optoelectronic device applications. In addition, dry etch induced preferential crystallographic etching in GaN microstructures is also demonstrated, which may be of great interest for applications requiring access to non- or semipolar GaN surfaces.« less

Anisotropic Hydrogen Etching of Chemical Vapor Deposited Graphene

NASA Astrophysics Data System (ADS)

Zhang, Yi; Li, Zhen; Zhang, Luyao; Kim, Pyojae; Zhou, Chongwu

2012-02-01

In terms of the preparation of graphene, chemical vapor deposition (CVD) has raised its popularity as a scalable and cost effective approach for graphene synthesis. While the formation of graphene on copper foil has been intensively studied, the reverse reaction of graphene reacts with hydrogen has not been systematically studied. In this talk we will present a simple, clean, and highly anisotropic hydrogen etching method for CVD graphene catalyzed by the copper substrate. By exposing CVD graphene on copper foil to hydrogen flow around 800 ^oC, we observed that the initially continuous graphene can be etched to have many hexagonal openings. In addition, we found that the etching is temperature dependent and the etching of graphene at 800 oC is most efficient and anisotropic. 80% of the angles of graphene edges after etching are 120^o, indicating the etching is highly anisotropic. No increase of D band along the etched edges indicates that the crystallographic orientation of etching is zigzag direction. Furthermore, we observed that copper played an important role in catalyzing the etching reaction, as no etching was observed for graphene transferred to Si/SiO2 under similar conditions. This highly anisotropic hydrogen etching technology may work as a simple and convenient way to determine graphene crystal orientation and grain size, and may enable the etching of graphene into nanoribbons for electronic applications.

Effect of additional etching and ethanol-wet bonding on the dentin bond strength of one-step self-etch adhesives

PubMed Central

Ahn, Joonghee; Jung, Kyoung-Hwa; Son, Sung-Ae; Hur, Bock; Kwon, Yong-Hoon

2015-01-01

Objectives This study examined the effects of additional acid etching on the dentin bond strength of one-step self-etch adhesives with different compositions and pH. The effect of ethanol wetting on etched dentin bond strength of self-etch adhesives was also evaluated. Materials and Methods Forty-two human permanent molars were classified into 21 groups according to the adhesive types (Clearfil SE Bond [SE, control]; G-aenial Bond [GB]; Xeno V [XV]; Beauti Bond [BB]; Adper Easy Bond [AE]; Single Bond Universal [SU]; All Bond Universal [AU]), and the dentin conditioning methods. Composite resins were placed on the dentin surfaces, and the teeth were sectioned. The microtensile bond strength was measured, and the failure mode of the fractured specimens was examined. The data were analyzed statistically using two-way ANOVA and Duncan's post hoc test. Results In GB, XV and SE (pH ≤ 2), the bond strength was decreased significantly when the dentin was etched (p < 0.05). In BB, AE and SU (pH 2.4 - 2.7), additional etching did not affect the bond strength (p > 0.05). In AU (pH = 3.2), additional etching increased the bond strength significantly (p < 0.05). When adhesives were applied to the acid etched dentin with ethanol-wet bonding, the bond strength was significantly higher than that of the no ethanol-wet bonding groups, and the incidence of cohesive failure was increased. Conclusions The effect of additional acid etching on the dentin bond strength was influenced by the pH of one-step self-etch adhesives. Ethanol wetting on etched dentin could create a stronger bonding performance of one-step self-etch adhesives for acid etched dentin. PMID:25671215

Separating semiconductor devices from substrate by etching graded composition release layer disposed between semiconductor devices and substrate including forming protuberances that reduce stiction

DOEpatents

Tauke-Pedretti, Anna; Nielson, Gregory N; Cederberg, Jeffrey G; Cruz-Campa, Jose Luis

2015-05-12

A method includes etching a release layer that is coupled between a plurality of semiconductor devices and a substrate with an etch. The etching includes etching the release layer between the semiconductor devices and the substrate until the semiconductor devices are at least substantially released from the substrate. The etching also includes etching a protuberance in the release layer between each of the semiconductor devices and the substrate. The etch is stopped while the protuberances remain between each of the semiconductor devices and the substrate. The method also includes separating the semiconductor devices from the substrate. Other methods and apparatus are also disclosed.

The potential for dental plaque to protect against erosion using an in vivo-in vitro model--a pilot study.

PubMed

Cheung, A; Zid, Z; Hunt, D; McIntyre, J

2005-12-01

Tooth erosion is a problem for professional wine tasters (exogenous erosion from frequent exposure to wine acids) and for people with gastro oesophageal reflux disease (GORD) and bulimia who experience frequent reflux of gastric contents into the mouth (endogenous erosion from mainly HCl). The objective in this study was to determine whether plaque/pellicle could provide teeth with any protection from two common erosive acids, using an in vivo-in vitro technique. Tiles of human tooth enamel and root surfaces were prepared from six extracted, unerupted third molar teeth and sterilized. Mandibular stents were prepared for six volunteer subjects and the tiles bonded to the buccal flanges of these stents. They were worn initially for three days to permit a layer of pellicle and plaque to form over the tile surfaces, and for a further 10 days of experimentation. Following cleaning of the plaque/ pellicle layer from the tiles on the right side flange, all the tiles were submerged in either 0.06M HCl or white wine for an accumulated time of 600 and 1500 minutes, respectively. Depths of erosion were determined using light microscopy of sections of the enamel and root tiles. SEM of the lesion surfaces was carried out to investigate the nature of erosive damage and of plaque/pellicle remnants. Retained plaque was found to significantly inhibit dental erosion on enamel, from contact with both HCl and wine, compared with that resulting following its removal. However, it was found to provide no significant protection on root surfaces. SEM analysis of the tile surfaces revealed marked etching of enamel on the cleaned surfaces, and considerable alteration to the appearance of remaining plaque and pellicle on most surfaces. Within the limitations of numbers of specimens, dental plaque/pellicle provided a significant level of protection to tooth enamel against dental erosion from simulated gastric acids and from white wine, using an in vivo-in vitro model. It was unable to provide any significant protection to root surfaces from these erosive agents. Possible reasons for this difference are explored.

High rate dry etching of (BiSb)2Te3 film by CH4/H2-based plasma

NASA Astrophysics Data System (ADS)

Song, Junqiang; Shi, Xun; Chen, Lidong

2014-10-01

Etching characteristics of p-type (BiSb)2Te3 films were studied with CH4/H2/Ar gas mixture using an inductively coupled plasma (ICP)-reactive ion etching (RIE) system. The effects of gas mixing ratio, working pressure and gas flow rate on the etch rate and the surface morphology were investigated. The vertical etched profile with the etch rate of 600 nm/min was achieved at the optimized processing parameters. X-ray photoelectron spectroscopy (XPS) analysis revealed the non-uniform etching of (BiSb)2Te3 films due to disparate volatility of the etching products. Micro-masking effects caused by polymer deposition and Bi-rich residues resulted in roughly etched surfaces. Smooth surfaces can be obtained by optimizing the CH4/H2/Ar mixing ratio.

Triangle pore arrays fabricated on Si (111) substrate by sphere lithography combined with metal-assisted chemical etching and anisotropic chemical etching

NASA Astrophysics Data System (ADS)

Asoh, Hidetaka; Fujihara, Kosuke; Ono, Sachiko

2012-07-01

The morphological change of silicon macropore arrays formed by metal-assisted chemical etching using shape-controlled Au thin film arrays was investigated during anisotropic chemical etching in tetramethylammonium hydroxide (TMAH) aqueous solution. After the deposition of Au as the etching catalyst on (111) silicon through a honeycomb mask prepared by sphere lithography, the specimens were etched in a mixed solution of HF and H2O2 at room temperature, resulting in the formation of ordered macropores in silicon along the [111] direction, which is not achievable by conventional chemical etching without a catalyst. In the anisotropic etching in TMAH, the macropores changed from being circular to being hexagonal and finally to being triangular, owing to the difference in etching rate between the crystal planes.

Correlation between surface chemistry and ion energy dependence of the etch yield in multicomponent oxides etching

NASA Astrophysics Data System (ADS)

Bérubé, P.-M.; Poirier, J.-S.; Margot, J.; Stafford, L.; Ndione, P. F.; Chaker, M.; Morandotti, R.

2009-09-01

The influence of surface chemistry in plasma etching of multicomponent oxides was investigated through measurements of the ion energy dependence of the etch yield. Using pulsed-laser-deposited CaxBa(1-x)Nb2O6 (CBN) and SrTiO3 thin films as examples, it was found that the etching energy threshold shifts toward values larger or smaller than the sputtering threshold depending on whether or not ion-assisted chemical etching is the dominant etching pathway and whether surface chemistry is enhancing or inhibiting desorption of the film atoms. In the case of CBN films etched in an inductively coupled Cl2 plasma, it is found that the chlorine uptake is inhibiting the etching reaction, with the desorption of nonvolatile NbCl2 and BaCl2 compounds being the rate-limiting step.

Metal etching composition

NASA Technical Reports Server (NTRS)

Otousa, Joseph E. (Inventor); Thomas, Clark S. (Inventor); Foster, Robert E. (Inventor)

1991-01-01

The present invention is directed to a chemical etching composition for etching metals or metallic alloys. The composition includes a solution of hydrochloric acid, phosphoric acid, ethylene glycol, and an oxidizing agent. The etching composition is particularly useful for etching metal surfaces in preparation for subsequent fluorescent penetrant inspection.

New frontiers of atomic layer etching

NASA Astrophysics Data System (ADS)

Sherpa, Sonam D.; Ranjan, Alok

2018-03-01

Interest in atomic layer etching (ALE) has surged recently because it offers several advantages over continuous or quasicontinuous plasma etching. These benefits include (1) independent control of ion energy, ion flux, and radical flux, (2) flux-independent etch rate that mitigates the iso-dense loading effects, and (3) ability to control the etch rate with atomic or nanoscale precision. In addition to these benefits, we demonstrate an area-selective etching for maskless lithography as a new frontier of ALE. In this paper, area-selective etching refers to the confinement of etching into the specific areas of the substrate. The concept of area-selective etching originated during our studies on quasi-ALE of silicon nitride which consists of sequential exposure of silicon nitride to hydrogen and fluorinated plasma. The findings of our studies reported in this paper suggest that it may be possible to confine the etching into specific areas of silicon nitride without using any mask by replacing conventional hydrogen plasma with a localized source of hydrogen ions.

Silicon etching using only Oxygen at high temperature: An alternative approach to Si micro-machining on 150 mm Si wafers

NASA Astrophysics Data System (ADS)

Chai, Jessica; Walker, Glenn; Wang, Li; Massoubre, David; Tan, Say Hwa; Chaik, Kien; Hold, Leonie; Iacopi, Alan

2015-12-01

Using a combination of low-pressure oxygen and high temperatures, isotropic and anisotropic silicon (Si) etch rates can be controlled up to ten micron per minute. By varying the process conditions, we show that the vertical-to-lateral etch rate ratio can be controlled from 1:1 isotropic etch to 1.8:1 anisotropic. This simple Si etching technique combines the main respective advantages of both wet and dry Si etching techniques such as fast Si etch rate, stiction-free, and high etch rate uniformity across a wafer. In addition, this alternative O2-based Si etching technique has additional advantages not commonly associated with dry etchants such as avoiding the use of halogens and has no toxic by-products, which improves safety and simplifies waste disposal. Furthermore, this process also exhibits very high selectivity (>1000:1) with conventional hard masks such as silicon carbide, silicon dioxide and silicon nitride, enabling deep Si etching. In these initial studies, etch rates as high as 9.2 μm/min could be achieved at 1150 °C. Empirical estimation for the calculation of the etch rate as a function of the feature size and oxygen flow rate are presented and used as proof of concepts.

In vitro bonding effectiveness of three different one-step self-etch adhesives with additional enamel etching.

PubMed

Batra, Charu; Nagpal, Rajni; Tyagi, Shashi Prabha; Singh, Udai Pratap; Manuja, Naveen

2014-08-01

To evaluate the effect of additional enamel etching on the shear bond strength of three self-etch adhesives. Class II box type cavities were made on extracted human molars. Teeth were randomly divided into one control group of etch and rinse adhesive and three test groups of self-etch adhesives (Clearfil S3 Bond, Futurabond NR, Xeno V). The teeth in the control group (n = 10) were treated with Adper™ Single Bond 2. The three test groups were further divided into two subgroups (n = 10): (i) self-etch adhesive was applied as per the manufacturer's instructions; (ii) additional etching of enamel surfaces was done prior to the application of self-etch adhesives. All cavities were restored with Filtek Z250. After thermocycling, shear bond strength was evaluated using a Universal testing machine. Data were analyzed using anova independent sample's 't' test and Dunnett's test. The failure modes were evaluated with a stereomicroscope at a magnification of 10×. Additional phosphoric acid etching of the enamel surface prior to the application of the adhesive system significantly increased the shear bond strength of all the examined self-etch adhesives. Additional phosphoric acid etching of enamel surface significantly improved the shear bond strength. © 2013 Wiley Publishing Asia Pty Ltd.

Inductively Coupled Plasma-Induced Electrical Damage on HgCdTe Etched Surface at Cryogenic Temperatures

NASA Astrophysics Data System (ADS)

Liu, L. F.; Chen, Y. Y.; Ye, Z. H.; Hu, X. N.; Ding, R. J.; He, L.

2018-03-01

Plasma etching is a powerful technique for transferring high-resolution lithographic patterns into HgCdTe material with low etch-induced damage, and it is important for fabricating small-pixel-size HgCdTe infrared focal plane array (IRFPA) detectors. P- to n-type conversion is known to occur during plasma etching of vacancy-doped HgCdTe; however, it is usually unwanted and its removal requires extra steps. Etching at cryogenic temperatures can reduce the etch-induced type conversion depth in HgCdTe via the electrical damage mechanism. Laser beam-induced current (LBIC) is a nondestructive photoelectric characterization technique which can provide information regarding the vertical and lateral electrical field distribution, such as defects and p-n junctions. In this work, inductively coupled plasma (ICP) etching of HgCdTe was implemented at cryogenic temperatures. For an Ar/CH4 (30:1 in SCCM) plasma with ICP input power of 1000 W and RF-coupled DC bias of ˜ 25 V, a HgCdTe sample was dry-etched at 123 K for 5 min using ICP. The sample was then processed to remove a thin layer of the plasma-etched region while maintaining a ladder-like damaged layer by continuously controlling the wet chemical etching time. Combining the ladder etching method and LBIC measurement, the ICP etching-induced electrical damage depth was measured and estimated to be about 20 nm. The results indicate that ICP etching at cryogenic temperatures can significantly suppress plasma etching-induced electrical damage, which is beneficial for defining HgCdTe mesa arrays.

Etching of enamel for direct bonding with a thulium fiber laser

NASA Astrophysics Data System (ADS)

Kabaş Sarp, Ayşe S.; Gülsoy, Murat

2011-03-01

Background: Laser etching of enamel for direct bonding can decrease the risk of surface enamel loss and demineralization which are the adverse effects of acid etching technique. However, in excess of +5.5°C can cause irreversible pulpal responses. In this study, a 1940- nm Thulium Fiber Laser in CW mode was used for laser etching. Aim: Determination of the suitable Laser parameters of enamel surface etching for direct bonding of ceramic brackets and keeping that intrapulpal temperature changes below the threshold value. Material and Method: Polycrystalline ceramic orthodontic brackets were bonded on bovine teeth by using 2 different kinds of etching techniques: Acid and Laser Etching. In addition to these 3 etched groups, there was also a group which was bonded without etching. Brackets were debonded with a material testing machine. Breaking time and the load at the breaking point were measured. Intrapulpal temperature changes were recorded by a K-type Thermocouple. For all laser groups, intrapulpal temperature rise was below the threshold value of 5.5°C. Results and Conclusion: Acid-etched group ( 11.73 MPa) significantly required more debonding force than 3- second- irradiated ( 5.03 MPa) and non-etched groups ( 3.4 MPa) but the results of acid etched group and 4- second- irradiated group (7.5 MPa) showed no significant difference. Moreover, 4- second irradiated group was over the minimum acceptable value for clinical use. Also, 3- second lasing caused a significant reduction in time according to acid-etch group. As a result, 1940- nm laser irradiation is a promising method for laser etching.

Does active application of universal adhesives to enamel in self-etch mode improve their performance?

PubMed

Loguercio, Alessandro D; Muñoz, Miguel Angel; Luque-Martinez, Issis; Hass, Viviane; Reis, Alessandra; Perdigão, Jorge

2015-09-01

To evaluate the effect of adhesion strategy on the enamel microshear bond strengths (μSBS), etching pattern, and in situ degree of conversion (DC) of seven universal adhesives. 84 extracted third molars were sectioned in four parts (buccal, lingual, proximal) and divided into 21 groups, according to the combination of the main factors adhesive (AdheSE Universal [ADU], All-Bond Universal [ABU], Clearfil Universal [CFU], Futurabond U [FBU], G-Bond Plus [GBP], Prime&Bond Elect (PBE), and Scotchbond Universal Adhesive [SBU]), and adhesion strategy (etch-and-rinse, active self-etch, and passive self-etch). Specimens were stored in water (37°C/24h) and tested at 1.0mm/min (μSBS). Enamel-resin interfaces were evaluated for DC using micro-Raman spectroscopy. The enamel-etching pattern was evaluated under a field-emission scanning electron microscope (direct and replica techniques). Data were analyzed with two-way ANOVA and Tukey's test (α=0.05). Active self-etch application increased μSBS and DC for five out of the seven universal adhesives when compared to passive application (p<0.001). A deeper enamel-etching pattern was observed for all universal adhesives in the etch-and-rinse strategy. A slight improvement in etching ability was observed in active self-etch application compared to that of passive self-etch application. Replicas of GBP and PBE applied in active self-etch mode displayed morphological features compatible with water droplets. The DC of GBP and PBE were not affected by the application/strategy mode. In light of the improved performance of universal adhesives when applied actively in SE mode, selective enamel etching with phosphoric acid may not be crucial for their adhesion to enamel. The active application of universal adhesives in self-etch mode may be a practical alternative to enamel etching in specific clinical situations. Copyright © 2015 Elsevier Ltd. All rights reserved.

A comparison of orthodontic bracket shear bond strength on enamel deproteinized by 5.25% sodium hypochlorite using total etch and self-etch primer

NASA Astrophysics Data System (ADS)

Ongkowidjaja, F.; Soegiharto, B. M.; Purbiati, M.

2017-08-01

The shear bond strength (SBS) can be increased by removing protein pellicles from the enamel surface by deproteinization using 5.25% sodium hypochlorite (NaOCl). The SBS of a self-etch primer is lower than that of a total etch primer; nonetheless, it prevents white spot lesions. This study aimed to assess the SBS of the Anyetch (AE) total etch primer and FL-Bond II Shofu (FL) self-etch primer after enamel deproteinization using 5.25% NaOCl. Forty eight human maxillary first premolars were extracted, cleaned, and divided into four groups. In group A, brackets were bonded to the enamel without deproteinization before etching (A1: 10 teeth using total etch primer (AE); A2: 10 teeth using self-etch primer (FL)). In group B, brackets were bonded to the enamel after deproteinization with 5.25% NaOCl before etching (B1: 10 teeth using total etch primer (AE); B2: 10 teeth using self-etch primer (FL)). Brackets were bonded using Transbond XT, stored in artificial saliva for 24 h at 37°C, mounted on acrylic cylinders, and debonded using a Shimadzu AG-5000 universal testing machine. There were no significant differences in SBS between the total etch (AE) groups (p > 0.05) and between the self-etch (FL) groups (p > 0.05). There were significant differences in SBS between groups A and B. The mean SBS for groups A1, A2, B1, and B2 was 12.91±3.99, 4.46±2.47, 13.06±3.66, and 3.62±2.36 MPa, respectively. Deproteinization using NaOCl did not affect the SBS of the total etch primer (AE) group; it reduced the SBS of the self-etch primer (FL) group, but not with a statistically significant difference.

Isotropic plasma etching of Ge Si and SiN x films

DOE PAGES

Henry, Michael David; Douglas, Erica Ann

2016-08-31

This study reports on selective isotropic dry etching of chemically vapor deposited (CVD) Ge thin film, release layers using a Shibaura chemical downstream etcher (CDE) with NF 3 and Ar based plasma chemistry. Relative etch rates between Ge, Si and SiN x are described with etch rate reductions achieved by adjusting plasma chemistry with O 2. Formation of oxides reducing etch rates were measured for both Ge and Si, but nitrides or oxy-nitrides created using direct injection of NO into the process chamber were measured to increase Si and SiN x etch rates while retarding Ge etching.

Cyclic etching of tin-doped indium oxide using hydrogen-induced modified layer

NASA Astrophysics Data System (ADS)

Hirata, Akiko; Fukasawa, Masanaga; Nagahata, Kazunori; Li, Hu; Karahashi, Kazuhiro; Hamaguchi, Satoshi; Tatsumi, Tetsuya

2018-06-01

The rate of etching of tin-doped indium oxide (ITO) and the effects of a hydrogen-induced modified layer on cyclic, multistep thin-layer etching were investigated. It was found that ITO cyclic etching is possible by precisely controlling the hydrogen-induced modified layer. Highly selective etching of ITO/SiO2 was also investigated, and it was suggested that cyclic etching by selective surface adsorption of Si can precisely control the etch rates of ITO and SiO2, resulting in an almost infinite selectivity for ITO over SiO2 and in improved profile controllability.

Ion-beam-assisted etching of diamond

NASA Technical Reports Server (NTRS)

Efremow, N. N.; Geis, M. W.; Flanders, D. C.; Lincoln, G. A.; Economou, N. P.

1985-01-01

The high thermal conductivity, low RF loss, and inertness of diamond make it useful in traveling wave tubes operating in excess of 500 GHz. Such use requires the controlled etching of type IIA diamond to produce grating like structures tens of micrometers deep. Previous work on reactive ion etching with O2 gave etching rates on the order of 20 nm/min and poor etch selectivity between the masking material (Ni or Cr) and the diamond. An alternative approach which uses a Xe(+) beam and a reactive gas flux of NO2 in an ion-beam-assisted etching system is reported. An etching rate of 200 nm/min was obtained with an etching rate ratio of 20 between the diamond and an aluminum mask.

Metal-assisted etch combined with regularizing etch

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yim, Joanne; Miller, Jeff; Jura, Michael

In an aspect of the disclosure, a process for forming nanostructuring on a silicon-containing substrate is provided. The process comprises (a) performing metal-assisted chemical etching on the substrate, (b) performing a clean, including partial or total removal of the metal used to assist the chemical etch, and (c) performing an isotropic or substantially isotropic chemical etch subsequently to the metal-assisted chemical etch of step (a). In an alternative aspect of the disclosure, the process comprises (a) performing metal-assisted chemical etching on the substrate, (b) cleaning the substrate, including removal of some or all of the assisting metal, and (c) performingmore » a chemical etch which results in regularized openings in the silicon substrate.« less

Difference in anisotropic etching characteristics of alkaline and copper based acid solutions for single-crystalline Si.

PubMed

Chen, Wei; Liu, Yaoping; Yang, Lixia; Wu, Juntao; Chen, Quansheng; Zhao, Yan; Wang, Yan; Du, Xiaolong

2018-02-21

The so called inverted pyramid arrays, outperforming conventional upright pyramid textures, have been successfully achieved by one-step Cu assisted chemical etching (CACE) for light reflection minimization in silicon solar cells. Due to the lower reduction potential of Cu 2+ /Cu and different electronic properties of different Si planes, the etching of Si substrate shows orientation-dependent. Different from the upright pyramid obtained by alkaline solutions, the formation of inverted pyramid results from the coexistence of anisotropic etching and localized etching process. The obtained structure is bounded by Si {111} planes which have the lowest etching rate, no matter what orientation of Si substrate is. The Si etching rate and (100)/(111) etching ratio are quantitatively analyzed. The different behaviors of anisotropic etching of Si by alkaline and Cu based acid etchant have been systematically investigated.

Silicon etching of difluoromethane atmospheric pressure plasma jet combined with its spectroscopic analysis

NASA Astrophysics Data System (ADS)

Sung, Yu-Ching; Wei, Ta-Chin; Liu, You-Chia; Huang, Chun

2018-06-01

A capacitivly coupled radio-frequency double-pipe atmospheric-pressure plasma jet is used for etching. An argon carrier gas is supplied to the plasma discharge jet; and CH2F2 etch gas is inserted into the plasma discharge jet, near the silicon substrate. Silicon etchings rate can be efficiently-controlled by adjusting the feeding etching gas composition and plasma jet operating parameters. The features of silicon etched by the plasma discharge jet are discussed in order to spatially spreading plasma species. Electronic excitation temperature and electron density are detected by increasing plasma power. The etched silicon profile exhibited an anisotropic shape and the etching rate was maximum at the total gas flow rate of 4500 sccm and CH2F2 concentration of 11.1%. An etching rate of 17 µm/min was obtained at a plasma power of 100 W.

Uniform lateral etching of tungsten in deep trenches utilizing reaction-limited NF3 plasma process

NASA Astrophysics Data System (ADS)

Kofuji, Naoyuki; Mori, Masahito; Nishida, Toshiaki

2017-06-01

The reaction-limited etching of tungsten (W) with NF3 plasma was performed in an attempt to achieve the uniform lateral etching of W in a deep trench, a capability required by manufacturing processes for three-dimensional NAND flash memory. Reaction-limited etching was found to be possible at high pressures without ion irradiation. An almost constant etching rate that showed no dependence on NF3 pressure was obtained. The effect of varying the wafer temperature was also examined. A higher wafer temperature reduced the threshold pressure for reaction-limited etching and also increased the etching rate in the reaction-limited region. Therefore, the control of the wafer temperature is crucial to controlling the etching amount by this method. We found that the uniform lateral etching of W was possible even in a deep trench where the F radical concentration was low.

Inverse metal-assisted chemical etching produces smooth high aspect ratio InP nanostructures.

PubMed

Kim, Seung Hyun; Mohseni, Parsian K; Song, Yi; Ishihara, Tatsumi; Li, Xiuling

2015-01-14

Creating high aspect ratio (AR) nanostructures by top-down fabrication without surface damage remains challenging for III-V semiconductors. Here, we demonstrate uniform, array-based InP nanostructures with lateral dimensions as small as sub-20 nm and AR > 35 using inverse metal-assisted chemical etching (I-MacEtch) in hydrogen peroxide (H2O2) and sulfuric acid (H2SO4), a purely solution-based yet anisotropic etching method. The mechanism of I-MacEtch, in contrast to regular MacEtch, is explored through surface characterization. Unique to I-MacEtch, the sidewall etching profile is remarkably smooth, independent of metal pattern edge roughness. The capability of this simple method to create various InP nanostructures, including high AR fins, can potentially enable the aggressive scaling of InP based transistors and optoelectronic devices with better performance and at lower cost than conventional etching methods.

Capabilities of ICP-RIE cryogenic dry etching of silicon: review of exemplary microstructures

NASA Astrophysics Data System (ADS)

Sökmen, Ü.; Stranz, A.; Fündling, S.; Wehmann, H.-H.; Bandalo, V.; Bora, A.; Tornow, M.; Waag, A.; Peiner, E.

2009-10-01

Inductively coupled plasma (ICP) cryogenic dry etching was used to etch submicron pores, nano contact lines, submicron diameter pillars, thin and thick cantilevers, membrane structures and anisotropic deep structures with high aspect ratios in silicon for bio-nanoelectronics, optoelectronics and nano-micro electromechanical systems (NMEMS). The ICP cryogenic dry etching gives us the advantage of switching plasmas between etch rates of 13 nm min-1 and 4 µm min-1 for submicron pores and for membrane structures, respectively. A very thin photoresist mask can endure at -75 °C even during etching 70 µm deep for cantilevers and 300 µm deep for membrane structures. Coating the backsides of silicon membrane substrates with a thin photoresist film inhibited the lateral etching of cantilevers during their front release. Between -95 °C and -140 °C, we realized crystallographic-plane-dependent etching that creates facets only at the etch profile bottom. By varying the oxygen content and the process temperature, we achieved good control over the shape of the etched structures. The formation of black silicon during membrane etching down to 300 µm was delayed by reducing the oxygen content.

A Study on Ohmic Contact to Dry-Etched p-GaN

NASA Astrophysics Data System (ADS)

Hu, Cheng-Yu; Ao, Jin-Ping; Okada, Masaya; Ohno, Yasuo

Low-power dry-etching process has been adopted to study the influence of dry-etching on Ohmic contact to p-GaN. When the surface layer of as-grown p-GaN was removed by low-power SiCl4/Cl2-etching, no Ohmic contact can be formed on the low-power dry-etched p-GaN. The same dry-etching process was also applied on n-GaN to understand the influence of the low-power dry-etching process. By capacitance-voltage (C-V) measurement, the Schottky barrier heights (SBHs) of p-GaN and n-GaN were measured. By comparing the change of measured SBHs on p-GaN and n-GaN, it was suggested that etching damage is not the only reason responsible for the degraded Ohmic contacts to dry-etched p-GaN and for Ohmic contact formatin, the original surface layer of as-grown p-GaN have some special properties, which were removed by dry-etching process. To partially recover the original surface of as-grown p-GaN, high temperature annealing (1000°C 30s) was tried on the SiCl4/Cl2-etched p-GaN and Ohmic contact was obtained.

ScAlN etch mask for highly selective silicon etching

DOE PAGES

Henry, Michael David; Young, Travis R.; Griffin, Ben

2017-09-08

Here, this work reports the utilization of a recently developed film, ScAlN, as a silicon etch mask offering significant improvements in high etch selectivity to silicon. Utilization of ScAlN as a fluorine chemistry based deep reactive ion etch mask demonstrated etch selectivity at 23 550:1, four times better than AlN, 11 times better than Al 2O 3, and 148 times better than silicon dioxide with significantly less resputtering at high bias voltage than either Al 2O 3 or AlN. Ellipsometry film thickness measurements show less than 0.3 nm/min mask erosion rates for ScAlN. Micromasking of resputtered Al for Al 2Omore » 3, AlN, and ScAlN etch masks is also reported here, utilizing cross-sectional scanning electron microscope and confocal microscope roughness measurements. With lower etch bias, the reduced etch rate can be optimized to achieve a trench bottom surface roughness that is comparable to SiO 2 etch masks. Etch mask selectivity enabled by ScAlN is likely to make significant improvements in microelectromechanical systems, wafer level packaging, and plasma dicing of silicon.« less

Photo-assisted etching of silicon in chlorine- and bromine-containing plasmas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhu, Weiye; Sridhar, Shyam; Liu, Lei

2014-05-28

Cl{sub 2}, Br{sub 2}, HBr, Br{sub 2}/Cl{sub 2}, and HBr/Cl{sub 2} feed gases diluted in Ar (50%–50% by volume) were used to study etching of p-type Si(100) in a rf inductively coupled, Faraday-shielded plasma, with a focus on the photo-assisted etching component. Etching rates were measured as a function of ion energy. Etching at ion energies below the threshold for ion-assisted etching was observed in all cases, with Br{sub 2}/Ar and HBr/Cl{sub 2}/Ar plasmas having the lowest and highest sub-threshold etching rates, respectively. Sub-threshold etching rates scaled with the product of surface halogen coverage (measured by X-ray photoelectron spectroscopy) andmore » Ar emission intensity (7504 Å). Etching rates measured under MgF{sub 2}, quartz, and opaque windows showed that sub-threshold etching is due to photon-stimulated processes on the surface, with vacuum ultraviolet photons being much more effective than longer wavelengths. Scanning electron and atomic force microscopy revealed that photo-etched surfaces were very rough, quite likely due to the inability of the photo-assisted process to remove contaminants from the surface. Photo-assisted etching in Cl{sub 2}/Ar plasmas resulted in the formation of 4-sided pyramidal features with bases that formed an angle of 45° with respect to 〈110〉 cleavage planes, suggesting that photo-assisted etching can be sensitive to crystal orientation.« less

Etching characteristics of Si{110} in 20 wt% KOH with addition of hydroxylamine for the fabrication of bulk micromachined MEMS

NASA Astrophysics Data System (ADS)

Rao, A. V. Narasimha; Swarnalatha, V.; Pal, P.

2017-12-01

Anisotropic wet etching is a most widely employed for the fabrication of MEMS/NEMS structures using silicon bulk micromachining. The use of Si{110} in MEMS is inevitable when a microstructure with vertical sidewall is to be fabricated using wet anisotropic etching. In most commonly employed etchants (i.e. TMAH and KOH), potassium hydroxide (KOH) exhibits higher etch rate and provides improved anisotropy between Si{111} and Si{110} planes. In the manufacturing company, high etch rate is demanded to increase the productivity that eventually reduces the cost of end product. In order to modify the etching characteristics of KOH for the micromachining of Si{110}, we have investigated the effect of hydroxylamine (NH2OH) in 20 wt% KOH solution. The concentration of NH2OH is varied from 0 to 20% and the etching is carried out at 75 °C. The etching characteristics which are studied in this work includes the etch rates of Si{110} and silicon dioxide, etched surface morphology, and undercutting at convex corners. The etch rate of Si{110} in 20 wt% KOH + 15% NH2OH solution is measured to be four times more than that of pure 20 wt% KOH. Moreover, the addition of NH2OH increases the undercutting at convex corners and enhances the etch selectivity between Si and SiO2.

Comparison of enamel bond fatigue durability of universal adhesives and two-step self-etch adhesives in self-etch mode.

PubMed

Tsujimoto, Akimasa; Barkmeier, Wayne W; Hosoya, Yumiko; Nojiri, Kie; Nagura, Yuko; Takamizawa, Toshiki; Latta, Mark A; Miyazaki, Masashi

2017-10-01

To comparatively evaluate universal adhesives and two-step self-etch adhesives for enamel bond fatigue durability in self-etch mode. Three universal adhesives (Clearfil Universal Bond; G-Premio Bond; Scotchbond Universal Adhesive) and three two-step self-etch adhesives (Clearfil SE Bond; Clearfil SE Bond 2; OptiBond XTR) were used. The initial shear bond strength and shear fatigue strength of the adhesive to enamel in self-etch mode were determined. The initial shear bond strengths of the universal adhesives to enamel in self-etch mode was significantly lower than those of two-step self-etch adhesives and initial shear bond strengths were not influenced by type of adhesive in each adhesive category. The shear fatigue strengths of universal adhesives to enamel in self-etch mode were significantly lower than that of Clearfil SE Bond and Clearfil SE Bond 2, but similar to that OptiBond XTR. Unlike two-step self-etch adhesives, the initial shear bond strength and shear fatigue strength of universal adhesives to enamel in self-etch mode was not influenced by the type of adhesive. This laboratory study showed that the enamel bond fatigue durability of universal adhesives was lower than Clearfil SE Bond and Clearfil SE Bond 2, similar to Optibond XTR, and was not influenced by type of adhesive, unlike two-step self-etch adhesives.

Determination of etching parameters for pulsed XeF2 etching of silicon using chamber pressure data

NASA Astrophysics Data System (ADS)

Sarkar, Dipta; Baboly, M. G.; Elahi, M. M.; Abbas, K.; Butner, J.; Piñon, D.; Ward, T. L.; Hieber, Tyler; Schuberth, Austin; Leseman, Z. C.

2018-04-01

A technique is presented for determination of the depletion of the etchant, etched depth, and instantaneous etch rate for Si etching with XeF2 in a pulsed etching system in real time. The only experimental data required is the pressure data collected temporally. Coupling the pressure data with the knowledge of the chemical reactions allows for the determination of the etching parameters of interest. Using this technique, it is revealed that pulsed etching processes are nonlinear, with the initial etch rate being the highest and monotonically decreasing as the etchant is depleted. With the pulsed etching system introduced in this paper, the highest instantaneous etch rate of silicon was recorded to be 19.5 µm min-1 for an initial pressure of 1.2 Torr for XeF2. Additionally, the same data is used to determine the rate constant for the reaction of XeF2 with Si; the reaction is determined to be second order in nature. The effect of varying the exposed surface area of Si as well as the effect that pressure has on the instantaneous etch rate as a function of time is shown applying the same technique. As a proof of concept, an AlN resonator is released using XeF2 pulses to remove a sacrificial poly-Si layer.

Comparative study of resist stabilization techniques for metal etch processing

NASA Astrophysics Data System (ADS)

Becker, Gerry; Ross, Matthew F.; Wong, Selmer S.; Minter, Jason P.; Marlowe, Trey; Livesay, William R.

1999-06-01

This study investigates resist stabilization techniques as they are applied to a metal etch application. The techniques that are compared are conventional deep-UV/thermal stabilization, or UV bake, and electron beam stabilization. The electron beam tool use din this study, an ElectronCure system from AlliedSignal Inc., ELectron Vision Group, utilizes a flood electron source and a non-thermal process. These stabilization techniques are compared with respect to a metal etch process. In this study, two types of resist are considered for stabilization and etch: a g/i-line resist, Shipley SPR-3012, and an advanced i-line, Shipley SPR 955- Cm. For each of these resist the effects of stabilization on resist features are evaluated by post-stabilization SEM analysis. Etch selectivity in all cases is evaluated by using a timed metal etch, and measuring resists remaining relative to total metal thickness etched. Etch selectivity is presented as a function of stabilization condition. Analyses of the effects of the type of stabilization on this method of selectivity measurement are also presented. SEM analysis was also performed on the features after a compete etch process, and is detailed as a function of stabilization condition. Post-etch cleaning is also an important factor impacted by pre-etch resist stabilization. Results of post- etch cleaning are presented for both stabilization methods. SEM inspection is also detailed for the metal features after resist removal processing.

Inorganic Bi/In thermal resist as a high-etch-ratio patterning layer for CF4/CHF3/O2 plasma etch

NASA Astrophysics Data System (ADS)

Tu, Yuqiang; Chapman, Glenn H.; Peng, Jun

2004-05-01

Bimetallic thin films containing indium and with low eutectic points, such as Bi/In, have been found to form highly sensitive thermal resists. They can be exposed by lasers with a wide range of wavelengths and be developed by diluted RCA2 solutions. The exposed bimetallic resist Bi/In can work as an etch masking layer for alkaline-based (KOH, TMAH and EDP) "wet" Si anisotropic etching. Current research shows that it can also act as a patterning and masking layer for Si and SiO2 plasma "dry" etch using CF4/CHF3. The profile of etched structures can be tuned by adding CHF3 and other gases such as Ar, and by changing the CF4/CHF3 ratio. Depending on the fluorocarbon plasma etching recipe the etch rate of laser exposed Bi/In can be as low as 0.1nm/min, 500 times lower than organic photoresists. O2 plasma ashing has little etching effect on exposed Bi/In, indicating that laser exposure is an oxidation process. Experiment result shows that single metal Indium film and bilayer Sn/In exhibit thermal resist characteristics but at higher exposure levels. They can be developed in diluted RCA2 solution and used as etch mask layers for Si anisotropic etch and plasma etch.

Controlled in situ etch-back

NASA Technical Reports Server (NTRS)

Mattauch, R. J.; Seabaugh, A. C. (Inventor)

1981-01-01

A controlled in situ etch-back technique is disclosed in which an etch melt and a growth melt are first saturated by a source-seed crystal and thereafter etch-back of a substrate takes place by the slightly undersaturated etch melt, followed by LPE growth of a layer by the growth melt, which is slightly supersaturated.

Method for anisotropic etching in the manufacture of semiconductor devices

NASA Technical Reports Server (NTRS)

Koontz, Steven L. (Inventor); Cross, Jon B. (Inventor)

1993-01-01

Hydrocarbon polymer coatings used in microelectronic manufacturing processes are anisotropically etched by hyperthermal atomic oxygen beams (translational energies of 0.2 to 20 eV, preferably 1 to 10 eV). Etching with hyperthermal oxygen atom species obtains highly anisotropic etching with sharp boundaries between etched and mask protected areas.

Method for anisotropic etching in the manufacture of semiconductor devices

DOEpatents

Koontz, Steven L.; Cross, Jon B.

1993-01-01

Hydrocarbon polymer coatings used in microelectronic manufacturing processes are anisotropically etched by atomic oxygen beams (translational energies of 0.2-20 eV, preferably 1-10 eV). Etching with hyperthermal (kinetic energy>1 eV) oxygen atom species obtains highly anisotropic etching with sharp boundaries between etched and mask-protected areas.

DOE Office of Scientific and Technical Information (OSTI.GOV)

Yin Yunpeng; Sawin, Herbert H.

The impact of etching kinetics and etching chemistries on surface roughening was investigated by etching thermal silicon dioxide and low-k dielectric coral materials in C{sub 4}F{sub 8}/Ar plasma beams in an inductive coupled plasma beam reactor. The etching kinetics, especially the angular etching yield curves, were measured by changing the plasma pressure and the feed gas composition which influence the effective neutral-to-ion flux ratio during etching. At low neutral-to-ion flux ratios, the angular etching yield curves are sputteringlike, with a peak around 60 deg. -70 deg. off-normal angles; the surface at grazing ion incidence angles becomes roughened due to ionmore » scattering related ion-channeling effects. At high neutral-to-ion flux ratios, ion enhanced etching dominates and surface roughening at grazing angles is mainly caused by the local fluorocarbon deposition induced micromasking mechanism. Interestingly, the etched surfaces at grazing angles remain smooth for both films at intermediate neutral-to-ion flux ratio regime. Furthermore, the oxygen addition broadens the region over which the etching without roughening can be performed.« less

Scanning electron microscopy evaluation of the effect of etching agents on human enamel surface.

PubMed

Zanet, Caio G; Arana-Chavez, Victor E; Fava, Marcelo

2006-01-01

Acid etching promotes microporosities on enamel surface, which provide a better bonding surface to adhesive materials. The purpose of this study was to comparatively analyze the microstructure of enamel surface after etching with 37% phosphoric acid or with two self-etching primers, Non-rinse conditioner (NRC) and Clearfil SE Bond (CSEB) using scanning electron microscopy. Thirty sound premolars were divided into 3 groups with ten teeth each: Group 1: the buccal surface was etched with 37% phosphoric acid for 15 seconds; Group 2: the buccal surface was etched with NRC for 20 seconds; Group 3: the buccal surface was etched with CSEB for 20 seconds. Teeth from Group 1 were rinsed with water; teeth from all groups were air-dried for 15 seconds. After that, all specimens were processed for scanning electron microscopy and analyzed in a Jeol 6100 SEM. The results showed deeper etching when the enamel surface was etched with 37% phosphoric acid, followed by NRC and CSEB. It is concluded that 37% phosphoric acid is still the best agent for a most effective enamel etching.

Enhancement of Device Performances in GaN-Based Light-Emitting Diodes Using Nano-Sized Surface Pit.

PubMed

Yeon, Seunghwan; Son, Taejoon; Shin, Dong Su; Jung, Kyung-Young; Park, Jinsub

2015-07-01

We report the improvement in optical and electrical properties of GaN-based green light-emitting diodes (LEDs) with nano-sized etch pits formed by the surface chemical etching. In order to control the density and sizes of etch pits formed on top surface of green LEDs, H3PO4 solution is used as a etchant with different etching time. When the etching time was increased from 0 min to 20 min, both the etch pit size and density were gradually increased. The improvement of extraction efficiency of LEDs using surface etching method can be attributed to the enlarged escape angle of generated photon by roughened p-GaN surface. The finite-difference time-domain (FDTD) simulation results well agreed with experimentally observed results. Moreover, the LED with etched p-GaN surface for 5 min shows the lowest leakage current value and the further increase of etching time resulting in increase of densities of the large-sized etch pit makes the degradation of electrical properties of LEDs.

Dry etching technologies for reflective multilayer

NASA Astrophysics Data System (ADS)

Iino, Yoshinori; Karyu, Makoto; Ita, Hirotsugu; Kase, Yoshihisa; Yoshimori, Tomoaki; Muto, Makoto; Nonaka, Mikio; Iwami, Munenori

2012-11-01

We have developed a highly integrated methodology for patterning Extreme Ultraviolet (EUV) mask, which has been highlighted for the lithography technique at the 14nm half-pitch generation and beyond. The EUV mask is characterized as a reflective-type mask which is completely different compared with conventional transparent-type of photo mask. And it requires not only patterning of absorber layer without damaging the underlying multi reflective layers (40 Si/Mo layers) but also etching multi reflective layers. In this case, the dry etch process has generally faced technical challenges such as the difficulties in CD control, etch damage to quartz substrate and low selectivity to the mask resist. Shibaura Mechatronics ARESTM mask etch system and its optimized etch process has already achieved the maximal etch performance at patterning two-layered absorber. And in this study, our process technologies of multi reflective layers will be evaluated by means of optimal combination of process gases and our optimized plasma produced by certain source power and bias power. When our ARES™ is used for multilayer etching, the user can choose to etch the absorber layer at the same time or etch only the multilayer.

Single Etch-Pit Shape on Off-Angled 4H-SiC(0001) Si-Face Formed by Chlorine Trifluoride

NASA Astrophysics Data System (ADS)

Hatayama, Tomoaki; Tamura, Tetsuya; Yano, Hiroshi; Fuyuki, Takashi

2012-07-01

The etch pit shape of an off-angled 4H-SiC Si-face formed by chlorine trifluoride (ClF3) in nitrogen (N2) ambient has been studied. One type of etch pit with a crooked hexagonal shape was formed at an etching temperature below 500 °C. The angle of the etch pit measured from a cross-sectional atomic force microscopy image was about 10° from the [11bar 20] view. The dislocation type of the etch pit was discussed in relation to the etch pit shape and an electron-beam-induced current image.

Photoelectrochemical fabrication of spectroscopic diffraction gratings, phase 2

NASA Technical Reports Server (NTRS)

Rauh, R. David; Carrabba, Michael M.; Li, Jianguo; Cartland, Robert F.; Hachey, John P.; Mathew, Sam

1990-01-01

This program was directed toward the production of Echelle diffraction gratings by a light-driven, electrochemical etching technique (photoelectrochemical etching). Etching is carried out in single crystal materials, and the differential rate of etching of the different crystallographic planes used to define the groove profiles. Etching of V-groove profiles was first discovered by us during the first phase of this project, which was initially conceived as a general exploration of photoelectrochemical etching techniques for grating fabrication. This highly controllable V-groove etching process was considered to be of high significance for producing low pitch Echelles, and provided the basis for a more extensive Phase 2 investigation.

Low-damage direct patterning of silicon oxide mask by mechanical processing

PubMed Central

2014-01-01

To realize the nanofabrication of silicon surfaces using atomic force microscopy (AFM), we investigated the etching of mechanically processed oxide masks using potassium hydroxide (KOH) solution. The dependence of the KOH solution etching rate on the load and scanning density of the mechanical pre-processing was evaluated. Particular load ranges were found to increase the etching rate, and the silicon etching rate also increased with removal of the natural oxide layer by diamond tip sliding. In contrast, the local oxide pattern formed (due to mechanochemical reaction of the silicon) by tip sliding at higher load was found to have higher etching resistance than that of unprocessed areas. The profile changes caused by the etching of the mechanically pre-processed areas with the KOH solution were also investigated. First, protuberances were processed by diamond tip sliding at lower and higher stresses than that of the shearing strength. Mechanical processing at low load and scanning density to remove the natural oxide layer was then performed. The KOH solution selectively etched the low load and scanning density processed area first and then etched the unprocessed silicon area. In contrast, the protuberances pre-processed at higher load were hardly etched. The etching resistance of plastic deformed layers was decreased, and their etching rate was increased because of surface damage induced by the pre-processing. These results show that etching depth can be controlled by controlling the etching time through natural oxide layer removal and mechanochemical oxide layer formation. These oxide layer removal and formation processes can be exploited to realize low-damage mask patterns. PMID:24948891

Ion track etching revisited: II. Electronic properties of aged tracks in polymers

NASA Astrophysics Data System (ADS)

Fink, D.; Muñoz Hernández, G.; Cruz, S. A.; Garcia-Arellano, H.; Vacik, J.; Hnatowicz, V.; Kiv, A.; Alfonta, L.

2018-02-01

We compile here electronic ion track etching effects, such as capacitive-type currents, current spike emission, phase shift, rectification and background currents that eventually emerge upon application of sinusoidal alternating voltages across thin, aged swift heavy ion-irradiated polymer foils during etching. Both capacitive-type currents and current spike emission occur as long as obstacles still prevent a smooth continuous charge carrier passage across the foils. In the case of sufficiently high applied electric fields, these obstacles are overcome by spike emission. These effects vanish upon etchant breakthrough. Subsequent transmitted currents are usually of Ohmic type, but shortly after breakthrough (during the track' core etching) often still exhibit deviations such as strong positive phase shifts. They stem from very slow charge carrier mobility across the etched ion tracks due to retarding trapping/detrapping processes. Upon etching the track's penumbra, one occasionally observes a split-up into two transmitted current components, one with positive and another one with negative phase shifts. Usually, these phase shifts vanish when bulk etching starts. Current rectification upon track etching is a very frequent phenomenon. Rectification uses to inverse when core etching ends and penumbra etching begins. When the latter ends, rectification largely vanishes. Occasionally, some residual rectification remains which we attribute to the aged polymeric bulk itself. Last not least, we still consider background currents which often emerge transiently during track etching. We could assign them clearly to differences in the electrochemical potential of the liquids on both sides of the etched polymer foils. Transient relaxation effects during the track etching cause their eventually chaotic behaviour.

Changes in deciduous and permanent dentinal tubules diameter after several conditioning protocols: In vitro study.

PubMed

de Los Angeles Moyaho-Bernal, María; Contreras-Bulnes, Rosalía; Rodríguez-Vilchis, Laura Emma; Rubio-Rosas, Efraín

2018-05-08

Innovators conditioning protocols are emerged in permanent dentin, however for deciduous dentin the information is limited; the aim of this study was to evaluate in vitro diameter of deciduous and permanent dentinal tubules after several conditioning protocols. Eighty dentin samples were distributed in sixteen groups (n = 5 p/g) and dentin surface was conditioned as follow: G1D/G1P acid etching; G2D/G2P, self-etch adhesive; G3D/G3P, G4D/G4P, Er: YAG laser irradiation at 200 mJ-25.5 J/cm 2 and 300 mJ-38.2 J/cm 2 , at 10 Hz under water spray respectively; G5D/G5P, G6D/G6P, G7D/G7P, and G8D/G8P were irradiated under the same energy densities followed phosphoric acid or self-etch adhesive conditioning. The sample dentin of deciduous and permanent teeth was analyzed with scanning electron microscopy and tubule diameter was evaluated by Image Tools Scandium program. Data were subjected to one-way analysis ANOVA to compare among groups with a level of significance at p ≤ .05. For deciduous dentin, diameters were from 1.52 ± 0.32 µm in G3D to 3.88 ± 0.37 µm in G1D; narrowest and widest diameter, respectively (p < .000). While permanent dentin tubules exhibited diameters from 1.16 ± 0.16/1.19 ± 0.12 µm in G7P/G8P to 2.76 ± 0.28 µm in G6P; narrowest and widest diameter, respectively (p < .000). All dentin conditioning protocols produced more open dentin tubules (diameter size) in deciduous dentin than permanent, specific conditioning protocols are required for each tissue (deciduous or permanent dentin), since same protocol produced stronger effects on primary dentin, which is important for dental clinical success in children and adolescents. © 2018 Wiley Periodicals, Inc.

The use of fixed appliances in the UK: a survey of specialist orthodontists.

PubMed

Banks, Phil; Elton, Victoria; Jones, Yvonne; Rice, Peter; Derwent, Serena; Odondi, Lang'o

2010-03-01

To investigate the use of fixed appliances in the UK. Prospective postal questionnaire. UK. All members of the General Dental Council Specialist List in Orthodontics still in active practice and not in training posts. A preemptive letter of explanation was sent inviting orthodontists to participate in the survey. The questionnaire was subsequently posted to 935 specialists. Data analysis investigated differences in clinical practice related to varying provider groups, level of operator experience and geographical region. The response rate achieved was 66.3%. A majority of orthodontists routinely used the 0.022 inch pre-adjusted edgewise system, standard size Siamese pattern stainless steel brackets, conventionally ligated and bonded using standard etch and light cured composite. Nickel titanium and stainless steel were the most popular archwire materials. Anchorage was supported routinely by palatal and lingual arches in up to 25% and by headgear in over a third of respondents. Newer innovations showed variable popularity. Self-etching primer was used routinely by one-third of respondents with 11% use of self-ligating brackets. Banding of first molars was preferred by over 60% of clinicians. Bone screw implants were used by only 0.2% of respondents. Clinicians with less than 10 years experience used more headgear, light curing, MBT prescription and molar bonding. Operators with over 20 years experience used more chemically cured bonding, Roth prescription, banded first molars, 0.018 inch slot size and Tip-Edge(TM), with less use of headgear. Fixed appliance use differed from that reported in the US with lower use in the UK of standard edgewise and Roth systems, aesthetic, miniaturised and 0.018 inch slot brackets and rapid maxillary expansion. Most UK orthodontic specialists routinely used the 0.022 inch pre-adjusted edgewise system with standard size Siamese steel brackets bonded using standard etch and light cured composite with conventional ligation. Variations were seen between different provider groups, types of treatment funding, levels of operator seniority and geographical regions. Differences were noted particularly in the use of bracket prescription and design, types of molar attachment and anchorage control.

Influence of Application Time and Etching Mode of Universal Adhesives on Enamel Adhesion.

PubMed

Sai, Keiichi; Takamizawa, Toshiki; Imai, Arisa; Tsujimoto, Akimasa; Ishii, Ryo; Barkmeier, Wayne W; Latta, Mark A; Miyazaki, Masashi

2018-01-01

To investigate the influence of application time and etching mode of universal adhesives on enamel adhesion. Five universal adhesives, Adhese Universal, Bondmer Lightless, Clearfil Universal Bond Quick, G-Premio Bond, and Scotchbond Universal, were used. Bovine incisors were prepared and divided into four groups of ten teeth each. SBS, Ra, and SFE were determined after the following procedures: 1. self-etch mode with immediate air blowing after application (IA); 2. self-etch mode with prolonged application time (PA); 3. etch-and-rinse mode with IA; 4. etch-and-rinse mode with PA. After 24-h water storage, the bonded assemblies were subjected to shear bond strength (SBS) tests. For surface roughness (Ra) and surface free energy (SFE) measurements, the adhesives were simply applied to the enamel and rinsed with acetone and water before the measurements were carried out. Significantly higher SBS and Ra values were obtained with etch-and-rinse mode than with self-etch mode regardless of the application time or type of adhesive. Although most adhesives showed decreased SFE values with increased application time in self-etch mode, SFE values in etch-and-rinse mode were dependent on the adhesive type and application time. Etching mode, application time, and type of adhesive significantly influenced the SBS, Ra, and SFE values.

Etching and Growth of GaAs

NASA Technical Reports Server (NTRS)

Seabaugh, A. C.; Mattauch, R., J.

1983-01-01

In-place process for etching and growth of gallium arsenide calls for presaturation of etch and growth melts by arsenic source crystal. Procedure allows precise control of thickness of etch and newly grown layer on substrate. Etching and deposition setup is expected to simplify processing and improve characteristics of gallium arsenide lasers, high-frequency amplifiers, and advanced integrated circuits.

High-performance etching of multilevel phase-type Fresnel zone plates with large apertures

NASA Astrophysics Data System (ADS)

Guo, Chengli; Zhang, Zhiyu; Xue, Donglin; Li, Longxiang; Wang, Ruoqiu; Zhou, Xiaoguang; Zhang, Feng; Zhang, Xuejun

2018-01-01

To ensure the etching depth uniformity of large-aperture Fresnel zone plates (FZPs) with controllable depths, a combination of a point source ion beam with a dwell-time algorithm has been proposed. According to the obtained distribution of the removal function, the latter can be used to optimize the etching time matrix by minimizing the root-mean-square error between the simulation results and the design value. Owing to the convolution operation in the utilized algorithm, the etching depth error is insensitive to the etching rate fluctuations of the ion beam, thereby reducing the requirement for the etching stability of the ion system. As a result, a 4-level FZP with a circular aperture of 300 mm was fabricated. The obtained results showed that the etching depth uniformity of the full aperture could be reduced to below 1%, which was sufficiently accurate for meeting the use requirements of FZPs. The proposed etching method may serve as an alternative way of etching high-precision diffractive optical elements with large apertures.

Optimization of KOH etching parameters for quantitative defect recognition in n- and p-type doped SiC

NASA Astrophysics Data System (ADS)

Sakwe, S. A.; Müller, R.; Wellmann, P. J.

2006-04-01

We have developed a KOH-based defect etching procedure for silicon carbide (SiC), which comprises in situ temperature measurement and control of melt composition. As benefit for the first time reproducible etching conditions were established (calibration plot, etching rate versus temperature and time); the etching procedure is time independent, i.e. no altering in KOH melt composition takes place, and absolute melt temperature values can be set. The paper describes this advanced KOH etching furnace, including the development of a new temperature sensor resistant to molten KOH. We present updated, absolute KOH etching parameters of n-type SiC and new absolute KOH etching parameters for low and highly p-type doped SiC, which are used for quantitative defect analysis. As best defect etching recipes we found T=530 °C/5 min (activation energy: 16.4 kcal/mol) and T=500 °C/5 min (activation energy: 13.5 kcal/mol) for n-type and p-type SiC, respectively.

Smooth and selective photo-electrochemical etching of heavily doped GaN:Si using a mode-locked 355 nm microchip laser

NASA Astrophysics Data System (ADS)

Lee, SeungGeun; Mishkat-Ul-Masabih, Saadat; Leonard, John T.; Feezell, Daniel F.; Cohen, Daniel A.; Speck, James S.; Nakamura, Shuji; DenBaars, Steven P.

2017-01-01

We investigate the photo-electrochemical (PEC) etching of Si-doped GaN samples grown on nonpolar GaN substrates, using a KOH/K2S2O8 solution and illuminated by a Xe arc lamp or a Q-switched 355 nm laser. The etch rate with the arc lamp decreased as the doping concentration increased, and the etching stopped for concentrations above 7.7 × 1018 cm-3. The high peak intensity of the Q-switched laser extended the etchable concentration to 2.4 × 1019 cm-3, with an etch rate of 14 nm/min. Compositionally selective etching was demonstrated, with an RMS surface roughness of 1.6 nm after etching down to an n-Al0.20Ga0.80N etch stop layer.

Comparing the effect of a desensitizing material and a self-etch adhesive on dentin sensitivity after periodontal surgery: a randomized clinical trial

PubMed Central

Hajizadeh, Hila; Majidinia, Sara; Moeintaghavi, Amir; Ghavamnasiri, Marjaneh

2017-01-01

Objectives This double-blind randomized placebo-controlled clinical trial evaluated the ability of a desensitizing agent and a self-etch adhesive on cervical dentin sensitivity (CDS) after periodontal surgery. Materials and Methods Ninety hypersensitive teeth of 13 subjects were included in the study. After periodontal surgery, the teeth of each posterior sextant treated with one of the following materials: G1: Clearfil S3 Bond (Kuraray Dental), G2: Gluma Desensitizer (Heraeus Kulzer), and G3: placebo (water). The sensitivity was assessed using evaporative stimuli before treatment (baseline, T0), 1 day after treatment (T1), after 1 week (T2), and after 1 month (T3) according to visual analog scale (VAS). Results Following the treatment, all the 3 groups showed significant reduction of CDS in T1 compared to T0. Reduction of CDS between T1 and T2 was observed only in G1 but there was no significant difference between T2 and T3 in this group. Although we observed a significant difference in T3 compared to T1 and T2 in G2 and G3, comparison of treatment groups in each assessment time showed a significant difference only in T3. According to paired comparison, this was due to the difference between G2 and G3. Conclusions Dentin sensitivity following periodontal surgery will decrease spontaneously over time, but treating the sensitive teeth with Gluma Desensitizer and Clearfil S3 Bond can have some benefits. PMID:28808633

Characteristics of contact and distance osteogenesis around modified implant surfaces in rabbit tibiae

PubMed Central

2017-01-01

Purpose Contact and distance osteogenesis occur around all endosseous dental implants. However, the mechanisms underlying these processes have not been fully elucidated. We hypothesized that these processes occur independently of each other. To test this, we used titanium (Ti) tubes to physically separate contact and distance osteogenesis, thus allowing contact osteogenesis to be measured in the absence of possible triggers from distance osteogenesis. Methods Sandblasted and acid-etched (SLA) and modified SLA (modSLA) implants were used. Both types had been sandblasted with large grit and then etched with acid. The modSLA implants then underwent additional treatment to increase hydrophilicity. The implants were implanted into rabbit tibiae, and half were implanted within Ti tubes. The bone-to-implant contact (BIC) ratio was calculated for each implant. Immunohistochemical analyses of bone morphogenetic protein (BMP)-2 expression and new bone formation (Masson trichrome stain) were performed. Results The implants outside of Ti tubes were associated with good bone formation along the implant surface. Implantation within a Ti tube significantly reduced the BIC ratio (P<0.001). Compared with the modSLA implants, the SLA implants were associated with significantly higher BIC ratios, regardless of the presence or absence of Ti tubes (P=0.043). In the absence of Ti tubes, the bone adjacent to the implant had areas of new bone formation that expressed BMP-2 at high levels. Conclusions This study disproved the null hypothesis and suggested that contact osteogenesis is initiated by signals from the old bone that undergoes distance osteogenesis after drilling. This signal may be BMP-2. PMID:28680714

Dry-plasma-free chemical etch technique for variability reduction in multi-patterning (Conference Presentation)

NASA Astrophysics Data System (ADS)

Kal, Subhadeep; Mohanty, Nihar; Farrell, Richard A.; Franke, Elliott; Raley, Angelique; Thibaut, Sophie; Pereira, Cheryl; Pillai, Karthik; Ko, Akiteru; Mosden, Aelan; Biolsi, Peter

2017-04-01

Scaling beyond the 7nm technology node demands significant control over the variability down to a few angstroms, in order to achieve reasonable yield. For example, to meet the current scaling targets it is highly desirable to achieve sub 30nm pitch line/space features at back-end of the line (BEOL) or front end of line (FEOL); uniform and precise contact/hole patterning at middle of line (MOL). One of the quintessential requirements for such precise and possibly self-aligned patterning strategies is superior etch selectivity between the target films while other masks/films are exposed. The need to achieve high etch selectivity becomes more evident for unit process development at MOL and BEOL, as a result of low density films choices (compared to FEOL film choices) due to lower temperature budget. Low etch selectivity with conventional plasma and wet chemical etch techniques, causes significant gouging (un-intended etching of etch stop layer, as shown in Fig 1), high line edge roughness (LER)/line width roughness (LWR), non-uniformity, etc. In certain circumstances this may lead to added downstream process stochastics. Furthermore, conventional plasma etches may also have the added disadvantage of plasma VUV damage and corner rounding (Fig. 1). Finally, the above mentioned factors can potentially compromise edge placement error (EPE) and/or yield. Therefore a process flow enabled with extremely high selective etches inherent to film properties and/or etch chemistries is a significant advantage. To improve this etch selectivity for certain etch steps during a process flow, we have to implement alternate highly selective, plasma free techniques in conjunction with conventional plasma etches (Fig 2.). In this article, we will present our plasma free, chemical gas phase etch technique using chemistries that have high selectivity towards a spectrum of films owing to the reaction mechanism ( as shown Fig 1). Gas phase etches also help eliminate plasma damage to the features during the etch process. Herein we will also demonstrate a test case on how a combination or plasma assisted and plasma free etch techniques has the potential to improve process performance of a 193nm immersion based self aligned quandruple patterning (SAQP) for BEOL compliant films (an example shown in Fig 2). In addition, we will also present on the application of gas etches for (1) profile improvement, (2) selective mandrel pull (3) critical dimension trim of mandrels, with an analysis of advantages over conventional techniques in terms of LER and EPE.

Radicals are required for thiol etching of gold particles

PubMed Central

Dreier, Timothy A.

2016-01-01

Etching of gold with excess thiol ligand is used in both synthesis and analysis of gold particles. Mechanistically, the process of etching gold with excess thiol is opaque. Previous studies have obliquely considered the role of oxygen in thiolate etching of gold. Herein, we show that oxygen or a radical initator is a necessary component for efficient etching of gold by thiolates. Attenuation of the etching process by radical scavengers in the presence of oxygen, and the restoration of activity by radical initiators under inert atmosphere, strongly implicate the oxygen radical. These data led us to propose an atomistic mechanism in which the oxygen radical initiates the etching process. PMID:26089294

Etching and oxidation of InAs in planar inductively coupled plasma

NASA Astrophysics Data System (ADS)

Dultsev, F. N.; Kesler, V. G.

2009-10-01

The surface of InAs (1 1 1)A was investigated under plasmachemical etching in the gas mixture CH 4/H 2/Ar. Etching was performed using the RF (13.56 MHz) and ICP plasma with the power 30-150 and 50-300 W, respectively; gas pressure in the reactor was 3-10 mTorr. It was demonstrated that the composition of the subsurface layer less than 5 nm thick changes during plasmachemical etching. A method of deep etching of InAs involving ICP plasma and hydrocarbon based chemistry providing the conservation of the surface relief is proposed. Optimal conditions and the composition of the gas phase for plasmachemical etching ensuring acceptable etch rates were selected.

Analysis of InP-based single photon avalanche diodes based on a single recess-etching process

NASA Astrophysics Data System (ADS)

Lee, Kiwon

2018-04-01

Effects of the different etching techniques have been investigated by analyzing electrical and optical characteristics of two-types of single-diffused single photon avalanche diodes (SPADs). The fabricated two-types of SPADs have no diffusion depth variation by using a single diffusion process at the same time. The dry-etched SPADs show higher temperature dependence of a breakdown voltage, larger dark-count-rate (DCR), and lower photon-detection-efficiency (PDE) than those of the wet-etched SPADs due to plasma-induced damage of dry-etching process. The results show that the dry etching damages can more significantly affect the performance of the SPADs based on a single recess-etching process.

Bonding effectiveness of self-etch adhesives to dentin after 24 h water storage.

PubMed

Sarr, Mouhamed; Benoist, Fatou Leye; Bane, Khaly; Aidara, Adjaratou Wakha; Seck, Anta; Toure, Babacar

2018-01-01

This study evaluated the immediate bonding effectiveness of five self-etch adhesive systems bonded to dentin. The microtensile bond strength of five self-etch adhesives systems, including one two-step and four one-step self-etch adhesives to dentin, was measured. Human third molars had their superficial dentin surface exposed, after which a standardized smear layer was produced using a medium-grit diamond bur. The selected adhesives were applied according to their respective manufacturer's instructions for μTBS measurement after storage in water at 37°C for 24 h. The μTBS varied from 11.1 to 44.3 MPa; the highest bond strength was obtained with the two-step self-etch adhesive Clearfil SE Bond and the lowest with the one-step self-etch adhesive Adper Prompt L-Pop. Pretesting failures mainly occurring during sectioning with the slow-speed diamond saw were observed only with the one-step self-etch adhesive Adper Prompt L-Pop (4 out of 18). When bonded to dentin, the self-etch adhesives with simplified application procedures (one-step self-etch adhesives) still underperform as compared to the two-step self-etch adhesive Clearfil SE Bond.

Bonding effectiveness of self-etch adhesives to dentin after 24 h water storage

PubMed Central

Sarr, Mouhamed; Benoist, Fatou Leye; Bane, Khaly; Aidara, Adjaratou Wakha; Seck, Anta; Toure, Babacar

2018-01-01

Purpose: This study evaluated the immediate bonding effectiveness of five self-etch adhesive systems bonded to dentin. Materials and Methods: The microtensile bond strength of five self-etch adhesives systems, including one two-step and four one-step self-etch adhesives to dentin, was measured. Human third molars had their superficial dentin surface exposed, after which a standardized smear layer was produced using a medium-grit diamond bur. The selected adhesives were applied according to their respective manufacturer's instructions for μTBS measurement after storage in water at 37°C for 24 h. Results: The μTBS varied from 11.1 to 44.3 MPa; the highest bond strength was obtained with the two-step self-etch adhesive Clearfil SE Bond and the lowest with the one-step self-etch adhesive Adper Prompt L-Pop. Pretesting failures mainly occurring during sectioning with the slow-speed diamond saw were observed only with the one-step self-etch adhesive Adper Prompt L-Pop (4 out of 18). Conclusions: When bonded to dentin, the self-etch adhesives with simplified application procedures (one-step self-etch adhesives) still underperform as compared to the two-step self-etch adhesive Clearfil SE Bond. PMID:29674814

Advanced plasma etch technologies for nanopatterning

NASA Astrophysics Data System (ADS)

Wise, Rich

2013-10-01

Advances in patterning techniques have enabled the extension of immersion lithography from 65/45 nm through 14/10 nm device technologies. A key to this increase in patterning capability has been innovation in the subsequent dry plasma etch processing steps. Multiple exposure techniques, such as litho-etch-litho-etch, sidewall image transfer, line/cut mask, and self-aligned structures, have been implemented to solution required device scaling. Advances in dry plasma etch process control across wafer uniformity and etch selectivity to both masking materials have enabled adoption of vertical devices and thin film scaling for increased device performance at a given pitch. Plasma etch processes, such as trilayer etches, aggressive critical dimension shrink techniques, and the extension of resist trim processes, have increased the attainable device dimensions at a given imaging capability. Precise control of the plasma etch parameters affecting across-design variation, defectivity, profile stability within wafer, within lot, and across tools has been successfully implemented to provide manufacturable patterning technology solutions. IBM has addressed these patterning challenges through an integrated total patterning solutions team to provide seamless and synergistic patterning processes to device and integration internal customers. We will discuss these challenges and the innovative plasma etch solutions pioneered by IBM and our alliance partners.

Advanced plasma etch technologies for nanopatterning

NASA Astrophysics Data System (ADS)

Wise, Rich

2012-03-01

Advances in patterning techniques have enabled the extension of immersion lithography from 65/45nm through 14/10nm device technologies. A key to this increase in patterning capability has been innovation in the subsequent dry plasma etch processing steps. Multiple exposure techniques such as litho-etch-litho-etch, sidewall image transfer, line/cut mask and self-aligned structures have been implemented to solution required device scaling. Advances in dry plasma etch process control, across wafer uniformity and etch selectivity to both masking materials and have enabled adoption of vertical devices and thin film scaling for increased device performance at a given pitch. Plasma etch processes such as trilayer etches, aggressive CD shrink techniques, and the extension of resist trim processes have increased the attainable device dimensions at a given imaging capability. Precise control of the plasma etch parameters affecting across design variation, defectivity, profile stability within wafer, within lot, and across tools have been successfully implemented to provide manufacturable patterning technology solutions. IBM has addressed these patterning challenges through an integrated Total Patterning Solutions team to provide seamless and synergistic patterning processes to device and integration internal customers. This paper will discuss these challenges and the innovative plasma etch solutions pioneered by IBM and our alliance partners.

Reactive ion etching of GaN using BCl 3, BCl 3/Ar and BCl 3/ N 2 gas plasmas

NASA Astrophysics Data System (ADS)

Basak, D.; Nakanishi, T.; Sakai, S.

2000-04-01

Reactive ion etching (RIE) of GaN has been performed using BCl 3 and additives, Ar and N 2, to BCl 3 plasma. The etch rate, surface roughness and the etch profile have been investigated. The etch rate of GaN is found to be 104 nm/min at rf power of 200 W, pressure of 2 Pa, with 9.5 sccm flow rate of BCl 3. The addition of 5 sccm of Ar to 9.5 sccm of BCl 3 reduces the etch rate of GaN while the addition of N 2 does not influence the etch rate significantly. The RIE of GaN layer with BCl 3/Ar and BCl 3/N 2 results in a smoother surface compared to surfaces etched with BCl 3 only. The etched side-wall in BCl 3 plasma makes an angle of 60° with the normal surface, and the angle of inclination is more in cases of BCl 3/Ar and BCl 3/N 2 plasmas. The RIE induced damage to the surface is measured qualitatively by PL measurements. It is observed that the damage to the etched surfaces is similar for all the plasmas.

Physics and chemistry of complex oxide etching and redeposition control

NASA Astrophysics Data System (ADS)

Margot, Joëlle

2012-10-01

Since its introduction in the 1970s, plasma etching has become the universal method for fine-line pattern transfer onto thin films and is anticipated to remain so in foreseeable future. Despite many success stories, plasma etching processes fail to meet the needs for several of the newest materials involved in advanced devices for photonic, electronic and RF applications like ferroelectrics, electro-optic materials, high-k dielectrics, giant magnetoresistance materials and unconventional conductors. In this context, the work achieved over the last decade on the etching of multicomponent oxides thin films such as barium strontium titanate (BST), strontium titanate (STO) and niobate of calcium and barium (CBN) will be reviewed. These materials present a low reactivity with usual etching gases such as fluorinated and chlorinated gases, their etching is mainly governed by ion sputtering and reactive gases sometimes interact with surface materials to form compounds that inhibit etching. The etching of platinum will also be presented as an example of unconventional conductor materials for which severe redeposition limits the achievable etching quality. Finally, it will be shown how simulation can help to understand the etching mechanisms and to define avenues for higher quality patterning.

Method for dry etching of transition metals

DOEpatents

Ashby, C.I.H.; Baca, A.G.; Esherick, P.; Parmeter, J.E.; Rieger, D.J.; Shul, R.J.

1998-09-29

A method for dry etching of transition metals is disclosed. The method for dry etching of a transition metal (or a transition metal alloy such as a silicide) on a substrate comprises providing at least one nitrogen- or phosphorus-containing {pi}-acceptor ligand in proximity to the transition metal, and etching the transition metal to form a volatile transition metal/{pi}-acceptor ligand complex. The dry etching may be performed in a plasma etching system such as a reactive ion etching (RIE) system, a downstream plasma etching system (i.e. a plasma afterglow), a chemically-assisted ion beam etching (CAIBE) system or the like. The dry etching may also be performed by generating the {pi}-acceptor ligands directly from a ligand source gas (e.g. nitrosyl ligands generated from nitric oxide), or from contact with energized particles such as photons, electrons, ions, atoms, or molecules. In some preferred embodiments of the present invention, an intermediary reactant species such as carbonyl or a halide ligand is used for an initial chemical reaction with the transition metal, with the intermediary reactant species being replaced at least in part by the {pi}-acceptor ligand for forming the volatile transition metal/{pi}-acceptor ligand complex.

Method for dry etching of transition metals

DOEpatents

Ashby, Carol I. H.; Baca, Albert G.; Esherick, Peter; Parmeter, John E.; Rieger, Dennis J.; Shul, Randy J.

1998-01-01

A method for dry etching of transition metals. The method for dry etching of a transition metal (or a transition metal alloy such as a silicide) on a substrate comprises providing at least one nitrogen- or phosphorous-containing .pi.-acceptor ligand in proximity to the transition metal, and etching the transition metal to form a volatile transition metal/.pi.-acceptor ligand complex. The dry etching may be performed in a plasma etching system such as a reactive ion etching (RIE) system, a downstream plasma etching system (i.e. a plasma afterglow), a chemically-assisted ion beam etching (CAIBE) system or the like. The dry etching may also be performed by generating the .pi.-acceptor ligands directly from a ligand source gas (e.g. nitrosyl ligands generated from nitric oxide), or from contact with energized particles such as photons, electrons, ions, atoms, or molecules. In some preferred embodiments of the present invention, an intermediary reactant species such as carbonyl or a halide ligand is used for an initial chemical reaction with the transition metal, with the intermediary reactant species being replaced at least in part by the .pi.-acceptor ligand for forming the volatile transition metal/.pi.-acceptor ligand complex.

Tridimensional morphology and kinetics of etch pit on the {l_brace}0 0 0 1{r_brace} plane of sapphire crystal

DOE Office of Scientific and Technical Information (OSTI.GOV)

Zhang Lunyong; Sun Jianfei, E-mail: jfsun_hit@263.net; Zuo Hongbo

2012-08-15

The tridimensional morphology and etching kinetics of the etch pit on the C-{l_brace}0 0 0 1{r_brace} plane of sapphire crystal ({alpha}-Al{sub 2}O{sub 3}) in molten KOH were studied experimentally. It was shown that the etch pit takes on tridimensional morphologies with triangular symmetry same as the symmetric property of the sapphire crystal. Pits like centric and eccentric triangular pyramid as well as hexagonal pyramid were observed, but the latter is less in density. In-depth analyses show the side walls of the etch pits belong to the {l_brace}1 1{sup Macron} 0 2{sup Macron }{r_brace} family, and the triangular pit contains edgesmore » full composed by Al{sup 3+} ions on the etching surface so it is more stable than the hexagonal pit since its edges on the etching surface contains Al{sup 2+} ions. The etch pits developed in a manner of kinematic wave by the step moving with constant speed, which is controlled by the chemical reaction with activation energy of 96.6 kJ/mol between Al{sub 2}O{sub 3} and KOH. - Graphical abstract: Schematic showing the atomic configuration of the predicted side walls of regular triangular pyramid shaped etch pit on the C-{l_brace}0 0 0 1{r_brace} plane of sapphire crystal. Highlights: Black-Right-Pointing-Pointer Observed the tridimensional morphology of etch pits. Black-Right-Pointing-Pointer Figured out the atomic configuration origin of the etch pits. Black-Right-Pointing-Pointer Quantitatively determined the etch rates of the etch pits.« less

Sealing effectiveness of fissure sealant bonded with universal adhesive systems on saliva-contaminated and noncontaminated enamel

PubMed Central

Shafiei, Fereshteh; Zarean, Mehran; Razmjoei, Faranak

2018-01-01

Background The effectiveness of sealants is dependent upon their adhesion to enamel surface. The aim of the study was to evaluate the sealing ability of a pit and fissure sealant used with a universal adhesive (etch-and-rinse vs. self-etch modes) when the site is contaminated with saliva. Adhesive properties were evaluated as microleakage and scanning electron microscopic (SEM) characteristics. Material and Methods A total of 72 mandibular third molars were randomly divided into 6 groups (n=12). Occlusal pits and fissures were sealed with an unfilled resin fissure sealant (FS) material with or without saliva contamination. The groups included: 1) phosphoric acid etching + FS (control), 2) phosphoric acid etching + Scotchbond Universal (etch-and-rinse) + FS, 3) phosphoric acid etching + saliva + Scotchbond Universal (etch-and-rinse) + FS, 4) Scotchbond Universal (self-etching) + FS,5) Scotchbond Universal (self-etching) + saliva + FS, and 6) Scotchbond Universal (self-etching) + saliva + Scotchbond Universal + FS. After thermocycling, the teeth were placed in 0.5% fuchsin, sectioned, and evaluated by digital microscopy. Two samples from each group were also observed by SEM. The data were analyzed with Kruskal-Wallis and Mann-Whitney tests for a significance of p<0.05. Results There were significant differences among groups. Groups 1,2 and 4 showed the least microleakage, with no significant differences among groups. Saliva contamination led to increased microleakage and gap formation in SEM images in groups 3, 5 and 6. Conclusions The fissure sealing ability of the universal adhesive in etch-and-rinse or self-etch modes was similar to that of conventional acid etching. Saliva contamination had a negative effect on sealant adhesion to pretreated enamel. Key words:Pit and fissure sealant, Universal adhesive, Saliva. PMID:29670708

Effects of Bias Pulsing on Etching of SiO2 Pattern in Capacitively-Coupled Plasmas for Nano-Scale Patterning of Multi-Level Hard Masks.

PubMed

Kim, Sechan; Choi, Gyuhyun; Chae, Heeyeop; Lee, Nae-Eung

2016-05-01

In order to study the effects of bias pulsing on the etching characteristics of a silicon dioxide (SiO2) layer using multi-level hard mask (MLHM) structures of ArF photoresist/bottom anti-reflected coating/SiO2/amorphous carbon layer (ACL)/SiO2, the effects of bias pulsing conditions on the etch characteristics of a SiO2 layer with an ACL mask pattern in C4F8/CH2F2/O2/Ar etch chemistries were investigated in a dual-frequency capacitively-coupled plasma (CCP) etcher. The effects of the pulse frequency, duty ratio, and pulse-bias power in the 2 MHz low-frequency (LF) power source were investigated in plasmas generated by a 27.12 MHz high-frequency (HF) power source. The etch rates of ACL and SiO2 decreased, but the etch selectivity of SiO2/ACL increased with decreasing duty ratio. When the ACL and SiO2 layers were etched with increasing pulse frequency, no significant change was observed in the etch rates and etch selectivity. With increasing LF pulse-bias power, the etch rate of ACL and SiO2 slightly increased, but the etch selectivity of SiO2/ACL decreased. Also, the precise control of the critical dimension (CD) values with decreasing duty ratio can be explained by the protection of sidewall etching of SiO2 by increased passivation. Pulse-biased etching was successfully applied to the patterning of the nano-scale line and space of SiO2 using an ACL pattern.

Shear bond strength of self-etch adhesives to enamel with additional phosphoric acid etching.

PubMed

Lührs, Anne-Katrin; Guhr, Silke; Schilke, Reinhard; Borchers, Lothar; Geurtsen, Werner; Günay, Hüsamettin

2008-01-01

This study evaluated the shear bond strength of self-etch adhesives to enamel and the effect of additional phosphoric acid etching. Seventy sound human molars were randomly divided into three test groups and one control group. The enamel surfaces of the control group (n=10) were treated with Syntac Classic (SC). Each test group was subdivided into two groups (each n=10). In half of each test group, ground enamel surfaces were coated with the self-etch adhesives AdheSe (ADH), Xeno III (XE) or Futurabond NR (FNR). In the remaining half of each test group, an additional phosphoric acid etching of the enamel surface was performed prior to applying the adhesives. The shear bond strength was measured with a universal testing machine at a crosshead speed of 1 mm/minute after storing the samples in distilled water at 37 degrees C for 24 hours. Fracture modes were determined by SEM examination. For statistical analysis, one-way ANOVA and the two-sided Dunnett Test were used (p>0.05). Additional phosphoric etching significantly increased the shear bond strength of all the examined self-etch adhesives (p<0.001). The highest shear bond strength was found for FNR after phosphoric acid etching. Without phosphoric acid etching, only FNR showed no significant differences compared to the control (SC). SEM evaluations showed mostly adhesive fractures. For all the self-etch adhesives, a slight increase in mixed fractures occurred after conditioning with phosphoric acid. An additional phosphoric acid etching of enamel should be considered when using self-etch adhesives. More clinical studies are needed to evaluate the long-term success of the examined adhesives.

Sealing effectiveness of fissure sealant bonded with universal adhesive systems on saliva-contaminated and noncontaminated enamel.

PubMed

Memarpour, Mahtab; Shafiei, Fereshteh; Zarean, Mehran; Razmjoei, Faranak

2018-01-01

The effectiveness of sealants is dependent upon their adhesion to enamel surface. The aim of the study was to evaluate the sealing ability of a pit and fissure sealant used with a universal adhesive (etch-and-rinse vs. self-etch modes) when the site is contaminated with saliva. Adhesive properties were evaluated as microleakage and scanning electron microscopic (SEM) characteristics. A total of 72 mandibular third molars were randomly divided into 6 groups (n=12). Occlusal pits and fissures were sealed with an unfilled resin fissure sealant (FS) material with or without saliva contamination. The groups included: 1) phosphoric acid etching + FS (control), 2) phosphoric acid etching + Scotchbond Universal (etch-and-rinse) + FS, 3) phosphoric acid etching + saliva + Scotchbond Universal (etch-and-rinse) + FS, 4) Scotchbond Universal (self-etching) + FS,5) Scotchbond Universal (self-etching) + saliva + FS, and 6) Scotchbond Universal (self-etching) + saliva + Scotchbond Universal + FS. After thermocycling, the teeth were placed in 0.5% fuchsin, sectioned, and evaluated by digital microscopy. Two samples from each group were also observed by SEM. The data were analyzed with Kruskal-Wallis and Mann-Whitney tests for a significance of p <0.05. There were significant differences among groups. Groups 1,2 and 4 showed the least microleakage, with no significant differences among groups. Saliva contamination led to increased microleakage and gap formation in SEM images in groups 3, 5 and 6. The fissure sealing ability of the universal adhesive in etch-and-rinse or self-etch modes was similar to that of conventional acid etching. Saliva contamination had a negative effect on sealant adhesion to pretreated enamel. Key words: Pit and fissure sealant, Universal adhesive, Saliva.

The research on conformal acid etching process of glass ceramic

NASA Astrophysics Data System (ADS)

Wang, Kepeng; Guo, Peiji

2014-08-01

A series of experiments have been done to explore the effect of different conditions on the hydrofluoric acid etching. The hydrofluoric acid was used to etch the glass ceramic called "ZERODUR", which is invented by SCHOTT in Germany. The glass ceramic was processed into cylindrical samples. The hydrofluoric acid etching was done in a plastic beaker. The concentration of hydrofluoric acid and the etching time were changed to measure the changes of geometric tolerance and I observed the surface using a microscope in order to find an appropriate condition of hydrofluoric acid etching.

Anisotropic etching of silicon in solutions containing tensioactive compounds

NASA Astrophysics Data System (ADS)

Zubel, Irena

2016-12-01

The results of investigations concerning anisotropic etching in 3M KOH and 25% TMAH solutions modified by tensioactive compounds such as alcohols, diols and a typical surfactant Triton X100 have been compared. Etching anisotropy was assessed on the basis of etch rates ratio V(110)/V(100). It was stated that the relation between surface tension of the solutions and etch rates of particular planes depend not only on the kind of surfactant but also on the kind of etching solution (KOH, TMAH). It points out an important role of TMA+ ions in the etching process, probably in the process of forming an adsorption layer, consisting of the molecules of tensioactive compounds on Si surface, which decides about etch rate. We have observed that this phenomenon occurs only at high concentration of TMA+ ions (25% TMAH). Reduction of TMAH concentration changes the properties of surfactant containing TMAH solutions. From all investigated solutions, the solutions that assured developing of (110) plane inclined at the angle of 45° to (100) substrate were selected. Such planes can be used as micromirrors in MOEMS structures. The solutions provide the etch rate ratio V(110)/V(100)<0.7, thus they were selected from hydroxide solutions containing surfactants. A simple way for etch rate anisotropy V(110)/V(100) assessment based on microscopic images etched structures has been proposed.

Post-processing of fused silica and its effects on damage resistance to nanosecond pulsed UV lasers.

PubMed

Ye, Hui; Li, Yaguo; Zhang, Qinghua; Wang, Wei; Yuan, Zhigang; Wang, Jian; Xu, Qiao

2016-04-10

HF-based (hydrofluoric acid) chemical etching has been a widely accepted technique to improve the laser damage performance of fused silica optics and ensure high-power UV laser systems at designed fluence. Etching processes such as acid concentration, composition, material removal amount, and etching state (etching with additional acoustic power or not) may have a great impact on the laser-induced damage threshold (LIDT) of treated sample surfaces. In order to find out the effects of these factors, we utilized the Taguchi method to determine the etching conditions that are helpful in raising the LIDT. Our results show that the most influential factors are concentration of etchants and the material etched away from the viewpoint of damage performance of fused silica optics. In addition, the additional acoustic power (∼0.6  W·cm^-2) may not benefit the etching rate and damage performance of fused silica. Moreover, the post-cleaning procedure of etched samples is also important in damage performances of fused silica optics. Different post-cleaning procedures were, thus, experiments on samples treated under the same etching conditions. It is found that the "spraying + rinsing + spraying" cleaning process is favorable to the removal of etching-induced deposits. Residuals on the etched surface are harmful to surface roughness and optical transmission as well as laser damage performance.

Comparison between universal adhesives and two-step self-etch adhesives in terms of dentin bond fatigue durability in self-etch mode.

PubMed

Tsujimoto, Akimasa; Barkmeier, Wayne W; Takamizawa, Toshiki; Watanabe, Hidehiko; Johnson, William W; Latta, Mark A; Miyazaki, Masashi

2017-06-01

This aim of this study was to compare universal adhesives and two-step self-etch adhesives in terms of dentin bond fatigue durability in self-etch mode. Three universal adhesives - Clearfil Universal, G-Premio Bond, and Scotchbond Universal Adhesive - and three-two-step self-etch adhesives - Clearfil SE Bond, Clearfil SE Bond 2, and OptiBond XTR - were used. The initial shear bond strength and shear fatigue strength of resin composite bonded to adhesive on dentin in self-etch mode were determined. Scanning electron microscopy observations of fracture surfaces after bond strength tests were also made. The initial shear bond strength of universal adhesives was material dependent, unlike that of two-step self-etch adhesives. The shear fatigue strength of Scotchbond Universal Adhesive was not significantly different from that of two-step self-etch adhesives, unlike the other universal adhesives. The shear fatigue strength of universal adhesives differed depending on the type of adhesive, unlike those of two-step self-etch adhesives. The results of this study encourage the continued use of two-step self-etch adhesive over some universal adhesives but suggest that changes to the composition of universal adhesives may lead to a dentin bond fatigue durability similar to that of two-step self-etch adhesives. © 2017 Eur J Oral Sci.

Single-crystal silicon trench etching for fabrication of highly integrated circuits

NASA Astrophysics Data System (ADS)

Engelhardt, Manfred

1991-03-01

The development of single crystal silicon trench etching for fabrication of memory cells in 4 16 and 64Mbit DRAMs is reviewed in this paper. A variety of both etch tools and process gases used for the process development is discussed since both equipment and etch chemistry had to be improved and changed respectively to meet the increasing requirements for high fidelity pattern transfer with increasing degree of integration. In additon to DRAM cell structures etch results for deep trench isolation in advanced bipolar ICs and ASICs are presented for these applications grooves were etched into silicon through a highly doped buried layer and at the borderline of adjacent p- and n-well areas respectively. Shallow trench etching of large and small exposed areas with identical etch rates is presented as an approach to replace standard LOCOS isolation by an advanced isolation technique. The etch profiles were investigated with SEM TEM and AES to get information on contathination and damage levels and on the mechanism leading to anisotropy in the dry etch process. Thermal wave measurements were performed on processed single crystal silicon substrates for a fast evaluation of the process with respect to plasma-induced substrate degradation. This useful technique allows an optimization ofthe etch process regarding high electrical performance of the fully processed memory chip. The benefits of the use of magnetic fields for the development of innovative single crystal silicon dry

Influence of application method on surface free-energy and bond strength of universal adhesive systems to enamel.

PubMed

Imai, Arisa; Takamizawa, Toshiki; Sai, Keiichi; Tsujimoto, Akimasa; Nojiri, Kie; Endo, Hajime; Barkmeier, Wayne W; Latta, Mark A; Miyazaki, Masashi

2017-10-01

The aim of the present study was to determine the influence of different adhesive application methods and etching modes on enamel bond effectiveness of universal adhesives using shear bond strength (SBS) testing and surface free-energy (SFE) measurements. The adhesives Scotchbond Universal, All-Bond Universal, Adhese Universal, and G-Premio Bond were used. Prepared bovine enamel specimens were divided into four groups, based on type of adhesive, and subjected to the following surface treatments: (i) total-etch mode with active application; (ii) total-etch mode with inactive application; (iii) self-etch mode with active application; and (iv) self-etch mode with inactive application. Bonded specimens were subjected to SBS testing. The SFE of the enamel surfaces with adhesive was measured after rinsing with acetone and water. The SBS values in total-etch mode were significantly higher than those in self-etch mode. In total-etch mode, significantly lower SBS values were observed with active application compared with inactive application; in contrast, in self-etch mode there were no significant differences in SBS between active and inactive applications. A reduction in total SFE was observed for active application compared with inactive application. The interaction between etching mode and application method was statistically significant, and the application method significantly affected enamel bond strength in total-etch mode. © 2017 Eur J Oral Sci.

Deep Reactive Ion Etching (DRIE) of High Aspect Ratio SiC Microstructures using a Time-Multiplexed Etch-Passivate Process

NASA Technical Reports Server (NTRS)

Evans, Laura J.; Beheim, Glenn M.

2006-01-01

High aspect ratio silicon carbide (SiC) microstructures are needed for microengines and other harsh environment micro-electro-mechanical systems (MEMS). Previously, deep reactive ion etching (DRIE) of low aspect ratio (AR less than or = 1) deep (greater than 100 micron) trenches in SiC has been reported. However, existing DRIE processes for SiC are not well-suited for definition of high aspect ratio features because such simple etch-only processes provide insufficient control over sidewall roughness and slope. Therefore, we have investigated the use of a time-multiplexed etch-passivate (TMEP) process, which alternates etching with polymer passivation of the etch sidewalls. An optimized TMEP process was used to etch high aspect ratio (AR greater than 5) deep (less than 100 micron) trenches in 6H-SiC. Power MEMS structures (micro turbine blades) in 6H-SiC were also fabricated.

Dry etching technologies for the advanced binary film

NASA Astrophysics Data System (ADS)

Iino, Yoshinori; Karyu, Makoto; Ita, Hirotsugu; Yoshimori, Tomoaki; Azumano, Hidehito; Muto, Makoto; Nonaka, Mikio

2011-11-01

ABF (Advanced Binary Film) developed by Hoya as a photomask for 32 (nm) and larger specifications provides excellent resistance to both mask cleaning and 193 (nm) excimer laser and thereby helps extend the lifetime of the mask itself compared to conventional photomasks and consequently reduces the semiconductor manufacturing cost [1,2,3]. Because ABF uses Ta-based films, which are different from Cr film or MoSi films commonly used for photomask, a new process is required for its etching technology. A patterning technology for ABF was established to perform the dry etching process for Ta-based films by using the knowledge gained from absorption layer etching for EUV mask that required the same Ta-film etching process [4]. Using the mask etching system ARES, which is manufactured by Shibaura Mechatronics, and its optimized etching process, a favorable CD (Critical Dimension) uniformity, a CD linearity and other etching characteristics were obtained in ABF patterning. Those results are reported here.

Process margin enhancement for 0.25-μm metal etch process

NASA Astrophysics Data System (ADS)

Lee, Chung Y.; Ma, Wei Wen; Lim, Eng H.; Cheng, Alex T.; Joy, Raymond; Ross, Matthew F.; Wong, Selmer S.; Marlowe, Trey

2000-06-01

This study evaluates electron beam stabilization of UV6, a positive tone Deep-UV (DUV) resist from Shipley, for a 0.25 micrometer metal etch application. Results are compared between untreated resist and resist treated with different levels of electron beam stabilization. The electron beam processing was carried out in an ElectronCureTM flood electron beam exposure system from Honeywell International Inc., Electron Vision. The ElectronCureTM system utilizes a flood electron beam source which is larger in diameter than the substrate being processed, and is capable of variable energy so that the electron range is matched to the resist film thickness. Changes in the UV6 resist material as a result of the electron beam stabilization are monitored via spectroscopic ellipsometry for film thickness and index of refraction changes and FTIR for analysis of chemical changes. Thermal flow stability is evaluated by applying hot plate bakes of 150 degrees Celsius and 200 degrees Celsius, to patterned resist wafers with no treatment and with an electron beam dose level of 2000 (mu) C/cm2. A significant improvement in the thermal flow stability of the patterned UV6 resist features is achieved with the electron beam stabilization process. Etch process performance of the UV6 resist was evaluated by performing a metal pattern transfer process on wafers with untreated resist and comparing these with etch results on wafers with different levels of electron beam stabilization. The etch processing was carried out in an Applied Materials reactor with an etch chemistry including BCl3 and Cl2. All wafers were etched under the same conditions and the resist was treated after etch to prevent further erosion after etch but before SEM analysis. Post metal etch SEM cross-sections show the enhancement in etch resistance provided by the electron beam stabilization process. Enhanced process margin is achieved as a result of the improved etch resistance, and is observed in reduced resist side-wall angles after etch. Only a slight improvement is observed in the isolated to dense bias effects of the etch process. Improved CD control is also achieved by applying the electron beam process, as more consistent CDs are observed after etch.

Self-Anchored Catalyst Interface Enables Ordered Via Array Formation from Submicrometer to Millimeter Scale for Polycrystalline and Single-Crystalline Silicon.

PubMed

Kim, Jeong Dong; Kim, Munho; Kong, Lingyu; Mohseni, Parsian K; Ranganathan, Srikanth; Pachamuthu, Jayavel; Chim, Wai Kin; Chiam, Sing Yang; Coleman, James J; Li, Xiuling

2018-03-14

Defying text definitions of wet etching, metal-assisted chemical etching (MacEtch), a solution-based, damage-free semiconductor etching method, is directional, where the metal catalyst film sinks with the semiconductor etching front, producing 3D semiconductor structures that are complementary to the metal catalyst film pattern. The same recipe that works perfectly to produce ordered array of nanostructures for single-crystalline Si (c-Si) fails completely when applied to polycrystalline Si (poly-Si) with the same doping type and level. Another long-standing challenge for MacEtch is the difficulty of uniformly etching across feature sizes larger than a few micrometers because of the nature of lateral etching. The issue of interface control between the catalyst and the semiconductor in both lateral and vertical directions over time and over distance needs to be systematically addressed. Here, we present a self-anchored catalyst (SAC) MacEtch method, where a nanoporous catalyst film is used to produce nanowires through the pinholes, which in turn physically anchor the catalyst film from detouring as it descends. The systematic vertical etch rate study as a function of porous catalyst diameter from 200 to 900 nm shows that the SAC-MacEtch not only confines the etching direction but also enhances the etch rate due to the increased liquid access path, significantly delaying the onset of the mass-transport-limited critical diameter compared to nonporous catalyst c-Si counterpart. With this enhanced mass transport approach, vias on multistacks of poly-Si/SiO 2 are also formed with excellent vertical registry through the polystack, even though they are separated by SiO 2 which is readily removed by HF alone with no anisotropy. In addition, 320 μm square through-Si-via (TSV) arrays in 550 μm thick c-Si are realized. The ability of SAC-MacEtch to etch through poly/oxide/poly stack as well as more than half millimeter thick silicon with excellent site specificity for a wide range of feature sizes has significant implications for 2.5D/3D photonic and electronic device applications.

SHI induced nano track polymer filters and characterization

NASA Astrophysics Data System (ADS)

Vijay, Y. K.

2009-07-01

Swift heavy ion irradiation produces damage in polymers in the form of latent tracks. Latent tracks can be enlarged by etching it in a suitable etchant and thus nuclear track etch membrane can be formed for gas permeation / purification in particular for hydrogen where the molecular size is very small. By applying suitable and controlled etching conditions well defined tracks can be formed for specific applications of the membranes. After etching gas permeation method is used for characterizing the tracks. In the present work polycarbonate (PC) of various thickness were irradiated with energetic ion beam at Inter University Accelerator Centre (IUAC), New Delhi. Nuclear tracks were modified by etching the PC in 6N NaOH at 60 (±1) °C from both sides for different times to produce track etch membranes. At critical etch time the etched pits from both the sides meet a rapid increase in gas permeation was observed. Permeability of hydrogen and carbon dioxide has been measured in samples etched for different times. The latent tracks produced by SHI irradiation in the track etch membranes show enhancement of free volume of the polymer. Nano filters are separation devices for the mixture of gases, different ions in the solution and isotopes and isobars separations. The polymer thin films with controlled porosity finding it self as best choice. However, the permeability and selectivity of these polymer based membrane filters are very important at the nano scale separation. The Swift Heavy Ion (SHI) induced nuclear track etched polymeric films with controlled etching have been attempted and characterized as nano scale filters.

Effects of hard mask etch on final topography of advanced phase shift masks

NASA Astrophysics Data System (ADS)

Hortenbach, Olga; Rolff, Haiko; Lajn, Alexander; Baessler, Martin

2017-07-01

Continuous shrinking of the semiconductor device dimensions demands steady improvements of the lithographic resolution on wafer level. These requirements challenge the photomask industry to further improve the mask quality in all relevant printing characteristics. In this paper topography of the Phase Shift Masks (PSM) was investigated. Effects of hard mask etch on phase shift uniformity and mask absorber profile were studied. Design of experiments method (DoE) was used for the process optimization, whereas gas composition, bias power of the hard mask main etch and bias power of the over-etch were varied. In addition, influence of the over-etch time was examined at the end of the experiment. Absorber depth uniformity, sidewall angle (SWA), reactive ion etch lag (RIE lag) and through pitch (TP) dependence were analyzed. Measurements were performed by means of Atomic-force microscopy (AFM) using critical dimension (CD) mode with a boot-shaped tip. Scanning electron microscope (SEM) cross-section images were prepared to verify the profile quality. Finally CD analysis was performed to confirm the optimal etch conditions. Significant dependence of the absorber SWA on hard mask (HM) etch conditions was observed revealing an improvement potential for the mask absorber profile. It was found that hard mask etch can leave a depth footprint in the absorber layer. Thus, the etch depth uniformity of hard mask etch is crucial for achieving a uniform phase shift over the active mask area. The optimized hard mask etch process results in significantly improved mask topography without deterioration of tight CD specifications.

Radicals Are Required for Thiol Etching of Gold Particles.

PubMed

Dreier, Timothy A; Ackerson, Christopher J

2015-08-03

Etching of gold with an excess of thiol ligand is used in both synthesis and analysis of gold particles. Mechanistically, the process of etching gold with excess thiol is unclear. Previous studies have obliquely considered the role of oxygen in thiolate etching of gold. Herein, we show that oxygen or a radical initiator is a necessary component for efficient etching of gold by thiolates. Attenuation of the etching process by radical scavengers in the presence of oxygen, and the restoration of activity by radical initiators under inert atmosphere, strongly implicate the oxygen radical. These data led us to propose an atomistic mechanism in which the oxygen radical initiates the etching process. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Etching fission tracks in zircons

USGS Publications Warehouse

Naeser, C.W.

1969-01-01

A new technique has been developed whereby fission tracks can be etched in zircon with a solution of sodium hydroxide at 220??C. Etching time varied between 15 minutes and 5 hours. Colored zircon required less etching time than the colorless varieties.

Alternative process for thin layer etching: Application to nitride spacer etching stopping on silicon germanium

DOE Office of Scientific and Technical Information (OSTI.GOV)

Posseme, N., E-mail: nicolas.posseme@cea.fr; Pollet, O.; Barnola, S.

2014-08-04

Silicon nitride spacer etching realization is considered today as one of the most challenging of the etch process for the new devices realization. For this step, the atomic etch precision to stop on silicon or silicon germanium with a perfect anisotropy (no foot formation) is required. The situation is that none of the current plasma technologies can meet all these requirements. To overcome these issues and meet the highly complex requirements imposed by device fabrication processes, we recently proposed an alternative etching process to the current plasma etch chemistries. This process is based on thin film modification by light ionsmore » implantation followed by a selective removal of the modified layer with respect to the non-modified material. In this Letter, we demonstrate the benefit of this alternative etch method in term of film damage control (silicon germanium recess obtained is less than 6 A), anisotropy (no foot formation), and its compatibility with other integration steps like epitaxial. The etch mechanisms of this approach are also addressed.« less

Modification of the Surface Topography and Composition of Ultrafine and Coarse Grained Titanium by Chemical Etching.

PubMed

Nazarov, Denis V; Zemtsova, Elena G; Solokhin, Alexandr Yu; Valiev, Ruslan Z; Smirnov, Vladimir M

2017-01-13

In this study, we present the detailed investigation of the influence of the etching medium (acidic or basic Piranha solutions) and the etching time on the morphology and surface relief of ultrafine grained (UFG) and coarse grained (CG) titanium. The surface relief and morphology have been studied by means of scanning electron microscopy (SEM), atomic force microscopy (AFM), and the spectral ellipsometry. The composition of the samples has been determined by X-ray fluorescence analysis (XRF) and X-ray Photoelectron Spectroscopy (XPS). Significant difference in the etching behavior of UFG and CG titanium has been found. UFG titanium exhibits higher etching activity independently of the etching medium. Formed structures possess higher homogeneity. The variation of the etching medium and time leads to micro-, nano-, or hierarchical micro/nanostructures on the surface. Significant difference has been found between surface composition for UFG titanium etched in basic and acidic Piranha solution. Based on the experimental data, the possible reasons and mechanisms are considered for the formation of nano- and microstructures. The prospects of etched UFG titanium as the material for implants are discussed.

Ion-enhanced chemical etching of ZrO2 in a chlorine discharge

NASA Astrophysics Data System (ADS)

Sha, Lin; Cho, Byeong-Ok; Chang, Jane P.

2002-09-01

Chlorine plasma is found to chemically etch ZrO2 thin films in an electron cyclotron resonance reactor, and the etch rate scaled linearly with the square root of ion energy at high ion energies with a threshold energy between 12-20 eV. The etching rate decreased monotonically with increasing chamber pressures, which corresponds to reduced electron temperatures. Optical emission spectroscopy and quadrupole mass spectrometry were used to identify the reaction etching products. No Zr, O, or ZrCl were detected as etching products, but highly chlorinated zirconium compounds (ZrCl2, ZrCl3, and ZrCl4) and ClO were found to be the dominant etching products. ZrCl3 was the dominant etching products at low ion energies, while ZrCl4 became dominant at higher ion energies. This is consistent with greater momentum transfer and enhanced surface chlorination, as determined by x-ray photoelectron spectroscopy, at increased ion energies. Several ion-enhanced chemical reactions are proposed to contribute to the ZrO2 etching. copyright 2002 American Vacuum Society.

Effect of Hydrofluoric Acid Etching Time on Titanium Topography, Chemistry, Wettability, and Cell Adhesion

PubMed Central

Zahran, R.; Rosales Leal, J. I.; Rodríguez Valverde, M. A.; Cabrerizo Vílchez, M. A.

2016-01-01

Titanium implant surface etching has proven an effective method to enhance cell attachment. Despite the frequent use of hydrofluoric (HF) acid, many questions remain unresolved, including the optimal etching time and its effect on surface and biological properties. The objective of this study was to investigate the effect of HF acid etching time on Ti topography, surface chemistry, wettability, and cell adhesion. These data are useful to design improved acid treatment and obtain an improved cell response. The surface topography, chemistry, dynamic wetting, and cell adhesiveness of polished Ti surfaces were evaluated after treatment with HF acid solution for 0, 2; 3, 5, 7, or 10 min, revealing a time-dependent effect of HF acid on their topography, chemistry, and wetting. Roughness and wetting increased with longer etching time except at 10 min, when roughness increased but wetness decreased. Skewness became negative after etching and kurtosis tended to 3 with longer etching time. Highest cell adhesion was achieved after 5–7 min of etching time. Wetting and cell adhesion were reduced on the highly rough surfaces obtained after 10-min etching time. PMID:27824875

Optimized plasma etch window of block copolymers and neutral brush layers for enhanced direct self-assembly pattern transfer into a hardmask layer

NASA Astrophysics Data System (ADS)

Brakensiek, Nickolas; Xu, Kui; Sweat, Daniel; Hockey, Mary Ann

2018-03-01

Directed self-assembly (DSA) of block copolymers (BCPs) is one of the most promising patterning technologies for future lithography nodes. However, one of the biggest challenges to DSA is the pattern transfer by plasma etching from BCP to hardmask (HM) because the etch selectivity between BCP and neutral brush layer underneath is usually not high enough to enable robust pattern transfer. This paper will explore the plasma etch conditions of both BCPs and neutral brush layers that may improve selectivity and allow a more robust pattern transfer of DSA patterns into the hardmask layer. The plasma etching parameters that are under investigation include the selection of oxidative or reductive etch chemistries, as well as plasma gas pressure, power, and gas mixture fractions. Investigation into the relationship between BCP/neutral brush layer materials with varying chemical compositions and the plasma etching conditions will be highlighted. The culmination of this work will demonstrate important etch parameters that allow BCPs and neutral brush layers to be etched into the underlying hardmask layer with a large process window.

Modification of the Surface Topography and Composition of Ultrafine and Coarse Grained Titanium by Chemical Etching

PubMed Central

Nazarov, Denis V.; Zemtsova, Elena G.; Solokhin, Alexandr Yu.; Valiev, Ruslan Z.; Smirnov, Vladimir M.

2017-01-01

In this study, we present the detailed investigation of the influence of the etching medium (acidic or basic Piranha solutions) and the etching time on the morphology and surface relief of ultrafine grained (UFG) and coarse grained (CG) titanium. The surface relief and morphology have been studied by means of scanning electron microscopy (SEM), atomic force microscopy (AFM), and the spectral ellipsometry. The composition of the samples has been determined by X-ray fluorescence analysis (XRF) and X-ray Photoelectron Spectroscopy (XPS). Significant difference in the etching behavior of UFG and CG titanium has been found. UFG titanium exhibits higher etching activity independently of the etching medium. Formed structures possess higher homogeneity. The variation of the etching medium and time leads to micro-, nano-, or hierarchical micro/nanostructures on the surface. Significant difference has been found between surface composition for UFG titanium etched in basic and acidic Piranha solution. Based on the experimental data, the possible reasons and mechanisms are considered for the formation of nano- and microstructures. The prospects of etched UFG titanium as the material for implants are discussed. PMID:28336849

DOE Office of Scientific and Technical Information (OSTI.GOV)

Henry, Michael David; Young, Travis R.; Griffin, Ben

Here, this work reports the utilization of a recently developed film, ScAlN, as a silicon etch mask offering significant improvements in high etch selectivity to silicon. Utilization of ScAlN as a fluorine chemistry based deep reactive ion etch mask demonstrated etch selectivity at 23 550:1, four times better than AlN, 11 times better than Al 2O 3, and 148 times better than silicon dioxide with significantly less resputtering at high bias voltage than either Al 2O 3 or AlN. Ellipsometry film thickness measurements show less than 0.3 nm/min mask erosion rates for ScAlN. Micromasking of resputtered Al for Al 2Omore » 3, AlN, and ScAlN etch masks is also reported here, utilizing cross-sectional scanning electron microscope and confocal microscope roughness measurements. With lower etch bias, the reduced etch rate can be optimized to achieve a trench bottom surface roughness that is comparable to SiO 2 etch masks. Etch mask selectivity enabled by ScAlN is likely to make significant improvements in microelectromechanical systems, wafer level packaging, and plasma dicing of silicon.« less

Chemical etching and organometallic chemical vapor deposition on varied geometries of GaAs

NASA Technical Reports Server (NTRS)

Bailey, Sheila G.; Landis, Geoffrey A.; Wilt, David M.

1989-01-01

Results of micron-spaced geometries produced by wet chemical etching and subsequent OMCVD growth on various GaAs surfaces are presented. The polar lattice increases the complexity of the process. The slow-etch planes defined by anisotropic etching are not always the same as the growth facets produced during MOCVD deposition, especially for deposition on higher-order planes produced by the hex groove etching.

Ion beam sputtering of fluoropolymers. [etching polymer films and target surfaces

NASA Technical Reports Server (NTRS)

Sovey, J. S.

1978-01-01

Ion beam sputter processing rates as well as pertinent characteristics of etched targets and films are described. An argon ion beam source was used to sputter etch and deposit the fluoropolymers PTFE, FEP, and CTFE. Ion beam energy, current density, and target temperature were varied to examine effects on etch and deposition rates. The ion etched fluoropolymers yield cone or spire-like surface structures which vary depending upon the type of polymer, ion beam power density, etch time, and target temperature. Sputter target and film characteristics documented by spectral transmittance measurements, X-ray diffraction, ESCA, and SEM photomicrographs are included.

Effects of etch-and-rinse and self-etch adhesives on dentin MMP-2 and MMP-9.

PubMed

Mazzoni, A; Scaffa, P; Carrilho, M; Tjäderhane, L; Di Lenarda, R; Polimeni, A; Tezvergil-Mutluay, A; Tay, F R; Pashley, D H; Breschi, L

2013-01-01

Auto-degradation of collagen matrices occurs within hybrid layers created by contemporary dentin bonding systems, by the slow action of host-derived matrix metalloproteinases (MMPs). This study tested the null hypothesis that there are no differences in the activities of MMP-2 and -9 after treatment with different etch-and-rinse or self-etch adhesives. Tested adhesives were: Adper Scotchbond 1XT (3M ESPE), PQ1 (Ultradent), Peak LC (Ultradent), Optibond Solo Plus (Kerr), Prime&Bond NT (Dentsply) (all 2-step etch-and-rinse adhesives), and Adper Easy Bond (3M ESPE), Tri-S (Kuraray), and Xeno-V (Dentsply) (1-step self-etch adhesives). MMP-2 and -9 activities were quantified in adhesive-treated dentin powder by means of an activity assay and gelatin zymography. MMP-2 and MMP-9 activities were found after treatment with all of the simplified etch-and-rinse and self-etch adhesives; however, the activation was adhesive-dependent. It is concluded that all two-step etch-and-rinse and the one-step self-etch adhesives tested can activate endogenous MMP-2 and MMP-9 in human dentin. These results support the role of endogenous MMPs in the degradation of hybrid layers created by these adhesives.

Improvement in etching rate for epilayer lift-off with surfactant

NASA Astrophysics Data System (ADS)

Wu, Fan-Lei; Horng, Ray-Hua; Lu, Jian-Heng; Chen, Chun-Li; Kao, Yu-Cheng

2013-03-01

In this study, the GaAs epilayer is quickly separated from GaAs substrate by epitaxial lift-off (ELO) process with mixture etchant solution. The HF solution mixes with surfactant as mixture etchant solution to etch AlAs sacrificial layer for the selective wet etching of AlAs sacrificial layer. Addiction surfactants etchant significantly enhance the etching rate in the hydrofluoric acid etching solution. It is because surfactant provides hydrophilicity to change the contact angle with enhances the fluid properties of the mixture etchant between GaAs epilayer and GaAs substrate. Arsine gas was released from the etchant solution because the critical reaction product in semiconductor etching is dissolved arsine gas. Arsine gas forms a bubble, which easily displaces the etchant solution, before the AlAs layer was undercut. The results showed that acetone and hydrofluoric acid ratio of about 1:1 for the fastest etching rate of 13.2 μm / min. The etching rate increases about 4 times compared with pure hydrofluoric acid, moreover can shorten the separation time about 70% of GaAs epilayer with GaAs substrate. The results indicate that etching ratio and stability are improved by mixture etchant solution. It is not only saving the epilayer and the etching solution exposure time, but also reducing the damage to the epilayer structure.

Alternating SiCl4/O2 passivation steps with SF6 etch steps for silicon deep etching

NASA Astrophysics Data System (ADS)

Duluard, C. Y.; Ranson, P.; Pichon, L. E.; Pereira, J.; Oubensaid, E. H.; Lefaucheux, P.; Puech, M.; Dussart, R.

2011-06-01

Deep etching of silicon has been investigated in an inductively coupled plasma etch reactor using short SiCl4/O2 plasma steps to passivate the sidewalls of the etched structures. A study was first carried out to define the appropriate parameters to create, at a substrate temperature of -20 °C, a passivation layer by SiCl4/O2 plasma that resists lateral chemical etching in SF6 plasma. The most efficient passivation layer was obtained for a SiCl4/O2 gas flow ratio of 2:1, a pressure of 1 Pa and a source power of 1000 W. Ex situ analyses on a film deposited with these parameters show that it is very rich in oxygen. Silicon etching processes that alternate SF6 plasma etch steps with SiCl4/O2 plasma passivation steps were then developed. Preliminary tests in pulsed-mode conditions have enabled etch rates greater than 2 µm min-1 with selectivities higher than 220. These results show that it is possible to develop a silicon deep etching process at substrate temperatures around -20 °C that uses low SiCl4 and O2 gas flows instead of conventional fluorocarbon gases for sidewall protection.

Self-etching aspects of a three-step etch-and-rinse adhesive.

PubMed

Bahillo, Jose; Roig, Miguel; Bortolotto, Tissiana; Krejci, Ivo

2013-11-01

The purpose of this study is to assess the marginal adaptation of cavities restored with a three-step etch-and-rinse adhesive, OptiBond FL (OFL) under different application protocols. Twenty-four class V cavities were prepared with half of the margins located in enamel and half in dentin. Cavities were restored with OFL and a microhybrid resin composite (Clearfil AP-X). Three groups (n = 8) that differed in the etching technique were tested with thermomechanical loading, and specimens were subjected to quantitative marginal analysis before and after loading. Micromorphology of etching patters on enamel and dentin were observed with SEM. Data was evaluated with Kruskal-Wallis and Bonferroni post hoc test. Significantly lower percent CM (46.9 ± 19.5) were found after loading on enamel in group 3 compared to group 1 (96.5 ± 5.1) and group 2 (93.1 ± 8.1). However, no significant differences (p = 0.30) were observed on dentin margins. Etching enamel with phosphoric acid but avoiding etching dentin before the application of OFL, optimal marginal adaptation could be obtained, evidencing a self-etching primer effect. A reliable adhesive interface was attained with the application of the three-step etch-and-rinse OFL adhesive with a selective enamel etching, representing an advantage on restoring deep cavities.

Development and Research on the Mechanism of Novel Mist Etching Method for Oxide Thin Films

NASA Astrophysics Data System (ADS)

Kawaharamura, Toshiyuki; Hirao, Takashi

2012-03-01

A novel etching process with etchant mist was developed and applied to oxide thin films such as zinc oxide (ZnO), zinc magnesium oxide (ZnMgO), and indium tin oxide (ITO). By using this process, it was shown that precise control of the etching characteristics is possible with a reasonable etching rate, for example, in the range of 10-100 nm/min, and a fine pattern of high accuracy can also be realized, even though this is usually very difficult by conventional wet etching processes, for ZnO and ZnMgO. The mist etching process was found to be similarly and successfully applied to ITO. The mechanism of mist etching has been studied by examining the etching temperature dependence of pattern accuracy, and it was shown that the mechanism was different from that of conventional liquid-phase spray etching. It was ascertained that fine pattern etching was attained using mist droplets completely (or partly) gasified by the heat applied to the substrate. This technique was applied to the fabrication of a ZnO thin-film transistor (TFT) with a ZnO active channel length of 4 µm. The electrical properties of the TFT were found to be excellent with fine uniformity over the entire 4-in. wafer.

Effects of Etch-and-Rinse and Self-etch Adhesives on Dentin MMP-2 and MMP-9

PubMed Central

Mazzoni, A.; Scaffa, P.; Carrilho, M.; Tjäderhane, L.; Di Lenarda, R.; Polimeni, A.; Tezvergil-Mutluay, A.; Tay, F.R.; Pashley, D.H.; Breschi, L.

2013-01-01

Auto-degradation of collagen matrices occurs within hybrid layers created by contemporary dentin bonding systems, by the slow action of host-derived matrix metalloproteinases (MMPs). This study tested the null hypothesis that there are no differences in the activities of MMP-2 and -9 after treatment with different etch-and-rinse or self-etch adhesives. Tested adhesives were: Adper Scotchbond 1XT (3M ESPE), PQ1 (Ultradent), Peak LC (Ultradent), Optibond Solo Plus (Kerr), Prime&Bond NT (Dentsply) (all 2-step etch-and-rinse adhesives), and Adper Easy Bond (3M ESPE), Tri-S (Kuraray), and Xeno-V (Dentsply) (1-step self-etch adhesives). MMP-2 and -9 activities were quantified in adhesive-treated dentin powder by means of an activity assay and gelatin zymography. MMP-2 and MMP-9 activities were found after treatment with all of the simplified etch-and-rinse and self-etch adhesives; however, the activation was adhesive-dependent. It is concluded that all two-step etch-and-rinse and the one-step self-etch adhesives tested can activate endogenous MMP-2 and MMP-9 in human dentin. These results support the role of endogenous MMPs in the degradation of hybrid layers created by these adhesives. PMID:23128110

Exploration of suitable dry etch technologies for directed self-assembly

NASA Astrophysics Data System (ADS)

Yamashita, Fumiko; Nishimura, Eiichi; Yatsuda, Koichi; Mochiki, Hiromasa; Bannister, Julie

2012-03-01

Directed self-assembly (DSA) has shown the potential to replace traditional resist patterns and provide a lower cost alternative for sub-20-nm patterns. One of the possible roadblocks for DSA implementation is the ability to etch the polymers to produce quality masks for subsequent etch processes. We have studied the effects of RF frequency and etch chemistry for dry developing DSA patterns. The results of the study showed a capacitively-coupled plasma (CCP) reactor with very high frequency (VHF) had superior pattern development after the block co-polymer (BCP) etch. The VHF CCP demonstrated minimal BCP height loss and line edge roughness (LER)/line width roughness (LWR). The advantage of CCP over ICP is the low dissociation so the etch rate of BCP is maintained low enough for process control. Additionally, the advantage of VHF is the low electron energy with a tight ion energy distribution that enables removal of the polymethyl methacrylate (PMMA) with good selectivity to polystyrene (PS) and minimal LER/LWR. Etch chemistries were evaluated on the VHF CCP to determine ability to treat the BCPs to increase etch resistance and feature resolution. The right combination of RF source frequencies and etch chemistry can help overcome the challenges of using DSA patterns to create good etch results.

A review of chemical-approach and ultramorphological studies on the development of fluoride-releasing dental adhesives comprising new pre-reacted glass ionomer (PRG) fillers.

PubMed

Ikemura, Kunio; Tay, Franklin R; Endo, Takeshi; Pashley, David H

2008-05-01

This paper reviews our recent studies on fluoride-releasing adhesives and the related studies in this field based on information from original research papers, reviews, and patent literatures. A revolutionary PRG (pre-reacted glass ionomer) filler technology--where fillers were prepared by the acid-base reaction of a fluoroaluminosilicate glass with polyalkenoic acid in water, was newly developed, and a new category as "Giomer" was introduced into the market. On fluoride release capability, SIMS examination revealed in vitro fluoride ion uptake by dentin substrate from the PRG fillers in dental adhesive. On bonding durability, it was found that the improved durability of resin-dentin bonds might be achieved not only via the strengthened dentin due to fluoride ion uptake from the PRG-Ca fillers, but also due to retention of relatively insoluble 4-AETCa formed around remnant apatite crystallites within the hybrid layer in 4-AET-containing self-etching adhesives. On ultramorphological study of the resin-dentin interface, TEM images of the PRG-Ca fillers revealed that the dehydrated hydrogel was barely distinguishable from normal glass fillers, if not for the concurrent presence of remnant, incompletely reacted glass cores. In conclusion, it was expected that uptake of fluoride ions with cariostatic effect from PRG-Ca fillers would endow dentin substrates with the benefit of secondary caries prevention, together with an effective and durable adhesion to dentin.

Development of β Type Ti23Mo-45S5 Bioglass Nanocomposites for Dental Applications

PubMed Central

Jurczyk, Karolina; Miklaszewski, Andrzej; Jurczyk, Mieczyslawa U.; Jurczyk, Mieczyslaw

2015-01-01

Titanium β-type alloys attract attention as biomaterials for dental applications. The aim of this work was the synthesis of nanostructured β type Ti23Mo-x wt % 45S5 Bioglass (x = 0, 3 and 10) composites by mechanical alloying and powder metallurgy methods and their characterization. The crystallization of the amorphous material upon annealing led to the formation of a nanostructured β type Ti23Mo alloy with a grain size of approximately 40 nm. With the increase of the 45S5 Bioglass contents in Ti23Mo, nanocomposite increase of the α-phase is noticeable. The electrochemical treatment in phosphoric acid electrolyte resulted in a porous surface, followed by bioactive ceramic Ca-P deposition. Corrosion resistance potentiodynamic testing in Ringer solution at 37 °C showed a positive effect of porosity and Ca-P deposition on nanostructured Ti23Mo 3 wt % 45S5 Bioglass nanocomposite. The contact angles of glycerol on the nanostructured Ti23Mo alloy were determined and show visible decrease for bulk Ti23Mo 3 wt % 45S5 Bioglass and etched Ti23Mo 3 wt % 45S5 Bioglass nanocomposites. In vitro tests culture of normal human osteoblast cells showed very good cell proliferation, colonization, and multilayering. The present study demonstrated that porous Ti23Mo 3 wt % 45S5 Bioglass nanocomposite is a promising biomaterial for bone tissue engineering. PMID:28793695

Thermographic analysis of surface damage in teeth

NASA Astrophysics Data System (ADS)

Conde-Contreras, M.; Bante-Guerra, J.; Hernandez-Garcia, E.; Hernandez, A. M.; Trujillo, S.; Quintana, P.; Alvarado-Gil, J. J.

2008-02-01

The analysis of the surface of teeth is an important field of research and technological development due to the importance of dental pieces in health and aesthetics. The presence of cracks as well as the etching effects on teeth surface, due to different chemical agents, affects not only the appearance of teeth but its integrity. In this work, laser thermography analysis of dental pieces with damage in the form of cracks is presented. The technique consists in the illumination of the surface at the center of the sample, using a 300 mW pulsed solid state laser beam focused with a gradium lens, and monitoring the spatial and temporal distribution of the temperature field. The heating of the sample is monitored using a focal plane array infrared camera, sensitive in the spectral range 7.5-13 μm with a noise equivalent temperature difference of 0.12°C. The data acquisition was performed by the PC firewire port using a PCI-8254R card and a home-made program in Labview 8.0 was used for data acquisition. The images were processed in a home-made linux program to obtain the experimental table values. Our results are compared with position and frequency scans obtained by infrared photothermal radiometry. It is shown that the crack in the tooth appears as an increase in the photothermal signal. In contrast, the thermographic image shows a more detailed structure in which close to the crack the temperature increases, but at the crack the signal falls.

Influence of rhBMP-2 on Guided Bone Regeneration for Placement and Functional Loading of Dental Implants: A Radiographic and Histologic Study in Dogs.

PubMed

Ben Amara, Heithem; Lee, Jung-Won; Kim, Jung-Ju; Kang, Yun-Mi; Kang, Eun-Jung; Koo, Ki-Tae

Evidence on the outcomes of functional loading placed in recombinant human bone morphogenetic protein 2 (rhBMP-2)/acellular collagen sponge (ACS)-induced bone is lacking. The aim of this study was to verify whether guided bone regeneration (GBR) with rhBMP-2/ACS enhances regeneration of missing bone and osseointegration of dental implants subject to functional loading. Two bilateral standardized large saddle-type defects (≈10 × 10 × 6 mm) were surgically created in each mandible of seven beagle dogs 2 months after tooth extraction. Defects were immediately reconstructed randomly using rhBMP-2 (O-BMP or InFuse) soaked in ACS, deproteinized bovine bone mineral (DBBM) granules, or ACS alone as surgical control and subsequently covered with collagen membrane. Screw-type sand-blasted, acid-etched dental implants were placed 3 months later into the reconstructed defects and into adjacent bone. Osseointegration was allowed to progress for 3 months before functional loading of 3 months until sacrifice. Significantly more bone fill was radiographically observed for GBR with rhBMP-2/ACS (O-BMP: 92.5%, InFuse: 79%) in comparison to the DBBM (52%) and ACS alone groups (56.6%). Osseointegration was achieved and maintained in all experimental defects challenged by prostheses-driven functional load. The bone density ranged from 37.49% in the ACS group to 64.9% in the rhBMP-2/ACS (InFuse) group with no significance. The highest mean percentage of BIC was found in rhBMP-2/ACS (InFuse: 52.98%) with no statistical difference. Crestal bone resorption was observed around implants placed in reconstructed areas without any significant difference. GBR with rhBMP-2/ACS provided the greatest bone fill among the three treatment procedures. GBR with rhBMP-2/ACS showed efficacy for placement, osseointegration, and functional loading of titanium implants in alveolar ridge defects.

Laser etching of austenitic stainless steels for micro-structural evaluation

NASA Astrophysics Data System (ADS)

Baghra, Chetan; Kumar, Aniruddha; Sathe, D. B.; Bhatt, R. B.; Behere, P. G.; Afzal, Mohd

2015-06-01

Etching is a key step in metallography to reveal microstructure of polished specimen under an optical microscope. A conventional technique for producing micro-structural contrast is chemical etching. As an alternate, laser etching is investigated since it does not involve use of corrosive reagents and it can be carried out without any physical contact with sample. Laser induced etching technique will be beneficial especially in nuclear industry where materials, being radioactive in nature, are handled inside a glove box. In this paper, experimental results of pulsed Nd-YAG laser based etching of few austenitic stainless steels such as SS 304, SS 316 LN and SS alloy D9 which are chosen as structural material for fabrication of various components of upcoming Prototype Fast Breeder Reactor (PFBR) at Kalpakkam India were reported. Laser etching was done by irradiating samples using nanosecond pulsed Nd-YAG laser beam which was transported into glass paneled glove box using optics. Experiments were carried out to understand effect of laser beam parameters such as wavelength, fluence, pulse repetition rate and number of exposures required for etching of austenitic stainless steel samples. Laser etching of PFBR fuel tube and plug welded joint was also carried to evaluate base metal grain size, depth of fusion at welded joint and heat affected zone in the base metal. Experimental results demonstrated that pulsed Nd-YAG laser etching is a fast and effortless technique which can be effectively employed for non-contact remote etching of austenitic stainless steels for micro-structural evaluation.

On the influence of etch pits in the overall dissolution rate of apatite basal sections

NASA Astrophysics Data System (ADS)

Alencar, Igor; Guedes, Sandro; Palissari, Rosane; Hadler, Julio C.

2015-09-01

Determination of efficiencies for particle detection plays a central role for proper estimation of reaction rates. If chemical etching is employed in the revelation of latent particle tracks in solid-state detectors, dissolution rates and etchable lengths are important factors governing the revelation and observation. In this work, the mask method, where a reference part of the sample is protected during dissolution, was employed to measure step heights in basal sections of apatite etched with a nitric acid, HNO, solution at a concentration of 1.1 M and a temperature of 20 °C. We show a drastic increase in the etching velocity as the number of etch pits in the surface augments, in accordance with the dissolution stepwave model, where the outcrop of each etch pit generates a continuous sequence of stepwaves. The number of etch pits was varied by irradiation with neutrons and perpendicularly incident heavy ions. The size dependence of the etch-pit opening with etching duration for ion (200-300 MeV 152Sm and 238U) tracks was also investigated. There is no distinction for the etch pits between the different ions, and the dissolution seems to be governed by the opening velocity when a high number of etch pits are present in the surface. Measurements of the etchable lengths of these ion tracks show an increase in these lengths when samples are not pre-annealed before irradiation. We discuss the implications of these findings for fission-track modelling.

Morphological Evaluation of the Adhesive/Enamel interfaces of Two-step Self-etching Adhesives and Multimode One-bottle Self-etching Adhesives.

PubMed

Sato, Takaaki; Takagaki, Tomohiro; Matsui, Naoko; Hamba, Hidenori; Sadr, Alireza; Nikaido, Toru; Tagami, Junji

To evaluate the acid-base resistant zone (ABRZ) at the adhesive/enamel interface of self-etching adhesives with or without prior phosphoric acid etching. Four adhesives were used in 8 groups: Clearfil SE Bond (SEB), Optibond XTR (XTR), Scotchbond Universal Adhesive (SBU), and Clearfil BOND SE ONE (ONE) without prior phosphoric-acid etching, and each adhesive with phosphoric acid etching for 10 s (P-SEB, P-XTR, P-SBU and P-ONE, respectively). After application of self-etching adhesives on ground enamel surfaces of human teeth, a flowable composite was placed. For observation of the acid-base resistant zone (ABRZ), the bonded interface was exposed to demineralizing solution (pH 4.5) for 4.5 h, followed by 5% NaOCl with ultrasonication for 20 min. After the acid-base challenge, morphological attributes of the interface were observed using SEM. ABRZ formation was confirmed in all groups. The funnel-shaped erosion beneath the interface was present in SBU and ONE, where nearly 10 to 15 μm of enamel was dissolved. With phosphoric acid etching, the ABRZs were obviously thicker compared with no phosphoric acid etching. Enamel beneath the bonding interface was more susceptible to acid dissolution in SBU and ONE. In the case of the one-bottle self-etching adhesives and universal adhesives that intrinsically have higher pH values, enamel etching should be recommended to improve the interfacial quality.

Self-etching adhesive on intact enamel, with and without pre-etching.

PubMed

Devarasa, G M; Subba Reddy, V V; Chaitra, N L; Swarna, Y M

2012-05-01

Bond strengths of composite resin to enamel using self-etch adhesive (SEA) Clearfil SE bond system on intact enamel and enamel pre-etched with phosphoric acid were compared. The objective was to determine if the pre-etching would increase the bond strengths of the SEA systems to intact enamel and to evaluate the effect of pre-etching on bond formation of self-etch adhesives on intact enamel. Labial surfaces of 40 caries free permanent upper central and lateral incisors were cleaned, sectioned of their roots. All specimens were mounted on acrylic block and divided randomly into four groups. In two groups the application of self-etch adhesive, Clearfil SE bond was carried as per manufacturer's instructions, composite cylinders were built, whereas in the other two groups, 37% phosphoric acid etching was done before the application of self-etching adhesives. Then the resin tags were analyzed using scanning electron microscope and shear bond strength was measured using Instron universal testing machine. When phosphoric acid was used, there was significant increase in the depth of penetration of resin tags and in the Shear Bond Strength of composite to enamel. The results indicate that out of both treatment groups, pre-etching the intact enamel with 37% phosphoric acid resulted in formation of longer resin tags and higher depth of penetration of resin tags of the Clearfil SE bond, and attaining higher bond strength of the Clearfil SE bond to intact enamel. Copyright © 2011 Wiley Periodicals, Inc.

Comparative Evaluation of the Etching Pattern of Er,Cr:YSGG & Acid Etching on Extracted Human Teeth-An ESEM Analysis

PubMed Central

Mazumdar, Dibyendu; Ranjan, Shashi; Krishna, Naveen Kumar; Kole, Ravindra; Singh, Priyankar; Lakiang, Deirimika; Jayam, Chiranjeevi

2016-01-01

Introduction Etching of enamel and dentin surfaces increases the surface area of the substrate for better bonding of the tooth colored restorative materials. Acid etching is the most commonly used method. Recently, hard tissue lasers have been used for this purpose. Aim The aim of the present study was to evaluate and compare the etching pattern of Er,Cr:YSGG and conventional etching on extracted human enamel and dentin specimens. Materials and Methods Total 40 extracted non-diseased teeth were selected, 20 anterior and 20 posterior teeth each for enamel and dentin specimens respectively. The sectioned samples were polished by 400 grit Silicon Carbide (SiC) paper to a thickness of 1.0 ± 0.5 mm. The enamel and dentin specimens were grouped as: GrE1 & GrD1 as control specimens, GrE2 & GrD2 were acid etched and GrE3 & GrD3 were lased. Acid etching was done using Conditioner 36 (37 % phosphoric acid) according to manufacturer instructions. Laser etching was done using Er,Cr:YSGG (Erbium, Chromium : Ytrium Scandium Gallium Garnet) at power settings of 3W, air 70% and water 20%. After surface treatment with assigned agents the specimens were analyzed under ESEM (Environmental Scanning Electron Microscope) at X1000 and X5000 magnification. Results Chi Square and Student “t” statistical analysis was used to compare smear layer removal and etching patterns between GrE2-GrE3. GrD2 and GrD3 were compared for smear layer removal and diameter of dentinal tubule opening using the same statistical analysis. Chi-square test for removal of smear layer in any of the treated surfaces i.e., GrE2-E3 and GrD2-D3 did not differ significantly (p>0.05). While GrE2 showed predominantly type I etching pattern (Chi-square=2.78, 0.05

0.10) and GrE3 showed type III etching (Chi-square=4.50, p<0.05). The tubule diameters were measured using GSA (Gesellschaft fur Softwareentwicklung und Analytik, Germany) image analyzer and the ‘t’ value of student ‘t’ test was 18.10 which was a highly significant result (p<.001). GrD2 had a mean dentinal tubule diameter of 2.78μm and GrD3 of 1.09μm. Conclusion The present study revealed type I etching pattern after acid etching, while type III etching pattern in enamel after laser etching. The lased dentin showed preferential removal of intertubular dentin while acid etching had more effect on the peritubular dentin. No significant differences was observed in removal of smear layer between the acid etched and lased groups. Although diameter of the exposed dentinal tubules was lesser after lased treatment in comparison to acid etching, further long term in vivo studies are needed with different parameters to establish the usage of Er,Cr:YSGG as a sole etching agent. PMID:27437337

Study of Gallium Arsenide Etching in a DC Discharge in Low-Pressure HCl-Containing Mixtures

NASA Astrophysics Data System (ADS)

Dunaev, A. V.; Murin, D. B.

2018-04-01

Halogen-containing plasmas are often used to form topological structures on semiconductor surfaces; therefore, spectral monitoring of the etching process is an important diagnostic tool in modern electronics. In this work, the emission spectra of gas discharges in mixtures of hydrogen chloride with argon, chlorine, and hydrogen in the presence of a semiconducting gallium arsenide plate were studied. Spectral lines and bands of the GaAs etching products appropriate for monitoring the etching rate were determined. It is shown that the emission intensity of the etching products is proportional to the GaAs etching rate in plasmas of HCl mixtures with Ar and Cl2, which makes it possible to monitor the etching process in real time by means of spectral methods.

Two-year clinical trial of a universal adhesive in total-etch and self-etch mode in non-carious cervical lesions☆

PubMed Central

Lawson, Nathaniel C.; Robles, Augusto; Fu, Chin-Chuan; Lin, Chee Paul; Sawlani, Kanchan; Burgess, John O.

2016-01-01

Objectives To compare the clinical performance of Scotchbond™ Universal Adhesive used in self- and total-etch modes and two-bottle Scotchbond™ Multi-purpose Adhesive in total-etch mode for Class 5 non-carious cervical lesions (NCCLs). Methods 37 adults were recruited with 3 or 6 NCCLs (>1.5 mm deep). Teeth were isolated, and a short cervical bevel was prepared. Teeth were restored randomly with Scotchbond Universal total-etch, Scotchbond Universal self-etch or Scotchbond Multi-purpose followed with a composite resin. Restorations were evaluated at baseline, 6, 12 and 24 months for marginal adaptation, marginal discoloration, secondary caries, and sensitivity to cold using modified USPHS Criteria. Patients and evaluators were blinded. Logistic and linear regression models using a generalized estimating equation were applied to evaluate the effects of time and adhesive material on clinical assessment outcomes over the 24 month follow-up period. Kaplan–Meier method was used to compare the retention between adhesive materials. Results Clinical performance of all adhesive materials deteriorated over time for marginal adaptation, and discoloration (p <0.0001). Both Scotchbond Universal self-etch and Scotchbond Multi-purpose materials were more than three times as likely to contribute to less satisfying performance in marginal discoloration over time than Scotchbond Universal total-etch. The retention rates up to 24 months were 87.6%, 94.9% and 100% for Scotchbond Multi-purpose and Scotchbond Universal self-etch and total-etch, respectively. Conclusions Scotchbond Universal in self- and total- etch modes performed similar to or better than Scotchbond Multipurpose, respectively. Clinical significance 24 month evaluation of a universal adhesive indicates acceptable clinical performance, particularly in a total-etch mode. PMID:26231300

Effect of source frequency and pulsing on the SiO2 etching characteristics of dual-frequency capacitive coupled plasma

NASA Astrophysics Data System (ADS)

Kim, Hoe Jun; Jeon, Min Hwan; Mishra, Anurag Kumar; Kim, In Jun; Sin, Tae Ho; Yeom, Geun Young

2015-01-01

A SiO2 layer masked with an amorphous carbon layer (ACL) has been etched in an Ar/C4F8 gas mixture with dual frequency capacitively coupled plasmas under variable frequency (13.56-60 MHz)/pulsed rf source power and 2 MHz continuous wave (CW) rf bias power, the effects of the frequency and pulsing of the source rf power on the SiO2 etch characteristics were investigated. By pulsing the rf power, an increased SiO2 etch selectivity was observed with decreasing SiO2 etch rate. However, when the rf power frequency was increased, not only a higher SiO2 etch rate but also higher SiO2 etch selectivity was observed for both CW and pulse modes. A higher CF2/F ratio and lower electron temperature were observed for both a higher source frequency mode and a pulsed plasma mode. Therefore, when the C 1s binding states of the etched SiO2 surfaces were investigated using X-ray photoelectron spectroscopy (XPS), the increase of C-Fx bonding on the SiO2 surface was observed for a higher source frequency operation similar to a pulsed plasma condition indicating the increase of SiO2 etch selectivity over the ACL. The increase of the SiO2 etch rate with increasing etch selectivity for the higher source frequency operation appears to be related to the increase of the total plasma density with increasing CF2/F ratio in the plasma. The SiO2 etch profile was also improved not only by using the pulsed plasma but also by increasing the source frequency.

Effect of Saliva on the Tensile Bond Strength of Different Generation Adhesive Systems: An In-Vitro Study.

PubMed

Gupta, Nimisha; Tripathi, Abhay Mani; Saha, Sonali; Dhinsa, Kavita; Garg, Aarti

2015-07-01

Newer development of bonding agents have gained a better understanding of factors affecting adhesion of interface between composite and dentin surface to improve longevity of restorations. The present study evaluated the influence of salivary contamination on the tensile bond strength of different generation adhesive systems (two-step etch-and-rinse, two-step self-etch and one-step self-etch) during different bonding stages to dentin where isolation is not maintained. Superficial dentin surfaces of 90 extracted human molars were randomly divided into three study Groups (Group A: Two-step etch-and-rinse adhesive system; Group B: Two-step self-etch adhesive system and Group C: One-step self-etch adhesive system) according to the different generation of adhesives used. According to treatment conditions in different bonding steps, each Group was further divided into three Subgroups containing ten teeth in each. After adhesive application, resin composite blocks were built on dentin and light cured subsequently. The teeth were then stored in water for 24 hours before sending for testing of tensile bond strength by Universal Testing Machine. The collected data were then statistically analysed using one-way ANOVA and Tukey HSD test. One-step self-etch adhesive system revealed maximum mean tensile bond strength followed in descending order by Two-step self-etch adhesive system and Two-step etch-and-rinse adhesive system both in uncontaminated and saliva contaminated conditions respectively. Unlike One-step self-etch adhesive system, saliva contamination could reduce tensile bond strength of the two-step self-etch and two-step etch-and-rinse adhesive system. Furthermore, the step of bonding procedures and the type of adhesive seems to be effective on the bond strength of adhesives contaminated with saliva.

Dry etched SiO2 Mask for HgCdTe Etching Process

NASA Astrophysics Data System (ADS)

Chen, Y. Y.; Ye, Z. H.; Sun, C. H.; Deng, L. G.; Zhang, S.; Xing, W.; Hu, X. N.; Ding, R. J.; He, L.

2016-09-01

A highly anisotropic etching process with low etch-induced damage is indispensable for advanced HgCdTe (MCT) infrared focal plane array (IRFPA) detectors. The inductively coupled plasma (ICP) enhanced reactive ion etching technique has been widely adopted in manufacturing HgCdTe IRFPA devices. An accurately patterned mask with sharp edges is decisive to accomplish pattern duplication. It has been reported by our group that the SiO2 mask functions well in etching HgCdTe with high selectivity. However, the wet process in defining the SiO2 mask is limited by ambiguous edges and nonuniform patterns. In this report, we patterned SiO2 with a mature ICP etching technique, prior to which a thin ZnS film was deposited by thermal evaporation. The SiO2 film etching can be terminated at the auto-stopping point of the ZnS layer thanks to the high selectivity of SiO2/ZnS in SF6 based etchant. Consequently, MCT etching was directly performed without any other treatment. This mask showed acceptable profile due to the maturity of the SiO2 etching process. The well-defined SiO2 pattern and the etched smooth surfaces were investigated with scanning electron microscopy and atomic force microscope. This new mask process could transfer the patterns exactly with very small etch-bias. A cavity with aspect-ratio (AR) of 1.2 and root mean square roughness of 1.77 nm was achieved first, slightly higher AR of 1.67 was also get with better mask profile. This masking process ensures good uniformity and surely benefits the delineation of shrinking pixels with its high resolution.

Deep Etching Process Developed for the Fabrication of Silicon Carbide Microsystems

NASA Technical Reports Server (NTRS)

Beheim, Glenn M.

2000-01-01

Silicon carbide (SiC), because of its superior electrical and mechanical properties at elevated temperatures, is a nearly ideal material for the microminiature sensors and actuators that are used in harsh environments where temperatures may reach 600 C or greater. Deep etching using plasma methods is one of the key processes used to fabricate silicon microsystems for more benign environments, but SiC has proven to be a more difficult material to etch, and etch depths in SiC have been limited to several micrometers. Recently, the Sensors and Electronics Technology Branch at the NASA Glenn Research Center at Lewis Field developed a plasma etching process that was shown to be capable of etching SiC to a depth of 60 mm. Deep etching of SiC is achieved by inductive coupling of radiofrequency electrical energy to a sulfur hexafluoride (SF6) plasma to direct a high flux of energetic ions and reactive fluorine atoms to the SiC surface. The plasma etch is performed at a low pressure, 5 mtorr, which together with a high gas throughput, provides for rapid removal of the gaseous etch products. The lateral topology of the SiC microstructure is defined by a thin film of etch-resistant material, such as indium-tin-oxide, which is patterned using conventional photolithographic processes. Ions from the plasma bombard the exposed SiC surfaces and supply the energy needed to initiate a reaction between SiC and atomic fluorine. In the absence of ion bombardment, no reaction occurs, so surfaces perpendicular to the wafer surface (the etch sidewalls) are etched slowly, yielding the desired vertical sidewalls.

Immediate bonding properties of universal adhesives to dentine.

PubMed

Muñoz, Miguel Angel; Luque, Issis; Hass, Viviane; Reis, Alessandra; Loguercio, Alessandro Dourado; Bombarda, Nara Hellen Campanha

2013-05-01

To evaluate the dentine microtensile bond strength (μTBS), nanoleakage (NL), degree of conversion (DC) within the hybrid layer for etch-and-rinse and self-etch strategies of universal simplified adhesive systems. forty caries free extracted third molars were divided into 8 groups for μTBS (n=5), according to the adhesive and etching strategy: Clearfil SE Bond [CSE] and Adper Single Bond 2 [SB], as controls; Peak Universal Adhesive System, self-etch [PkSe] and etch-and-rinse [PkEr]; Scotchbond Universal Adhesive, self-etch [ScSe] and etch-and-rinse [ScEr]; All Bond Universal, self-etch [AlSe] and etch-and-rinse [AlEr]. After restorations were constructed, specimens were stored in water (37°C/24h) and then resin-dentine sticks were prepared (0.8mm(2)). The sticks were tested under tension at 0.5mm/min. Some sticks from each tooth group were used for DC determination by micro-Raman spectroscopy or nanoleakage evaluation (NL). The pH for each solution was evaluated using a pH metre. Data were analyzed with one-way ANOVA and Tukey's test (α=0.05). For μTBS, only PkSe and PkEr were similar to the respective control groups (p>0.05). AlSe showed the lowest μTBS mean (p<0.05). For NL, ScEr, ScSe, AlSe, and AlEr showed the lowest NL similar to control groups (p<0.05). For DC, only ScSe showed lower DC than the other materials (p<0.05). Performance of universal adhesives was shown to be material-dependent. The results indicate that this new category of universal adhesives used on dentine as either etch-and-rinse or self-etch strategies were inferior as regards at least one of the properties evaluated (μTBS, NL and DC) in comparison with the control adhesives (CSE for self-etch and SB for etch-and-rinse). Copyright © 2013 Elsevier Ltd. All rights reserved.

CR-39 track etching and blow-up method

DOEpatents

Hankins, Dale E.

1987-01-01

This invention is a method of etching tracks in CR-39 foil to obtain uniformly sized tracks. The invention comprises a step of electrochemically etching the foil at a low frequency and a "blow-up" step of electrochemically etching the foil at a high frequency.

Evaluation of microtensile bond strength of self-etching adhesives on normal and caries-affected dentin.

PubMed

Shibata, Shizuma; Vieira, Luiz Clovis Cardoso; Baratieri, Luiz Narciso; Fu, Jiale; Hoshika, Shuhei; Matsuda, Yasuhiro; Sano, Hidehiko

2016-01-01

The purpose of this study was to evaluate the µTBS (microtensile bond strength) of currently available self-etching adhesives with an experimental self-etch adhesive in normal and caries-affected dentin, using a portable hardness measuring device, in order to standardize dentin Knoop hardness. Normal (ND) and caries-affected dentin (CAD) were obtained from twenty human molars with class II natural caries. The following adhesive systems were tested: Mega Bond (MB), a 2-step self-etching adhesive; MTB-200 (MTB), an experimental 1-step self-etching adhesive (1-SEA), and two commercially available one-step self-etching systems, G-Bond Plus (GB) and Adper Easy Bond (EB). MB-ND achieved the highest µTBS (p<0.05). The mean µTBS was statistically lower in CAD than in ND for all adhesives tested (p<0.05), and the 2-step self-etch adhesive achieved better overall performance than the 1-step self-etch adhesives.

Vertical Si nanowire arrays fabricated by magnetically guided metal-assisted chemical etching

NASA Astrophysics Data System (ADS)

Chun, Dong Won; Kim, Tae Kyoung; Choi, Duyoung; Caldwell, Elizabeth; Kim, Young Jin; Paik, Jae Cheol; Jin, Sungho; Chen, Renkun

2016-11-01

In this work, vertically aligned Si nanowire arrays were fabricated by magnetically guided metal-assisted directional chemical etching. Using an anodized aluminum oxide template as a shadow mask, nanoscale Ni dot arrays were fabricated on an Si wafer to serve as a mask to protect the Si during the etching. For the magnetically guided chemical etching, we deposited a tri-layer metal catalyst (Au/Fe/Au) in a Swiss-cheese configuration and etched the sample under the magnetic field to improve the directionality of the Si nanowire etching and increase the etching rate along the vertical direction. After the etching, the nanowires were dried with minimal surface-tension-induced aggregation by utilizing a supercritical CO2 drying procedure. High-resolution transmission electron microscopy (HR-TEM) analysis confirmed the formation of single-crystal Si nanowires. The method developed here for producing vertically aligned Si nanowire arrays could find a wide range of applications in electrochemical and electronic devices.

Effect of the addition of SF6 and N2 in inductively coupled SiCl4 plasma for GaN etching

NASA Astrophysics Data System (ADS)

Oubensaid, E. H.; Duluard, C. Y.; Pichon, L. E.; Pereira, J.; Boufnichel, M.; Lefaucheux, P.; Dussart, R.; Ranson, P.

2009-07-01

The GaN etching by SiCl4 plasma is considered in an ICP tool. By respecting some material limitations, it has been possible to etch the gallium nitride in pure SiCl4 plasma, with an etch rate of 19 nm min-1. This result is comparable to other reported results. Thereafter, the combination of SiCl4 with SF6 and N2 was tested in order to increase the etch rate. The addition of SF6 in the plasma has enabled us to reach an etch rate of 53 nm min-1. However, best results were obtained with the addition of N2, with an increase of the etch rate by a factor of 6. Mass spectrometry was also performed in order to determine the effects of the additional gases. The surface morphology of the GaN was also analysed by scanning electron microscope after etching.

Influence of pretreatment on the surface characteristics of PLLA fibers and subsequent hydroxyapatite coating.

PubMed

Peng, F; Olson, J R; Shaw, M T; Wei, M

2009-01-01

A fibrous precursor for bone repair composites was made by coating poly(L-lactide) (PLLA) fibers with hydroxyapatite (HA) using a biomimetic method. To enhance the bonding between the HA coating and the PLLA fiber, PLLA fibers were etched with either sodium hydroxide or sodium hypochlorite to generate carboxyl groups on fiber surfaces. The experiments were designed to determine the influence of etching on the fiber surface morphology and chemistry as well as the subsequent HA coating on the etched fiber surfaces. It was found that the etching pretreatment increased the roughness as well as the hydrophilicity of fibers, indicating that hydrolysis of PLLA chains had taken place on fiber surfaces. The etching pretreatment also promoted HA coating formation by introducing thicker coating on the surface of fibers with a longer etching time, a higher etching concentration, or with NaOCl as the etching agent. A mechanism of surface hydrolysis and oxidation of PLLA was proposed. (c) 2008 Wiley Periodicals, Inc.

Effect of tetramethylammonium hydroxide/isopropyl alcohol wet etching on geometry and surface roughness of silicon nanowires fabricated by AFM lithography

PubMed Central

Yusoh, Siti Noorhaniah

2016-01-01

Summary The optimization of etchant parameters in wet etching plays an important role in the fabrication of semiconductor devices. Wet etching of tetramethylammonium hydroxide (TMAH)/isopropyl alcohol (IPA) on silicon nanowires fabricated by AFM lithography is studied herein. TMAH (25 wt %) with different IPA concentrations (0, 10, 20, and 30 vol %) and etching time durations (30, 40, and 50 s) were investigated. The relationships between etching depth and width, and etching rate and surface roughness of silicon nanowires were characterized in detail using atomic force microscopy (AFM). The obtained results indicate that increased IPA concentration in TMAH produced greater width of the silicon nanowires with a smooth surface. It was also observed that the use of a longer etching time causes more unmasked silicon layers to be removed. Importantly, throughout this study, wet etching with optimized parameters can be applied in the design of the devices with excellent performance for many applications. PMID:27826521

Reactive ion etching effects on carbon-doped Ge2Sb2Te5 phase change material in CF4/Ar plasma

NASA Astrophysics Data System (ADS)

Shen, Lanlan; Song, Sannian; Song, Zhitang; Li, Le; Guo, Tianqi; Liu, Bo; Wu, Liangcai; Cheng, Yan; Feng, Songlin

2016-10-01

Recently, carbon-doped Ge2Sb2Te5 (CGST) has been proved to be a high promising material for future phase change memory technology. In this article, reactive ion etching (RIE) of phase change material CGST films is studied using CF4/Ar gas mixture. The effects on gas-mixing ratio, RF power, gas pressure on the etch rate, etch profile and roughness of the CGST film are investigated. Conventional phase change material Ge2Sb2Te5 (GST) films are simultaneously studied for comparison. Compared with GST film, 10 % more CF4 is needed for high etch rate and 10% less CF4 for good anisotropy of CGST due to more fluorocarbon polymer deposition during CF4 etching. The trends of etch rates and roughness of CGST with varying RF power and chamber pressure are similar with those of GST. Furthermore, the etch rate of CGST are more easily to be saturated when higher RF power is applied.

Neutral beam and ICP etching of HKMG MOS capacitors: Observations and a plasma-induced damage model

NASA Astrophysics Data System (ADS)

Kuo, Tai-Chen; Shih, Tzu-Lang; Su, Yin-Hsien; Lee, Wen-Hsi; Current, Michael Ira; Samukawa, Seiji

2018-04-01

In this study, TiN/HfO2/Si metal-oxide-semiconductor (MOS) capacitors were etched by a neutral beam etching technique under two contrasting conditions. The configurations of neutral beam etching technique were specially designed to demonstrate a "damage-free" condition or to approximate "reactive-ion-etching-like" conditions to verify the effect of plasma-induced damage on electrical characteristics of MOS capacitors. The results show that by neutral beam etching (NBE), the interface state density (Dit) and the oxide trapped charge (Qot) were lower than routine plasma etching. Furthermore, the decrease in capacitor size does not lead to an increase in leakage current density, indicating less plasma induced side-wall damage. We present a plasma-induced gate stack damage model which we demonstrate by using these two different etching configurations. These results show that NBE is effective in preventing plasma-induced damage at the high-k/Si interface and on the high-k oxide sidewall and thus improve the electrical performance of the gate structure.

Wet etching mechanism and crystallization of indium-tin oxide layer for application in light-emitting diodes

NASA Astrophysics Data System (ADS)

Su, Shui-Hsiang; Kong, Hsieng-Jen; Tseng, Chun-Lung; Chen, Guan-Yu

2018-01-01

In the article, we describe the etching mechanism of indium-tin oxide (ITO) film, which was wet-etched using a solution of hydrochloric acid (HCl) and ferric chloride (FeCl3). The etching mechanism is analyzed at various etching durations of ITO films by scanning electron microscopy (SEM), high-resolution transmission electron microscopy (HR-TEM), and selective area diffraction (SAD) analysis. In comparison with the crystalline phase of SnO2, the In2O3 phase can be more easily transformed to In3+ and can form an inverted conical structure during the etching process. By adjusting the etching duration, the residual ITO is completely removed to show a designed pattern. This is attributed to the negative Gibbs energy of In2O3 transformed to In3+. The result also corresponds to the finding of energy-dispersive X-ray spectroscopy (EDS) analysis that the Sn/In ratio increases with increasing etching duration.

Trends in Dielectric Etch for Microelectronics Processing

NASA Astrophysics Data System (ADS)

Hudson, Eric A.

2003-10-01

Dielectric etch technology faces many challenges to meet the requirements for leading-edge microelectronics processing. The move to sub 100-nm device design rules increases the aspect ratios of certain features, imposes tighter restrictions on etched features' critical dimensions, and increases the density of closely packed arrays of features. Changes in photolithography are driving transitions to new photoresist materials and novel multilayer resist methods. The increasing use of copper metallization and low-k interlayer dielectric materials has introduced dual-damascene integration methods, with specialized dielectric etch applications. A common need is the selective removal of multiple layers which have very different compositions, while maintaining close control of the etched features' profiles. To increase productivity, there is a growing trend toward in-situ processing, which allows several films to be successively etched during a single pass through the process module. Dielectric etch systems mainly utilize capacitively coupled etch reactors, operating with medium-density plasmas and low gas residence time. Commercial technology development increasingly relies upon plasma diagnostics and modeling to reduce development cycle time and maximize performance.

Selective etching of TiN over TaN and vice versa in chlorine-containing plasmas

DOE Office of Scientific and Technical Information (OSTI.GOV)

Shin, Hyungjoo; Zhu Weiye; Liu Lei

2013-05-15

Selectivity of etching between physical vapor-deposited TiN and TaN was studied in chlorine-containing plasmas, under isotropic etching conditions. Etching rates for blanket films were measured in-situ using optical emission of the N{sub 2} (C{sup 3}{Pi}{sub u}{yields}B{sup 3}{Pi}{sub g}) bandhead at 337 nm to determine the etching time, and transmission electron microscopy to determine the starting film thickness. The etching selectivity in Cl{sub 2}/He or HCl/He plasmas was poor (<2:1). There was a window of very high selectivity of etching TiN over TaN by adding small amounts (<1%) of O{sub 2} in the Cl{sub 2}/He plasma. Reverse selectivity (10:1 of TaNmore » etching over TiN) was observed when adding small amounts of O{sub 2} to the HCl/He plasma. Results are explained on the basis of the volatility of plausible reaction products.« less

Nanoparticle-based etching of silicon surfaces

DOEpatents

Branz, Howard [Boulder, CO; Duda, Anna [Denver, CO; Ginley, David S [Evergreen, CO; Yost, Vernon [Littleton, CO; Meier, Daniel [Atlanta, GA; Ward, James S [Golden, CO

2011-12-13

A method (300) of texturing silicon surfaces (116) such to reduce reflectivity of a silicon wafer (110) for use in solar cells. The method (300) includes filling (330, 340) a vessel (122) with a volume of an etching solution (124) so as to cover the silicon surface 116) of a wafer or substrate (112). The etching solution (124) is made up of a catalytic nanomaterial (140) and an oxidant-etchant solution (146). The catalytic nanomaterial (140) may include gold or silver nanoparticles or noble metal nanoparticles, each of which may be a colloidal solution. The oxidant-etchant solution (146) includes an etching agent (142), such as hydrofluoric acid, and an oxidizing agent (144), such as hydrogen peroxide. Etching (350) is performed for a period of time including agitating or stirring the etching solution (124). The etch time may be selected such that the etched silicon surface (116) has a reflectivity of less than about 15 percent such as 1 to 10 percent in a 350 to 1000 nanometer wavelength range.

Power ultrasound irradiation during the alkaline etching process of the 2024 aluminum alloy

NASA Astrophysics Data System (ADS)

Moutarlier, V.; Viennet, R.; Rolet, J.; Gigandet, M. P.; Hihn, J. Y.

2015-11-01

Prior to any surface treatment on an aluminum alloy, a surface preparation is necessary. This commonly consists in performing an alkaline etching followed by acid deoxidizing. In this work, the use of power ultrasound irradiation during the etching step on the 2024 aluminum alloy was studied. The etching rate was estimated by weight loss, and the alkaline film formed during the etching step was characterized by glow discharge optical emission spectrometry (GDOES) and scanning electron microscope (SEM). The benefit of power ultrasound during the etching step was confirmed by pitting potential measurement in NaCl solution after a post-treatment (anodizing).

Anisotropic Etching Using Reactive Cluster Beams

NASA Astrophysics Data System (ADS)

Koike, Kunihiko; Yoshino, Yu; Senoo, Takehiko; Seki, Toshio; Ninomiya, Satoshi; Aoki, Takaaki; Matsuo, Jiro

2010-12-01

The characteristics of Si etching using nonionic cluster beams with highly reactive chlorine-trifluoride (ClF3) gas were examined. An etching rate of 40 µm/min or higher was obtained even at room temperature when a ClF3 molecular cluster was formed and irradiated on a single-crystal Si substrate in high vacuum. The etching selectivity of Si with respect to a photoresist and SiO2 was at least 1:1000. We also succeeded in highly anisotropic etching with an aspect ratio of 10 or higher. Moreover, this etching method has a great advantage of low damage, compared with the conventional plasma process.

Uniformly thinned optical fibers produced via HF etching with spectral and microscopic verification.

PubMed

Bal, Harpreet K; Brodzeli, Zourab; Dragomir, Nicoleta M; Collins, Stephen F; Sidiroglou, Fotios

2012-05-01

A method for producing uniformly thinned (etched) optical fibers is described, which can also be employed to etch optical fibers containing a Bragg grating (FBG) uniformly for evanescent-field-based sensing and other applications. Through a simple modification of this method, the fabrication of phase-shifted FBGs based on uneven etching is also shown. The critical role of how a fiber is secured is shown, and the success of the method is illustrated, by differential interference contrast microscopy images of uniformly etched FBGs. An etched FBG sensor for the monitoring of the refractive index of different glycerin solutions is demonstrated.

Controlled ion track etching

NASA Astrophysics Data System (ADS)

George, J.; Irkens, M.; Neumann, S.; Scherer, U. W.; Srivastava, A.; Sinha, D.; Fink, D.

2006-03-01

It is a common practice since long to follow the ion track-etching process in thin foils via conductometry, i.e . by measurement of the electrical current which passes through the etched track, once the track breakthrough condition has been achieved. The major disadvantage of this approach, namely the absence of any major detectable signal before breakthrough, can be avoided by examining the track-etching process capacitively. This method allows one to define precisely not only the breakthrough point before it is reached, but also the length of any non-transient track. Combining both capacitive and conductive etching allows one to control the etching process perfectly. Examples and possible applications are given.

Evaluation of Pentafluoroethane and 1,1-Difluoroethane for a Dielectric Etch Application in an Inductively Coupled Plasma Etch Tool

NASA Astrophysics Data System (ADS)

Karecki, Simon; Chatterjee, Ritwik; Pruette, Laura; Reif, Rafael; Sparks, Terry; Beu, Laurie; Vartanian, Victor

2000-07-01

In this work, a combination of two hydrofluorocarbon compounds, pentafluoroethane (FC-125, C2HF5) and 1,1-difluoroethane (FC-152a, CF2H-CH3), was evaluated as a potential replacement for perfluorocompounds in dielectric etch applications. A high aspect ratio oxide via etch was used as the test vehicle for this study, which was conducted in a commercial inductively coupled high density plasma etch tool. Both process and emissions data were collected and compared to those provided by a process utilizing a standard perfluorinated etch chemistry (C2F6). Global warming (CF4, C2F6, CHF3) and hygroscopic gas (HF, SiF4) emissions were characterized using Fourier transform infrared (FTIR) spectroscopy. FC-125/FC-152a was found to produce significant reductions in global warming emissions, on the order of 68 to 76% relative to the reference process. Although etch stopping, caused by a high degree of polymer deposition inside the etched features, was observed, process data otherwise appeared promising for an initial study, with good resist selectivity and etch rates being achieved.

Anisotropic Etching of Hexagonal Boron Nitride and Graphene: Question of Edge Terminations.

PubMed

Stehle, Yijing Y; Sang, Xiahan; Unocic, Raymond R; Voylov, Dmitry; Jackson, Roderick K; Smirnov, Sergei; Vlassiouk, Ivan

2017-12-13

Chemical vapor deposition (CVD) has been established as the most effective way to grow large area two-dimensional materials. Direct study of the etching process can reveal subtleties of this competing with the growth reaction and thus provide the necessary details of the overall growth mechanism. Here we investigate hydrogen-induced etching of hBN and graphene and compare the results with the classical kinetic Wulff construction model. Formation of the anisotropically etched holes in the center of hBN and graphene single crystals was observed along with the changes in the crystals' circumference. We show that the edges of triangular holes in hBN crystals formed at regular etching conditions are parallel to B-terminated zigzags, opposite to the N-terminated zigzag edges of hBN triangular crystals. The morphology of the etched hBN holes is affected by a disbalance of the B/N ratio upon etching and can be shifted toward the anticipated from the Wulff model N-terminated zigzag by etching in a nitrogen buffer gas instead of a typical argon. For graphene, etched hexagonal holes are terminated by zigzag, while the crystal circumference is gradually changing from a pure zigzag to a slanted angle resulting in dodecagons.

High-aspect ratio micro- and nanostructures enabled by photo-electrochemical etching for sensing and energy harvesting applications

NASA Astrophysics Data System (ADS)

Alhalaili, Badriyah; Dryden, Daniel M.; Vidu, Ruxandra; Ghandiparsi, Soroush; Cansizoglu, Hilal; Gao, Yang; Saif Islam, M.

2018-03-01

Photo-electrochemical (PEC) etching can produce high-aspect ratio features, such as pillars and holes, with high anisotropy and selectivity, while avoiding the surface and sidewall damage caused by traditional deep reactive ion etching (DRIE) or inductively coupled plasma (ICP) RIE. Plasma-based techniques lead to the formation of dangling bonds, surface traps, carrier leakage paths, and recombination centers. In pursuit of effective PEC etching, we demonstrate an optical system using long wavelength (λ = 975 nm) infra-red (IR) illumination from a high-power laser (1-10 W) to control the PEC etching process in n-type silicon. The silicon wafer surface was patterned with notches through a lithography process and KOH etching. Then, PEC etching was introduced by illuminating the backside of the silicon wafer to enhance depth, resulting in high-aspect ratio structures. The effect of the PEC etching process was optimized by varying light intensities and electrolyte concentrations. This work was focused on determining and optimizing this PEC etching technique on silicon, with the goal of expanding the method to a variety of materials including GaN and SiC that are used in designing optoelectronic and electronic devices, sensors and energy harvesting devices.

Solid-State Nanopore.

PubMed

Yuan, Zhishan; Wang, Chengyong; Yi, Xin; Ni, Zhonghua; Chen, Yunfei; Li, Tie

2018-02-20

Solid-state nanopore has captured the attention of many researchers due to its characteristic of nanoscale. Now, different fabrication methods have been reported, which can be summarized into two broad categories: "top-down" etching technology and "bottom-up" shrinkage technology. Ion track etching method, mask etching method chemical solution etching method, and high-energy particle etching and shrinkage method are exhibited in this report. Besides, we also discussed applications of solid-state nanopore fabrication technology in DNA sequencing, protein detection, and energy conversion.

Solid-State Nanopore

NASA Astrophysics Data System (ADS)

Yuan, Zhishan; Wang, Chengyong; Yi, Xin; Ni, Zhonghua; Chen, Yunfei; Li, Tie

2018-02-01

Solid-state nanopore has captured the attention of many researchers due to its characteristic of nanoscale. Now, different fabrication methods have been reported, which can be summarized into two broad categories: "top-down" etching technology and "bottom-up" shrinkage technology. Ion track etching method, mask etching method chemical solution etching method, and high-energy particle etching and shrinkage method are exhibited in this report. Besides, we also discussed applications of solid-state nanopore fabrication technology in DNA sequencing, protein detection, and energy conversion.

Microtensile bond strength of eleven contemporary adhesives to enamel.

PubMed

Inoue, Satoshi; Vargas, Marcos A; Abe, Yasuhiko; Yoshida, Yasuhiro; Lambrechts, Paul; Vanherle, Guido; Sano, Hidehiko; Van Meerbeek, Bart

2003-10-01

To compare the microtensile bond strength (microTBS) to enamel of 10 contemporary adhesives, including three one-step self-etch systems, four two-step self-etch systems and three two-step total-etch systems, with that of a conventional three-step total-etch adhesive. Resin composite (Z100, 3M) was bonded to flat, #600-grit wet-sanded enamel surfaces of 18 extracted human third molars using the adhesives strictly according to the respective manufacturer's instructions. After storage overnight in 37 degrees C water, the bonded specimens were sectioned into 2-4 thin slabs of approximately 1 mm thickness and 2.5 mm width. They were then trimmed into an hourglass shape with an interface area of approximately 1 mm2, and subsequently subjected to microTBS-testing with a cross-head speed of 1 mm/minute. The microTBS to enamel varied from 3.2 MPa for the experimental one-step self-etch adhesive PQ/Universal (self-etch) to 43.9 MPa for the two-step total-etch adhesive Scotchbond 1. When compared with the conventional three-step total-etch adhesive OptiBond FL, the bond strengths of most adhesives with simplified application procedures were not significantly different, except for two one-step self-etch adhesives, experimental PQ/Universal (self-etch) and One-up Bond F, that showed lower bond strengths. Specimen failures during sample preparation were recorded for the latter adhesives as well.

Effect of etching on bonding of a self-etch adhesive to dentine affected by amelogenesis imperfecta.

PubMed

Epasinghe, Don Jeevanie; Yiu, Cynthia Kar Yung

2018-02-01

Dentine affected by amelogenesis imperfecta (AI) is histologically altered due to loss of hypoplastic enamel and becomes hypermineralized. In the present study, we examined the effect of additional acid etching on microtensile bond strength of a self-etch adhesive to AI-affected dentine. Flat coronal dentine obtained from extracted AI-affected and non-carious permanent molars were allocated to two groups: (a) Clearfil SE Bond (control); and (b) Clearfil SE Bond and additional etching with 34% phosphoric acid for 15 seconds. The bonded teeth were sectioned into .8-mm 2 beams for microtensile bond strength testing, and stressed to failure under tension. The bond strength data were analyzed using two-way analysis of variance (dentine type and etching step) and Student-Newman-Keuls multiple comparison test (P<.05). Representative fractured beams from each group were examined under scanning electron microscopy. Both factors, dentine substrate (P<.001) and etching step (P<.05), and their interactions (P<.001), were statistically significant. Additional etching had an adverse effect on the bond strength of Clearfil SE Bond to normal dentine (P<.005), and no significant improvement was found for AI-affected dentine (P=.479). Additional acid etching does not improve the bond strength of a self-etch adhesive to AI-affected dentine. © 2017 John Wiley & Sons Australia, Ltd.

Etching method for photoresists or polymers

NASA Technical Reports Server (NTRS)

Lerner, Narcinda R. (Inventor); Wydeven, Theodore J., Jr. (Inventor)

1991-01-01

A method for etching or removing polymers, photoresists, and organic contaminants from a substrate is disclosed. The method includes creating a more reactive gas species by producing a plasma discharge in a reactive gas such as oxygen and contacting the resulting gas species with a sacrificial solid organic material such as polyethylene or polyvinyl fluoride, reproducing a highly reactive gas species, which in turn etches the starting polymer, organic contaminant, or photoresist. The sample to be etched is located away from the plasma glow discharge region so as to avoid damaging the substrate by exposure to high energy particles and electric fields encountered in that region. Greatly increased etching rates are obtained. This method is highly effective for etching polymers such as polyimides and photoresists that are otherwise difficult or slow to etch downstream from an electric discharge in a reactive gas.

Direct mapping and characterization of dry etch damage-induced PN junction for long-wavelength HgCdTe infrared detector arrays.

PubMed

Li, Yantao; Hu, Weida; Ye, Zhenhua; Chen, Yiyu; Chen, Xiaoshuang; Lu, Wei

2017-04-01

Mercury cadmium telluride is the standard material to fabricate high-performance infrared focal plane array (FPA) detectors. However, etch-induced damage is a serious obstacle for realizing highly uniform and damage-free FPA detectors. In this Letter, the high signal-to-noise ratio and high spatial resolution scanning photocurrent microscopy (SPCM) is used to characterize the dry etch-induced inversion layer of vacancy-doped p-type Hg_1-xCd_xTe (x=0.22) material under different etching temperatures. It is found that the peak-to-peak magnitude of the SPCM profile decreases with a decrease in etching temperature, showing direct proof of controlling dry etch-induced type conversion. Our work paves the way toward seeking optimal etching processes in large-scale infrared FPAs.

Cl 2-based dry etching of the AlGaInN system in inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Cho, Hyun; Vartuli, C. B.; Abernathy, C. R.; Donovan, S. M.; Pearton, S. J.; Shul, R. J.; Han, J.

1998-12-01

Cl 2-Based inductively coupled plasmas with low additional d.c. self-biases (-100 V) produce convenient etch rates (500-1500 Å·min -1) for GaN, AlN, InN, InAlN and InGaN. A systematic study of the effects of additive gas (Ar, N 2, H 2), discharge composition and ICP source power and chuck power on etch rate and surface morphology has been performed. The general trends are to go through a maximum in etch rate with percent Cl 2 in the discharge for all three mixtures and to have an increase (decrease) in etch rate with source power (pressure). Since the etching is strongly ion-assisted, anisotropic pattern transfer is readily achieved. Maximum etch selectivities of approximately 6 for InN over the other nitrides were obtained.

Thermal etching rate of GaN during MOCVD growth interruption in hydrogen and ammonia ambient determined by AlGaN/GaN superlattice structures

NASA Astrophysics Data System (ADS)

Zhang, Feng; Ikeda, Masao; Zhang, Shuming; Liu, Jianping; Tian, Aiqin; Wen, Pengyan; Cheng, Yang; Yang, Hui

2017-10-01

Thermal etching effect of GaN during growth interruption in the metalorganic chemical vapor deposition reactor was investigated in this paper. The thermal etching rate was determined by growing a series of AlGaN/GaN superlattice structures with fixed GaN growth temperature at 735 °C and various AlGaN growth temperature changing from 900 °C to 1007 °C. It was observed that the GaN layer was etched off during the growth interruption when the growth temperature ramped up to AlGaN growth temperature. The etching thickness was determined by high resolution X-ray diffractometer and the etching rate was deduced accordingly. An activation energy of 2.53 eV was obtained for the thermal etching process.

Laser-driven fusion etching process

DOEpatents

Ashby, C.I.H.; Brannon, P.J.; Gerardo, J.B.

1987-08-25

The surfaces of solids are etched by a radiation-driven chemical reaction. The process involves exposing a substrate coated with a layer of a reactant material on its surface to radiation, e.g., a laser, to induce localized melting of the substrate which results in the occurrence of a fusion reaction between the substrate and coating material. The resultant reaction product and excess reactant salt are then removed from the surface of the substrate with a solvent which is relatively inert towards the substrate. The laser-driven chemical etching process is especially suitable for etching ionic substrates, e.g., LiNbO/sub 3/, such as used in electro-optical/acousto-optic devices. It is also suitable for applications wherein the etching process is required to produce an etched ionic substrate having a smooth surface morphology or when a very rapid etching rate is desired.

Inductively coupled BCl 3/Cl 2 /Ar plasma etching of Al-rich AlGaN

DOE PAGES

Douglas, Erica A.; Sanchez, Carlos A.; Kaplar, Robert J.; ...

2016-12-01

Varying atomic ratios in compound semiconductors is well known to have large effects on the etching properties of the material. The use of thin device barrier layers, down to 25 nm, adds to the fabrication complexity by requiring precise control over etch rates and surface morphology. The effects of bias power and gas ratio of BCl 3 to Cl 2 for inductively coupled plasma etching of high Al content AlGaN were contrasted with AlN in this study for etch rate, selectivity, and surface morphology. Etch rates were greatly affected by both bias power and gas chemistry. Here we detail themore » effects of small variations in Al composition for AlGaN and show substantial changes in etch rate with regards to bias power as compared to AlN.« less

Cryogenic Etching of High Aspect Ratio 400 nm Pitch Silicon Gratings.

PubMed

Miao, Houxun; Chen, Lei; Mirzaeimoghri, Mona; Kasica, Richard; Wen, Han

2016-10-01

The cryogenic process and Bosch process are two widely used processes for reactive ion etching of high aspect ratio silicon structures. This paper focuses on the cryogenic deep etching of 400 nm pitch silicon gratings with various etching mask materials including polymer, Cr, SiO 2 and Cr-on-polymer. The undercut is found to be the key factor limiting the achievable aspect ratio for the direct hard masks of Cr and SiO 2 , while the etch selectivity responds to the limitation of the polymer mask. The Cr-on-polymer mask provides the same high selectivity as Cr and reduces the excessive undercut introduced by direct hard masks. By optimizing the etching parameters, we etched a 400 nm pitch grating to ≈ 10.6 μ m depth, corresponding to an aspect ratio of ≈ 53.

Etch bias inversion during EUV mask ARC etch

NASA Astrophysics Data System (ADS)

Lajn, Alexander; Rolff, Haiko; Wistrom, Richard

2017-07-01

The introduction of EUV lithography to high volume manufacturing is now within reach for 7nm technology node and beyond (1), at least for some steps. The scheduling is in transition from long to mid-term. Thus, all contributors need to focus their efforts on the production requirements. For the photo mask industry, these requirements include the control of defectivity, CD performance and lifetime of their masks. The mask CD performance including CD uniformity, CD targeting, and CD linearity/ resolution, is predominantly determined by the photo resist performance and by the litho and etch processes. State-of-the-art chemically amplified resists exhibit an asymmetric resolution for directly and indirectly written features, which usually results in a similarly asymmetric resolution performance on the mask. This resolution gap may reach as high as multiple tens of nanometers on the mask level in dependence of the chosen processes. Depending on the printing requirements of the wafer process, a reduction or even an increase of this gap may be required. A potential way of tuning via the etch process, is to control the lateral CD contribution during etch. Aside from process tuning knobs like pressure, RF powers and gases, which usually also affect CD linearity and CD uniformity, the simplest knob is the etch time itself. An increased over etch time results in an increased CD contribution in the normal case. , We found that the etch CD contribution of ARC layer etch on EUV photo masks is reduced by longer over etch times. Moreover, this effect can be demonstrated to be present for different etch chambers and photo resists.

Modeling of block copolymer dry etching for directed self-assembly lithography

NASA Astrophysics Data System (ADS)

Belete, Zelalem; Baer, Eberhard; Erdmann, Andreas

2018-03-01

Directed self-assembly (DSA) of block copolymers (BCP) is a promising alternative technology to overcome the limits of patterning for the semiconductor industry. DSA exploits the self-assembling property of BCPs for nano-scale manufacturing and to repair defects in patterns created during photolithography. After self-assembly of BCPs, to transfer the created pattern to the underlying substrate, selective etching of PMMA (poly (methyl methacrylate)) to PS (polystyrene) is required. However, the etch process to transfer the self-assemble "fingerprint" DSA patterns to the underlying layer is still a challenge. Using combined experimental and modelling studies increases understanding of plasma interaction with BCP materials during the etch process and supports the development of selective process that form well-defined patterns. In this paper, a simple model based on a generic surface model has been developed and an investigation to understand the etch behavior of PS-b-PMMA for Ar, and Ar/O2 plasma chemistries has been conducted. The implemented model is calibrated for etch rates and etch profiles with literature data to extract parameters and conduct simulations. In order to understand the effect of the plasma on the block copolymers, first the etch model was calibrated for polystyrene (PS) and poly (methyl methacrylate) (PMMA) homopolymers. After calibration of the model with the homopolymers etch rate, a full Monte-Carlo simulation was conducted and simulation results are compared with the critical-dimension (CD) and selectivity of etch profile measurement. In addition, etch simulations for lamellae pattern have been demonstrated, using the implemented model.

Overlapping double etch technique for evaluation of metallic alloys to stress corrosion cracking

DOEpatents

Steeves, Arthur F.; Stewart, James C.

1981-01-01

A double overlapping etch zone technique for evaluation of the resistance of metallic alloys to stress corrosion cracking. The technique involves evaluating the metallic alloy along the line of demarcation between an overlapping double etch zone and single etch zone formed on the metallic alloy surface.

Sequential infiltration synthesis for enhancing multiple-patterning lithography

DOE Office of Scientific and Technical Information (OSTI.GOV)

Darling, Seth B.; Elam, Jeffrey W.; Tseng, Yu-Chih

Simplified methods of multiple-patterning photolithography using sequential infiltration synthesis to modify the photoresist such that it withstands plasma etching better than unmodified resist and replaces one or more hard masks and/or a freezing step in MPL processes including litho-etch-litho-etch photolithography or litho-freeze-litho-etch photolithography.

Studies and testing of antireflective (AR) coatings for soda-lime glass

NASA Technical Reports Server (NTRS)

Pastirik, E. M.; Sparks, T. G.; Coleman, M. G.

1978-01-01

Processes for producing antireflection films on glass are concentrated in three areas: acid etching of glass, plasma etching of glass, and acid development of sodium silicate films on glass. The best transmission was achieved through the acid etching technique, while the most durable films were produced from development of sodium silicate films. Control of the acid etching technique is presently inadequate for production implementation. While films having excellent antireflective properties were fabricated by plasma etching techniques, all were water soluble.

Lateral electrochemical etching of III-nitride materials for microfabrication

DOE Office of Scientific and Technical Information (OSTI.GOV)

Han, Jung

Conductivity-selective lateral etching of III-nitride materials is described. Methods and structures for making vertical cavity surface emitting lasers with distributed Bragg reflectors via electrochemical etching are described. Layer-selective, lateral electrochemical etching of multi-layer stacks is employed to form semiconductor/air DBR structures adjacent active multiple quantum well regions of the lasers. The electrochemical etching techniques are suitable for high-volume production of lasers and other III-nitride devices, such as lasers, HEMT transistors, power transistors, MEMs structures, and LEDs.

Research on InGaAs FETs.

DTIC Science & Technology

1981-09-01

is to reduce resistance and to allow wirebonding. Finally, the excess p-region is etched away (Figs. 2f and 2g) using 25 citric acid (50% by weight...found to be parallel to the grains. Gates etched in the citric acid /hydrogen perioxide etch that are oriented parallel to the grains have the cross...occur at IV reverse bias (i.e., negative gate voltage and IDSS is typically z 45 mA. After 60 sec of etch- ing in the citric acid etch (i.e., 25 citric

Electrodeposited silk coatings for bone implants.

PubMed

Elia, Roberto; Michelson, Courtney D; Perera, Austin L; Brunner, Teresa F; Harsono, Masly; Leisk, Gray G; Kugel, Gerard; Kaplan, David L

2015-11-01

The aim of this study was to characterize the mechanical properties and drug elution features of silk protein-based electrodeposited dental implant coatings. Silk processing conditions were modified to obtain coatings with a range of mechanical properties on titanium studs. These coatings were assessed for adhesive strength and dissolution, with properties tuned using water vapor annealing or glycerol incorporation to modulate crystalline content. Coating reproducibility was demonstrated over a range of silk concentrations from 1% to 10%. Surface roughness of titanium substrates was altered using industry relevant acid etching and grit blasting, and the effect of surface topography on silk coating adhesion was assessed. Florescent compounds were incorporated into the silk coatings, which were modulated for crystalline content, to achieve four days of sustained release of the compounds. This silk electrogelation technique offers a safe and relatively simple approach to generate mechanically robust, biocompatible, and degradable implant coatings that can also be functionalized with bioactive compounds to modulate the local regenerative tissue environment. © 2014 Wiley Periodicals, Inc.

Electrodeposited silk coatings for bone implants

PubMed Central

Elia, Roberto; Michelson, Courtney D.; Perera, Austin L.; Brunner, Teresa F.; Harsono, Masly; Leisk, Gray G.; Kugel, Gerard; Kaplan, David L.

2014-01-01

The aim of this study was to characterize the mechanical properties and drug elution features of silk protein-based electrodeposited dental implant coatings. Silk processing conditions were modified to obtain coatings with a range of mechanical properties on titanium studs. These coatings were assessed for adhesive strength and dissolution, with properties tuned using water vapor annealing or glycerol incorporation to modulate crystalline content. Coating reproducibility was demonstrated over a range of silk concentrations from 1 to 10%. Surface roughness of titanium substrates was altered using industry relevant acid etching and grit blasting, and the effect of surface topography on silk coating adhesion was assessed. Florescent compounds were incorporated into the silk coatings, which were modulated for crystalline content, to achieve four days of sustained release of the compounds. This silk electrogelation technique offers a safe and relatively simple approach to generate mechanically robust, biocompatible and degradable implant coatings that can also be functionalized with bioactive compounds to modulate the local regenerative tissue environment. PMID:25545462

4-META opaque resin--a new resin strongly adhesive to nickel-chromium alloy.

PubMed

Tanaka, T; Nagata, K; Takeyama, M; Atsuta, M; Nakabayashi, N; Masuhara, E

1981-09-01

1) A new adhesive opaque resin containing a reactive monomer, 4-methacryloxy-ethyl trimellitate anhydride (4-META), was prepared, and its application to thermosetting acrylic resin veneer crowns was studied. 2) The 4-META opaque resin was applied to a variety of nickel-chromium dental alloy specimens which had undergone different treatment, and endurance tests were conducted to evaluate the durability of adhesion. 3) Stable adhesion against water penetration was achieved with metal surfaces first etched with HCl and then oxidized with HNO3. A bond strength of 250 kg/cm2 was maintained even after immersion in water at 37 degrees C for 30 wk or at 80 degrees C for ten wk. Furthermore, this value did not decrease even after the specimens were subjected to 500 thermal cycles. 4) The 4-META opaque resin studied can eliminate the necessity for retention devices on metal castings. 5) The smooth 4-META opaque resin should have no adverse effects on gingivae.

Photonic jet μ-etching: from static to dynamic process

NASA Astrophysics Data System (ADS)

Abdurrochman, A.; Lecler, S.; Zelgowski, J.; Mermet, F.; Fontaine, J.; Tumbelaka, B. Y.

2017-05-01

Photonic jet etching is a direct-laser etching method applying photonic jet phenomenon to concentrate the laser beam onto the proceeded material. We call photonic jet the phenomenon of the localized sub-wavelength propagative beam generated at the shadow-side surfaces of micro-scale dielectric cylinders or spheres, when they are illuminated by an electromagnetic plane-wave or laser beam. This concentration has made possible the laser to yield sub-μ etching marks, despite the laser was a near-infrared with nano-second pulses sources. We will present these achievements from the beginning when some spherical glasses were used for static etching to dynamic etching using an optical fiber with a semi-elliptical tip.

A comparison of etched-geometry and overgrown silicon permeable base transistors by two-dimensional numerical simulations

NASA Astrophysics Data System (ADS)

Vojak, B. A.; Alley, G. D.

1983-08-01

Two-dimensional numerical simulations are used to compare etched geometry and overgrown Si permeable base transistors (PTBs), considering both the etched collector and etched emitter biasing conditions made possible by the asymmetry of the etched structure. In PTB devices, the two-dimensional nature of the depletion region near the Schottky contact base grating results in a smaller electron barrier and, therefore, a larger collector current in the etched than in the overgrown structure. The parasitic feedback effects which result at high base-to-emitter bias levels lead to a deviation from the square-law behavior found in the collector characteristics of the overgrown PBT. These structures also have lower device capacitances and smaller transconductances at high base-to-emitter voltages. As a result, overgrown and etched structures have comparable predicted maximum values of the small signal unity short-circuit current gain frequency and maximum oscillation frequency.

Low damage dry etch for III-nitride light emitters

NASA Astrophysics Data System (ADS)

Nedy, Joseph G.; Young, Nathan G.; Kelchner, Kathryn M.; Hu, Yanling; Farrell, Robert M.; Nakamura, Shuji; DenBaars, Steven P.; Weisbuch, Claude; Speck, James S.

2015-08-01

We have developed a dry etch process for the fabrication of lithographically defined features close to light emitting layers in the III-nitride material system. The dry etch was tested for its effect on the internal quantum efficiency of c-plane InGaN quantum wells using the photoluminescence of a test structure with two active regions. No change was observed in the internal quantum efficiency of the test active region when the etched surface was greater than 71 nm away. To demonstrate the application of the developed dry etch process, surface-etched air gaps were fabricated 275 nm away from the active region of an m-plane InGaN/GaN laser diode and served as the waveguide upper cladding. Electrically injected lasing was observed without the need for regrowth or recovery anneals. This dry etch opens up a new design tool that can be utilized in the next generation of GaN light emitters.

Micro-pyramidal structure fabrication on polydimethylsiloxane (PDMS) by Si (100) KOH wet etching

NASA Astrophysics Data System (ADS)

Hwang, Shinae; Lim, Kyungsuk; Shin, Hyeseon; Lee, Seongjae; Jang, Moongyu

2017-10-01

A high degree of accuracy in bulk micromachining is essential to fabricate micro-electro-mechanical systems (MEMS) devices. A series of etching experiments is carried out using 40 wt% KOH solutions at the constant temperature of 70 °C. Before wet etching, SF6 and O2 are used as the dry etching gas to etch the masking layers of a 100 nm thick Si3N4 and SiO2, respectively. The experimental results indicate that (100) silicon wafer form the pyramidal structures with (111) single crystal planes. All the etch profiles are analyzed using Scanning Electron Microscope (SEM) and the wet etch rates depend on the opening sizes. The manufactured pyramidal structures are used as the pattern of silicon mold. After a short hardening of coated polydimethylsiloxane (PDMS) layer, micro pyramidal structures are easily transferred to PDMS layer.

Pulsed Laser-Assisted Focused Electron-Beam-Induced Etching of Titanium with XeF 2 : Enhanced Reaction Rate and Precursor Transport

DOE PAGES

Noh, J. H.; Fowlkes, J. D.; Timilsina, R.; ...

2015-01-28

We introduce a laser-assisted focused electron-beam-induced etching (LA-FEBIE) process which is a versatile, direct write nanofabrication method that allows nanoscale patterning and editing; we do this in order to enhance the etch rate of electron-beam-induced etching. The results demonstrate that the titanium electron stimulated etch rate via the XeF2 precursor can be enhanced up to a factor of 6 times with an intermittent pulsed laser assist. Moreover, the evolution of the etching process is correlated to in situ stage current measurements and scanning electron micrographs as a function of time. Finally, the increased etch rate is attributed to photothermally enhancedmore » Ti–F reaction and TiF4 desorption and in some regimes enhanced XeF2 surface diffusion to the reaction zone.« less

Formation and metrology of dual scale nano-morphology on SF(6) plasma etched silicon surfaces.

PubMed

Boulousis, G; Constantoudis, V; Kokkoris, G; Gogolides, E

2008-06-25

Surface roughness and nano-morphology in SF(6) plasma etched silicon substrates are investigated in a helicon type plasma reactor as a function of etching time and process parameters. The plasma etched surfaces are analyzed by atomic force microscopy. It is found that dual scale nano-roughness is formatted on the silicon surface comprising an underlying nano-roughness and superimposed nano-mounds. Detailed metrological quantification is proposed for the characterization of dual scale surface morphology. As etching proceeds, the mounds become higher, fewer and wider, and the underlying nano-roughness also increases. Increase in wafer temperature leads to smoother surfaces with lower, fewer and wider nano-mounds. A mechanism based on the deposition of etch inhibiting particles during the etching process is proposed for the explanation of the experimental behavior. In addition, appropriately designed experiments are conducted, and they confirm the presence of this mechanism.

Mesoporous carbon-supported Pd nanoparticles with high specific surface area for cyclohexene hydrogenation: Outstanding catalytic activity of NaOH-treated catalysts

NASA Astrophysics Data System (ADS)

Puskás, R.; Varga, T.; Grósz, A.; Sápi, A.; Oszkó, A.; Kukovecz, Á.; Kónya, Z.

2016-06-01

Extremely high specific surface area mesoporous carbon-supported Pd nanoparticle catalysts were prepared with both impregnation and polyol-based sol methods. The silica template used for the synthesis of mesoporous carbon was removed by both NaOH and HF etching. Pd/mesoporous carbon catalysts synthesized with the impregnation method has as high specific surface area as 2250 m2/g. In case of NaOH-etched impregnated samples, the turnover frequency of cyclohexene hydrogenation to cyclohexane at 313 K was obtained 14 molecules • site- 1 • s- 1. The specific surface area of HF-etched samples was higher compared to NaOH-etched samples. However, catalytic activity was 3-6 times higher on NaOH-etched samples compared to HF-etched samples, which can be attributed to the presence of sodium and surface hydroxylgroups of the catalysts etched with NaOH solution.

Cryogenic Etching of Silicon: An Alternative Method For Fabrication of Vertical Microcantilever Master Molds

PubMed Central

Addae-Mensah, Kweku A.; Retterer, Scott; Opalenik, Susan R.; Thomas, Darrell; Lavrik, Nickolay V.; Wikswo, John P.

2013-01-01

This paper examines the use of deep reactive ion etching (DRIE) of silicon with fluorine high-density plasmas at cryogenic temperatures to produce silicon master molds for vertical microcantilever arrays used for controlling substrate stiffness for culturing living cells. The resultant profiles achieved depend on the rate of deposition and etching of a SiOxFy polymer, which serves as a passivation layer on the sidewalls of the etched structures in relation to areas that have not been passivated with the polymer. We look at how optimal tuning of two parameters, the O2 flow rate and the capacitively coupled plasma (CCP) power, determine the etch profile. All other pertinent parameters are kept constant. We examine the etch profiles produced using e-beam resist as the main etch mask, with holes having diameters of 750 nm, 1 µm, and 2 µm. PMID:24223478

Ion track etching revisited: I. Correlations between track parameters in aged polymers

NASA Astrophysics Data System (ADS)

Fink, D.; Muñoz H., G.; García A., H.; Vacik, J.; Hnatowicz, V.; Kiv, A.; Alfonta, L.

2018-04-01

Some yet poorly understood problems of etching of pristine and swift heavy ion track-irradiated aged polymers were treated, by applying conductometry across the irradiated foils during etching. The onset times of etchant penetration across pristine foils, and the onset times of the different etched track regimes in irradiated foils were determined for polymers of various proveniences, fluences and ages, as well as their corresponding etching speeds. From the results, correlations of the parameters with each other were deduced. The normalization of these parameters enables one to compare irradiated polymer foils of different origin and treatment with one another. In a number of cases, also polymeric gel formation and swelling occur which influence the track etching behaviour. The polymer degradation during aging influences the track etching parameters, which differ from each other on both sides of the foils. With increasing sample age, these differences increase.

Laser-driven fusion etching process

DOEpatents

Ashby, Carol I. H.; Brannon, Paul J.; Gerardo, James B.

1989-01-01

The surfaces of solid ionic substrates are etched by a radiation-driven chemical reaction. The process involves exposing an ionic substrate coated with a layer of a reactant material on its surface to radiation, e.g. a laser, to induce localized melting of the substrate which results in the occurrance of a fusion reaction between the substrate and coating material. The resultant reaction product and excess reactant salt are then removed from the surface of the substrate with a solvent which is relatively inert towards the substrate. The laser-driven chemical etching process is especially suitable for etching ionic salt substrates, e.g., a solid inorganic salt such as LiNbO.sub.3, such as used in electro-optical/acousto-optic devices. It is also suitable for applications wherein the etching process is required to produce an etched ionic substrate having a smooth surface morphology or when a very rapid etching rate is desired.

SEMICONDUCTOR TECHNOLOGY Texturization of mono-crystalline silicon solar cells in TMAH without the addition of surfactant

NASA Astrophysics Data System (ADS)

Weiying, Ou; Yao, Zhang; Hailing, Li; Lei, Zhao; Chunlan, Zhou; Hongwei, Diao; Min, Liu; Weiming, Lu; Jun, Zhang; Wenjing, Wang

2010-10-01

Etching was performed on (100) silicon wafers using silicon-dissolved tetramethylammonium hydroxide (TMAH) solutions without the addition of surfactant. Experiments were carried out in different TMAH concentrations at different temperatures for different etching times. The surface phenomena, etching rates, surface morphology and surface reflectance were analyzed. Experimental results show that the resulting surface covered with uniform pyramids can be realized with a small change in etching rates during the etching process. The etching mechanism is explained based on the experimental results and the theoretical considerations. It is suggested that all the components in the TMAH solutions play important roles in the etching process. Moreover, TMA+ ions may increase the wettability of the textured surface. A good textured surface can be obtained in conditions where the absorption of OH-/H2O is in equilibrium with that of TMA+/SiO2 (OH)22-.

Method to control artifacts of microstructural fabrication

DOEpatents

Shul, Randy J.; Willison, Christi G.; Schubert, W. Kent; Manginell, Ronald P.; Mitchell, Mary-Anne; Galambos, Paul C.

2006-09-12

New methods for fabrication of silicon microstructures have been developed. In these methods, an etching delay layer is deposited and patterned so as to provide differential control on the depth of features being etched into a substrate material. Compensation for etching-related structural artifacts can be accomplished by proper use of such an etching delay layer.

Dopant Selective Reactive Ion Etching of Silicon Carbide

NASA Technical Reports Server (NTRS)

Okojie, Robert (Inventor)

2016-01-01

A method for selectively etching a substrate is provided. In one embodiment, an epilayer is grown on top of the substrate. A resistive element may be defined and etched into the epilayer. On the other side of the substrate, the substrate is selectively etched up to the resistive element, leaving a suspended resistive element.

Overlapping double etch technique for evaluation of metallic alloys to stress corrosion cracking

DOEpatents

Not Available

1980-05-28

A double overlapping etch zone technique for evaluation of the resistance of metallic alloys to stress corrosion cracking is described. The technique involves evaluating the metallic alloy along the line of demarcation between an overlapping double etch zone and single etch zone formed on the metallic alloy surface.

Formation of nanostructured silicon surfaces by stain etching

PubMed Central

2014-01-01

In this work, we report the fabrication of ordered silicon structures by chemical etching of silicon in vanadium oxide (V2O5)/hydrofluoric acid (HF) solution. The effects of the different etching parameters including the solution concentration, temperature, and the presence of metal catalyst film deposition (Pd) on the morphologies and reflective properties of the etched Si surfaces were studied. Scanning electron microscopy (SEM) was carried out to explore the morphologies of the etched surfaces with and without the presence of catalyst. In this case, the attack on the surfaces with a palladium deposit begins by creating uniform circular pores on silicon in which we distinguish the formation of pyramidal structures of silicon. Fourier transform infrared spectroscopy (FTIR) demonstrates that the surfaces are H-terminated. A UV-Vis-NIR spectrophotometer was used to study the reflectance of the structures obtained. A reflectance of 2.21% from the etched Si surfaces in the wavelength range of 400 to 1,000 nm was obtained after 120 min of etching while it is of 4.33% from the Pd/Si surfaces etched for 15 min. PMID:25435830

Deep reactive ion etching of 4H-SiC via cyclic SF6/O2 segments

NASA Astrophysics Data System (ADS)

Luna, Lunet E.; Tadjer, Marko J.; Anderson, Travis J.; Imhoff, Eugene A.; Hobart, Karl D.; Kub, Fritz J.

2017-10-01

Cycles of inductively coupled SF6/O2 plasma with low (9%) and high (90%) oxygen content etch segments are used to produce up to 46.6 µm-deep trenches with 5.5 µm-wide openings in single-crystalline 4H-SiC substrates. The low oxygen content segment serves to etch deep in SiC whereas the high oxygen content segment serves to etch SiC at a slower rate, targeting carbon-rich residues on the surface as the combination of carbon-rich and fluorinated residues impact sidewall profile. The cycles work in concert to etch past 30 µm at an etch rate of ~0.26 µm min-1 near room temperature, while maintaining close to vertical sidewalls, high aspect ratio, and high mask selectivity. In addition, power ramps during the low oxygen content segment is used to produce a 1:1 ratio of mask opening to trench bottom width. The effect of process parameters such as cycle time and backside substrate cooling on etch depth and micromasking of the electroplated nickel etch mask are investigated.

Microtrenching-free two-step reactive ion etching of 4H-SiC using NF{sub 3}/HBr/O{sub 2} and Cl{sub 2}/O{sub 2}

DOE Office of Scientific and Technical Information (OSTI.GOV)

Tseng, Yuan-Hung, E-mail: yhtseng.ee99g@nctu.edu.tw; Tsui, Bing-Yue

2014-05-15

In this paper, the authors performed a reactive ion etch of a 4H-SiC substrate with a gas mixture of NF{sub 3}, HBr, and O{sub 2}, resulting in a microtrenching-free etch. The etch rate was 107.8 nm/min, and the selectivity over the oxide hard mask was ∼3.85. Cross-sectional scanning electron microscopy showed no microtrenching compared with etches using plasmas of NF{sub 3}, NF{sub 3}/HBr, and NF{sub 3}/O{sub 2}. Analyzing a variety of HBr/O{sub 2} mixing ratios, the authors discuss the additive effect of each gas and their respective potential mechanisms for alleviating microtrenching. To increase the radius of gyration of the bottommore » corners, they introduced a second etch step with Cl{sub 2}/O{sub 2} plasma. Fabricating simple metal-oxide-semiconductor capacitors on the two-step etched surface, the authors found that the electrical characteristics of the etched sample were nearly the same as the nonetched sample.« less

Adhesive capability of total-etch, self-etch, and self-adhesive systems for fiber post cementation

NASA Astrophysics Data System (ADS)

Theodor, Y.; Koesmaningati, H.; Gita, F.

2017-08-01

The aim of this study was to analyze whether self-etch and self-adhesive systems are comparable to the total-etch system for fiber post cementation. This experimental laboratory study, which was approved by an ethics committee, was performed using 27 mandibular premolar teeth randomly divided into three groups. Fiber post cementation was done using three different adhesive systems. Specimens were prepared with a thickness of 5 mm, which was measured from the cervical to medial areas of the root, and stored for 24 h in saline solution at room temperature. A push-out test was performed using a universal testing machine (Shimidzu AG-5000E) with a crosshead speed of 0.5 mm/min. The results of one way ANOVA bivariate testing showed that the total-etch and self-etch systems have comparable adhesion capability (p<0.05) and that the self-adhesive system has the lowest adhesion capability (p>0.05). With easier application, the self-etch system has a comparable adhesion capability to the total-etch system.

Porous silicon formation during Au-catalyzed etching

DOE Office of Scientific and Technical Information (OSTI.GOV)

Algasinger, Michael; Bernt, Maximilian; Koynov, Svetoslav

2014-04-28

The formation of “black” nano-textured Si during the Au-catalyzed wet-chemical etch process was investigated with respect to photovoltaic applications. Cross-sectional scanning electron microscopy (SEM) images recorded at different stages of the etch process exhibit an evolution of a two-layer structure, consisting of cone-like Si hillocks covered with a nano-porous Si (np-Si) layer. Optical measurements confirm the presence of a np-Si phase which appears after the first ∼10 s of the etch process and continuously increases with the etch time. Furthermore, the etch process was investigated on Si substrates with different doping levels (∼0.01–100 Ω cm). SEM images show a transition frommore » the two-layer morphology to a structure consisting entirely of np-Si for higher doping levels (<0.1 Ω cm). The experimental results are discussed on the basis of the model of a local electrochemical etch process. A better understanding of the metal-catalyzed etch process facilitates the fabrication of “black” Si on various Si substrates, which is of significant interest for photovoltaic applications.« less

Anisotropic Etching of Hexagonal Boron Nitride and Graphene: Question of Edge Terminations

DOE Office of Scientific and Technical Information (OSTI.GOV)

Stehle, Yijing Y.; Sang, Xiahan; Unocic, Raymond R.

Here, chemical vapor deposition (CVD) has been established as the most effective way to grow large area two-dimensional materials. Direct study of the etching process can reveal subtleties of this competing with the growth reaction and thus provide the necessary details of the overall growth mechanism. Here we investigate hydrogen-induced etching of hBN and graphene and compare the results with the classical kinetic Wulff construction model. Formation of the anisotropically etched holes in the center of hBN and graphene single crystals was observed along with the changes in the crystals' circumference. We show that the edges of triangular holes inmore » hBN crystals formed at regular etching conditions are parallel to B-terminated zigzags, opposite to the N-terminated zigzag edges of hBN triangular crystals. The morphology of the etched hBN holes is affected by a disbalance of the B/N ratio upon etching and can be shifted toward the anticipated from the Wulff model N-terminated zigzag by etching in a nitrogen buffer gas instead of a typical argon. For graphene, etched hexagonal holes are terminated by zigzag, while the crystal circumference is gradually changing from a pure zigzag to a slanted angle resulting in dodecagons.« less

Suppression of Lateral Diffusion and Surface Leakage Currents in nBn Photodetectors Using an Inverted Design

NASA Astrophysics Data System (ADS)

Du, X.; Savich, G. R.; Marozas, B. T.; Wicks, G. W.

2018-02-01

Surface leakage and lateral diffusion currents in InAs-based nBn photodetectors have been investigated. Devices fabricated using a shallow etch processing scheme that etches through the top contact and stops at the barrier exhibited large lateral diffusion current but undetectably low surface leakage. Such large lateral diffusion current significantly increased the dark current, especially in small devices, and causes pixel-to-pixel crosstalk in detector arrays. To eliminate the lateral diffusion current, two different approaches were examined. The conventional solution utilized a deep etch process, which etches through the top contact, barrier, and absorber. This deep etch processing scheme eliminated lateral diffusion, but introduced high surface current along the device mesa sidewalls, increasing the dark current. High device failure rate was also observed in deep-etched nBn structures. An alternative approach to limit lateral diffusion used an inverted nBn structure that has its absorber grown above the barrier. Like the shallow etch process on conventional nBn structures, the inverted nBn devices were fabricated with a processing scheme that only etches the top layer (the absorber, in this case) but avoids etching through the barrier. The results show that inverted nBn devices have the advantage of eliminating the lateral diffusion current without introducing elevated surface current.

Qualitative modeling of silica plasma etching using neural network

NASA Astrophysics Data System (ADS)

Kim, Byungwhan; Kwon, Kwang Ho

2003-01-01

An etching of silica thin film is qualitatively modeled by using a neural network. The process was characterized by a 23 full factorial experiment plus one center point, in which the experimental factors and ranges include 100-800 W radio-frequency source power, 100-400 W bias power and gas flow rate ratio CHF3/CF4. The gas flow rate ratio varied from 0.2 to 5.0. The backpropagation neural network (BPNN) was trained on nine experiments and tested on six experiments, not pertaining to the original training data. The prediction ability of the BPNN was optimized as a function of the training parameters. Prediction errors are 180 Å/min and 1.33, for the etch rate and anisotropy models, respectively. Physical etch mechanisms were estimated from the three-dimensional plots generated from the optimized models. Predicted response surfaces were consistent with experimentally measured etch data. The dc bias was correlated to the etch responses to evaluate its contribution. Both the source power (plasma density) and bias power (ion directionality) strongly affected the etch rate. The source power was the most influential factor for the etch rate. A conflicting effect between the source and bias powers was noticed with respect to the anisotropy. The dc bias played an important role in understanding or separating physical etch mechanisms.

Microtensile bond strength of silorane-based composite specific adhesive system using different bonding strategies.

PubMed

Bastos, Laura Alves; Sousa, Ana Beatriz Silva; Drubi-Filho, Brahim; Panzeri Pires-de-Souza, Fernanda de Carvalho; Garcia, Lucas da Fonseca Roberti

2015-02-01

The aim of this study was to evaluate the effect of pre-etching on the bond strength of silorane-based composite specific adhesive system to dentin. Thirty human molars were randomly divided into 5 groups according to the different bonding strategies. For teeth restored with silorane-based composite (Filtek Silorane, 3M ESPE), the specific self-etching adhesive system (Adhesive System P90, 3M ESPE) was used with and without pre-etching (Pre-etching/Silorane and Silorane groups). Teeth restored with methacrylate based-composite (Filtek Z250, 3M ESPE) were hybridized with the two-step self-etching system (Clearfil SE Bond, Kuraray), with and without pre-etching (Pre-etching/Methacrylate and Methacrylate groups), or three-step adhesive system (Adper Scotchbond Multi-Purpose, 3M ESPE) (Three-step/Methacrylate group) (n = 6). The restored teeth were sectioned into stick-shaped test specimens (1.0 × 1.0 mm), and coupled to a universal test machine (0.5 mm/min) to perform microtensile testing. Pre-etching/Methacrylate group presented the highest bond strength values, with significant difference from Silorane and Three-step/Methacrylate groups (p < 0.05). However, it was not significantly different from Preetching/Silorane and Methacrylate groups. Pre-etching increased bond strength of silorane-based composite specific adhesive system to dentin.

Anisotropic Etching of Hexagonal Boron Nitride and Graphene: Question of Edge Terminations

DOE PAGES

Stehle, Yijing Y.; Sang, Xiahan; Unocic, Raymond R.; ...

2017-11-14

Here, chemical vapor deposition (CVD) has been established as the most effective way to grow large area two-dimensional materials. Direct study of the etching process can reveal subtleties of this competing with the growth reaction and thus provide the necessary details of the overall growth mechanism. Here we investigate hydrogen-induced etching of hBN and graphene and compare the results with the classical kinetic Wulff construction model. Formation of the anisotropically etched holes in the center of hBN and graphene single crystals was observed along with the changes in the crystals' circumference. We show that the edges of triangular holes inmore » hBN crystals formed at regular etching conditions are parallel to B-terminated zigzags, opposite to the N-terminated zigzag edges of hBN triangular crystals. The morphology of the etched hBN holes is affected by a disbalance of the B/N ratio upon etching and can be shifted toward the anticipated from the Wulff model N-terminated zigzag by etching in a nitrogen buffer gas instead of a typical argon. For graphene, etched hexagonal holes are terminated by zigzag, while the crystal circumference is gradually changing from a pure zigzag to a slanted angle resulting in dodecagons.« less

Quantum cascade laser based monitoring of CF{sub 2} radical concentration as a diagnostic tool of dielectric etching plasma processes

DOE Office of Scientific and Technical Information (OSTI.GOV)

Hübner, M.; Lang, N.; Röpcke, J.

2015-01-19

Dielectric etching plasma processes for modern interlevel dielectrics become more and more complex by the introduction of new ultra low-k dielectrics. One challenge is the minimization of sidewall damage, while etching ultra low-k porous SiCOH by fluorocarbon plasmas. The optimization of this process requires a deeper understanding of the concentration of the CF{sub 2} radical, which acts as precursor in the polymerization of the etch sample surfaces. In an industrial dielectric etching plasma reactor, the CF{sub 2} radical was measured in situ using a continuous wave quantum cascade laser (cw-QCL) around 1106.2 cm{sup −1}. We measured Doppler-resolved ro-vibrational absorption lines andmore » determined absolute densities using transitions in the ν{sub 3} fundamental band of CF{sub 2} with the aid of an improved simulation of the line strengths. We found that the CF{sub 2} radical concentration during the etching plasma process directly correlates to the layer structure of the etched wafer. Hence, this correlation can serve as a diagnostic tool of dielectric etching plasma processes. Applying QCL based absorption spectroscopy opens up the way for advanced process monitoring and etching controlling in semiconductor manufacturing.« less

Method for forming suspended micromechanical structures

DOEpatents

Fleming, James G.

2000-01-01

A micromachining method is disclosed for forming a suspended micromechanical structure from {111} crystalline silicon. The micromachining method is based on the use of anisotropic dry etching to define lateral features of the structure which are etched down into a {111}-silicon substrate to a first etch depth, thereby forming sidewalls of the structure. The sidewalls are then coated with a protection layer, and the substrate is dry etched to a second etch depth to define a spacing of the structure from the substrate. A selective anisotropic wet etchant (e.g. KOH, EDP, TMAH, NaOH or CsOH) is used to laterally undercut the structure between the first and second etch depths, thereby forming a substantially planar lower surface of the structure along a {111} crystal plane that is parallel to an upper surface of the structure. The lateral extent of undercutting by the wet etchant is controlled and effectively terminated by either timing the etching, by the location of angled {111}-silicon planes or by the locations of preformed etch-stops. This present method allows the formation of suspended micromechanical structures having large vertical dimensions and large masses while allowing for detailed lateral features which can be provided by dry etch definition. Additionally, the method of the present invention is compatible with the formation of electronic circuitry on the substrate.

Minimizing Isolate Catalyst Motion in Metal-Assisted Chemical Etching for Deep Trenching of Silicon Nanohole Array.

PubMed

Kong, Lingyu; Zhao, Yunshan; Dasgupta, Binayak; Ren, Yi; Hippalgaonkar, Kedar; Li, Xiuling; Chim, Wai Kin; Chiam, Sing Yang

2017-06-21

The instability of isolate catalysts during metal-assisted chemical etching is a major hindrance to achieve high aspect ratio structures in the vertical and directional etching of silicon (Si). In this work, we discussed and showed how isolate catalyst motion can be influenced and controlled by the semiconductor doping type and the oxidant concentration ratio. We propose that the triggering event in deviating isolate catalyst motion is brought about by unequal etch rates across the isolate catalyst. This triggering event is indirectly affected by the oxidant concentration ratio through the etching rates. While the triggering events are stochastic, the doping concentration of silicon offers a good control in minimizing isolate catalyst motion. The doping concentration affects the porosity at the etching front, and this directly affects the van der Waals (vdWs) forces between the metal catalyst and Si during etching. A reduction in the vdWs forces resulted in a lower bending torque that can prevent the straying of the isolate catalyst from its directional etching, in the event of unequal etch rates. The key understandings in isolate catalyst motion derived from this work allowed us to demonstrate the fabrication of large area and uniformly ordered sub-500 nm nanoholes array with an unprecedented high aspect ratio of ∼12.

Recovery of GaN surface after reactive ion etching

NASA Astrophysics Data System (ADS)

Fan, Qian; Chevtchenko, S.; Ni, Xianfeng; Cho, Sang-Jun; Morko, Hadis

2006-02-01

Surface properties of GaN subjected to reactive ion etching and the impact on device performance have been investigated by surface potential, optical and electrical measurements. Different etching conditions were studied and essentially high power levels and low chamber pressures resulted in higher etch rates accompanying with the roughening of the surface morphology. Surface potential for the as-grown c-plane GaN was found to be in the range of 0.5~0.7 V using Scanning Kevin Probe Microscopy. However, after reactive ion etching at a power level of 300 W, it decreased to 0.1~0.2 V. A nearly linear reduction was observed on c-plane GaN with increasing power. The nonpolar a-plane GaN samples also showed large surface band bending before and after etching. Additionally, the intensity of the near band-edge photoluminescence decreased and the free carrier density increased after etching. These results suggest that the changes in the surface potential may originate from the formation of possible nitrogen vacancies and other surface oriented defects and adsorbates. To recover the etched surface, N II plasma, rapid thermal annealing, and etching in wet KOH were performed. For each of these methods, the surface potential was found to increase by 0.1~0.3 V, also the reverse leakage current in Schottky diodes fabricated on treated samples was reduced considerably compared with as-etched samples, which implies a partial-to-complete recovery from the plasma-induced damage.

Atomic precision etch using a low-electron temperature plasma

NASA Astrophysics Data System (ADS)

Dorf, L.; Wang, J.-C.; Rauf, S.; Zhang, Y.; Agarwal, A.; Kenney, J.; Ramaswamy, K.; Collins, K.

2016-03-01

Sub-nm precision is increasingly being required of many critical plasma etching processes in the semiconductor industry. Accurate control over ion energy and ion/radical composition is needed during plasma processing to meet these stringent requirements. Described in this work is a new plasma etch system which has been designed with the requirements of atomic precision plasma processing in mind. In this system, an electron sheet beam parallel to the substrate surface produces a plasma with an order of magnitude lower electron temperature Te (~ 0.3 eV) and ion energy Ei (< 3 eV without applied bias) compared to conventional radio-frequency (RF) plasma technologies. Electron beam plasmas are characterized by higher ion-to-radical fraction compared to RF plasmas, so a separate radical source is used to provide accurate control over relative ion and radical concentrations. Another important element in this plasma system is low frequency RF bias capability which allows control of ion energy in the 2-50 eV range. Presented in this work are the results of etching of a variety of materials and structures performed in this system. In addition to high selectivity and low controllable etch rate, an important requirement of atomic precision etch processes is no (or minimal) damage to the remaining material surface. It has traditionally not been possible to avoid damage in RF plasma processing systems, even during atomic layer etch. The experiments for Si etch in Cl2 based plasmas in the aforementioned etch system show that damage can be minimized if the ion energy is kept below 10 eV. Layer-by-layer etch of Si is also demonstrated in this etch system using electrical and gas pulsing.

Bond strength of universal adhesives: A systematic review and meta-analysis.

PubMed

Rosa, Wellington Luiz de Oliveira da; Piva, Evandro; Silva, Adriana Fernandes da

2015-07-01

A systematic review was conducted to determine whether the etch-and-rinse or self-etching mode is the best protocol for dentin and enamel adhesion by universal adhesives. This report followed the PRISMA Statement. A total of 10 articles were included in the meta-analysis. Two reviewers performed a literature search up to October 2014 in eight databases: PubMed, Web of Science, Scopus, BBO, SciELO, LILACS, IBECS and The Cochrane Library. In vitro studies evaluating the bond strength of universal adhesives to dentin and/or enamel by the etch-and-rinse and self-etch strategies were eligible to be selected. Statistical analyses were conducted using RevMan 5.1 (The Cochrane Collaboration, Copenhagen, Denmark). A global comparison was performed with random-effects models at a significance level of p<0.05. The analysis of dentin micro-tensile bond strength showed no statistically significant difference between the etch-and-rinse and self-etch strategies for mild universal adhesives (p≥0.05). However, for the ultra-mild All-Bond Universal adhesive, the etch-and-rinse strategy was significantly different than the self-etch mode in terms of dentin micro-tensile bond strength, as well as in the global analysis of enamel micro-tensile and micro-shear bond strength (p≤0.05). The enamel bond strength of universal adhesives is improved with prior phosphoric acid etching. However, this effect was not evident for dentin with the use of mild universal adhesives with the etch-and-rinse strategy. Selective enamel etching prior to the application of a mild universal adhesive is an advisable strategy for optimizing bonding. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of EDTA and phosphoric Acid pretreatment on the bonding effectiveness of self-etch adhesives to ground enamel.

PubMed

Ibrahim, Ihab M; Elkassas, Dina W; Yousry, Mai M

2010-10-01

This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9-1.0), intermediary strong AdheSE (pH=1.6-1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel.

Defying ageing: An expectation for dentine bonding with universal adhesives?

PubMed

Zhang, Zheng-yi; Tian, Fu-cong; Niu, Li-na; Ochala, Kirsten; Chen, Chen; Fu, Bai-ping; Wang, Xiao-yan; Pashley, David H; Tay, Franklin R

2016-02-01

The present study evaluated the long-term dentine bonding effectiveness of five universal adhesives in etch-and-rinse or self-etch mode after 12 months of water-ageing. The adhesives evaluated included All-Bond Universal, Clearfil Universal Bond, Futurabond U Prime&Bond Elect and Scotchbond Universal. Microtensile bond strength and transmission electron microscopy of the resin-dentine interfaces created in human coronal dentine were examined after 24h or 12 months. Microtensile bond strength were significantly affected by bonding strategy (etch-and-rinse vs self-etch) and ageing (24h vs 12 months). All subgroups showed significantly decreased bond strength after ageing except for Prime&Bond Elect and Scotchbond Universal used in self-etch mode. All five adhesives employed in etch-and-rinse mode exhibited ultrastructural features characteristic of collagen degradation and resin hydrolysis. A previously-unobserved inside-out collagen degradation pattern was identified in hybrid layers created by 10-MDP containing adhesives (All-Bond Universal, Scotchbond Universal and Clearfil Universal Bond) in the etch-and-rinse mode, producing partially degraded collagen fibrils with intact periphery and a hollow core. In the self-etch mode, all adhesives except for Prime&Bond Elect exhibited degradation of the collagen fibrils along the thin hybrid layers. The three 10-MDP containing universal adhesives did not protect surface collagen fibrils from degradation when bonding was performed in the self-etch mode. Despite the adjunctive conclusion that bonds created by universal adhesives in the self-etch bonding mode are more resistant to decline in bond strength when compared with those bonds created using the etch-and-rinse mode, bonds created by universal adhesives are generally incapable of defying ageing. Copyright © 2015 Elsevier Ltd. All rights reserved.

Effect of EDTA and Phosphoric Acid Pretreatment on the Bonding Effectiveness of Self-Etch Adhesives to Ground Enamel

PubMed Central

Ibrahim, Ihab M.; Elkassas, Dina W.; Yousry, Mai M.

2010-01-01

Objectives: This in vitro study determined the effect of enamel pretreatment with phosphoric acid and ethylenediaminetetraacetic acid (EDTA) on the bond strength of strong, intermediary strong, and mild self-etching adhesive systems. Methods: Ninety sound human premolars were used. Resin composite cylinders were bonded to flat ground enamel surfaces using three self-etching adhesive systems: strong Adper Prompt L-Pop (pH=0.9–1.0), intermediary strong AdheSE (pH=1.6–1.7), and mild Frog (pH=2). Adhesive systems were applied either according to manufacturer instructions (control) or after pretreatment with either phosphoric acid or EDTA (n=10). After 24 hours, shear bond strength was tested using a universal testing machine at a cross-head speed of 0.5 mm/minute. Ultra-morphological characterization of the surface topography and resin/enamel interfaces as well as representative fractured enamel specimens were examined using scanning electron microscopy (SEM). Results: Neither surface pretreatment statistically increased the mean shear bond strength values of either the strong or the intermediary strong self-etching adhesive systems. However, phosphoric acid pretreatment significantly increased the mean shear bond strength values of the mild self-etching adhesive system. SEM examination of enamel surface topography showed that phosphoric acid pretreatment deepened the same etching pattern of the strong and intermediary strong adhesive systems but converted the irregular etching pattern of the mild self-etching adhesive system to a regular etching pattern. SEM examination of the resin/enamel interface revealed that deepening of the etching pattern was consistent with increase in the length of resin tags. EDTA pretreatment had a negligible effect on ultra-morphological features. Conclusions: Use of phosphoric acid pretreatment can be beneficial with mild self-etching adhesive systems for bonding to enamel. PMID:20922162

Guiding gate-etch process development using 3D surface reaction modeling for 7nm and beyond

NASA Astrophysics Data System (ADS)

Dunn, Derren; Sporre, John R.; Deshpande, Vaibhav; Oulmane, Mohamed; Gull, Ronald; Ventzek, Peter; Ranjan, Alok

2017-03-01

Increasingly, advanced process nodes such as 7nm (N7) are fundamentally 3D and require stringent control of critical dimensions over high aspect ratio features. Process integration in these nodes requires a deep understanding of complex physical mechanisms to control critical dimensions from lithography through final etch. Polysilicon gate etch processes are critical steps in several device architectures for advanced nodes that rely on self-aligned patterning approaches to gate definition. These processes are required to meet several key metrics: (a) vertical etch profiles over high aspect ratios; (b) clean gate sidewalls free of etch process residue; (c) minimal erosion of liner oxide films protecting key architectural elements such as fins; and (e) residue free corners at gate interfaces with critical device elements. In this study, we explore how hybrid modeling approaches can be used to model a multi-step finFET polysilicon gate etch process. Initial parts of the patterning process through hardmask assembly are modeled using process emulation. Important aspects of gate definition are then modeled using a particle Monte Carlo (PMC) feature scale model that incorporates surface chemical reactions.1 When necessary, species and energy flux inputs to the PMC model are derived from simulations of the etch chamber. The modeled polysilicon gate etch process consists of several steps including a hard mask breakthrough step (BT), main feature etch steps (ME), and over-etch steps (OE) that control gate profiles at the gate fin interface. An additional constraint on this etch flow is that fin spacer oxides are left intact after final profile tuning steps. A natural optimization required from these processes is to maximize vertical gate profiles while minimizing erosion of fin spacer films.2

Enamel Surface with Pit and Fissure Sealant Containing 45S5 Bioactive Glass.

PubMed

Yang, S-Y; Kwon, J-S; Kim, K-N; Kim, K-M

2016-05-01

Enamel demineralization adjacent to pit and fissure sealants leads to the formation of marginal caries, which can necessitate the replacement of existing sealants. Dental materials with bioactive glass, which releases ions that inhibit dental caries, have been studied. The purpose of this study was to evaluate the enamel surface adjacent to sealants containing 45S5 bioactive glass (BAG) under simulated microleakage between the material and the tooth in a cariogenic environment. Sealants containing 45S5BAG filler were prepared as follows: 0% 45S5BAG + 50.0% glass (BAG0 group), 12.5% 45S5BAG + 37.5% glass (BAG12.5 group), 25.0% 45S5BAG + 25.0% glass (BAG25.0 group), 37.5% 45S5BAG + 12.5% glass (BAG37.5 group), and 50.0% 45S5BAG + 0% glass (BAG50.0 group). A cured sealant disk was placed over a flat bovine enamel disk, separated by a 60-µm gap, and immersed in lactic acid solution (pH 4.0) at 37 °C for 15, 30, and 45 d. After the storage period, each enamel disk was separated from the cured sealant disk, and the enamel surface was examined with optical 3-dimensional surface profilometer, microhardness tester, and scanning electron microscopy. The results showed a significant increase in roughness and a decrease in microhardness of the enamel surface as the proportion of 45S5BAG decreased (P< 0.05). In the scanning electron microscopy images, enamel surfaces with BAG50.0 showed a smooth surface, similar to those in the control group with distilled water, even after prolonged acid storage. Additionally, an etched pattern was observed on the surface of the demineralized enamel with a decreasing proportion of 45S5BAG. Increasing the 45S5BAG filler contents of the sealants had a significant impact in preventing the demineralization of the enamel surface within microgaps between the material and the tooth when exposed to a cariogenic environment. Therefore, despite some marginal leakage, these novel sealants may be effective preventive dental materials for inhibiting secondary caries at the margins. © International & American Associations for Dental Research 2016.

Surface engineering on CeO2 nanorods by chemical redox etching and their enhanced catalytic activity for CO oxidation

NASA Astrophysics Data System (ADS)

Gao, Wei; Zhang, Zhiyun; Li, Jing; Ma, Yuanyuan; Qu, Yongquan

2015-07-01

Controllable surface properties of nanocerias are desired for various catalytic processes. There is a lack of efficient approaches to adjust the surface properties of ceria to date. Herein, a redox chemical etching method was developed to controllably engineer the surface properties of ceria nanorods. Ascorbic acid and hydrogen peroxide were used to perform the redox chemical etching process, resulting in a rough surface and/or pores on the surface of ceria nanorods. Increasing the etching cycles induced a steady increase of the specific surface area, oxygen vacancies and surface Ce3+ fractions. As a result, the etched nanorods delivered enhanced catalytic activity for CO oxidation, compared to the non-etched ceria nanorods. Our method provides a novel and facile approach to continuously adjust the surface properties of ceria for practical applications.Controllable surface properties of nanocerias are desired for various catalytic processes. There is a lack of efficient approaches to adjust the surface properties of ceria to date. Herein, a redox chemical etching method was developed to controllably engineer the surface properties of ceria nanorods. Ascorbic acid and hydrogen peroxide were used to perform the redox chemical etching process, resulting in a rough surface and/or pores on the surface of ceria nanorods. Increasing the etching cycles induced a steady increase of the specific surface area, oxygen vacancies and surface Ce3+ fractions. As a result, the etched nanorods delivered enhanced catalytic activity for CO oxidation, compared to the non-etched ceria nanorods. Our method provides a novel and facile approach to continuously adjust the surface properties of ceria for practical applications. Electronic supplementary information (ESI) available: Diameter distributions of as-prepared and etched samples, optical images, specific catalytic data of CO oxidation and comparison of CO oxidation. See DOI: 10.1039/c5nr01846c

High-density plasma etching of III-nitrides: Process development, device applications and damage remediation

NASA Astrophysics Data System (ADS)

Singh, Rajwinder

Plasma-assisted etching is a key technology for III-nitride device fabrication. The inevitable etch damage resulting from energetic pattern transfer is a challenge that needs to be addressed in order to optimize device performance and reliability. This dissertation focuses on the development of a high-density inductively-coupled plasma (ICP) etch process for III-nitrides, the demonstration of its applicability to practical device fabrication using a custom built ICP reactor, and development of techniques for remediation of etch damage. A chlorine-based standard dry etch process has been developed and utilized in fabrication of a number of electronic and optoelectronic III-nitride devices. Annealing studies carried out at 700°C have yielded the important insight that the annealing time necessary for making good-quality metal contacts to etch processed n-GaN is very short (<30 sec), comparable with the annealing times necessary for dopant activation of p-GaN films and provides an opportunity for streamlining process flow. Plasma etching degrades contact quality on n-GaN films and this degradation has been found to increase with the rf bias levels (ion energies) used, most notably in films with higher doping levels. Immersion in 1:1 mixture of hydrochloric acid and de-ionized water, prior to metallization, removes some of the etch damage and is helpful in recovering contact quality. In-situ treatment consisting of a slow ramp-down of rf bias at the end of the etch is found to achieve the same effect as the ex-situ treatment. This insitu technique is significantly advantageous in a large-scale production environment because it eliminates a process step, particularly one involving treatment in hydrochloric acid. ICP equipment customization for scaling up the process to full 2-inch wafer size is described. Results on etching of state of the art 256 x 256 AlGaN focal plane arrays of ultraviolet photodetectors are reported, with excellent etch uniformity over the wafer area.

Etude fondamentale des mecanismes de gravure par plasma de materiaux de pointe: Application a la fabrication de dispositifs photoniques

NASA Astrophysics Data System (ADS)

Stafford, Luc

Advances in electronics and photonics critically depend upon plasma-based materials processing either for transferring small lithographic patterns into underlying materials (plasma etching) or for the growth of high-quality films. This thesis deals with the etching mechanisms of materials using high-density plasmas. The general objective of this work is to provide an original framework for the plasma-material interaction involved in the etching of advanced materials by putting the emphasis on complex oxides such as SrTiO3, (Ba,Sr)TiO 3 and SrBi2Ta2O9 films. Based on a synthesis of the descriptions proposed by different authors to explain the etching characteristics of simple materials in noble and halogenated plasma mixtures, we propose comprehensive rate models for physical and chemical plasma etching processes. These models have been successfully validated using experimental data published in literature for Si, Pt, W, SiO2 and ZnO. As an example, we have been able to adequately describe the simultaneous dependence of the etch rate on ion and reactive neutral fluxes and on the ion energy. From an exhaustive experimental investigation of the plasma and etching properties, we have also demonstrated that the validity of the proposed models can be extended to complex oxides such as SrTiO3, (Ba,Sr)TiO 3 and SrBi2Ta2O9 films. We also reported for the first time physical aspects involved in plasma etching such as the influence of the film microstructural properties on the sputter-etch rate and the influence of the positive ion composition on the ion-assisted desorption dynamics. Finally, we have used our deep investigation of the etching mechanisms of STO films and the resulting excellent control of the etch rate to fabricate a ridge waveguide for photonic device applications. Keywords: plasma etching, sputtering, adsorption and desorption dynamics, high-density plasmas, plasma diagnostics, advanced materials, photonic applications.

Bond efficacy and interface morphology of self-etching adhesives to ground enamel.

PubMed

Abdalla, Ali I; El Zohairy, Ahmed A; Abdel Mohsen, Mohamed M; Feilzer, Albert J

2010-02-01

This study compared the microshear bond strengths to ground enamel of three one-step self-etching adhesive systems, a self-etching primer system and an etch-and-rinse adhesive system. Three self-etching adhesives, Futurabond DC (Voco), Clearfil S Tri Bond (Kuraray) and Hybrid bond (Sun-Medical), a self-etching primer, Clearfil SE Bond (Kuraray), and an etch-and-rinse system, Admira Bond (Voco), were selected. Thirty human molars were used. The root of each tooth was removed and the crown was sectioned into halves. The convex enamel surfaces were reduced by polishing on silicone paper to prepare a flat surface. The bonding systems were applied on this surface. Prior to adhesive curing, a hollow cylinder (2.0 mm height/0.75 mm internal diameter) was placed on the treated surfaces. A resin composite was then inserted into the tube and cured. After water storage for 24 h, the tube was removed and shear bond strength was determined in a universal testing machine at a crosshead speed of 0.5 mm/min. The results were analyzed with ANOVA and the Tukey.-Kramer test at a 59 degrees confidence level. The enamel of five additional teeth was ground, and the etching component of each adhesive was applied and removed with absolute ethanol instead of being light cured. These teeth and selected fractured surfaces were examined by SEM. Adhesion to ground enamel of the Futurabond DC (25 +/- 3.5 MPa) and Clearfil SE Bond (23 +/- 2.9 MPa) self-etching systems was not significantly different from the etch-and-rinse system Admira Bond (27 +/- 2.3 MPa). The two self-etching adhesives Clearfil S Tri bond and Hybrid Bond demonstrated significantly lower bond strengths (14 +/- 1.4 MPa; 11 +/- 1.9 MPa) with no significant differences between them (p < 0.05). Bond strengths to ground enamel of self-etching adhesive systems are dependent on the type of adhesive system. Some of the new adhesive systems showed bond strength values comparable to that of etch-and-rinse systems. There was no correlation between bond strength and morphological changes in enamel.

Modeling Cl2/O2/Ar inductively coupled plasmas used for silicon etching: effects of SiO2 chamber wall coating

NASA Astrophysics Data System (ADS)

Tinck, S.; Boullart, W.; Bogaerts, A.

2011-08-01

In this paper, simulations are performed to gain a better insight into the properties of a Cl2/Ar plasma, with and without O2, during plasma etching of Si. Both plasma and surface properties are calculated in a self-consistent manner. Special attention is paid to the behavior of etch products coming from the wafer or the walls, and how the chamber walls can affect the plasma and the resulting etch process. Two modeling cases are considered. In the first case, the reactor walls are defined as clean (Al2O3), whereas in the second case a SiO2 coating is introduced on the reactor walls before the etching process, so that oxygen will be sputtered from the walls and introduced into the plasma. For this reason, a detailed reaction set is presented for a Cl2/O2/Ar plasma containing etched species, as well as an extensive reaction set for surface processes, including physical and chemical sputtering, chemical etching and deposition processes. Density and flux profiles of various species are presented for a better understanding of the bulk plasma during the etching process. Detailed information is also given on the composition of the surfaces at various locations of the reactor, on the etch products in the plasma and on the surface loss probabilities of the plasma species at the walls, with different compositions. It is found that in the clean chamber, walls are mostly chlorinated (Al2Cl3), with a thin layer of etch products residing on the wall. In the coated chamber, an oxy-chloride layer is grown on the walls for a few nanometers during the etching process. The Cl atom wall loss probability is found to decrease significantly in the coated chamber, hence increasing the etch rate. SiCl2, SiCl4 and SiCl3 are found to be the main etch products in the plasma, with the fraction of SiCl2 being always slightly higher. The simulation results compare well with experimental data available from the literature.

CDU improvement technology of etching pattern using photo lithography

NASA Astrophysics Data System (ADS)

Tadokoro, Masahide; Shinozuka, Shinichi; Jyousaka, Megumi; Ogata, Kunie; Morimoto, Tamotsu; Konishi, Yoshitaka

2008-03-01

Semiconductor manufacturing technology has shifted towards finer design rules, and demands for critical dimension uniformity (CDU) of resist patterns have become greater than ever. One of the methods for improving Resist Pattern CDU is to control post-exposure bake (PEB) temperature. When ArF resist is used, there is a certain relationship between critical dimension (CD) and PEB temperature. By utilizing this relationship, Resist Pattern CDU can be improved through control of within-wafer temperature distribution in the PEB process. Resist Pattern CDU improvement contributes to Etching Pattern CDU improvement to a certain degree. To further improve Etching Pattern CDU, etcher-specific CD variation needs to be controlled. In this evaluation, 1. We verified whether etcher-specific CD variation can be controlled and consequently Etching Pattern CDU can be further improved by controlling resist patterns through PEB control. 2. Verifying whether Etching Pattern CDU improvement through has any effect on the reduction in wiring resistance variation. The evaluation procedure is as follows.1. Wafers with base film of Doped Poly-Si (D-Poly) were prepared. 2. Resist patterns were created on them. 3. To determine etcher-specific characteristics, the first etching was performed, and after cleaning off the resist and BARC, CD of etched D-Poly was measured. 4. Using the obtained within-wafer CD distribution of the etching patterns, within-wafer temperature distribution in the PEB process was modified. 5. Resist patterns were created again, followed by the second etching and cleaning, which was followed by CD measurement. We used Optical CD Measurement (OCD) for measurement of resist patterns and etching patterns as OCD is minimally affected by Line Edge Roughness (LER). As a result, 1. We confirmed the effect of Resist Pattern CD control through PEB control on the reduction in etcher-specific CD variation and the improvement in Etching Pattern CDU. 2. The improvement in Etching Pattern CDU has an effect on the reduction in wiring resistance variation. The method for Etching Pattern CDU improvement through PEB control reduces within-wafer variation of MOS transistor's gate length. Therefore, with this method, we can expect to observe uniform within-wafer MOS transistor characteristics.

Effect of bromelain and papain gel on enamel deproteinisation before orthodontic bracket bonding.

PubMed

Pithon, Matheus Melo; Campos, Matheus Souza; Coqueiro, Raildo da Silva

2016-05-01

To test the hypothesis that enamel surface deproteinisation with different concentrations of bromelain in association with 10% papain increases the shear bond strength (SBS) of brackets bonded with orthodontic composite and resin modified glass ionomer cement (RMGIC). Orthodontic brackets were attached according to the following protocols to 195 bovine incisors, which were acquired and divided into 13 groups: 1) Transbond XT (TXT) according to the manufacturer's recommendations; 2) Deproteinisation with 3% bromelain (BD) plus 10% papain and TXT; 3) 6% BD plus 10% Papain and TXT; 4) RMGIC, without enamel deproteinisation and without acid etching; 5) RMGIC, with 3% BD plus 10% papain and without acid etching; 6) RMGIC, with 6% BD plus 10% papain and without acid etching; 7) attachment using RMGIC following etching with polyacrylic acid; 8) 3% BD plus 10% papain, attachment using RMGIC and etching with polyacrylic acid; 9) 6% BD plus 10% papain, and attachment using RMGIC following etching with polyacrylic acid; 10) etching with 37% phosphoric acid and attachment using RMGIC; 11) 3% BD plus 10% papain, etching with 37% phosphoric acid and attachment using RMGIC; 12) 6% BD plus 10% papain, etching with 37% phosphoric acid and attachment using RMGIC; 13) deproteinisation with 2.5% sodium hypochlorite (NaOCl), etching with polyacrylic acid and RMGIC. After bonding, the brackets were removed by a universal mechanical testing machine, which recorded shear bond strength at failure. The material remaining on the tooth was assessed using the adhesive remnant index (ARI). Deproteinisation with 3% and 6% bromelain gel plus papain significantly increased the shear bond strength (p < 0.05), when acid etching was performed with phosphoric acid, followed by primer application and attachment using Transbond XT (Group 3) and when attached with RMGIC without etching. Deproteinisation with 6% bromelain gel plus papain significantly increased (p < 0.05) the ARI score only when attachment was performed using RMGIC, without etching (Group 6). Deproteinisation with bromelain associated with papain in a gel increased the shear bond strength and is recommended before orthodontic bracket attachment.

Process for Smoothing an Si Substrate after Etching of SiO2

NASA Technical Reports Server (NTRS)

Turner, Tasha; Wu, Chi

2003-01-01

A reactive-ion etching (RIE) process for smoothing a silicon substrate has been devised. The process is especially useful for smoothing those silicon areas that have been exposed by etching a pattern of holes in a layer of silicon dioxide that covers the substrate. Applications in which one could utilize smooth silicon surfaces like those produced by this process include fabrication of optical waveguides, epitaxial deposition of silicon on selected areas of silicon substrates, and preparation of silicon substrates for deposition of adherent metal layers. During etching away of a layer of SiO2 that covers an Si substrate, a polymer becomes deposited on the substrate, and the substrate surface becomes rough (roughness height approximately equal to 50 nm) as a result of over-etching or of deposition of the polymer. While it is possible to smooth a silicon substrate by wet chemical etching, the undesired consequences of wet chemical etching can include compromising the integrity of the SiO2 sidewalls and undercutting of the adjacent areas of the silicon dioxide that are meant to be left intact. The present RIE process results in anisotropic etching that removes the polymer and reduces height of roughness of the silicon substrate to less than 10 nm while leaving the SiO2 sidewalls intact and vertical. Control over substrate versus sidewall etching (in particular, preferential etching of the substrate) is achieved through selection of process parameters, including gas flow, power, and pressure. Such control is not uniformly and repeatably achievable in wet chemical etching. The recipe for the present RIE process is the following: Etch 1 - A mixture of CF4 and O2 gases flowing at rates of 25 to 75 and 75 to 125 standard cubic centimeters per minute (stdcm3/min), respectively; power between 44 and 55 W; and pressure between 45 and 55 mtorr (between 6.0 and 7.3 Pa). The etch rate lies between approximately equal to 3 and approximately equal to 6 nm/minute. Etch 2 - O2 gas flowing at 75 to 125 stdcm3/min, power between 44 and 55 W, and pressure between 50 and 100 mtorr (between 6.7 and 13.3 Pa).

Effect of universal adhesive etching modes on bond strength to dual-polymerizing composite resins.

PubMed

Michaud, Pierre-Luc; Brown, Matthew

2018-04-01

Information is lacking as to the effect on bond strength of the etching modes of universal adhesives when they are used to bond dual-polymerizing composite resins to dentin. The purpose of this in vitro study was to investigate the bonding of dual-polymerizing foundation composite resins to dentin when universal bonding agents are used in self-etch or etch-and-rinse modes. Sixty caries-free, extracted third molar teeth were sectioned transversely in the apical third of the crown and allocated to 12 groups (n=5). Three different bonding agents (Scotchbond Universal, OptiBond XTR, All-Bond Universal) were used to bond 2 different dual-polymerizing composite resins (CompCore AF or CoreFlo DC) to dentin, using 2 different etching approaches (etch-and-rinse or self-etch). The specimens were sectioned into sticks (1×1×8 mm) with a precision saw. The bond strength of the specimens was tested under microtensile force at a crosshead speed of 0.5 mm/min. The data were analyzed using a 3-way ANOVA, a Games-Howell post hoc comparisons model, and Student t tests with Bonferroni corrections (α=.05). In the overall model, the composite resin used had no effect on bond strength (P=.830). The etching protocol by itself also did not have a significant effect (P=.059), although a trend was present. The bonding agent, however, did have an effect (P<.001) on bond strength. Also, a significant interaction effect was found for the bonding agent and etching protocol on bond strength (P<.001). The etching protocol influenced the bond strength when Scotchbond Universal (P<.008) and All-Bond Universal (P<.004) were used but not when OptiBond XTR was used (P=1.00). A self-etch protocol provided significantly higher bond strength when Scotchbond Universal was used, whereas with All-Bond Universal, an etch-and-rinse protocol, provided higher bond strength. When universal bonding agents were used to secure dual-polymerizing composite resins to dentin, no single etching protocol is better than another. Depending on which bonding agent is being used, one etching mode may perform better. Copyright © 2017 Editorial Council for the Journal of Prosthetic Dentistry. Published by Elsevier Inc. All rights reserved.

High density plasma etching of magnetic devices

NASA Astrophysics Data System (ADS)

Jung, Kee Bum

Magnetic materials such as NiFe (permalloy) or NiFeCo are widely used in the data storage industry. Techniques for submicron patterning are required to develop next generation magnetic devices. The relative chemical inertness of most magnetic materials means they are hard to etch using conventional RIE (Reactive Ion Etching). Therefore ion milling has generally been used across the industry, but this has limitations for magnetic structures with submicron dimensions. In this dissertation, we suggest high density plasmas such as ECR (Electron Cyclotron Resonance) and ICP (Inductively Coupled Plasma) for the etching of magnetic materials (NiFe, NiFeCo, CoFeB, CoSm, CoZr) and other related materials (TaN, CrSi, FeMn), which are employed for magnetic devices like magnetoresistive random access memories (MRAM), magnetic read/write heads, magnetic sensors and microactuators. This research examined the fundamental etch mechanisms occurring in high density plasma processing of magnetic materials by measuring etch rate, surface morphology and surface stoichiometry. However, one concern with using Cl2-based plasma chemistry is the effect of residual chlorine or chlorinated etch residues remaining on the sidewalls of etched features, leading to a degradation of the magnetic properties. To avoid this problem, we employed two different processing methods. The first one is applying several different cleaning procedures, including de-ionized water rinsing or in-situ exposure to H2, O2 or SF6 plasmas. Very stable magnetic properties were achieved over a period of ˜6 months except O2 plasma treated structures, with no evidence of corrosion, provided chlorinated etch residues were removed by post-etch cleaning. The second method is using non-corrosive gas chemistries such as CO/NH3 or CO2/NH3. There is a small chemical contribution to the etch mechanism (i.e. formation of metal carbonyls) as determined by a comparison with Ar and N2 physical sputtering. The discharge should be NH3-rich to achieve the highest etch rates. Several different mask materials were investigated, including photoresist, thermal oxide and deposited oxide. Photoresist etches very rapidly in CO/NH 3 and use of a hard mask is necessary to achieve pattern transfer. Due to its physically dominated nature, the CO/NH3 chemistry appears suited to shallow etch depth (≤0.5mum) applications, but mask erosion leads to sloped feature sidewalls for deeper features.

Effect of Fluoride-Releasing Adhesive Systems on the Mechanical Properties of Eroded Dentin.

PubMed

Guedes, Ana Paula Albuquerque; Moda, Mariana Dias; Suzuki, Thaís Yumi Umeda; Godas, André Gustavo de Lima; Sundfeld, Renato Herman; Briso, André Luiz Fraga; Santos, Paulo Henrique dos

2016-01-01

The aim of the study was to evaluate the effect of erosive pH cycling with solutions that simulate dental erosion on Martens hardness (HMV) and elastic modulus (Eit) of dentin restored with fluoride-releasing adhesive systems. Twenty-seven bovine dentin slabs were restored with three adhesive systems: Adper Single Bond 2 total-etch adhesive system, One Up Bond F and Clearfil SE Protect fluoride-containing self-etching adhesive systems. The restorations were made with Filtek Z250. The HMV and Eit values at distances of 10, 30, 50 and 70 µm from the interface were evaluated using a dynamic ultra microhardness tester before and after immersion in deionized water, citric acid and hydrochloric acid (n=9). Data were submitted to repeated-measures ANOVA and Fisher's PLSD tests (=0.05). After erosive cycling, HMV values of dentin decreased in all groups. For dentin restored with Adper Single Bond 2, the lowest values were found closer to the hybrid layer, while for One Up Bond F and Clearfil SE Protect, the values remained unaltered at all distances. For dentin restored with fluoride-releasing adhesive systems, a decrease in Eit was found, but after 30 µm this difference was not significant. The acid substances were able to alter HMV and Eit of the underlying dentin. For fluoride-releasing adhesives, the greater the distance from bonded interface, the lower the Eit values. The fluoride in One Up Bond F and Clearfil SE Protect was able to protect the underlying dentin closer to the materials. In this way, the fluoride from adhesive systems could have some positive effect in the early stages of erosive lesions.

Six-year clinical performance of etch-and-rinse and self-etch adhesives.

PubMed

Boushell, Lee W; Heymann, Harald O; Ritter, Andre V; Sturdevant, John R; Swift, Edward J; Wilder, Aldridge D; Chung, Yunro; Lambert, Cynthia A; Walter, Ricardo

2016-09-01

To evaluate the 6-year clinical performance of Xeno IV, Xeno III, and XP Bond adhesives in the restoration of non-carious cervical lesions (NCCLs). This was a randomized controlled clinical trial where 39 participants met the inclusion/exclusion criteria and were enrolled. Lesions restored were notch-shaped NCCLs. Prior to adhesive procedures, NCCLs were roughened. No enamel bevel was placed and no mechanical retention was created. Adhesive systems were applied following manufacturer's instructions and the NCCLs were restored with composite resin (TPH(3)). Restorations were finished immediately after placement and scored with regard to retention, marginal discoloration, marginal adaptation, sensitivity, and secondary caries using modified USPHS criteria. Descriptive statistics were performed. Logistic regression models were performed for each outcome separately with compound symmetry correlation structure where teeth were clustered by participants. All analyses were conducted using SAS 9.2. The 6-year recall rate was 77.5% of the restorations (76.9% of the participants). No statistical differences were found between adhesives for retention, marginal discoloration, and marginal adaptation. Restorations failed by loss of retention (16.7%, 27.6%, and 11.8% of Xeno IV, Xeno III, and XP Bond restorations, respectively) and marginal discoloration (7.4% of Xeno IV restorations). For every unit increase in restoration volume it was 1.31 (95%C.I. 1.05, 1.63, P=0.01) times more likely that the restoration retention would be maintained. The tested adhesive systems presented similar clinical performance after six years of service, with annual failure rates of 2.8%, 4.6%, and 2.0% for Xeno IV, Xeno III, and XP Bond, respectively. Copyright © 2016 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Hydrophilicity of dentin bonding systems influences in vitro Streptococcus mutans biofilm formation

PubMed Central

Brambilla, Eugenio; Ionescu, Andrei; Mazzoni, Annalisa; Cadenaro, Milena; Gagliani, Massimo; Ferraroni, Monica; Tay, Franklin; Pashley, David; Breschi, Lorenzo

2014-01-01

Objectives To evaluate in vitro Streptococcus mutans (S. mutans) biofilm formation on the surface of five light-curing experimental dental bonding systems (DBS) with increasing hydrophilicity. The null hypothesis tested was that resin chemical composition and hydrophilicity does not affect S. mutans biofilm formation. Methods Five light-curing versions of experimental resin blends with increasing hydrophilicity were investigated (R1, R2, R3, R4 and R5). R1 and R2 contained ethoxylated BisGMA/TEGDMA or BisGMA/TEGDMA, respectively, and were very hydrophobic, were representative of pit-and-fissure bonding agents. R3 was representative of a typical two-step etch- and-rinse adhesive, while R4 and R5 were very hydrophilic resins analogous to self-etching adhesives. Twenty-eight disks were prepared for each resin blend. After a 24 h-incubation at 37 °C, a multilayer monospecific biofilm of S. mutans was obtained on the surface of each disk. The adherent biomass was determined using the MTT assay and evaluated morphologically with confocal laser scanning microscopy (CLSM) and scanning electron microscopy (SEM). Results R2 and R3 surfaces showed the highest biofilm formation while R1 and R4 showed a similar intermediate biofilm formation. R5 was more hydrophilic and acidic and was significantly less colonized than all the other resins. A significant quadratic relationship between biofilm formation and hydrophilicity of the resin blends was found. CLSM and SEM evaluation confirmed MTT assay results. Conclusions The null hypothesis was rejected since S. mutans biofilm formation was influenced by hydrophilicity, surface acidity and chemical composition of the experimental resins. Further studies using a bioreactor are needed to confirm the results and clarify the role of the single factors. PMID:24954666

Biomimetic remineralization of dentin.

PubMed

Niu, Li-Na; Zhang, Wei; Pashley, David H; Breschi, Lorenzo; Mao, Jing; Chen, Ji-Hua; Tay, Franklin R

2014-01-01

Remineralization of demineralized dentin is important for improving dentin bonding stability and controlling primary and secondary caries. Nevertheless, conventional dentin remineralization strategy is not suitable for remineralizing completely demineralized dentin within hybrid layers created by etch-and-rinse and moderately aggressive self-etch adhesive systems, or the superficial part of a caries-affected dentin lesion left behind after minimally invasive caries removal. Biomimetic remineralization represents a different approach to this problem by attempting to backfill the demineralized dentin collagen with liquid-like amorphous calcium phosphate nanoprecursor particles that are stabilized by biomimetic analogs of noncollagenous proteins. This paper reviewed the changing concepts in calcium phosphate mineralization of fibrillar collagen, including the recently discovered, non-classical particle-based crystallization concept, formation of polymer-induced liquid-precursors (PILP), experimental collagen models for mineralization, and the need for using phosphate-containing biomimetic analogs for biomimetic mineralization of collagen. Published work on the remineralization of resin-dentin bonds and artificial caries-like lesions by various research groups was then reviewed. Finally, the problems and progress associated with the translation of a scientifically sound concept into a clinically applicable approach are discussed. The particle-based biomimetic remineralization strategy based on the PILP process demonstrates great potential in remineralizing faulty hybrid layers or caries-like dentin. Based on this concept, research in the development of more clinically feasible dentin remineralization strategy, such as incorporating poly(anionic) acid-stabilized amorphous calcium phosphate nanoprecursor-containing mesoporous silica nanofillers in dentin adhesives, may provide a promising strategy for increasing of the durability of resin-dentin bonding and remineralizing caries-affected dentin. Copyright © 2013 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Water interaction and bond strength to dentin of dye-labelled adhesive as a function of the addition of rhodamine B.

PubMed

Wang, Linda; Bim, Odair; Lopes, Adolfo Coelho de Oliveira; Francisconi-Dos-Rios, Luciana Fávaro; Maenosono, Rafael Massunari; D'Alpino, Paulo Henrique Perlatti; Honório, Heitor Marques; Atta, Maria Teresa

2016-01-01

This study investigated the effect of the fluorescent dye rhodamine B (RB) for interfacial micromorphology analysis of dental composite restorations on water sorption/solubility (WS/WSL) and microtensile bond strength to dentin (µTBS) of a 3-step total etch and a 2-step self-etch adhesive system. The adhesives Adper Scotchbond Multi-Purpose (MP) and Clearfil SE Bond (SE) were mixed with 0.1 mg/mL of RB. For the WS/WSL tests, cured resin disks (5.0 mm in diameter x 0.8 mm thick) were prepared and assigned into four groups (n=10): MP, MP-RB, SE, and SE-RB. For µTBS assessment, extracted human third molars (n=40) had the flat occlusal dentin prepared and assigned into the same experimental groups (n=10). After the bonding and restoration procedures, specimens were sectioned in rectangular beams, stored in water and tested after seven days or after 12 months. The failure mode of fractured specimens was qualitatively evaluated under optical microscope (x40). Data from WS/WSL and µTBS were assessed by one-way and three-way ANOVA, respectively, and Tukey's test (α=5%). RB increased the WSL of MP and SE. On the other hand, WS of both MP and SE was not affected by the addition of RB. No significance in µTBS between MP and MP-RB for seven days or one year was observed, whereas for SE a decrease in the µTBS means occurred in both storage times. RB should be incorporated into non-simplified DBSs with caution, as it can interfere with their physical-mechanical properties, leading to a possible misinterpretation of bonded interface.

Water interaction and bond strength to dentin of dye-labelled adhesive as a function of the addition of rhodamine B

PubMed Central

WANG, Linda; BIM, Odair; LOPES, Adolfo Coelho de Oliveira; FRANCISCONI-DOS-RIOS, Luciana Fávaro; MAENOSONO, Rafael Massunari; D’ALPINO, Paulo Henrique Perlatti; HONÓRIO, Heitor Marques; ATTA, Maria Teresa

2016-01-01

ABSTRACT Objective This study investigated the effect of the fluorescent dye rhodamine B (RB) for interfacial micromorphology analysis of dental composite restorations on water sorption/solubility (WS/WSL) and microtensile bond strength to dentin (µTBS) of a 3-step total etch and a 2-step self-etch adhesive system. Material and Methods The adhesives Adper Scotchbond Multi-Purpose (MP) and Clearfil SE Bond (SE) were mixed with 0.1 mg/mL of RB. For the WS/WSL tests, cured resin disks (5.0 mm in diameter x 0.8 mm thick) were prepared and assigned into four groups (n=10): MP, MP-RB, SE, and SE-RB. For µTBS assessment, extracted human third molars (n=40) had the flat occlusal dentin prepared and assigned into the same experimental groups (n=10). After the bonding and restoration procedures, specimens were sectioned in rectangular beams, stored in water and tested after seven days or after 12 months. The failure mode of fractured specimens was qualitatively evaluated under optical microscope (x40). Data from WS/WSL and µTBS were assessed by one-way and three-way ANOVA, respectively, and Tukey’s test (α=5%). Results RB increased the WSL of MP and SE. On the other hand, WS of both MP and SE was not affected by the addition of RB. No significance in µTBS between MP and MP-RB for seven days or one year was observed, whereas for SE a decrease in the µTBS means occurred in both storage times. Conclusions RB should be incorporated into non-simplified DBSs with caution, as it can interfere with their physical-mechanical properties, leading to a possible misinterpretation of bonded interface. PMID:27556201

Leucine-rich amelogenin peptide (LRAP) as a surface primer for biomimetic remineralization of superficial enamel defects: An in vitro study.

PubMed

Shafiei, Farhad; Hossein, Bagheri G; Farajollahi, Mohammad M; Fathollah, Moztarzadeh; Marjan, Behroozibakhsh; Tahereh, Jafarzadeh Kashi

2015-01-01

This study was carried out to obtain more information about the assembly of hydroxyapatite bundles formed in the presence of Leucine-Rich Amelogenin Peptide (LRAP) and to evaluate its effect on the remineralization of enamel defects through a biomimetic approach. One or 2 mg/mL LRAP solutions containing 2.5 mM of Ca(+2) and 1.5 mM phosphate were prepared (pH = 7.2) and stored at 37 °C for 24 h. The products of the reaction were studied using atomic force microscopy (AFM), transmission electron microscopy (TEM), and selected area electron diffraction (SAED). Vickers surface microhardness recovery (SMR%) of acid-etched bovine enamel, with or without LRAP surface treatment, were calculated to evaluate the influence of peptide on the lesion remineralization. Distilled water and 1 or 2 mg/mL LRAP solution (pH = 7.2) were applied on the lesions and the specimens were incubated in mineralization solution (2.5mM Ca(+2) , 1.5mM PO4 (-3) , pH = 7.2) for 24 h. One-way ANOVA and Tukey's multi-comparison tests were used for statistical analysis. The pattern of enamel surface repair was studied using FE-SEM. AFM showed the formation of highly organized hierarchical structures, composed of hydroxyapatite (HA) crystals, similar to the dental enamel microstructure. ANOVA procedure showed significant effect of peptide treatment on the calculated SMR% (p < 0.001). Tukey's test revealed that peptide treated groups had significantly higher values of SMR%. In conclusion, LRAP is able to regulate the formation of HA and enhances the remineralization of acid-etched enamel as a surface treatment agent. © Wiley Periodicals, Inc.

Effect of two-step and one-step surface conditioning of glass ceramic on adhesion strength of orthodontic bracket and effect of thermo-cycling on adhesion strength.

PubMed

Asiry, Moshabab A; AlShahrani, Ibrahim; Alaqeel, Samer M; Durgesh, Bangalore H; Ramakrishnaiah, Ravikumar

2018-08-01

The adhesion strength of orthodontic brackets bonded to dental glass ceramics was evaluated after ceramic surface was treated with two-step and one-step surface conditioning systems, and subjecting to thermo-cycling. A total of forty specimens were fabricated from silica based glass ceramic (lithium disilicate) by duplicating the buccal surface of maxillary first premolar. The specimens were randomly assigned to two experimental groups (n = 20), group one specimens were treated with two-step surface conditioning system (IPS ceramic etching gel™ and Monobond plus™) and group two specimens were treated with one-step surface conditioning system (Monobond etch and prime™). The surface roughness of the specimens after treatment with two-step and one-step surface conditioning system was measured using non-contact surface profilometer. Ten randomly selected specimens from each group were subjected to thermo-cycling and the remaining ten served as baseline. The shear bond strength of the specimens was measured using universal material testing machine. The adhesive remnant index score was calculated, and the results of surface roughness and bond strength were tabulated and subjected to analysis of variance and post hoc tukey's test at a significance level of p < 0.05. The results of the study showed that the specimens treated with two-step conditioning system had higher surface roughness and bond strength than one-step conditioning system. The majority of the specimens treated with both two-step and one-step conditioned specimens showed adhesive failure after subjecting thermo-cycling. Traditional two-step conditioning provides better bond strength. The clinical importance of the study is that, the silane promoted adhesion significantly reduces on exposure to thermo-cycling. Copyright © 2018 Elsevier Ltd. All rights reserved.

The influence of Y-TZP surface treatment on topography and ceramic/resin cement interfacial fracture toughness.

PubMed

Paes, P N G; Bastian, F L; Jardim, P M

2017-09-01

Consider the efficacy of glass infiltration etching (SIE) treatment as a procedure to modify the zirconia surface resulting in higher interfacial fracture toughness. Y-TZP was subjected to 5 different surface treatments conditions consisting of no treatment (G1), SIE followed by hydrofluoric acid treatment (G2), heat treated at 750°C (G3), hydrofluoric acid treated (G4) and airborne-particle abrasion with alumina particles (G5). The effect of surface treatment on roughness was evaluated by Atomic Force Microscopy providing three different parameters: R a , R sk and surface area variation. The ceramic/resin cement interface was analyzed by Fracture Mechanics K I test with failure mode determined by fractographic analysis. Weibull's analysis was also performed to evaluate the structural integrity of the adhesion zone. G2 and G4 specimens showed very similar, and high R a values but different surface area variation (33% for G2 and 13% for G4) and they presented the highest fracture toughness (K IC ). Weibull's analysis showed G2 (SIE) tendency to exhibit higher K IC values than the other groups but with more data scatter and a higher early failure probability than G4 specimens. Selective glass infiltration etching surface treatment was effective in modifying the zirconia surface roughness, increasing the bonding area and hence the mechanical imbrications at the zirconia/resin cement interface resulting in higher fracture toughness (K IC ) values with higher K IC values obtained when failure probability above 20% was expected (Weibull's distribution) among all the experimental groups. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Ceramic strengthening by tuning the elastic moduli of resin-based luting agents.

PubMed

Spazzin, Aloísio O; Bacchi, Ataís; Alessandretti, Rodrigo; Santos, Mateus B; Basso, Gabriela R; Griggs, Jason; Moraes, Rafael R

2017-03-01

Resin-based luting agents (RBLAs) with tuned elastic moduli (E) were prepared and their influence on the strengthening, reliability, and mode of failure of luted feldspar ceramic was investigated. RBLAs with low E (2.6GPa), intermediate E (6.6GPa), and high E (13.3GPa) were prepared and used to coat acid-etched ceramic disks. Positive (untreated ceramic) and negative (acid-etched ceramic) control groups were tested. The response variables (n=30) were biaxial flexural strength (σ bf , MPa), characteristic strength (σ 0 , MPa), and Weibull modulus at the ceramic surface (z=0) and luting agent surface (z=-t 2 ). A 3D finite element analysis simulated the biaxial flexural test. Fractographic analysis and morphology of the bonded interfaces were analyzed using scanning electron microscopy. The RBLAs improved σ bf and σ 0 at z=0, particularly those with intermediate and high E, whereas the mechanical reliability was only affected in the negative control. At z=-t 2 , differences between all RBLAs were observed but the structural reliability was independent of the RBLA tested. Increasing E of the RBLA was associated with increased stress concentration at the RBLA and reduced stresses reaching the ceramic. Failures originated on the ceramic surface at the ceramic-cement interface. In the high E group, failure sometimes originated from the RBLA free surface. All RBLAs completely filled the ceramic irregularities. Increased E of the RBLA reduced the variability of strength, the stress reaching the ceramic structure, and sometimes altered the origin of failure. The use of high E RBLAs seems beneficial for luting feldspar ceramics. Copyright © 2017 The Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Zn-doped etch-and-rinse model dentin adhesives: Dentin bond integrity, biocompatibility, and properties.

PubMed

Barcellos, Daphne Câmara; Fonseca, Beatriz Maria; Pucci, César Rogério; Cavalcanti, Bruno das Neves; Persici, Erasmo De Souza; Gonçalves, Sérgio Eduardo de Paiva

2016-07-01

This study assessed a 6 month resin/dentin bond's durability and cytotoxic effect of Zn-doped model dentin adhesives. The mechanical and physicochemical properties were also tested. A model etch-and-rinse single-bottle adhesive was formulated (55wt.% Bis-GMA, 45wt.% HEMA, 0.5wt.% CQ, 0.5wt.% DMAEMA) and Zinc methacrylate (Zn-Mt) or ZnO nanoparticles (ZnOn) were added to the model's adhesive, resulting in three groups: Group Control (control model adhesive); Group Zn-Mt (1wt.% Zn-Mt incorporated to adhesive) and Group ZnOn (1wt.% ZnOn incorporated to adhesive). The microtensile bond strength (mTBS) was assessed after 24h or 6 months in water storage. Mechanical properties (diametral tensile strength/DTS, flexural strength/FS, flexural modulus/FM, resilience modulus/RM, and compressive strength/CS) and physicochemical properties (polymerization shrinkage/PS, contact angle/CA, water sorption/WS, and water solubility/WS) were also tested. Cytotoxicity was evaluated with SRB biochemical assay. No significant difference in the DTS, FS, FM, CS, CA, WS, and WS were found when 1% of ZnOn or Zn-Mt was added to the model dentin adhesive. Group Zn-Mt decreased the RM of adhesive. Groups Zn-Mt and ZnOn decreased the PS of adhesives. Group ZnOn reduced the cytotoxicity of adhesive. Group ZnOn preserved mTBS after 6 months storage without degradation areas as seen by SEM analysis. The 1wt.% ZnOn may preserve the integrity of the hybrid layer and may reduce cytotoxicity and polymerization shrinkage of model dentin adhesive. The addition of Zn-Mt to the adhesive had no beneficial effects. Copyright © 2016 The Academy of Dental Materials. All rights reserved.

Semiconductor etching by hyperthermal neutral beams

NASA Technical Reports Server (NTRS)

Minton, Timothy K. (Inventor); Giapis, Konstantinos P. (Inventor)

1999-01-01

An at-least dual chamber apparatus and method in which high flux beams of fast moving neutral reactive species are created, collimated and used to etch semiconductor or metal materials from the surface of a workpiece. Beams including halogen atoms are preferably used to achieve anisotropic etching with good selectivity at satisfactory etch rates. Surface damage and undercutting are minimized.

Method of inducing differential etch rates in glow discharge produced amorphous silicon

DOEpatents

Staebler, David L.; Zanzucchi, Peter J.

1980-01-01

A method of inducing differential etch rates in glow discharge produced amorphous silicon by heating a portion of the glow discharge produced amorphous silicon to a temperature of about 365.degree. C. higher than the deposition temperature prior to etching. The etch rate of the exposed amorphous silicon is less than the unheated amorphous silicon.

Characteristics of n-GaN after ICP etching

NASA Astrophysics Data System (ADS)

Han, Yanjun; Xue, Song; Guo, Wenping; Hao, Zhi-Biao; Sun, Changzheng; Luo, Yi

2002-09-01

In this work, a systematic study on the plasma-induced damage on n-type GaN by inductively coupled plasma (ICP) etching is presented. After n-contact metal formation and annealing, electrical property is evaluated by the I-V characteristics. Room temperature photoluminescence (PL) measurement of etched GaN surfaces is performed to investigate the etching damage on the optical properties of n-type GaN. Investigation of the effect of additive gas RF chuck power on these characteristics has also been carried out. The better etching conditions have been obtained based on these results.

3D memory: etch is the new litho

NASA Astrophysics Data System (ADS)

Petti, Christopher

2018-03-01

This paper discusses the process challenges and limitations for 3D NAND processes, focusing on vertical 3D architectures. The effect of deep memory hole etches on die cost is calculated, with die cost showing a minimum at a given number of layers because of aspect-ratio dependent etch effects. Techniques to mitigate these etch effects are summarized, as are other etch issues, such as bowing and twisting. Metal replacement gate processes and their challenges are also described. Lastly, future directions of vertical 3D NAND technologies are explored.

Incident angle dependence of proton response of CR-39 (TS-16) track detector

NASA Technical Reports Server (NTRS)

Oda, K.; Csige, I.; Yamauchi, T.; Miyake, H.; Benton, E. V.

1993-01-01

The proton response of the TS-16 type of CR-39 plastic nuclear track detector has been studied with accelerated and fast neutron induced protons in vacuum and in air. The diameters of etched tracks were measured as a function of etching time and the etch rate ratio and the etch induction layer were determined from the growth curve of the diameter using a variable etch rate ratio model. In the case of the accelerated protons in vacuum an anomalous incident angle dependence of the response is observed.

Etching Behavior of Aluminum Alloy Extrusions

NASA Astrophysics Data System (ADS)

Zhu, Hanliang

2014-11-01

The etching treatment is an important process step in influencing the surface quality of anodized aluminum alloy extrusions. The aim of etching is to produce a homogeneously matte surface. However, in the etching process, further surface imperfections can be generated on the extrusion surface due to uneven materials loss from different microstructural components. These surface imperfections formed prior to anodizing can significantly influence the surface quality of the final anodized extrusion products. In this article, various factors that influence the materials loss during alkaline etching of aluminum alloy extrusions are investigated. The influencing variables considered include etching process parameters, Fe-rich particles, Mg-Si precipitates, and extrusion profiles. This study provides a basis for improving the surface quality in industrial extrusion products by optimizing various process parameters.

Ion beam sputtering of fluoropolymers

NASA Technical Reports Server (NTRS)

Sovey, J. S.

1978-01-01

Etching and deposition of fluoropolymers are of considerable industrial interest for applications dealing with adhesion, chemical inertness, hydrophobicity, and dielectric properties. This paper describes ion beam sputter processing rates as well as pertinent characteristics of etched targets and films. An argon ion beam source was used to sputter etch and deposit the fluoropolymers PTFE, FEP, and CTFE. Ion beam energy, current density, and target temperature were varied to examine effects on etch and deposition rates. The ion etched fluoropolymers yield cone or spire-like surface structures which vary depending upon the type of polymer, ion beam power density, etch time, and target temperature. Also presented are sputter target and film characteristics which were documented by spectral transmittance measurements, X-ray diffraction, ESCA, and SEM photomicrographs.

Determination of Etch Rate Behavior of 4H-SiC Using Chlorine Trifluoride Gas

NASA Astrophysics Data System (ADS)

Miura, Yutaka; Habuka, Hitoshi; Katsumi, Yusuke; Oda, Satoko; Fukai, Yasushi; Fukae, Katsuya; Kato, Tomohisa; Okumura, Hajime; Arai, Kazuo

2007-12-01

The etch rate of single-crystalline 4H-SiC is studied using chlorine trifluoride gas at 673-973 K and atmospheric pressure in a cold wall horizontal reactor. The 4H-SiC etch rate can be higher than 10 μm/min at substrate temperatures higher than 723 K. The etch rate increases with the chlorine trifluoride gas flow rate. The etch rate is calculated by taking into account the transport phenomena in the reactor including the chemical reaction at the substrate surface. The flat etch rate at the higher substrate temperatures is caused mainly by the relationship between the transport rate and the surface chemical reaction rate of chlorine trifluoride gas.

More vertical etch profile using a Faraday cage in plasma etching

NASA Astrophysics Data System (ADS)

Cho, Byeong-Ok; Hwang, Sung-Wook; Ryu, Jung-Hyun; Moon, Sang Heup

1999-05-01

Scanning electron microscope images of sidewalls obtained by plasma etching of an SiO2 film with and without a Faraday cage have been compared. When the substrate film is etched in the Faraday cage, faceting is effectively suppressed and the etch profile becomes more vertical regardless of the process conditions. This is because the electric potential in the cage is nearly uniform and therefore distortion of the electric field at the convex corner of a microfeature is prevented. The most vertical etch profile is obtained when the cage is used in fluorocarbon plasmas, where faceting is further suppressed due to the decrease in the chemical sputtering yield and the increase in the radical/ion flux on the substrate.

Note: Dissolved hydrogen detection in power transformer oil based on chemically etched fiber Bragg grating.

PubMed

Jiang, Jun; Ma, Guo-ming; Song, Hong-tu; Zhou, Hong-yang; Li, Cheng-rong; Luo, Ying-ting; Wang, Hong-bin

2015-10-01

A fiber Bragg grating (FBG) sensor based on chemically etched cladding to detect dissolved hydrogen is proposed and studied in this paper. Low hydrogen concentration tests have been carried out in mixed gases and transformer oil to investigate the repeatability and sensitivity. Moreover, to estimate the influence of etched cladding thickness, a physical model of FBG-based hydrogen sensor is analyzed. Experimental results prove that thin cladding chemically etched by HF acid solution improves the response to hydrogen detection in oil effectively. At last, the sensitivity of FBG sensor chemically etched 16 μm could be as high as 0.060 pm/(μl/l), increased by more than 30% in comparison to un-etched FBG.

Graphene nanoribbons: Relevance of etching process

DOE Office of Scientific and Technical Information (OSTI.GOV)

Simonet, P., E-mail: psimonet@phys.ethz.ch; Bischoff, D.; Moser, A.

2015-05-14

Most graphene nanoribbons in the experimental literature are patterned using plasma etching. Various etching processes induce different types of defects and do not necessarily result in the same electronic and structural ribbon properties. This study focuses on two frequently used etching techniques, namely, O{sub 2} plasma ashing and O{sub 2 }+ Ar reactive ion etching (RIE). O{sub 2} plasma ashing represents an alternative to RIE physical etching for sensitive substrates, as it is a more gentle chemical process. We find that plasma ashing creates defective graphene in the exposed trenches, resulting in instabilities in the ribbon transport. These are probably caused bymore » more or larger localized states at the edges of the ashed device compared to the RIE defined device.« less

Composition/bandgap selective dry photochemical etching of semiconductor materials

DOEpatents

Ashby, Carol I. H.; Dishman, James L.

1987-01-01

A method of selectively photochemically dry etching a first semiconductor material of a given composition and direct bandgap Eg.sub.1 in the presence of a second semiconductor material of a different composition and direct bandgap Eg.sub.2, wherein Eg.sub.2 >Eg.sub.1, said second semiconductor material substantially not being etched during said method, comprises subjecting both materials to the same photon flux and to the same gaseous etchant under conditions where said etchant would be ineffective for chemical etching of either material were the photons not present, said photons being of an energy greater than Eg.sub.1 but less than Eg.sub.2, whereby said first semiconductor material is photochemically etched and said second material is substantially not etched.

Influence of duration of phosphoric acid pre-etching on bond durability of universal adhesives and surface free-energy characteristics of enamel.

PubMed

Tsujimoto, Akimasa; Barkmeier, Wayne W; Takamizawa, Toshiki; Watanabe, Hidehiko; Johnson, William W; Latta, Mark A; Miyazaki, Masashi

2016-08-01

The purpose of this study was to evaluate the influence of duration of phosphoric acid pre-etching on the bond durability of universal adhesives and the surface free-energy characteristics of enamel. Three universal adhesives and extracted human molars were used. Two no-pre-etching groups were prepared: ground enamel; and enamel after ultrasonic cleaning with distilled water for 30 s to remove the smear layer. Four pre-etching groups were prepared: enamel pre-etched with phosphoric acid for 3, 5, 10, and 15 s. Shear bond strength (SBS) values of universal adhesive after no thermal cycling and after 30,000 or 60,000 thermal cycles, and surface free-energy values of enamel surfaces, calculated from contact angle measurements, were determined. The specimens that had been pre-etched showed significantly higher SBS and surface free-energy values than the specimens that had not been pre-etched, regardless of the aging condition and adhesive type. The SBS and surface free-energy values did not increase for pre-etching times of longer than 3 s. There were no significant differences in SBS values and surface free-energy characteristics between the specimens with and without a smear layer. The results of this study suggest that phosphoric acid pre-etching of enamel improves the bond durability of universal adhesives and the surface free-energy characteristics of enamel, but these bonding properties do not increase for phosphoric acid pre-etching times of longer than 3 s. © 2016 Eur J Oral Sci.

Dynamic secondary ion mass spectroscopy of Au nanoparticles on Si wafer using Bi3+ as primary ion coupled with surface etching by Ar cluster ion beam: The effect of etching conditions on surface structure

NASA Astrophysics Data System (ADS)

Park, Eun Ji; Choi, Chang Min; Kim, Il Hee; Kim, Jung-Hwan; Lee, Gaehang; Jin, Jong Sung; Ganteför, Gerd; Kim, Young Dok; Choi, Myoung Choul

2018-01-01

Wet-chemically synthesized Au nanoparticles were deposited on Si wafer surfaces, and the secondary ions mass spectra (SIMS) from these samples were collected using Bi3+ with an energy of 30 keV as the primary ions. In the SIMS, Au cluster cations with a well-known, even-odd alteration pattern in the signal intensity were observed. We also performed depth profile SIMS analyses, i.e., etching the surface using an Ar gas cluster ion beam (GCIB), and a subsequent Bi3+ SIMS analysis was repetitively performed. Here, two different etching conditions (Ar1600 clusters of 10 keV energy or Ar1000 of 2.5 keV denoted as "harsh" or "soft" etching conditions, respectively) were used. Etching under harsh conditions induced emission of the Au-Si binary cluster cations in the SIMS spectra of the Bi3+ primary ions. The formation of binary cluster cations can be induced by either fragmentation of Au nanoparticles or alloying of Au and Si, increasing Au-Si coordination on the sample surface during harsh GCIB etching. Alternatively, use of the soft GCIB etching conditions resulted in exclusive emission of pure Au cluster cations with nearly no Au-Si cluster cation formation. Depth profile analyses of the Bi3+ SIMS combined with soft GCIB etching can be useful for studying the chemical environments of atoms at the surface without altering the original interface structure during etching.

Effect of clearfil protect bond and transbond plus self-etch primer on shear bond strength of orthodontic brackets

PubMed Central

Raji, S. Hamid; Ghorbanipour, Reza; Majdzade, Fateme

2011-01-01

Background: The aim of this study was to evaluate the shear bond strength of an antimicrobial and fluoride-releasing self-etch primer (clearfil protect bond) and compare it with transbond plus self-etch primer and conventional acid etching and priming system. Materials and Methods: Forty-eight extracted human premolars were divided randomly to three groups. In group 1, the teeth were bonded with conventional acid etching and priming method. In group 2, the teeth were bonded with clearfil protect bond self-etch primer, and transbond plus self-etch primer was used to bond the teeth in group 3. The samples were stored in 37°C distilled water and thermocycled. Then, the SBS of the sample was evaluated with Zwick testing machine. Descriptive statistics and the analysis of variances (ANOVA) and Tukey's test and Kruskal-Wallis were used to analyze the data. Results: The results of the ANOVA showed that the mean of group 3 was significantly lower than that of other groups. Most of the sample showed a pattern of failure within the adhesive resin. Conclusion: The shear bond strength of clearfil protect bond and transbond plus self-etch primer was enough for bonding the orthodontic brackets. The mode of failure of bonded brackets with these two self-etch primers is safe for enamel. PMID:23372605

Microtensile bond strength of silorane-based composite specific adhesive system using different bonding strategies

PubMed Central

Bastos, Laura Alves; Sousa, Ana Beatriz Silva; Drubi-Filho, Brahim; Panzeri Pires-de-Souza, Fernanda de Carvalho

2015-01-01

Objectives The aim of this study was to evaluate the effect of pre-etching on the bond strength of silorane-based composite specific adhesive system to dentin. Materials and Methods Thirty human molars were randomly divided into 5 groups according to the different bonding strategies. For teeth restored with silorane-based composite (Filtek Silorane, 3M ESPE), the specific self-etching adhesive system (Adhesive System P90, 3M ESPE) was used with and without pre-etching (Pre-etching/Silorane and Silorane groups). Teeth restored with methacrylate based-composite (Filtek Z250, 3M ESPE) were hybridized with the two-step self-etching system (Clearfil SE Bond, Kuraray), with and without pre-etching (Pre-etching/Methacrylate and Methacrylate groups), or three-step adhesive system (Adper Scotchbond Multi-Purpose, 3M ESPE) (Three-step/Methacrylate group) (n = 6). The restored teeth were sectioned into stick-shaped test specimens (1.0 × 1.0 mm), and coupled to a universal test machine (0.5 mm/min) to perform microtensile testing. Results Pre-etching/Methacrylate group presented the highest bond strength values, with significant difference from Silorane and Three-step/Methacrylate groups (p < 0.05). However, it was not significantly different from Preetching/Silorane and Methacrylate groups. Conclusions Pre-etching increased bond strength of silorane-based composite specific adhesive system to dentin. PMID:25671209

Influence of enamel conditioning on the shear bond strength of different adhesives.

PubMed

Brauchli, Lorenz; Muscillo, Teodoro; Steineck, Markus; Wichelhaus, Andrea

2010-11-01

Phosphoric acid etching is the gold standard for enamel conditioning. However, it is possible that air abrasion or a combination of air abrasion and etching might result in enhanced adhesion. The aim of this study was to investigate the effect of different enamel conditioning methods on the bond strength of six adhesives. Three different enamel conditioning procedures (phosphoric acid etching, air abrasion, air abrasion + phosphoric acid etching) were evaluated for their influence on the shear bond strength of six different adhesives (Transbond™ XT, Cool-Bond™, Fuji Ortho LC, Ultra Band-Lok, Tetric(®) Flow, Light-Bond™). Each group consisted of 15 specimens. Shear forces were measured with a universal testing machine. The scores of the Adhesive Remnant Index (ARI) were also analyzed. There were no significant differences between phosphoric acid etching and air abrasion + phosphoric acid etching. Air abrasion as a single conditioning technique led to significantly lower shear forces. The ARI scores did not correlate with the shear strengths measured. There were greater variations in shear forces for the different adhesives than for the conditioning techniques. The highest shear forces were found for the conventional composites Transbond™ XT and Cool- Bond™ in combination with conventional etching. Air abrasion alone and in combination with phosphoric acid etching showed no advantages compared with phosphoric acid etching alone and, therefore, cannot be recommended.

Method to fabricate multi-level silicon-based microstructures via use of an etching delay layer

DOEpatents

Manginell, Ronald P.; Schubert, W. Kent; Shul, Randy J.

2005-08-16

New methods for fabrication of silicon microstructures have been developed. In these methods, an etching delay layer is deposited and patterned so as to provide differential control on the depth of features being etched into a substrate material. Structures having features with different depth can be formed thereby in a single etching step.

High-uniformity centimeter-wide Si etching method for MEMS devices with large opening elements

NASA Astrophysics Data System (ADS)

Okamoto, Yuki; Tohyama, Yukiya; Inagaki, Shunsuke; Takiguchi, Mikio; Ono, Tomoki; Lebrasseur, Eric; Mita, Yoshio

2018-04-01

We propose a compensated mesh pattern filling method to achieve highly uniform wafer depth etching (over hundreds of microns) with a large-area opening (over centimeter). The mesh opening diameter is gradually changed between the center and the edge of a large etching area. Using such a design, the etching depth distribution depending on sidewall distance (known as the local loading effect) inversely compensates for the over-centimeter-scale etching depth distribution, known as the global or within-die(chip)-scale loading effect. Only a single DRIE with test structure patterns provides a micro-electromechanical systems (MEMS) designer with the etched depth dependence on the mesh opening size as well as on the distance from the chip edge, and the designer only has to set the opening size so as to obtain a uniform etching depth over the entire chip. This method is useful when process optimization cannot be performed, such as in the cases of using standard conditions for a foundry service and of short turn-around-time prototyping. To demonstrate, a large MEMS mirror that needed over 1 cm2 of backside etching was successfully fabricated using as-is-provided DRIE conditions.

Characterization of the high density plasma etching process of CCTO thin films for the fabrication of very high density capacitors

NASA Astrophysics Data System (ADS)

Altamore, C.; Tringali, C.; Sparta', N.; Di Marco, S.; Grasso, A.; Ravesi, S.

2010-02-01

In this work the feasibility of CCTO (Calcium Copper Titanate) patterning by etching process is demonstrated and fully characterized in a hard to etch materials etcher. CCTO sintered in powder shows a giant relative dielectric constant (105) measured at 1 MHz at room temperature. This feature is furthermore coupled with stability from 101 Hz to 106 Hz in a wide temperature range (100K - 600K). In principle, this property can allow to fabricate very high capacitance density condenser. Due to its perovskite multi-component structure, CCTO can be considered a hard to etch material. For high density capacitor fabrication, CCTO anisotropic etching is requested by using high density plasma. The behavior of etched CCTO was studied in a HRe- (High Density Reflected electron) plasma etcher using Cl2/Ar chemistry. The relationship between the etch rate and the Cl2/Ar ratio was also studied. The effects of RF MHz, KHz Power and pressure variation, the impact of HBr addiction to the Cl2/Ar chemistry on the CCTO etch rate and on its selectivity to Pt and photo resist was investigated.

Scalloping minimization in deep Si etching on Unaxis DSE tools

NASA Astrophysics Data System (ADS)

Lai, Shouliang; Johnson, Dave J.; Westerman, Russ J.; Nolan, John J.; Purser, David; Devre, Mike

2003-01-01

Sidewall smoothness is often a critical requirement for many MEMS devices, such as microfludic devices, chemical, biological and optical transducers, while fast silicon etch rate is another. For such applications, the time division multiplex (TDM) etch processes, so-called "Bosch" processes are widely employed. However, in the conventional TDM processes, rough sidewalls result due to scallop formation. To date, the amplitude of the scalloping has been directly linked to the silicon etch rate. At Unaxis USA Inc., we have developed a proprietary fast gas switching technique that is effective for scalloping minimization in deep silicon etching processes. In this technique, process cycle times can be reduced from several seconds to as little as a fraction of second. Scallop amplitudes can be reduced with shorter process cycles. More importantly, as the scallop amplitude is progressively reduced, the silicon etch rate can be maintained relatively constant at high values. An optimized experiment has shown that at etch rate in excess of 7 μm/min, scallops with length of 116 nm and depth of 35 nm were obtained. The fast gas switching approach offers an ideal manufacturing solution for MEMS applications where extremely smooth sidewall and fast etch rate are crucial.

Submicron patterned metal hole etching

DOEpatents

McCarthy, Anthony M.; Contolini, Robert J.; Liberman, Vladimir; Morse, Jeffrey

2000-01-01

A wet chemical process for etching submicron patterned holes in thin metal layers using electrochemical etching with the aid of a wetting agent. In this process, the processed wafer to be etched is immersed in a wetting agent, such as methanol, for a few seconds prior to inserting the processed wafer into an electrochemical etching setup, with the wafer maintained horizontal during transfer to maintain a film of methanol covering the patterned areas. The electrochemical etching setup includes a tube which seals the edges of the wafer preventing loss of the methanol. An electrolyte composed of 4:1 water: sulfuric is poured into the tube and the electrolyte replaces the wetting agent in the patterned holes. A working electrode is attached to a metal layer of the wafer, with reference and counter electrodes inserted in the electrolyte with all electrodes connected to a potentiostat. A single pulse on the counter electrode, such as a 100 ms pulse at +10.2 volts, is used to excite the electrochemical circuit and perform the etch. The process produces uniform etching of the patterned holes in the metal layers, such as chromium and molybdenum of the wafer without adversely effecting the patterned mask.

Dopant type and/or concentration selective dry photochemical etching of semiconductor materials

DOEpatents

Ashby, Carol I. H.; Dishman, James L.

1987-01-01

A method of selectively photochemically dry etching a first semiconductor material of a given composition in the presence of a second semiconductor material which is of a composition different from said first material, said second material substantially not being etched during said method, comprises subjecting both materials to the same photon flux of an energy greater than their respective direct bandgaps and to the same gaseous chemical etchant under conditions where said etchant would be ineffective for chemical etching of either material were the photons not present, said conditions also being such that the resultant electronic structure of the first semiconductor material under said photon flux is sufficient for the first material to undergo substantial photochemical etching under said conditions and being such that the resultant electronic structure of the second semiconductor material under said photon flux is not sufficient for the second material to undergo substantial photochemical etching under said conditions. In a preferred mode, the materials are subjected to a bias voltage which suppresses etching in n- or p- type material but not in p- or n-type material, respectively; or suppresses etching in the more heavily doped of two n-type or two p-type materials.

Dopant type and/or concentration selective dry photochemical etching of semiconductor materials

DOEpatents

Ashby, C.R.H.; Dishman, J.L.

1985-10-11

Disclosed is a method of selectively photochemically dry etching a first semiconductor material of a given composition in the presence of a second semiconductor material which is of a composition different from said first material, said second material substantially not being etched during said method. The method comprises subjecting both materials to the same photon flux of an energy greater than their respective direct bandgaps and to the same gaseous chemical etchant under conditions where said etchant would be ineffective for chemical etching of either material were the photons not present, said conditions also being such that the resultant electronic structure of the first semiconductor material under said photon flux is sufficient for the first material to undergo substantial photochemical etching under said conditions and being such that the resultant electronic structure of the second semiconductor material under said photon flux is not sufficient for the second material to undergo substantial photochemical etching under said conditions. In a preferred mode, the materials are subjected to a bias voltage which suppresses etching in n- or p-type material but not in p- or n-type material, respectively; or suppresses etching in the more heavily doped of two n-type or two p-type materials.

Use of hydrogen etching to remove existing dislocations in GaN epitaxial layers

NASA Astrophysics Data System (ADS)

Yeh, Yen-Hsien; Chu, Chung-Ming; Wu, Yin-Hao; Hsu, Ying-Chia; Yu, Tzu-Yi; Lee, Wei-I.

2015-08-01

In this paper, based on the anisotropic nature of hydrogen (H2) etching on GaN, we describe a new approach to the removal of threading dislocations in GaN layers. The top surfaces of c-plane (Ga-face) and a-plane GaNs are considered stable in H2; therefore, H2 etches only crystal imperfections such as dislocation and basal plane stacking fault (BSF) sites. We used H2 to etch undoped c-plane GaN, n-type c-plane GaN, a-plane GaN, and an InGaN/GaN multiple quantum well structure. Several examinations were performed, indicating deep cavities on the c-plane GaN samples after H2 etching; furthermore, gorge-like grooves were observed on the a-plane GaN samples. The deep cavities on the c-plane GaN were considered the etched dislocation sites, and the gorge-like grooves on the a-plane GaN were considered the etched BSF sites. Photoluminescence measurements were performed and the results indicated that the H2-etched samples demonstrate superior optoelectronic properties, probably because of the elimination of dislocations.

Extreme wettability of nanostructured glass fabricated by non-lithographic, anisotropic etching

PubMed Central

Yu, Eusun; Kim, Seul-Cham; Lee, Heon Ju; Oh, Kyu Hwan; Moon, Myoung-Woon

2015-01-01

Functional glass surfaces with the properties of superhydrophobicity/or superhydrohydrophilicity, anti-condensation or low reflectance require nano- or micro-scale roughness, which is difficult to fabricate directly on glass surfaces. Here, we report a novel non-lithographic method for the fabrication of nanostructures on glass; this method introduces a sacrificial SiO2 layer for anisotropic plasma etching. The first step was to form nanopillars on SiO2 layer-coated glass by using preferential CF4 plasma etching. With continuous plasma etching, the SiO2 pillars become etch-resistant masks on the glass; thus, the glass regions covered by the SiO2 pillars are etched slowly, and the regions with no SiO2 pillars are etched rapidly, resulting in nanopatterned glass. The glass surface that is etched with CF4 plasma becomes superhydrophilic because of its high surface energy, as well as its nano-scale roughness and high aspect ratio. Upon applying a subsequent hydrophobic coating to the nanostructured glass, a superhydrophobic surface was achieved. The light transmission of the glass was relatively unaffected by the nanostructures, whereas the reflectance was significantly reduced by the increase in nanopattern roughness on the glass. PMID:25791414

The effect of reactive ion etch (RIE) process conditions on ReRAM device performance

NASA Astrophysics Data System (ADS)

Beckmann, K.; Holt, J.; Olin-Ammentorp, W.; Alamgir, Z.; Van Nostrand, J.; Cady, N. C.

2017-09-01

The recent surge of research on resistive random access memory (ReRAM) devices has resulted in a wealth of different materials and fabrication approaches. In this work, we describe the performance implications of utilizing a reactive ion etch (RIE) based process to fabricate HfO2 based ReRAM devices, versus a more unconventional shadow mask fabrication approach. The work is the result of an effort to increase device yield and reduce individual device size. Our results show that choice of RIE etch gas (SF6 versus CF4) is critical for defining the post-etch device profile (cross-section), and for tuning the removal of metal layers used as bottom electrodes in the ReRAM device stack. We have shown that etch conditions leading to a tapered profile for the device stack cause poor electrical performance, likely due to metal re-deposition during etching, and damage to the switching layer. These devices exhibit nonlinear I-V during the low resistive state, but this could be improved to linear behavior once a near-vertical etch profile was achieved. Device stacks with vertical etch profiles also showed an increase in forming voltage, reduced switching variability and increased endurance.

Dry etch challenges for CD shrinkage in memory process

NASA Astrophysics Data System (ADS)

Matsushita, Takaya; Matsumoto, Takanori; Mukai, Hidefumi; Kyoh, Suigen; Hashimoto, Kohji

2015-03-01

Line pattern collapse attracts attention as a new problem of the L&S formation in sub-20nm H.P feature. Line pattern collapse that occurs in a slight non-uniformity of adjacent CD (Critical dimension) space using double patterning process has been studied with focus on micro-loading effect in Si etching. Bias RF pulsing plasma etching process using low duty cycle helped increase of selectivity Si to SiO2. In addition to the effect of Bias RF pulsing process, the thin mask obtained from improvement of selectivity has greatly suppressed micro-loading in Si etching. However it was found that micro-loading effect worsen again in sub-20nm space width. It has been confirmed that by using cycle etch process to remove deposition with CFx based etching micro-loading effect could be suppressed. Finally, Si etching process condition using combination of results above could provide finer line and space without "line pattern collapse" in sub-20nm.

Morphological Study on Porous Silicon Carbide Membrane Fabricated by Double-Step Electrochemical Etching

NASA Astrophysics Data System (ADS)

Omiya, Takuma; Tanaka, Akira; Shimomura, Masaru

2012-07-01

The structure of porous silicon carbide membranes that peeled off spontaneously during electrochemical etching was studied. They were fabricated from n-type 6H SiC(0001) wafers by a double-step electrochemical etching process in a hydrofluoric electrolyte. Nanoporous membranes were obtained after double-step etching with current densities of 10-20 and 60-100 mA/cm2 in the first and second steps, respectively. Microporous membranes were also fabricated after double-step etching with current densities of 100 and 200 mA/cm2. It was found that the pore diameter is influenced by the etching current in step 1, and that a higher current is required in step 2 when the current in step 1 is increased. During the etching processes in steps 1 and 2, vertical nanopore and lateral crack formations proceed, respectively. The influx pathway of hydrofluoric solution, expansion of generated gases, and transfer limitation of positive holes to the pore surface are the key factors in the peeling-off mechanism of the membrane.

Effects of gas flow rate on the etch characteristics of a low- k sicoh film with an amorphous carbon mask in dual-frequency CF4/C4F8/Ar capacitively-coupled plasmas

NASA Astrophysics Data System (ADS)

Kwon, Bong-Soo; Lee, Hea-Lim; Lee, Nae-Eung; Kim, Chang-Young; Choi, Chi Kyu

2013-01-01

Highly selective nanoscale etching of a low-dielectric constant (low- k) organosilicate (SiCOH) layer using a mask pattern of chemical-vapor-deposited (CVD) amorphous carbon layer (ACL) was carried out in CF4/C4F8/Ar dual-frequency superimposed capacitively-coupled plasmas. The etching characteristics of the SiCOH layers, such as the etch rate, etch selectivity, critical dimension (CD), and line edge roughness (LER) during the plasma etching, were investigated by varying the C4F8 flow rate. The C4F8 gas flow rate primarily was found to control the degree of polymerization and to cause variations in the selectivity, CD and LER of the patterned SiCOH layer. Process windows for ultra-high etch selectivity of the SiCOH layer to the CVD ACL are formed due to the disproportionate degrees of polymerization on the SiCOH and the ACL surfaces.

Etching Characteristics of VO2 Thin Films Using Inductively Coupled Cl2/Ar Plasma

NASA Astrophysics Data System (ADS)

Ham, Yong-Hyun; Efremov, Alexander; Min, Nam-Ki; Lee, Hyun Woo; Yun, Sun Jin; Kwon, Kwang-Ho

2009-08-01

A study on both etching characteristics and mechanism of VO2 thin films in the Cl2/Ar inductively coupled plasma was carried. The variable parameters were gas pressure (4-10 mTorr) and input power (400-700 W) at fixed bias power of 150 W and initial mixture composition of 25% Cl2 + 75% Ar. It was found that an increase in both gas pressure and input power results in increasing VO2 etch rate while the etch selectivity over photoresist keeps a near to constant values. Plasma diagnostics by Langmuir probes and zero-dimensional plasma model provided the data on plasma parameters, steady-state densities and fluxes of active species on the etched surface. The model-based analysis of the etch mechanism showed that, for the given ranges of operating conditions, the VO2 etch kinetics corresponds to the transitional regime of ion-assisted chemical reaction and is influenced by both neutral and ion fluxes with a higher sensitivity to the neutral flux.

A junction-level optoelectronic characterization of etching-induced damage for third-generation HgCdTe infrared focal-plane array photodetectors

NASA Astrophysics Data System (ADS)

Wang, Peng; Wang, Yueming; Wu, Mingzai; Ye, Zhenhua

2018-06-01

Third-generation HgCdTe-based infrared focal plane arrays require high aspect ratio trenches with admissible etch induced damage at the surface and sidewalls for effectively isolating the pixels. In this paper, the high-density inductively coupled plasma enhanced reaction ion etching technique has been used for micro-mesa delineation of HgCdTe for third-generation infrared focal-plane array detectors. A nondestructive junction-level optoelectronic characterization method called laser beam induced current (LBIC) is used to evaluate the lateral junction extent of HgCdTe etch-induced damage scanning electron microscopy. It is found that the LBIC profiles exhibit evident double peaks and valleys phenomena. The lateral extent of etch induced mesa damage of ∼2.4 μm is obtained by comparing the LBIC profile and the scanning electron microscopy image of etched sample. This finding will guide us to nondestructively identify the distributions of the etching damages in large scale HgCdTe micro-mesa.

Barium-strontium-titanate etching characteristics in chlorinated discharges

NASA Astrophysics Data System (ADS)

Stafford, Luc; Margot, Joëlle; Langlois, Olivier; Chaker, Mohamed

2003-07-01

The etching characteristics of barium-strontium-titanate (BST) were investigated using a high-density plasma sustained by surface waves at 190 MHz in Ar/Cl2 gas mixtures. The etch rate was examined as a function of both the total gas pressure and the Cl2 fraction in Ar/Cl2 using a wafer temperature of 10 °C. The results were correlated to positive ion density and plasma composition obtained from Langmuir probes and mass spectrometry. The BST etch rate was found to increase linearly with the positive ion density and to decrease with increasing chlorine atom concentration. This result indicates that for the temperature conditions used, the interaction between chlorine and BST yields compounds having a volatility that is lower than the original material. As a consequence, the contribution of neutral atomic Cl atoms to the etch mechanism is detrimental, thereby reducing the etch rate. As the wafer temperature increases, the role of chemistry in the etching process is enhanced.

Anisotropic selective etching between SiGe and Si

NASA Astrophysics Data System (ADS)

Ishii, Yohei; Scott-McCabe, Ritchie; Yu, Alex; Okuma, Kazumasa; Maeda, Kenji; Sebastian, Joseph; Manos, Jim

2018-06-01

In Si/SiGe dual-channel FinFETs, it is necessary to simultaneously control the etched amounts of SiGe and Si. However, the SiGe etch rate is higher than the Si etch rate in not only halogen plasmas but also physical sputtering. In this study, we found that hydrogen plasma selectively etches Si over SiGe. The result shows that the selectivity of Si over SiGe can be up to 38 with increasing Ge concentration in SiGe. Attenuated total reflectance Fourier transform infrared spectroscopy (ATR-FTIR) results indicate that hydrogen selectively bonds with Si rather than with Ge in SiGe. During the etching, hydrogen-induced Si surface segregation is also observed. It is also observed that the difference in etched amount between SiGe and Si can be controlled from positive to negative values even in Si/SiGe dual-channel fin patterning while maintaining the vertical profiles. Furthermore, no plasma-induced lattice damage was observed by transmission electron microscopy for both Si and SiGe fin sidewalls.

Composition/bandgap selective dry photochemical etching of semiconductor materials

DOEpatents

Ashby, C.I.H.; Dishman, J.L.

1985-10-11

Disclosed is a method of selectively photochemically dry etching a first semiconductor material of a given composition and direct bandgap Eg/sub 1/ in the presence of a second semiconductor material of a different composition and direct bandgap Eg/sub 2/, wherein Eg/sub 2/ > Eg/sub 1/, said second semiconductor material substantially not being etched during said method. The method comprises subjecting both materials to the same photon flux and to the same gaseous etchant under conditions where said etchant would be ineffective for chemical etching of either material were the photons not present, said photons being of an energy greater than Eg/sub 1/ but less than Eg/sub 2/, whereby said first semiconductor material is photochemically etched and said second material is substantially not etched.

TrackEtching - A Java based code for etched track profile calculations in SSNTDs

NASA Astrophysics Data System (ADS)

Muraleedhara Varier, K.; Sankar, V.; Gangadathan, M. P.

2017-09-01

A java code incorporating a user friendly GUI has been developed to calculate the parameters of chemically etched track profiles of ion-irradiated solid state nuclear track detectors. Huygen's construction of wavefronts based on secondary wavelets has been used to numerically calculate the etched track profile as a function of the etching time. Provision for normal incidence and oblique incidence on the detector surface has been incorporated. Results in typical cases are presented and compared with experimental data. Different expressions for the variation of track etch rate as a function of the ion energy have been utilized. The best set of values of the parameters in the expressions can be obtained by comparing with available experimental data. Critical angle for track development can also be calculated using the present code.

Improving contact layer patterning using SEM contour based etch model

NASA Astrophysics Data System (ADS)

Weisbuch, François; Lutich, Andrey; Schatz, Jirka; Hertzsch, Tino; Moll, Hans-Peter

2016-10-01

The patterning of the contact layer is modulated by strong etch effects that are highly dependent on the geometry of the contacts. Such litho-etch biases need to be corrected to ensure a good pattern fidelity. But aggressive designs contain complex shapes that can hardly be compensated with etch bias table and are difficult to characterize with standard CD metrology. In this work we propose to implement a model based etch compensation method able to deal with any contact configuration. With the help of SEM contours, it was possible to get reliable 2D measurements particularly helpful to calibrate the etch model. The selections of calibration structures was optimized in combination with model form to achieve an overall errRMS of 3nm allowing the implementation of the model in production.

Differentiation of grain orientation with corrosive and colour etching on a granular bainitic steel.

PubMed

Reisinger, S; Ressel, G; Eck, S; Marsoner, S

2017-08-01

This study presents a detailed verification of the etching methods with Nital and Klemm on a granular bainitic steel. It is shown that both methods allow the identification of the crystal orientation, whereas Klemm etching enables also a quantification of the apparent phases, as also retained austenite can be distinguished from the other bainitic microstructures. A combination of atom probe tomography with electron-back-scattered-diffraction showed that both etching methods emphasize the bainitic {100} crystal orientation. However, a cross-section produced by focused ion beam evidenced that Klemm etching leads to the formation of a topography of the different oriented bainitic crystals that directly affects the thickness and therefore the apparent colour of the deposited layer formed during etching. Copyright © 2017 Elsevier Ltd. All rights reserved.

The endpoint detection technique for deep submicrometer plasma etching

NASA Astrophysics Data System (ADS)

Wang, Wei; Du, Zhi-yun; Zeng, Yong; Lan, Zhong-went

2009-07-01

The availability of reliable optical sensor technology provides opportunities to better characterize and control plasma etching processes in real time, they could play a important role in endpoint detection, fault diagnostics and processes feedback control and so on. The optical emission spectroscopy (OES) method becomes deficient in the case of deep submicrometer gate etching. In the newly developed high density inductively coupled plasma (HD-ICP) etching system, Interferometry endpoint (IEP) is introduced to get the EPD. The IEP fringe count algorithm is investigated to predict the end point, and then its signal is used to control etching rate and to call end point with OES signal in over etching (OE) processes step. The experiment results show that IEP together with OES provide extra process control margin for advanced device with thinner gate oxide.

Effects of a power and photon energy of incident light on near-field etching properties

NASA Astrophysics Data System (ADS)

Yatsui, T.; Saito, H.; Nishioka, K.; Leuschel, B.; Soppera, O.; Nobusada, K.

2017-12-01

We developed a near-field etching technique for realizing an ultra-flat surfaces of various materials and structures. To elucidate the near-field etching properties, we have investigated the effects of power and the photon energy of the incident light. First, we established theoretically that an optical near-field with photon energy lower than the absorption edge of the molecules can induce molecular vibrations. We used nanodiamonds to study the power dependence of the near-field etching properties. From the topological changes of the nanodiamonds, we confirmed the linear-dependence of the etching volume with the incident power. Furthermore, we studied the photon energy dependence using TiO2 nanostriped structures, which revealed that a lower photon energy results in a lower etching rate.

Microfabricated Cantilevers Based on Sputtered Thin-Film Ni50Ti50 Shape Memory Alloy (SMA)

DTIC Science & Technology

2015-08-01

surface coating developed during the NiTi deposition or anneal that is relatively resistant to the wet etch. Fig. 2 SEMs after the NiTi wet -etch...SEMs of NiTi devices after the 600 °C anneal , wet -etch patterning of the NiTi. A 120-nm Au capping layer was also sputtered. Figure 3a shows a 200-nm...Ni50Ti50 Cantilever 2 3. Results and Discussion 3 3.1 Wet -Etch Patterning NiTi 3 3.2 Dry-Etch Release of NiTi Devices 5 3.3 Thermal Actuation of

Effects of etching time on enamel bond strengths.

PubMed

Triolo, P T; Swift, E J; Mudgil, A; Levine, A

1993-12-01

This study evaluated the effects of etching time on bond strengths of composite to enamel. Proximal surfaces of extracted molars were etched with either a conventional etchant (35% phosphoric acid) or one of two dentin/enamel conditioners, 10% maleic acid (Scotchbond Multi-Purpose Etchant), or a solution of oxalic acid, aluminum nitrate, and glycine (Gluma 1 & 2 Conditioner). Each agent was applied for 15, 30, or 60 seconds. Specimens etched with 35% phosphoric acid had the highest mean bond strengths at each etching time. At the manufacturer's recommended application times, the other two agents gave significantly lower shear bond strengths than phosphoric acid.

Process Development for Automated Solar Cell and Module Production. Task 4: Automated Array Assembly

NASA Technical Reports Server (NTRS)

1979-01-01

A baseline sequence for the manufacture of solar cell modules was specified. Starting with silicon wafers, the process goes through damage etching, texture etching, junction formation, plasma edge etch, aluminum back surface field formation, and screen printed metallization to produce finished solar cells. The cells were then series connected on a ribbon and bonded into a finished glass tedlar module. A number of steps required additional developmental effort to verify technical and economic feasibility. These steps include texture etching, plasma edge etch, aluminum back surface field formation, array layup and interconnect, and module edge sealing and framing.

Characterizing fluorocarbon assisted atomic layer etching of Si using cyclic Ar/C4F8 and Ar/CHF3 plasma

NASA Astrophysics Data System (ADS)

Metzler, Dominik; Li, Chen; Engelmann, Sebastian; Bruce, Robert L.; Joseph, Eric A.; Oehrlein, Gottlieb S.

2017-02-01

With the increasing interest in establishing directional etching methods capable of atomic scale resolution for fabricating highly scaled electronic devices, the need for development and characterization of atomic layer etching processes, or generally etch processes with atomic layer precision, is growing. In this work, a flux-controlled cyclic plasma process is used for etching of SiO2 and Si at the Angstrom-level. This is based on steady-state Ar plasma, with periodic, precise injection of a fluorocarbon (FC) precursor (C4F8 and CHF3) and synchronized, plasma-based Ar+ ion bombardment [D. Metzler et al., J. Vac. Sci. Technol., A 32, 020603 (2014) and D. Metzler et al., J. Vac. Sci. Technol., A 34, 01B101 (2016)]. For low energy Ar+ ion bombardment conditions, physical sputter rates are minimized, whereas material can be etched when FC reactants are present at the surface. This cyclic approach offers a large parameter space for process optimization. Etch depth per cycle, removal rates, and self-limitation of removal, along with material dependence of these aspects, were examined as a function of FC surface coverage, ion energy, and etch step length using in situ real time ellipsometry. The deposited FC thickness per cycle is found to have a strong impact on etch depth per cycle of SiO2 and Si but is limited with regard to control over material etching selectivity. Ion energy over the 20-30 eV range strongly impacts material selectivity. The choice of precursor can have a significant impact on the surface chemistry and chemically enhanced etching. CHF3 has a lower FC deposition yield for both SiO2 and Si and also exhibits a strong substrate dependence of FC deposition yield, in contrast to C4F8. The thickness of deposited FC layers using CHF3 is found to be greater for Si than for SiO2. X-ray photoelectron spectroscopy was used to study surface chemistry. When thicker FC films of 11 Å are employed, strong changes of FC film chemistry during a cycle are seen whereas the chemical state of the substrate varies much less. On the other hand, for FC film deposition of 5 Å for each cycle, strong substrate surface chemical changes are seen during an etching cycle. The nature of this cyclic etching with periodic deposition of thin FC films differs significantly from conventional etching with steady-state FC layers since surface conditions change strongly throughout each cycle.

Understanding and controlling the step bunching instability in aqueous silicon etching

NASA Astrophysics Data System (ADS)

Bao, Hailing

Chemical etching of silicon has been widely used for more than half a century in the semiconductor industry. It not only forms the basis for current wafer cleaning processes, it also serves as a powerful tool to create a variety of surface morphologies for different applications. Its potential for controlling surface morphology at the atomic scale over micron-size regions is especially appealing. In spite of its wide usage, the chemistry of silicon etching is poorly understood. Many seemingly simple but fundamental questions have not been answered. As a result, the development of new etchants and new etching protocols are based on expensive and tedious trial-and-error experiments. A better understanding of the etching mechanism would direct the rational formulation of new etchants that produce controlled etch morphologies. Particularly, micron-scale step bunches spontaneously develop on the vicinal Si(111) surface etched in KOH or other anisotropic aqueous etchants. The ability to control the size, orientation, density and regularity of these surface features would greatly improve the performance of microelectromechanical devices. This study is directed towards understanding the chemistry and step bunching instability in aqueous anisotropic etching of silicon through a combination of experimental techniques and theoretical simulations. To reveal the cause of step-bunching instability, kinetic Monte Carlo simulations were constructed based on an atomistic model of the silicon lattice and a modified kinematic wave theory. The simulations showed that inhomogeneity was the origin of step-bunching, which was confirmed through STM studies of etch morphologies created under controlled flow conditions. To quantify the size of the inhomogeneities in different etchants and to clarify their effects, a five-parallel-trench pattern was fabricated. This pattern used a nitride mask to protect most regions of the wafer; five evenly spaced etch windows were opened to the Si(110) substrate. Combining data from these etched patterns and surface IR spectra, a modified mechanism, which explained most experimental observations, was proposed. Control of the step-bunching instability was accomplished with a second micromachined etch barrier pattern which consisted of a circular array of seventy-two long, narrow trenches in an etch mask. Using this pattern, well aligned, regularly shaped, evenly-distributed, near-atomically flat terraces in micron size were produced controllably.

Method of fabricating vertically aligned group III-V nanowires

DOEpatents

Wang, George T; Li, Qiming

2014-11-25

A top-down method of fabricating vertically aligned Group III-V micro- and nanowires uses a two-step etch process that adds a selective anisotropic wet etch after an initial plasma etch to remove the dry etch damage while enabling micro/nanowires with straight and smooth faceted sidewalls and controllable diameters independent of pitch. The method enables the fabrication of nanowire lasers, LEDs, and solar cells.

Evaluating the shear bond strength of enamel and dentin with or without etching: A comparative study between dimethacrylate-based and silorane-based adhesives

PubMed Central

Hajizadeh, Hila; Nasseh, Atefeh; Rahmanpour, Naim

2015-01-01

Background Silorane-based composites and their specific self-etch adhesive were introduced to conquest the polymerization shrinkage of methacrylate-based composites. It has been shown that additional etching of enamel and dentin can improve the bond strength of self-etch methacrylate-based adhesives but this claim is not apparent about silorane-based adhesives. Our objective was to compare the shear bond strength (SBS) of enamel and dentin between silorane-based adhesive resin and a methacrylate-based resin with or without additional etching. Material and Methods 40 sound human premolars were prepared and divided into two groups: 1- Filtek P60 composite and Clearfil SE Bond adhesive; 2- Filtek P90 composite and Silorane adhesive. Each group divided into two subgroups: with or without additional etching. For additional etching, 37% acid phosphoric was applied before bonding procedure. A cylinder of the composite was bonded to the surface. After 24 hours storage and 500 thermo cycling between 5-55°C, shear bond strength was assessed with the cross head speed of 0.5 mm/min. Then, bonded surfaces were observed under stereomicroscope to determine the failure mode. Data were analyzed with two-way ANOVA and Fischer exact test. Results Shear bond strength of Filtek P60 composite was significantly higher than Filtek P90 composite both in enamel and dentin surfaces (P<0.05). However, additional etching had no significant effect on shear bond strength in enamel or dentin for each of the composites (P>0.05). There was no interaction between composite type and additional etching (P>0.05). Failure pattern was mainly adhesive and no significant correlation was found between failure and composite type or additional etching (P>0.05). Conclusions Shear bond strength of methacrylate-based composite was significantly higher than silorane-based composite both in enamel and dentin surfaces and additional etching had no significant effect on shear bond strength in enamel or dentin for each of the composites. The mode of failure had no meaningful relation to the type of composite and etching factor. Key words:Shear bond strength, adhesive, composite resin, silorane, methacrylate. PMID:26644830

Selective dry etching of silicon containing anti-reflective coating

NASA Astrophysics Data System (ADS)

Sridhar, Shyam; Nolan, Andrew; Wang, Li; Karakas, Erdinc; Voronin, Sergey; Biolsi, Peter; Ranjan, Alok

2018-03-01

Multi-layer patterning schemes involve the use of Silicon containing Anti-Reflective Coating (SiARC) films for their anti-reflective properties. Patterning transfer completion requires complete and selective removal of SiARC which is very difficult due to its high silicon content (>40%). Typically, SiARC removal is accomplished through a non-selective etch during the pattern transfer process using fluorine containing plasmas, or an ex-situ wet etch process using hydrofluoric acid is employed to remove the residual SiARC, post pattern transfer. Using a non-selective etch may result in profile distortion or wiggling, due to distortion of the underlying organic layer. The drawbacks of using wet etch process for SiARC removal are increased overall processing time and the need for additional equipment. Many applications may involve patterning of active structures in a poly-Si layer with an underlying oxide stopping layer. In such applications, SiARC removal selective to oxide using a wet process may prove futile. Removing SiARC selectively to SiO2 using a dry etch process is also challenging, due to similarity in the nature of chemical bonds (Si - O) in the two materials. In this work, we present highly selective etching of SiARC, in a plasma driven by a surface wave radial line slot antenna. The first step in the process involves an in-situ modification of the SiARC layer in O2 plasma followed by selective etching in a NF3/H2 plasma. Surface treatment in O2 plasma resulted in enhanced etching of the SiARC layer. For the right processing conditions, in-situ NF3/H2 dry etch process demonstrated selectivity values greater than 15:1 with respect to SiO2. The etching chemistry, however, was sensitive to NF3:H2 gas ratio. For dilute NF3 in H2, no SiARC etching was observed. Presumably, this is due to the deposition of ammonium fluorosilicate layer that occurs for dilute NF3/H2 plasmas. Additionally, challenges involved in selective SiARC removal (selective to SiO2, organic and Si layers) post pattern transfer, in a multi-layer structure will be discussed.

The effect of water storage, elapsed time and contaminants on the bond strength and interfacial polymerization of a nanohybrid composite.

PubMed

Perriard, Jean; Lorente, Maria Cattani; Scherrer, Susanne; Belser, Urs C; Wiskott, H W Anselm

2009-12-01

To systematically characterize the effect of time lapse, water storage, and selected contaminants on the bond strength of a nanofilled dental composite. Half-dumbbell-shaped samples were fabricated out of light-polymerizing composite resin. To function as substrates they were aged for 30 days in water. Prior to bonding, the substrates' surfaces were subjected to the following treatments: 1) Removing a 0.2- to 0.4-mm layer using a fluted carbide bur; 2) grit blasting with 50 microm alumina particles; 3) etching with phosphoric acid gel; 4) grit blasting followed by etching; 5) blasting with tribochemical particles followed by silane application; 6) sanding with 400-grit paper, air aging of the adherent half-sample before bonding; 7) surface contamination with saliva; 8) surface contamination with blood. In each group (n = 30), freshly polymerized (except in group 6) adherent half-samples were bonded to the substrate half-samples by a layer of unfilled adhesive resin. Fifteen full dumbbell-shaped specimens were subjected to tensile testing after 1 h and 15 after 7 days water storage. In a positive control group, freshly cured half-samples were bonded shortly after fabrication. The tensile strength was analyzed using Weibull statistics and presented in terms of the material's characteristic strength and shape parameter. Fractographs of the two weakest and strongest samples of each group were produced. The surfaces were searched to locate hackle, wake hackle and the origin of the fracture. Surface roughness and time lapse increased the bond strength of the repaired specimens. All groups in which surface roughness was produced before bonding increased in repair strength. Post-bonding aging improved strength. Fractographs yielded interpretable data whenever larger surfaces of single phase bonding resin were present. 1) Roughening and etching an aged composite's surface prior to applying a coat of unfilled resin and the filled material increases repair bond strength by up to 100%. 2) The repair bond strength of a roughened aged composite is 25% to 30% inferior to the tensile strength of solid specimens. 3) After 7 days' storage in water, no detrimental effect could be seen from saliva or blood contamination if the surfaces were properly rinsed.

Performance of a new one-step multi-mode adhesive on etched vs non-etched enamel on bond strength and interfacial morphology.

PubMed

de Goes, Mario Fernando; Shinohara, Mirela Sanae; Freitas, Marcela Santiago

2014-06-01

To compare microtensile bond strength (μTBS) and interfacial morphology of a new one-step multimode adhesive with a two-step self-etching adhesive and two etch-and-rinse adhesives systems on enamel. Thirty human third molars were sectioned to obtain two enamel fragments. For μTBS, 48 enamel surfaces were ground using 600-grit SiC paper and randomly assigned into 6 groups (n = 8): nonetched Scotchbond Universal [SBU]; etched SBU [SBU-et]; non-etched Clearfil SE Bond [CSE]; etched CSE [CSE-et]; Scotchbond Multi-PURPOSE [SBMP]; Excite [EX]. The etched specimens were conditioned with 37% phosphoric acid for 30 s, each adhesive system was applied according to manufacturers' instructions, and composite resin blocks (Filtek Supreme Plus, 3M ESPE) were incrementally built up. Specimens were sectioned into beams with a cross-sectional area of 0.8-mm2 and tested under tension (1 mm/min). The data were analyzed with oneway ANOVA and Fisher's PLSD (α = 0.05). For interface analysis, two samples from each group were embedded in epoxy resin, polished, and then observed using scanning electron microscopy (SEM). The μTBS values (in MPa) and the standard deviations were: SBU = 27.4 (8.5); SBU-et = 33.6 (9.3); CSE = 28.5 (8.3); CSE-et = 34.2 (9.0); SBMP = 30.4 (11.0); EX = 23.3 (8.2). CSE-et and SBU-et presented the highest bond strength values, followed by SBMP, CSE, and SBU which did not differ significantly from each other. EX showed the statistically significantly lowest bond strength values. SEM images of interfaces from etched samples showed long adhesive-resin tags penetrating into demineralized enamel. Preliminary etching of enamel significantly increased bond strength for the new one-step multimode adhesive SBU and two-step self-etching adhesive CSE.

Antibacterial Effect and Tensile Bond Strength of Self-etching Adhesive Resins with and without Methacryloyloxydodecylpyridinium Bromide: An in vitro Study.

PubMed

Krishnamurthy, Madhuram; Kumar, V Naveen; Leburu, Ashok; Dhanavel, Chakravarthy; Selvendran, Kasiswamy E; Praveen, Nehrudhas

2018-04-01

Aim: The aim of the present study was to compare the antibacterial activity of a self-etching primer containing antibacterial monomer methacryloyloxydodecylpyridinium bromide (MDPB) (Clearfil protect bond) with a conventional self-etching primer without MDPB (Clearfil SE bond) against Streptococcus mutans and the effect of incorporation of MDPB on the tensile bond strength of the experimental self-etching primer (Clearfil protect bond). Materials and methods: The antibacterial activity of the self-etching primers was assessed using agar disk diffusion method and the diameters of the zones of inhibition were measured and ranked. For tensile bond strength testing, 20 noncarious human molars were selected and randomly divided into two groups comprising 10 teeth in each group. Group I specimens were treated with Clearfil SE bond (without MDPB). Group II specimens were treated with Clearfil protect bond (with MDPB). Composite material was placed incrementally and cured for 40 seconds in all the specimens. Tensile bond strength was estimated using the Instron Universal testing machine at a crosshead speed of 1 mm/min. Results: The addition of MDPB into a self-etching primer exerts potential antibacterial effect against S. mutans. The tensile bond strength of MDPB containing self-etching primer was slightly lower than that of the conventional self-etching Clearfil protect bond primer, but the difference was not statistically significant. Conclusion: Thus, a self-etching primer containing MDPB will be a boon to adhesive dentistry as it has bactericidal property with adequate tensile bond strength. Clinical significance: The concept of prevention of extension in adhesive dentistry would result in micro/nanoleakage due to the presence of residual bacteria in the cavity. Self-etching primers with MDPB would improve the longevity of such restorations by providing adequate antibacterial activity without compromising the bond strength. Keywords: Antibacterial property, Methacryloyloxydodecy-lpyridinium bromide, Self-etching primers, Tensile bond strength.

Inductively coupled plasma etching of GaAs low loss waveguides for a traveling waveguide polarization converter, using chlorine chemistry

NASA Astrophysics Data System (ADS)

Lu, J.; Meng, X.; Springthorpe, A. J.; Shepherd, F. R.; Poirier, M.

2004-05-01

A traveling waveguide polarization converter [M. Poirier et al.] has been developed, which involves long, low loss, weakly confined waveguides etched in GaAs (epitaxially grown by molecular beam epitaxy), with electroplated ``T electrodes'' distributed along the etched floor adjacent to the ridge walls, and airbridge interconnect metallization. This article describes the development of the waveguide fabrication, based on inductively coupled plasma (ICP) etching of GaAs using Cl2 chemistry; the special processes required to fabricate the electrodes and metallization [X. Meng et al.], and the device characteristics [M. Poirier et al.], are described elsewhere. The required waveguide has dimensions nominally 4 μm wide and 2.1 μm deep, with dimensional tolerances ~0.1 μm across the wafer and wafer to wafer. A vertical etch profile with very smooth sidewalls and floors is required to enable the plated metal electrodes to be fabricated within 0.1 μm of the ridge. The ridges were fabricated using Cl2 ICP etching and a photoresist mask patterned with an I-line stepper; He backside cooling, combined with an electrostatic chuck, was employed to ensure good heat transfer to prevent resist reticulation. The experimental results showed that the ridge profile is very sensitive to ICP power and platen rf power. High ICP power and low platen power tend to result in more isotropic etching, whereas increasing platen power increases the photoresist etch rate, which causes rougher ridge sidewalls. No strong dependence of GaAs etch rate and ridge profile were observed with small changes in process temperature (chuck temperature). However, when the chuck temperature was decreased from 25 to 0 °C, etch uniformity across a 3 in. wafer improved from 6% to 3%. Photoresist and polymer residues present after the ICP etch were removed using a combination of wet and dry processes. .

A systematic review of the influence of different titanium surfaces on proliferation, differentiation and protein synthesis of osteoblast-like MG63 cells.

PubMed

Bächle, Maria; Kohal, Ralf J

2004-12-01

Titanium is the standard material for dental and orthopaedical implants. The good biocompatibility has been proven in many experimental and clinical investigations. Different titanium topographies were tested in vitro using different cell culture models. The aim of this systematic review was to evaluate and summarize the medical/dental literature to assess on which kind of titanium surface structure the osteoblast-like osteosarcoma cells MG63 show the best proliferation and differentiation rate, and the best protein synthesis. A systematic search was carried out using different on-line databases (PubMed, Web of Science, Cochrane Library, International Poster Journal), supplemented by handsearch in selected journals and by examination of the bibliographies of the identified articles. Inclusion and exclusion criterias were applied when considering relevant articles. Studies which met the inclusion criteria were included and data extraction was undertaken by one reviewer. The search yielded 348 references. Nine articles referring to nine different studies were relevant to our question. Additionally 8 less relevant articles were identified. It was found that regularly textured surfaces of pure titanium with R(a) values (average roughness) of around 4 mum are well-accepted by MG63 cells. The surfaces and culture conditions vary widely. Therefore it is still difficult to recommend one particular surface. It seems that there are no differences in cell proliferation and differentiation on surfaces treated by blasting and etching. Standardization in fabrication and size of the different test surfaces as well as homogeneity in culture times and plating densities should be aspects for future research.

Effects of coating materials on nanoindentation hardness of enamel and adjacent areas.

PubMed

Alsayed, Ehab Z; Hariri, Ilnaz; Nakashima, Syozi; Shimada, Yasushi; Bakhsh, Turki A; Tagami, Junji; Sadr, Alireza

2016-06-01

Materials that can be applied as thin coatings and actively release fluoride or other bioavailable ions for reinforcing dental hard tissue deserve further investigation. In this study we assessed the potential of resin coating materials in protection of underlying and adjacent enamel against demineralization challenge using nanoindentation. Enamel was coated using Giomer (PRG Barrier Coat, PBC), resin-modified glass-ionomer (Clinpro XT Varnish, CXT), two-step self-etch adhesive (Clearfil SE Protect, SEP) or no coating (control). After 5000 thermal cycles and one-week demineralization challenge, Martens hardness of enamel beneath the coating, uncoated area and intermediate areas was measured using a Berkovich tip under 2mN load up to 200μm depth. Integrated hardness and 10-μm surface zone hardness were compared among groups. Nanoindentation and scanning electron microscopy suggested that all materials effectively prevented demineralization in coated area. Uncoated areas presented different hardness trends; PBC showed a remarkable peak at the surface zone before reaching as low as the control, while CXT showed relatively high hardness values at all depths. Ion-release from coating materials affects different layers of enamel. Coatings with fluoride-releasing glass fillers contributed to reinforcement of adjacent enamel. Surface prereacted glass filler-containing PBC superficially protected neighboring enamel against demineralization, while resin-modified glass-ionomer with calcium (CXT) improved in-depth protection. Cross-sectional hardness mapping of enamel on a wide range of locations revealed minute differences in its structure. Copyright © 2016 Academy of Dental Materials. Published by Elsevier Ltd. All rights reserved.

Effect of sandblasting, silica coating, and laser treatment on the microtensile bond strength of a dental zirconia ceramic to resin cements.

PubMed

Mahmoodi, Nasrin; Hooshmand, Tabassom; Heidari, Solmaz; Khoshro, Kimia

2016-02-01

The purpose of this in vitro study was to evaluate the effect of laser irradiation as well as other surface treatment methods on the microtensile bond strength of a dental zirconia ceramic to the two types of resin cements. Zirconia ceramic blocks (ICE Zirkon) were sintered according to the manufacturer's instructions and duplicated in resin composites. The ceramic specimens were divided into four groups according to the following surface treatments: no surface treatment (control), sandblasting with alumina, silica coating plus silanization, and Nd:YAG laser irradiation. The specimens were divided equally and then bonded with Panavia F2.0 (self-etching resin cement) and Clearfil SA Luting (self-adhesive resin cement) to the composite blocks. The bonded ceramic-composite blocks were stored in distilled water at 37 °C for 72 h, cut to prepare bar-shaped specimens with a bonding area of approximately 1 mm(2), and thermocycled for 3000 cycles between 5 and 55 °C, and the microtensile bond strengths were measured using a universal testing machine. The data were analyzed by ANOVA and Tukey post hoc test. The results showed that the self-adhesive resin cement used in this study did not improve the microtensile bond strength when the zirconia surface was sandblasted by alumina. The use of the Nd:YAG laser did not enhance the bond strength between the zirconia and both types of resin cements. In addition, silica coating of the zirconia surfaces plus silane application significantly improved the bond strength regardless of the type of resin cement utilized.

Cytotoxicity Evaluation of Self Adhesive Composite Resin Cements by Dentin Barrier Test on 3D Pulp Cells.

PubMed

Ulker, Hayriye Esra; Sengun, Abdulkadir

2009-04-01

The aim of this study was to evaluate the effects of five self-etch dental composite resin cements on the cell viability of bovine dental papilla-derived cells. The cytotoxicity of composite resin cements (Rely X Unicem Clicker, 3M ESPE; MaxCem; KERR, Panavia F 2.0; Kuraray, BisCem; Bisco and Bistite II DC; Tokuyama) was analyzed in a dentin barrier test device using three-dimensional (3D) pulp cell cultures. A commercially available cell culture perfusion chamber was separated into two compartments by 500 mum dentin disc. The three dimensional cultures placed on a dentin disk held in place by a special biocompatible stainless-steel holder. Test materials were introduced into the upper compartment in direct contact with the cavity side of the dentin disks according to the manufacturer's instructions. Subsequently, the pulpal part of the perfusion chamber containing the cell cultures was perfused with medium (2 ml/h). After an exposure period of 24 h, the cell survival was determined by the MTT assay. Statistical analyses were performed using the Mann-Whitney U-test. In dentin barrier test, cell survival was similar with Maxcem and negative control group (P>.05), and all other tested materials were cytotoxic for the three dimensional cell cultures (P>.05). The significance of composite resin cements is being more important in dentistry. The cytotoxic potencies demonstrated by these materials might be of clinical relevance. Some composite resin cements include biologically active ingredients and may modify pulp cell metabolism when the materials are used in deep cavities or directly contact pulp tissue.

The effect of zoledronate-containing primer on dentin bonding of a universal adhesive.

PubMed

Zenobi, Walter; Feitosa, Victor Pinheiro; Moura, Maria Elisa Martins; D'arcangelo, Camillo; Rodrigues, Lidiany Karla de Azevedo; Sauro, Salvatore

2018-01-01

To evaluate the bonding ability and nanoleakage of a universal adhesive applied to dentin pre-treated using a zoledronate-containing primer (zol-primer) before and after mechanical load cycling. Flat dentin surfaces obtained from human molars were assigned to one of the following adhesion procedures (n=6): 1-Single Bond Universal (SBU) applied in etch-and-rinse mode; 2- SBU applied as etch-and-rinse after the application of zol-primer; 3- SBU applied in self-etch strategy; 4- SBU applied as self-etch after the use of zol-primer. Half of the specimens were processed for microtensile bond strength test after 24h, while the other half part was submitted to 200,000 mechanical cycles. Further specimens were silver-impregnated and assessed for interface nanoleakage by SEM. Data were analyzed with two-way ANOVA and Tukey's test (p<0.05). At 24h evaluation, the four groups presented similar bond strengths, whilst both groups bonded with etch-and-rinse technique showed significant bond strength reduction after mechanical load (p<0.05), with the highest drop in bond strength for the specimens pre-treated with the zol-primer. No negative effects were found for self-etch strategy (p>0.05) in microtensile test. Lower nanoleakage expression was observed for etch-and-rinse specimens treated with zol-primer. However, noteworthy reduction of adhesive layer thickness was observed when combining the zol-primer with the self-etch bonding approach. It can be concluded that zol-primer should not be used along with a universal adhesive in etch-and-rinse mode, but its application before self-etch application may provide less degradation of the resin-dentin interface. Copyright © 2017 Elsevier Ltd. All rights reserved.

Evaluation of different types of enamel conditioning before application of a fissure sealant.

PubMed

Ciucchi, Philip; Neuhaus, Klaus W; Emerich, Marta; Peutzfeldt, Anne; Lussi, Adrian

2015-01-01

The aim of the study was to compare fissure sealant quality after mechanical conditioning of erbium-doped yttrium aluminium garnet (Er:YAG) laser or air abrasion prior to chemical conditioning of phosphoric acid etching or of a self-etch adhesive. Twenty-five permanent molars were initially divided into three groups: control group (n = 5), phosphoric acid etching; test group 1 (n = 10), air abrasion; and test group 2, (n = 10) Er:YAG laser. After mechanical conditioning, the test group teeth were sectioned buccolingually and the occlusal surface of one half tooth (equal to one sample) was acid etched, while a self-etch adhesive was applied on the other half. The fissure system of each sample was sealed, thermo-cycled and immersed in 5% methylene dye for 24 h. Each sample was sectioned buccolingually, and one slice was analysed microscopically. Using specialized software microleakage, unfilled margin, sealant failure and unfilled area proportions were calculated. A nonparametric ANOVA model was applied to compare the Er:YAG treatment with that of air abrasion and the self-etch adhesive with phosphoric acid (α = 0.05). Test groups were compared to the control group using Wilcoxon rank sum tests (α = 0.05). The control group displayed significantly lower microleakage but higher unfilled area proportions than the Er:YAG laser + self-etch adhesive group and displayed significantly higher unfilled margin and unfilled area proportions than the air-abrasion + self-etch adhesive group. There was no statistically significant difference in the quality of sealants applied in fissures treated with either Er:YAG laser or air abrasion prior to phosphoric acid etching, nor in the quality of sealants applied in fissures treated with either self-etch adhesive or phosphoric acid following Er:YAG or air-abrasion treatment.

Effects of acid etching and adhesive treatments on host-derived cysteine cathepsin activity in dentin.

PubMed

Zhang, Wenhao; Yang, Weixiang; Wu, Shuyi; Zheng, Kaibin; Liao, Weili; Chen, Boli; Yao, Ke; Liang, Guobin; Li, Yan

2014-10-01

To analyze the effects of different processes during bonding on endogenous cysteine cathepsin activity in dentin. Dentin powder, prepared from extracted human third molars, was divided into 10 groups. Two lots of dentin powder were used to detect the effects of the procedure of protein extraction on endogenous cathepsin activity. The others were used to study effects of different acid-etching or adhesive treatments on enzyme activity. Concentrations of 37% phosphoric acid or 10% phosphoric acid, two etch-and-rinse adhesive systems, and two self-etching adhesive systems were used as dentin powder treatments. The untreated mineralized dentin powder was set as the control. After treatment, the proteins of each group were extracted. The total cathepsin activity in the extracts of each group was monitored with a fluorescence reader. In the control group, there were no significant differences in cathepsin activity between the protein extract before EDTA treatment and the protein extract after EDTA treatment (p > 0.05). The cathepsin activities of the three different extracts in the 37% phosphoric acid-treated group were different from each other (p < 0.05). The two acid-etching groups and two etch-and-rinse groups showed significant enzyme activity reduction vs the control group (p < 0.05). There were no significant differences between those four groups (p > 0.05). Treating the dentin powder with any of the two self-etching adhesives resulted in an increase in cathepsin activity (p < 0.05). The activity of cysteine cathepsins can be detected in dentin powder. Treatment with EDTA during protein extraction exerted an influence on cathepsin activity. Acid etching or etch-and-rinse adhesive systems may reduce the activity of endogenous cathepsins in dentin. Self-etching adhesive systems may increase the enzyme activity.

Consequences of atomic layer etching on wafer scale uniformity in inductively coupled plasmas

NASA Astrophysics Data System (ADS)

Huard, Chad M.; Lanham, Steven J.; Kushner, Mark J.

2018-04-01

Atomic layer etching (ALE) typically divides the etching process into two self-limited reactions. One reaction passivates a single layer of material while the second preferentially removes the passivated layer. As such, under ideal conditions the wafer scale uniformity of ALE should be independent of the uniformity of the reactant fluxes onto the wafers, provided all surface reactions are saturated. The passivation and etch steps should individually asymptotically saturate after a characteristic fluence of reactants has been delivered to each site. In this paper, results from a computational investigation are discussed regarding the uniformity of ALE of Si in Cl2 containing inductively coupled plasmas when the reactant fluxes are both non-uniform and non-ideal. In the parameter space investigated for inductively coupled plasmas, the local etch rate for continuous processing was proportional to the ion flux. When operated with saturated conditions (that is, both ALE steps are allowed to self-terminate), the ALE process is less sensitive to non-uniformities in the incoming ion flux than continuous etching. Operating ALE in a sub-saturation regime resulted in less uniform etching. It was also found that ALE processing with saturated steps requires a larger total ion fluence than continuous etching to achieve the same etch depth. This condition may result in increased resist erosion and/or damage to stopping layers using ALE. While these results demonstrate that ALE provides increased etch depth uniformity, they do not show an improved critical dimension uniformity in all cases. These possible limitations to ALE processing, as well as increased processing time, will be part of the process optimization that includes the benefits of atomic resolution and improved uniformity.