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 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.

Comparison of microleakage on one composite etched with phosphoric acid or a combination of phosphoric and hydrofluoric acids and bonded with several different systems.

PubMed

Szep, Susanne; Langner, Nicole; Bayer, Silja; Börnichen, Diana; Schulz, Christoph; Gerhardt, Thomas; Schriever, Anette; Becker, Joachim; Heidemann, Detlef

2003-02-01

There are no data available on whether or to what extent hydrofluoric acid affects the marginal integrity of dentin-bonded composite restorations when it is used instead of phosphoric acid in the total-etch technique. This in vitro study examined the etching effects of phosphoric acid versus a combination of phosphoric and hydrofluoric acid by evaluation of microleakage in a composite restoration bonded with different dentin adhesive systems. Extracted teeth (n = 90) containing 2 class II preparations, mesial occlusal (MO) and distal occlusal (DO) standarized (cervical margins in dentin) were perfused with Ringer solution and etched in 1 of 2 ways: with phosphoric acid only or with phosphoric combined with hydrofluoric acid. Different dentin bonding agents were then applied (Etch & Prime 3.0, Optibond Solo, Prime & Bond NT, Scotchbond 1, Syntac Single Component, or Syntac Sprint; (n = 15 for each etching material)). The preparations were restored with a hybrid composite (Herculite XRV) and submitted to 5000 thermocycles (5 degrees C to 55 degrees C) to simulate the in vivo situation. Microleakage was assessed with 2% methylene blue diffusion for 24 hours. Dye penetration was calculated as a percentage of the total length of the gingival margins of the preparation with light microscopy at original magnification x 32. The results were analyzed with the Kruskal-Wallis multiple comparison z-value assay (alpha = .05). Differences in dye penetration were significant, both as a function of the dentin adhesive and the conditioning mode applied. In the specimen groups conditioned with phosphoric acid, Optibond Solo (54% +/- 44%) and Syntac Sprint (74% +/- 39%) demonstrated the lowest penetration values. Higher values were obtained for Prime & Bond NT (81% +/- 34%), Scotchbond 1 (83% +/- 31%), Etch & Prime 3.0 (85% +/- 33%), and Syntac Single Component (95% +/- 16%), with no significant differences (alpha=.05) between specimen groups. The best results were obtained for Syntac Sprint (24% +/- 26% dye penetration) after conditioning with a mixture of phosphoric and hydrofluoric acid. The least favorable result was obtained for Optibond Solo (65% +/- 31%). It was significantly different from Prime & Bond NT (76% +/- 37%), Scotchbond 1 (85% +/- 29%), and Etch & Prime 3.0 (88% +/- 24%). Syntac Single Component (75% +/- 32%) was significantly different from Syntac Sprint. Syntac Single Component and Syntac Sprint exhibited significantly better results when conditioned with a combination of phosphoric acid and hydrofluoric acid than with phosphoric acid only. Within the limitations of this in vitro study, total-etching water-based (Syntac Single Component) and acetone-based (Syntac Sprint) bonding agents with a combination of phosphoric acid and hydrofluoric acid led to significant reductions (alpha=.05) in dye penetration compared to phosphoric acid conditioning only. Ethanol-based dentin bonding agents (Etch & Prime 3.0, Optibond Solo, and Scotchbond 1) were not significantly influenced by the type of conditioner used.

Fabrication Techniques for III-V Micro-Opto-Electro-Mechanical Systems

DTIC Science & Technology

2002-03-26

Trifluoride . . . . . . . . . . . . . . . . . . . . . 2-33 ClF3 Chlorine Trifluoride . . . . . . . . . . . . . . . . . . . . . 2-33 xix Symbol Page O2 Oxygen...dimensionless) . . . . . . . . . . . . 2-36 HCl Hydrochloric Acid . . . . . . . . . . . . . . . . . . . . . . 3-16 M Molarity (moles/liter...interhalogen etch gases have been synthesized and used to etch silicon. These gases include bromine triflouride (BrF3) and chlorine trifluoride (ClF3) [27

Ultrasonic recovery of copper and iron through the simultaneous utilization of Printed Circuit Boards (PCB) spent acid etching solution and PCB waste sludge.

PubMed

Huang, Zhiyuan; Xie, Fengchun; Ma, Yang

2011-01-15

A method was developed to recover the copper and iron from Printed Circuit Boards (PCB) manufacturing generated spent acid etching solution and waste sludge with ultrasonic energy at laboratory scale. It demonstrated that copper-containing PCB spent etching solution could be utilized as a leaching solution to leach copper from copper contained PCB waste sludge. It also indicated that lime could be used as an alkaline precipitating agent in this method to precipitate iron from the mixture of acidic PCB spent etching solution and waste sludge. This method provided an effective technique for the recovery of copper and iron through simultaneous use of PCB spent acid solution and waste sludge. The leaching rates of copper and iron enhanced with ultrasound energy were reached at 93.76% and 2.07% respectively and effectively separated copper from iron. Followed by applying lime to precipitate copper from the mixture of leachate and rinsing water produced by the copper and iron separation, about 99.99% and 1.29% of soluble copper and calcium were settled as the solids respectively. Furthermore the settled copper could be made as commercial rate copper. The process performance parameters studied were pH, ultrasonic power, and temperature. This method provided a simple and reliable technique to recover copper and iron from waste streams generated by PCB manufacturing, and would significantly reduce the cost of chemicals used in the recovery. Copyright © 2010 Elsevier B.V. All rights reserved.

Effect of Surface Treatment on Enamel Cracks After Orthodontic Bracket Debonding: Er,Cr:YSGG Laser-Etching Versus Acid-Etching

PubMed Central

Ghaffari, Hassanali; Mirhashemi, Amirhossein; Baherimoghadam, Tahereh; Azmi, Amir

2017-01-01

Objectives: This study sought to compare enamel cracks after orthodontic bracket debonding in the surfaces prepared with erbium, chromium: yttrium-scandium-galliumgarnet (Er,Cr:YSGG) laser and the conventional acid-etching technique. Materials and Methods: This in-vitro experimental study was conducted on 60 sound human premolars extracted for orthodontic purposes. The teeth were randomly divided into two groups (n=30). The teeth in group A were etched with 37% phosphoric acid gel, while the teeth in group B were subjected to Er,Cr:YSGG laser irradiation (gold handpiece, MZ8 tip, 50Hz, 4.5W, 60μs, 80% water and 60% air). Orthodontic brackets were bonded to the enamel surfaces and were then debonded in both groups. The samples were inspected under a stereomicroscope at ×38 magnification to assess the number and length of enamel cracks before bonding and after debonding. Independent-samples t-test was used to compare the frequency of enamel cracks in the two groups. Levene’s test was applied to assess the equality of variances. Results: No significant difference was noted in the frequency or length of enamel cracks between the two groups after debonding (P>0.05). Conclusions: Despite the same results of the frequency and length of enamel cracks in the two groups and by considering the side effects of acid-etching (demineralization and formation of white spot lesions), Er,Cr:YSGG laser may be used as an alternative to acid-etching for enamel surface preparation prior to bracket bonding. PMID:29296111

Advanced light-scattering materials: Double-textured ZnO:B films grown by LP-MOCVD

NASA Astrophysics Data System (ADS)

Addonizio, M. L.; Spadoni, A.; Antonaia, A.

2013-12-01

Double-textured ZnO:B layers with enhanced optical scattering in both short and long wavelength regions have been successfully fabricated using MOCVD technique through a three step process. Growth of double-textured structures has been induced by wet etching on polycrystalline ZnO surface. Our double-layer structure consists of a first ZnO:B layer wet etched and subsequently used as substrate for a second ZnO:B layer deposition. Polycrystalline ZnO:B layers were etched by utilizing diluted solutions of fluoridic acid (HF), chloridric acid (HCl) and phosphoric acid (H3PO4) and their effect on surface morphology modification was systematically investigated. The morphology of the second deposited ZnO layer strongly depended on the surface properties of the etched ZnO first layer. Growth of cauliflower-like texture was induced by protrusions presence on the HCl etched surface. Optimized double-layer structure shows a cauliflower-like double texture with higher RMS roughness and increased spectral haze values in both short and long wavelength regions, compared to conventional pyramidal-like single texture. Furthermore, this highly scattering structure preserves excellent optical and electrical properties.

Comparative efficacy of Er,Cr:YSGG and Er:YAG lasers for etching of composite for orthodontic bracket bonding.

PubMed

Mirhashemi, Amir Hossein; Chiniforush, Nasim; Sharifi, Nastaran; Hosseini, Amir Mehdi

2018-05-01

Several techniques have been proposed to obtain a durable bond, and the efficacy of these techniques is assessed by measuring parameters such as bond strength. Laser has provided a bond strength as high as that of acid etching in vitro and has simpler use with shorter clinical time compared to acid etching. This study aimed to compare the efficacy of Er:YAG and Er,Cr:YSGG lasers for etching and bonding of composite to orthodontic brackets. No previous study has evaluated the effect of these particular types of laser. A total of 70 composite blocks were randomly divided into five groups (n = 14): group 1, etching with phosphoric acid for 20 s; group 2, Er:YAG laser irradiation with 2 W power for 10 s; group 3, Er:YAG laser with 3 W power for 10 s; group 4, Er,Cr:YSGG laser with 2 W power for 10 s; group 5, Er,Cr:YSGG laser with 3 W power for 10 s. Metal brackets were then bonded to composites, and after 5000 thermal cycles, they were subjected to shear bond strength test in a universal testing machine after 24 h of water storage. One sample of each group was evaluated under a scanning electron microscope (SEM) to assess changes in composite surface after etching. The adhesive remnant index (ARI) was calculated under a stereomicroscope. Data were statistically analyzed. The mean and standard deviation of shear bond strength were 18.65 ± 3.36, 19.68 ± 5.34, 21.31 ± 4.03, 17.38 ± 6.94, and 16.45 ± 4.26 MPa in groups 1-5, respectively. The ARI scores showed that the bond failure mode in all groups was mainly mixed. The groups were not significantly different in terms of shear bond strength. Er:YAG and Er,Cr:YSGG lasers with the mentioned parameters yield optimal shear bond strength and can be used as an alternative to acid etching for bracket bond to composite.

Distinguishing shocked from tectonically deformed quartz by the use of the SEM and chemical etching

USGS Publications Warehouse

Gratz, A.J.; Fisler, D.K.; Bohor, B.F.

1996-01-01

Multiple sets of crystallographically-oriented planar deformation features (PDFs) are generated by high-strain-rate shock waves at pressures of > 12 GPa in naturally shocked quartz samples. On surfaces, PDFs appear as narrow (50-500 nm) lamellae filled with amorphosed quartz (diaplectic glass) which can be etched with hydrofluoric acid or with hydrothermal alkaline solutions. In contrast, slow-strain-rate tectonic deformation pressure produces wider, semi-linear and widely spaced arrays of dislocation loops that are not glass filled. Etching samples with HF before examination in a scanning electron microscope (SEM) allows for unambiguous visual distinction between glass-filled PDFs and glass-free tectonic deformation arrays in quartz. This etching also reveals the internal 'pillaring' often characteristic of shock-induced PDFs. This technique is useful for easily distinguishing between shock and tectonic deformation in quartz, but does not replace optical techniques for characterizing the shock features.

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.

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.

Nanoporous Gallium Nitride Through Anisotropic Metal-Assisted Electroless Photochemical Wet Etching Technique

NASA Astrophysics Data System (ADS)

Perumal, R.; Hassan, Z.

2016-12-01

Nanoporous gallium nitride (GaN) has many potential applications in light-emitting diodes (LEDs), photovoltaics, templates and chemical sensors. This article reports the porosification of GaN through UV enhanced metal-assisted electroless photochemical wet etching technique using three different acid-based etchants and platinum served as catalyst for porosification. The etching process was conducted at room temperature for a duration of 90min. The morphological, structural, spectral and optical features of the developed porous GaN were studied with appropriate characterization techniques and the obtained results were presented. Field emission scanning electron micrographs exhibited the porosity nature along with excellent porous network of the etched samples. Structural studies confirmed the mono crystalline quality of the porous nanostructures. Raman spectral analyzes inferred the presenting phonon modes such as E2 (TO) and A1 (LO) in fabricated nanoporous structures. The resulted porous nanostructures hold the substantially enhanced photoluminescence intensity compared with the pristine GaN epitaxial film that is interesting and desirable for several advances in the applications of Nano-optoelectronic devices.

Marginal adaptation of composite resins under two adhesive techniques.

PubMed

Dačić, Stefan; Veselinović, Aleksandar M; Mitić, Aleksandar; Nikolić, Marija; Cenić, Milica; Dačić-Simonović, Dragica

2016-11-01

In the present research, different adhesive techniques were used to set up fillings with composite resins. After the application of etch and rinse or self etch adhesive technique, marginal adaptation of composite fillings was estimated by the length of margins without gaps, and by the microretention of resin in enamel and dentin. The study material consisted of 40 extracted teeth. Twenty Class V cavities were treated with 35% phosphorous acid and restored after rinsing by Adper Single Bond 2 and Filtek Ultimate-ASB/FU 3M ESPE composite system. The remaining 20 cavities were restored by Adper Easy One-AEO/FU 3M ESPE composite system. Marginal adaptation of composite fillings was examined using a scanning electron microscope (SEM). The etch and rinse adhesive technique showed a significantly higher percentage of margin length without gaps (in enamel: 92.5%, in dentin: 57.3%), compared with the self-etch technique with lower percentage of margin length without gaps, in enamel 70.4% (p < .001), and in dentin-22.6% (p < .05). In the first technique, microretention was composed of adhesive and hybrid layers as well as resin tugs in interprismatic spaces of enamel, while the dentin microretention was composed of adhesive and hybrid layers with resin tugs in dentin canals. In the second technique, resin tugs were rarely seen and a microgap was dominant along the border of restoration margins. The SEM analysis showed a better marginal adaptation of composite resin to enamel and dentin with better microretention when the etch and rinse adhesive procedure was applied. © 2016 Wiley Periodicals, Inc.

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.

Multiscale characterization of partially demineralized superficial and deep dentin surfaces.

PubMed

Pelin, Irina M; Trunfio-Sfarghiu, Ana-Maria; Farge, Pierre; Piednoir, Agnes; Pirat, Christophe; Ramos, Stella M M

2013-08-01

The objective of this study was to address the following question: 'Which properties are modified in partially demineralized surfaces, compared with non-demineralized dentin surfaces, following orthophosphoric acid-etching as performed in clinical procedures?'. For this purpose, the complementary techniques atomic force microscopy/spectroscopy, scanning electron microscopy, energy-dispersive X-ray spectroscopy, and contact angle measurements were used to provide a multiscale characterization of the dentin substrate undergoing the acidic preconditioning designed to enhance wetting. Special attention was given to the influence of the etching pretreatment on the nanomechanical properties at different levels of dentin surfaces, in both dry and hydrated conditions. The four-sided pyramid model (extended Hertz contact model) proved to be accurate for calculating the apparent Young's modulus, offering new information on the elasticity of dentin. The modulus value notably decreased following etching and surface hydration. This study underlines that after the acid etching pretreatment the contribution of the nanomechanical, morphological, and physicochemical modifications has a strong influence on the dentin adhesion properties and thus plays a significant role in the coupling of the adhesive-resin composite build-up material at the dentin surface. © 2013 Eur J Oral Sci.

Automated and inexpensive method to manufacture solid- state nanopores and micropores in robust silicon wafers

NASA Astrophysics Data System (ADS)

Vega, M.; Granell, P.; Lasorsa, C.; Lerner, B.; Perez, M.

2016-02-01

In this work an easy, reproducible and inexpensive technique for the production of solid state nanopores and micropores using silicon wafer substrate is proposed. The technique is based on control of pore formation, by neutralization etchant (KOH) with a strong acid (HCl). Thus, a local neutralization is produced around the nanopore, which stops the silicon etching. The etching process was performed with 7M KOH at 80°C, where 1.23µm/min etching speed was obtained, similar to those published in literature. The control of the pore formation with the braking acid method was done using 12M HCl and different extreme conditions: i) at 25°C, ii) at 80°C and iii) at 80°C applying an electric potential. In these studies, it was found that nanopores and micropores can be obtained automatically and at a low cost. Additionally, the process was optimized to obtain clean silicon wafers after the pore fabrication process. This method opens the possibility for an efficient scale-up from laboratory production.

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

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.

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.

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.

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.

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.

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.

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.

Fabrication of low reflective nanopore-type black Si layer using one-step Ni-assisted chemical etching for Si solar cell application

NASA Astrophysics Data System (ADS)

Takaloo, AshkanVakilipour; Kolahdouz, Mohammadreza; Poursafar, Jafar; Es, Firat; Turan, Rasit; Ki-Joo, Seung

2018-03-01

Nanotextured Si fabricated through metal-assisted chemical etching (MACE) technique exhibits a promising potential for producing antireflective layer for photovoltaic (PV) application. In this study, a novel single-step nickel (Ni) assisted etching technique was applied to produce an antireflective, nonporous Si (black Si) in an aqueous solution containing hydrofluoric acid (HF), hydrogen peroxide (H2O2) and NiSO4 at 40 °C. Field emission scanning electron microscope was used to characterize different morphologies of the textured Si. Optical reflection measurements of samples were carried out to compare the reflectivity of different morphologies. Results indicated that vertical as well as horizontal pores with nanosized diameters were bored in the Si wafer after 1 h treatment in the etching solution containing different molar ratios of H2O2 to HF. Increasing H2O2 concentration in electrochemical etching solution had a considerable influence on the morphology due to higher injection of positive charges from Ni atoms onto the Si surface. Optimized concentration of H2O2 led to formation of an antireflective layer with 2.1% reflectance of incident light.

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.

Fourier transform infrared photoacoustic spectroscopy study of physicochemical interaction between human dentin and etch-&-rinse adhesives in a simulated moist bond technique.

PubMed

Ubaldini, Adriana L M; Baesso, Mauro L; Sehn, Elizandra; Sato, Francielle; Benetti, Ana R; Pascotto, Renata C

2012-06-01

The purpose of this study was to provide the physicochemical interactions at the interfaces between two commercial etch-&-rinse adhesives and human dentin in a simulated moist bond technique. Six dentin specimens were divided into two groups (n=3) according to the use of two different adhesive systems: (a) 2-hydroxyethylmethacrylate (HEMA) and 4-methacryloxyethyl trimellitate anhydrate (4-META), and (b) HEMA. The Fourier transform infrared photoacoustic spectroscopy was performed before and after dentin treatment with 37% phosphoric acid, with adhesive systems and also for the adhesive systems alone. Acid-conditioning resulted in a decalcification pattern. Adhesive treated spectra subtraction suggested the occurrence of chemical bonding to dentin expressed through modifications of the OH stretching peak (3340 cm(-1)) and symmetric CH stretching (2900 cm(-1)) for both adhesives spectra; a decrease of orthophosphate absorption band (1040 to 970 cm(-1)) for adhesive A and a better resolved complex band formation (1270 to 970 cm(-1)) for adhesive B were observed. These results suggested the occurrence of chemical bonding between sound human dentin and etch-&-rinse adhesives through a clinical typical condition.

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.

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

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.

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

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.

Recovering obliterated engraved marks on aluminium surfaces by etching technique.

PubMed

Baharum, Mohd Izhar Mohd; Kuppuswamy, R; Rahman, Azari Abd

2008-05-20

A study has been made of the characteristics of restoration of obliterated engraved marks on aluminium surfaces by etching technique. By etching different reagents on 0.61mm thick sheets of aluminium (99wt%) on which some engraved marks had been erased to different depths it was found that the reagent 60% hydrochloric acid and 40% sodium hydroxide on alternate swabbing on the surfaces was found to be the most sensitive one for these metal surfaces. This reagent was able to restore marks in the above plates erased down to 0.04mm below the bottom of the engraving. The marks also presented excellent contrast with the background. This reagent was further experimented with similar aluminium surfaces, but of relatively greater thickness of 1.5mm. It was noticed that the recovery depth increased slightly to 0.06mm; this suggested the dependence of recovery depth on the thickness of the sheet metal. Further, the depth of restoration decreased in cases where the original number was erased and over which a new number was engraved; the latter results are similar to those of steel surfaces reported earlier [M.A.M. Zaili, R. Kuppuswamy, H. Harun, Restoration of engraved marks on steel surfaces by etching technique, Forensic Sci. Int. 171 (2007) 27-32].

Shear bond strength and debonding characteristics of metal and ceramic brackets bonded with conventional acid-etch and self-etch primer systems: An in-vivo study.

PubMed

Mirzakouchaki, Behnam; Shirazi, Sajjad; Sharghi, Reza; Shirazi, Samaneh; Moghimi, Mahsan; Shahrbaf, Shirin

2016-02-01

Different in-vitro studies have reported various results regarding shear bond strength (SBS) of orthodontic brackets when SEP technique is compared to conventional system. This in-vivo study was designed to compare the effect of conventional acid-etching and self-etching primer adhesive (SEP) systems on SBS and debonding characteristics of metal and ceramic orthodontic brackets. 120 intact first maxillary and mandibular premolars of 30 orthodontic patients were selected and bonded with metal and ceramic brackets using conventional acid-etch or self-etch primer system. The bonded brackets were incorporated into the wire during the study period to simulate the real orthodontic treatment condition. The teeth were extracted and debonded after 30 days. The SBS, debonding characteristics and adhesive remnant indices (ARI) were determined in all groups. The mean SBS of metal brackets was 10.63±1.42 MPa in conventional and 9.38±1.53 MPa in SEP system, (P=0.004). No statistically significant difference was noted between conventional and SEP systems in ceramic brackets. The frequency of 1, 2 and 3 ARI scores and debonding within the adhesive were the most common among all groups. No statistically significant difference was observed regarding ARI or failure mode of debonded specimens in different brackets or bonding systems. The SBS of metal brackets bonded using conventional system was significantly higher than SEP system, although the SBS of SEP system was clinically acceptable. No significant difference was found between conventional and SEP systems used with ceramic brackets. Total SBS of metal brackets was significantly higher than ceramic brackets. Due to adequate SBS of SEP system in bonding the metal brackets, it can be used as an alternative for conventional system. Shear bond strength, Orthodontic brackets, Adhesive remnant index, self-etch.

Shear bond strength and debonding characteristics of metal and ceramic brackets bonded with conventional acid-etch and self-etch primer systems: An in-vivo study

PubMed Central

Mirzakouchaki, Behnam; Sharghi, Reza; Shirazi, Samaneh; Moghimi, Mahsan; Shahrbaf, Shirin

2016-01-01

Background Different in-vitro studies have reported various results regarding shear bond strength (SBS) of orthodontic brackets when SEP technique is compared to conventional system. This in-vivo study was designed to compare the effect of conventional acid-etching and self-etching primer adhesive (SEP) systems on SBS and debonding characteristics of metal and ceramic orthodontic brackets. Material and Methods 120 intact first maxillary and mandibular premolars of 30 orthodontic patients were selected and bonded with metal and ceramic brackets using conventional acid-etch or self-etch primer system. The bonded brackets were incorporated into the wire during the study period to simulate the real orthodontic treatment condition. The teeth were extracted and debonded after 30 days. The SBS, debonding characteristics and adhesive remnant indices (ARI) were determined in all groups. Results The mean SBS of metal brackets was 10.63±1.42 MPa in conventional and 9.38±1.53 MPa in SEP system, (P=0.004). No statistically significant difference was noted between conventional and SEP systems in ceramic brackets. The frequency of 1, 2 and 3 ARI scores and debonding within the adhesive were the most common among all groups. No statistically significant difference was observed regarding ARI or failure mode of debonded specimens in different brackets or bonding systems. Conclusions The SBS of metal brackets bonded using conventional system was significantly higher than SEP system, although the SBS of SEP system was clinically acceptable. No significant difference was found between conventional and SEP systems used with ceramic brackets. Total SBS of metal brackets was significantly higher than ceramic brackets. Due to adequate SBS of SEP system in bonding the metal brackets, it can be used as an alternative for conventional system. Key words:Shear bond strength, Orthodontic brackets, Adhesive remnant index, self-etch. PMID:26855704

Electrowetting Lens Employing Hemispherical Cavity Formed by Hydrofluoric Acid, Nitric Acid, and Acetic Acid Etching of Silicon

NASA Astrophysics Data System (ADS)

Lee, June Kyoo; Choi, Ju Chan; Jang, Won Ick; Kim, Hak-Rin; Kong, Seong Ho

2012-06-01

We demonstrate the design of an electrowetting lens employing a high-aspect-ratio hemispherical lens cavity and its micro-electro-mechanical-system (MEMS) fabrication process in this study. Our preliminary simulation results showed that the physical and electrical durability of the lens can be improved by the mitigation of stresses on the insulator at the hemispherical cavity. High-aspect-ratio hemispherical cavities with various diameters and very smooth sidewall surfaces were uniformly fabricated on a silicon wafer by a sophisticated isotropic wet etching technique. Moreover, we experimentally investigated the optical properties of the MEMS-based electrowetting lens with the proposed cavity. Two immiscible liquids in the proposed lens cavity were electrostatically controlled with negligible optical distortion and low focal-length hysteresis due to the fully axis-symmetrical geometry and smooth sidewall of the cavity.

Effect of acid and laser etching on shear bond strength of conventional and resin-modified glass-ionomer cements to composite resin.

PubMed

Navimipour, Elmira Jafari; Oskoee, Siavash Savadi; Oskoee, Parnian Alizadeh; Bahari, Mahmoud; Rikhtegaran, Sahand; Ghojazadeh, Morteza

2012-03-01

Success in sandwich technique procedures can be achieved through an acceptable bond between the materials. The aim of this study was to compare the effect of 35% phosphoric acid and Er,Cr:YSGG laser on shear bond strength of conventional glass-ionomer cement (GIC) and resin-modified glass-ionomer cement (RMGIC) to composite resin in sandwich technique. Sixty-six specimens were prepared from each type of glass-ionomer cements and divided into three treatment groups as follows: without pretreatment, acid etching by 35% phosphoric acid for 15 s, and 1-W Er,Cr:YSGG laser treatment for 15 s with a 600-μm-diameter tip aligned perpendicular to the target area at a distance of 1 mm from the surface. Energy density of laser irradiation was 17.7 J/cm(2). Two specimens in each group were prepared for evaluation under a scanning electron microscope (SEM) after surface treatment and the remainder underwent bonding procedure with a bonding agent and composite resin. Then the shear bond strength was measured at a crosshead speed of 0.5 mm/min. Two-factor analysis of variance and post-hoc Tukey test showed that the cement type, surface treatment method, and the interaction of these two factors significantly affect the shear bond strength between glass-ionomer cements and composite resin (p < 0.05). Surface treatment with phosphoric acid or Er,Cr:YSGG laser increased the shear bond strength of GIC to composite resin; however, in RMGIC only laser etching resulted in significantly higher bond strength. These findings were supported by SEM results. The fracture mode was evaluated under a stereomicroscope at ×20.

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.

Self-etching adhesives: review of adhesion to tooth structure part II.

PubMed

Strydom, C

2005-02-01

Self-etching adhesives are steadily increasing in popularity among dental practitioners with their easy handling technique and their promise of no post-op sensitivity. As with any new bonding material, in vitro and in vivo investigations are required to assess the clinical efficacy of these systems. The current literature was reviewed to provide information on these systems, including the influence of their acidity and permeability on the quality of the bond, the role of water in long-term degradation of the bond in in vivo and in vitro studies, and the clinical efficacy of the self-etching adhesives in clinical research studies. Published abstracts, reviews, laboratory reports and clinical research papers in the dental literature. Very little information is available on self-etching systems pertaining to the long-term in vitro and in vivo durability of their bond and their medium- to long-term clinical outcome. Although post-op sensitivity seems to be something of the past, short-term clinical studies show that some self-etching adhesives do not perform as well as total-etch systems.

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

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.

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.

Photolithography-free laser-patterned HF acid-resistant chromium-polyimide mask for rapid fabrication of microfluidic systems in glass

NASA Astrophysics Data System (ADS)

Zamuruyev, Konstantin O.; Zrodnikov, Yuriy; Davis, Cristina E.

2017-01-01

Excellent chemical and physical properties of glass, over a range of operating conditions, make it a preferred material for chemical detection systems in analytical chemistry, biology, and the environmental sciences. However, it is often compromised with SU8, PDMS, or Parylene materials due to the sophisticated mask preparation requirements for wet etching of glass. Here, we report our efforts toward developing a photolithography-free laser-patterned hydrofluoric acid-resistant chromium-polyimide tape mask for rapid prototyping of microfluidic systems in glass. The patterns are defined in masking layer with a diode-pumped solid-state laser. Minimum feature size is limited to the diameter of the laser beam, 30 µm minimum spacing between features is limited by the thermal shrinkage and adhesive contact of the polyimide tape to 40 µm. The patterned glass substrates are etched in 49% hydrofluoric acid at ambient temperature with soft agitation (in time increments, up to 60 min duration). In spite of the simplicity, our method demonstrates comparable results to the other current more sophisticated masking methods in terms of the etched depth (up to 300 µm in borosilicate glass), feature under etch ratio in isotropic etch (~1.36), and low mask hole density. The method demonstrates high yield and reliability. To our knowledge, this method is the first proposed technique for rapid prototyping of microfluidic systems in glass with such high performance parameters. The proposed method of fabrication can potentially be implemented in research institutions without access to a standard clean-room facility.

Development of Novel Decontamination Techniques for Chemical Agents (GB, VX, HD) Contaminated Facilities. Phase 1. Identification and Evaluation of Novel Decontamination Concepts. Volume 2

DTIC Science & Technology

1983-02-01

Phosphoric, citric or other acids may be used as coupling agent/solvents in the cleaning tank. Decontamination solutions may also be used. Ultrasonics may be...111-54 "THERMAL DECOMPOSITION USING CO2 LASER . . . . . . . . . . . . . . 111-63 >’HYDROBLASTING. III-70 (-7, ACID ETCH/ NUTRALIZATION...111-192 NITRIC ACID . . .*. . . . .\\. . . . . . . . . . . . . . . TII-197 AMMONIA • • . . . • . . . . • . . . . . .... . ...... . 111-202 DANC .1

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.

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.

In situ chemical functionalization of gallium nitride with phosphonic acid derivatives during etching.

PubMed

Wilkins, Stewart J; Greenough, Michelle; Arellano, Consuelo; Paskova, Tania; Ivanisevic, Albena

2014-03-04

In situ functionalization of polar (c plane) and nonpolar (a plane) gallium nitride (GaN) was performed by adding (3-bromopropyl) phosphonic acid or propyl phosphonic acid to a phosphoric acid etch. The target was to modulate the emission properties and oxide formation of GaN, which was explored through surface characterization with atomic force microscopy, X-ray photoelectron spectroscopy, photoluminescence (PL), inductively coupled plasma-mass spectrometry, and water contact angle. The use of (3-bromopropyl) phosphonic acid and propyl phosphonic acid in phosphoric acid demonstrated lower amounts of gallium oxide formation and greater hydrophobicity for both sample sets, while also improving PL emission of polar GaN samples. In addition to crystal orientation, growth-related factors such as defect density in bulk GaN versus thin GaN films residing on sapphire substrates were investigated as well as their responses to in situ functionalization. Thin nonpolar GaN layers were the most sensitive to etching treatments due in part to higher defect densities (stacking faults and threading dislocations), which accounts for large surface depressions. High-quality GaN (both free-standing bulk polar and bulk nonpolar) demonstrated increased sensitivity to oxide formation. Room-temperature PL stands out as an excellent technique to identify nonradiative recombination as observed in the spectra of heteroepitaxially grown GaN samples. The chemical methods applied to tune optical and physical properties of GaN provide a quantitative framework for future novel chemical and biochemical sensor development.

Effects of attrition, prior acid-etching, and cyclic loading on the bond strength of a self-etching adhesive system to dentin.

PubMed

Shinkai, Koichi; Ebihara, Takashi; Shirono, Manabu; Seki, Hideaki; Wakaki, Suguru; Suzuki, Masaya; Suzuki, Shiro; Katoh, Yoshiroh

2009-03-01

The purpose of this study was to evaluate the effects of dentin attrition, phosphoric acid etching, and cyclic loading on the microtensile bond strength (microTBS) of a self-etching adhesive system to dentin. Flat dentin surfaces of human molars were assigned to eight experimental groups based on those with or without attrition, prior acid-etching, and cyclic loading. Resin composite paste was placed and polymerized after the bonding procedure according to manufacturer's instructions. The specimens were subjected to microTBS testing at a crosshead speed of 0.5 mm/min. Results showed that the minimum mean value of microTBS was 14.9 MPa in the group without attrition and acid-etching but with loading, while the maximum mean value of microTBS was 40.0 MPa in the group without attrition and loading but with acid etching. Therefore, the value of microTBS to dentin without attrition was significantly decreased by cyclic loading but that to dentin with attrition was not affected.

Improvement of enamel bond strengths for conventional and resin-modified glass ionomers: acid-etching vs. conditioning*

PubMed Central

Zhang, Ling; Tang, Tian; Zhang, Zhen-liang; Liang, Bing; Wang, Xiao-miao; Fu, Bai-ping

2013-01-01

Objective: This study deals with the effect of phosphoric acid etching and conditioning on enamel micro-tensile bond strengths (μTBSs) of conventional and resin-modified glass ionomer cements (GICs/RMGICs). Methods: Forty-eight bovine incisors were prepared into rectangular blocks. Highly-polished labial enamel surfaces were either acid-etched, conditioned with liquids of cements, or not further treated (control). Subsequently, two matching pre-treated enamel surfaces were cemented together with one of four cements [two GICs: Fuji I (GC), Ketac Cem Easymix (3M ESPE); two RMGICs: Fuji Plus (GC), RelyX Luting (3M ESPE)] in preparation for μTBS tests. Pre-treated enamel surfaces and cement-enamel interfaces were analyzed by scanning electron microscopy (SEM). Results: Phosphoric acid etching significantly increased the enamel μTBS of GICs/RMGICs. Conditioning with the liquids of the cements produced significantly weaker or equivalent enamel μTBS compared to the control. Regardless of etching, RMGICs yielded stronger enamel μTBS than GICs. A visible hybrid layer was found at certain enamel-cement interfaces of the etched enamels. Conclusions: Phosphoric acid etching significantly increased the enamel μTBSs of GICs/RMGICs. Phosphoric acid etching should be recommended to etch the enamel margins before the cementation of the prostheses such as inlays and onlays, using GICs/RMGICs to improve the bond strengths. RMGICs provided stronger enamel bond strength than GICs and conditioning did not increase enamel bond strength. PMID:24190447

Nanofabrication on monocrystalline silicon through friction-induced selective etching of Si3N4 mask

PubMed Central

2014-01-01

A new fabrication method is proposed to produce nanostructures on monocrystalline silicon based on the friction-induced selective etching of its Si3N4 mask. With low-pressure chemical vapor deposition (LPCVD) Si3N4 film as etching mask on Si(100) surface, the fabrication can be realized by nanoscratching on the Si3N4 mask and post-etching in hydrofluoric acid (HF) and potassium hydroxide (KOH) solution in sequence. Scanning Auger nanoprobe analysis indicated that the HF solution could selectively etch the scratched Si3N4 mask and then provide the gap for post-etching of silicon substrate in KOH solution. Experimental results suggested that the fabrication depth increased with the increase of the scratching load or KOH etching period. Because of the excellent masking ability of the Si3N4 film, the maximum fabrication depth of nanostructure on silicon can reach several microns. Compared to the traditional friction-induced selective etching technique, the present method can fabricate structures with lesser damage and deeper depths. Since the proposed method has been demonstrated to be a less destructive and flexible way to fabricate a large-area texture structure, it will provide new opportunities for Si-based nanofabrication. PMID:24940174

Observation of Biological Tissues Using Common Path Optical Coherence Tomography with Gold Coated Conical Tip Lens Fiber

NASA Astrophysics Data System (ADS)

Taguchi, K.; Sugiyama, J.; Totsuka, M.; Imanaka, S.

2012-03-01

In this paper, we proposed a high lateral resolution common-path Fourier domain optical coherence tomography(OCT) system with the use of a chemically etched single mode fiber. In our experiments, single mode optical fiber for 1310nm was used for preparing the tapered tips. Our system used a conical microlens that was chemically etched by selective chemical etching technique using an etching solution of buffered hydrofluoric acid (BHF). From experimental results, we verified that our proposed optical coherence tomography system could operate as a common-path Fourier domain OCT system and conical tip lens fiber was very useful for a high lateral resolution common-path Fourier domain OCT system. Furthermore, we could observe a surface of paramecium bursaria and symbiotic chlorella in the paramecium bursaria using gold coated conical-tip fiber in the water.

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.

Bond strength of a pit-and-fissure sealant associated to etch-and-rinse and self-etching adhesive systems to saliva-contaminated enamel: individual vs. simultaneous light curing.

PubMed

Gomes-Silva, Jaciara Miranda; Torres, Carolina Paes; Contente, Marta Maria Martins Giamatei; Oliveira, Maria Angélica Hueb de Menezes; Palma-Dibb, Regina Guenka; Borsatto, Maria Cristina

2008-01-01

This study evaluated in vitro the shear bond strength (SBS) of a resin-based pit-and-fissure sealant [Fluroshield (F), Dentsply/Caulk] associated with either an etch-and-rinse [Adper Single Bond 2 (SB), 3M/ESPE] or a self-etching adhesive system [Clearfil S3 Bond (S3), Kuraray Co., Ltd.] to saliva-contaminated enamel, comparing two curing protocols: individual light curing of the adhesive system and the sealant or simultaneous curing of both materials. Mesial and distal enamel surfaces from 45 sound third molars were randomly assigned to 6 groups (n=15), according to the bonding technique: I - F was applied to 37% phosphoric acid etched enamel. The other groups were contaminated with fresh human saliva (0.01 mL; 10 s) after acid etching: II - SB and F were light cured separately; III - SB and F were light cured together; IV - S3 and F were light cured separately; V - S3 and F were light cured simultaneously; VI - F was applied to saliva-contaminated, acid-etched enamel without an intermediate bonding agent layer. SBS was tested to failure in a universal testing machine at 0.5 mm/min. Data were analyzed by one-way ANOVA and Fisher's test (alpha=0.05).The debonded specimens were examined with a stereomicroscope to assess the failure modes. Three representative specimens from each group were observed under scanning electron microscopy for a qualitative analysis. Mean SBS in MPa were: I-12.28 (+/-4.29); II-8.57 (+/-3.19); III-7.97 (+/-2.16); IV-12.56 (+/-3.11); V-11.45 (+/-3.77); and VI-7.47 (+/-1.99). In conclusion, individual or simultaneous curing of the intermediate bonding agent layer and the resin sealant did not seem to affect bond strength to saliva-contaminated enamel. S3/F presented significantly higher SBS than the that of the groups treated with SB etch-and-rinse adhesive system and similar SBS to that of the control group, in which the sealant was applied under ideal dry, noncontaminated conditions.

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 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

An Ex-vivo Shear and tensile bond strengths of orthodontic molar tubes bonded using different techniques.

PubMed

Abu-Alhaija, Elham; Jaradat, Mohammad; Alwahadni, Ahed

2017-03-01

Molar bonding procedures need continuous improvement to be widely accepted clinically and eventually replace molar bands. The purpose of this study was to determine the effects of enamel micro-abrasion and silane coating of the base of molar tubes on shear and tensile bond strengths of orthodontic molar tubes. A total of 200 third molars were randomly allocated into five groups of 40 teeth as follows: group 1: molar tubes bonded to etched teeth (37% phosphoric acid gel; control group); group 2: molar tubes bonded to etched teeth (37% phosphoric acid) with the addition of silane to the base of molar tubes; group 3: molar tubes bonded to teeth pre-treated with 18% hydrochloric acid and pumice (micro-abrasion); group 4: molar tubes bonded to teeth pre-treated with microabrasion with the addition of silane to the base of molar tubes; group 5: molar tubes bonded to teeth pre-treated with microabrasion before conventional acid etching combined with the addition of silane to the base of molar tubes. The bond strength testing was performed using a computer control electromechanical universal testing machine. The highest mean shear and tensile bond strengths were recorded in group 5 (13.81±2.54MPa and 13.97±2.29 MPa, respectively). Micro-abrasion alone (group 3) and the combination of enamel micro-abrasion and the addition of silane (group 4) produced bond strength values comparable to the control. Enamel surface pre-treatment (micro abrasion) before conventional acid etching combined with the addition of silane to the base of the molar tube produced the highest bond strengths among all tested groups. Key words: Molar, shear strength, tensile strength, orthodontic appliances.

An Ex-vivo Shear and tensile bond strengths of orthodontic molar tubes bonded using different techniques

PubMed Central

Alwahadni, Ahed

2017-01-01

Background Molar bonding procedures need continuous improvement to be widely accepted clinically and eventually replace molar bands. Material and Methods The purpose of this study was to determine the effects of enamel micro-abrasion and silane coating of the base of molar tubes on shear and tensile bond strengths of orthodontic molar tubes. A total of 200 third molars were randomly allocated into five groups of 40 teeth as follows: group 1: molar tubes bonded to etched teeth (37% phosphoric acid gel; control group); group 2: molar tubes bonded to etched teeth (37% phosphoric acid) with the addition of silane to the base of molar tubes; group 3: molar tubes bonded to teeth pre-treated with 18% hydrochloric acid and pumice (micro-abrasion); group 4: molar tubes bonded to teeth pre-treated with microabrasion with the addition of silane to the base of molar tubes; group 5: molar tubes bonded to teeth pre-treated with microabrasion before conventional acid etching combined with the addition of silane to the base of molar tubes. The bond strength testing was performed using a computer control electromechanical universal testing machine. Results The highest mean shear and tensile bond strengths were recorded in group 5 (13.81±2.54MPa and 13.97±2.29 MPa, respectively). Micro-abrasion alone (group 3) and the combination of enamel micro-abrasion and the addition of silane (group 4) produced bond strength values comparable to the control. Conclusions Enamel surface pre-treatment (micro abrasion) before conventional acid etching combined with the addition of silane to the base of the molar tube produced the highest bond strengths among all tested groups. Key words:Molar, shear strength, tensile strength, orthodontic appliances. PMID:28298990

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.

Electron and Light Microscopy Techniques Suitable for Studying Fatigue Damage in a Crystallized Glass Ceramic

NASA Technical Reports Server (NTRS)

Harrell, Shelley; Zaretsky, Erwin V.

1961-01-01

The crystals of Pyroceram are randomly oriented and highly reflective so that standard microscopy techniques are not satisfactory for studying this material. Standard replicating procedures proved difficult to use. New microscopy techniques and procedures have therefore been developed. A method for locating, orienting, and identifying specific areas to be viewed with an electron microscope is described. This method not require any special equipment. Plastic replicas were found to be unsatisfactory because of their tendency to adhere to Pryoceram. This caused them to tear when released or resulted in artifacts. Preshadowed silicon monoxide replicas were satisfactory but required a releasing agent. A method of depositing the releasing agent is described. To polish specimens without evidence of fire-polishing, it was found necessary to use a vibratory polishing technique. Chrome oxide was used as the abrasive and either water or kerosene as the lubricant. Vibratory polishing is extremely slow, but surfaces so polished show no evidence of fire polishing, even when examined by electron microscopy. The most satisfactory etching process used for Pyroceram 9608 consisted of a primary etch of 5 milliliters of hydrochloric acid (concentrated), 5 milliliters of hydrogen fluoride (45 percent), and 45 milliliters of water, and a secondary etch with methyl alcohol replacing the water. Best results were obtained with total etching times from 25 to 30 seconds. Staining of the Pyroceram surface with a Sanford's marker was found to be an expedient way to reduce the glare of reflected light.

Smart Pixels for Optical Processing and Communications: Design, Models, Fabrication and Test

DTIC Science & Technology

1998-06-01

11.3 Mobility-Lifetime Product 115 11.4 P-IforVCSEL 116 Chapter 12: Developing a Reliable Etch 12.1 Etch Rates and Selectivity for Citric Acid 126...eGa0.4As etch-stop layer beneath the GaAs buffer. The gate recess was performed with a timed citric acid / hydrogen peroxide wet etch. The conducting...alkalinity. The wet etchant tested in this effort was a citric acid / hydrogen peroxide mixture,8൓ due to its availability, ease of preparation

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.

Carbon Nanotube Spaceframes for Low-Density Aerospace Materials

DTIC Science & Technology

2012-01-26

different types of oxidative etching chemistries have been reported in the literature, with acidic conditions such as nitric acid etching and piranha...and reduce the production of adhered fulvic acid species.1 A range of RCA type different etching conditions were investigated involving different...carboxylic and hydroxyl type sites together by first using a dicarboxylic acid (preferably in a highly reactive form such as oxalic chloride or succinic

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.

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.

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

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.

Technology development for phosphoric acid fuel cell powerplant, phase 2

NASA Technical Reports Server (NTRS)

Christner, L.

1979-01-01

A technique for producing an acid inventory control member by spraying FEP onto a partially screened carbon paper backing is discussed. Theoretical analysis of the acid management indicates that the vapor composition of 103% H3PO4 is approximately 1.0 ppm P4O10. An SEM evaluation of corrosion resistance of phenolic resins and graphite/phenolic resin composites in H3PO4 at 185 C shows specific surface etching. Carbonization of graphite/phenolic bipolar plates is achieved without blistering.

Effect of reducing acid etching time on bond strength to noncarious and caries-affected primary and permanent dentin.

PubMed

Scheffel, Débora Lopes Salles; Ricci, Hérica Adad; de Souza Costa, Carlos Alberto; Pashley, David Henry; Hebling, Josimeri

2013-01-01

The purpose was to evaluate the effect of acid etching time on the bond strength of a simplified etch-and-rinse adhesive system to noncarious and caries-affected dentin of primary and permanent teeth. Twenty-four extracted primary and permanent teeth were divided into three groups, according to the acid etching time. Four teeth from each group were exposed to a microbiological caries-inducing protocol. After caries removal, noncarious and caries-affected dentin surfaces were etched with 37 percent phosphoric acid for five, 10, or 15 seconds prior to the application of Prime & Bond NT adhesive. Crowns were restored with resin composite and prepared for microtensile testing. Data were submitted to Kruskal-Wallis and Mann-Whitney tests (α=0.05). Higher bond strengths were obtained for noncarious dentin vs. caries-affected dentin for both primary and permanent teeth. Reducing the acid etching time from 15 to five seconds did not affect the bond strength to caries-affected or noncarious dentin in primary teeth. For permanent teeth, lower bond strength values were observed when the noncarious dentin was etched for five seconds, while no difference was seen between 10 and 15 seconds. For Prime & Bond NT, the etching of dentin for five seconds could be recommended for primary teeth, while 10 seconds would be the minimum time for permanent teeth.

Sputtered gold mask for deep chemical etching of silicon

NASA Technical Reports Server (NTRS)

Pisciotta, B. P.; Gross, C.; Olive, R. S.

1975-01-01

Sputtered mask resists chemical attack from acid and has adherence to withstand prolonged submergence in etch solution without lifting from silicon surface. Even under prolonged etch conditions with significant undercutting, gold mask maintained excellent adhesion to silicon surface and imperviousness to acid.

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

Effects of a pulsed Nd:YAG laser on enamel and dentin

NASA Astrophysics Data System (ADS)

Myers, Terry D.

1990-06-01

Enamel and dentin samples were exposed extraorally to a pulsed neodymium yttriuma1uminumgarnet (Nd:YAG) laser. The lased samples were observed using both scanning electron microscopy and histological techniques to determine the effects of the laser. The present study has provided the following points: (1) Properly treated, enamel can be 1aser etched to a depth comparable to that achieved with phosphoric acid etching; and (2) both carious and noncarious dentin can be vaporized by the Nd:YAG laser. No cracking or chipping of any enamel or dentin sample was observed histologically or under the SEM.

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.

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.

Comparison of shear bond strength and surface structure between conventional acid etching and air-abrasion of human enamel.

PubMed

Olsen, M E; Bishara, S E; Damon, P; Jakobsen, J R

1997-11-01

Recently, air-abrasion technology has been examined for potential applications within dentistry, including the field of orthodontics. The purpose of this study was to compare the traditional acid-etch technique with an air-abrasion surface preparation technique, with two different sizes of abrading particles. The following parameters were evaluated: (a) shear bond strength, (b) bond failure location, and (c) enamel surface preparation, as viewed through a scanning electron microscope. Sixty extracted human third molars were pumiced and divided into three groups of 20. The first group was etched with a 37% phosphoric acid gel for 30 seconds, rinsed for 30 seconds, and dried for 20 seconds. The second and third groups were air-abraded with (a) a 50 microm particle and (b) a 90 microm particle of aluminum oxide, with the Micro-etcher microabrasion machine (Danville Engineering Inc.). All three groups had molar stainless steel orthodontic brackets bonded to the buccal surface of each tooth with Transbond XT bonding system (3M Unitek). A Zwick Universal Testing Machine (Calitek Corp.) was used to determine shear bond strengths. The analysis of variance was used to compare the three groups. The Adhesive Remnant Index (ARI) was used to evaluate the residual adhesive on the enamel after bracket removal. The chi square test was used to evaluate differences in the ARI scores among the groups. The significance for all tests was predetermined at p < or = 0.05. The results indicated that there was a significant difference in shear bond strength among the three groups (p = 0.0001). The Duncan Multiple Range test showed a significant decrease in shear bond strength in the air-abraded groups. The chi square test revealed significant differences among the ARI scores of the acid-etched group and the air-abraded groups (chi(2) = 0.0001), indicating no adhesive remained on the enamel surface after debonding when air-abrasion was used. In conclusion, the current findings indicate that enamel surface preparation using air-abrasion results in a significant lower bond strength and should not be advocated for routine clinical use as an enamel conditioner at this time.

Process for etching mixed metal oxides

DOEpatents

Ashby, Carol I. H.; Ginley, David S.

1994-01-01

An etching process using dicarboxylic and tricarboxylic acids as chelating etchants for mixed metal oxide films such as high temperature superconductors and ferroelectric materials. Undesirable differential etching rates between different metal oxides are avoided by selection of the proper acid or combination of acids. Feature sizes below one micron, excellent quality vertical edges, and film thicknesses in the 100 Angstom range may be achieved by this method.

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.

Effect of different surface treatments on the push-out bond strength of fiber post to root canal dentin.

PubMed

Demiryürek, Ebru Ozsezer; Külünk, Safak; Saraç, Duygu; Yüksel, Gözde; Bulucu, Bilinç

2009-08-01

The purpose of this study was to evaluate the effects of different surface treatments on the bond strength of a fiber post to dentin. Sixty extracted human maxillary incisor teeth were manually shaped with K-files using the step-back technique. ISO size 45 files were used as master apical files. Post spaces were prepared and then the root canals were subjected to one of the following 5 surface treatments: irrigation with 5% sodium hypochlorite (NaOCl); treatment with ethanol, ethyl acetate, and acetone-based cleansing agent (Sikko Tim); irrigation with 17% EDTA; etching with 37% orthophosphoric acid for 15 seconds; and etching with 10% citric acid for 15 seconds. Fiber posts were luted using self-etching/self-priming dual polymerized resin cement. From the coronal part of each root, 3 slides of 0.6-mm thickness were obtained. A push-out bond strength test was performed by a universal testing machine at a crosshead speed of 0.5 mm/min. Dentin surfaces were examined under scanning electron microscopy (SEM) after different surface treatments. Data were analyzed with a one-way analysis of variance (ANOVA) and Tukey HSD test. ANOVA revealed that canal surface treatment affected the bond strength (P < .001). The highest bond strength was obtained in the Sikko Tim group. The results also showed that surface treatment methods increased the bond strength to dentin when compared with the control group. Sikko Tim group was the more effective surface treatment agent compared with EDTA, orthophosphoric acid, citric acid, and control groups; however, it could not remove the smear layer and sealer remnants effectively on radicular dentin surfaces. Removal of the smear layer and opening of dentinal tubules are not recommended when a self-etching/self-priming adhesive system is used.

Effect of different monomer-based composites and acid etching pre-treatment of enamel on the microleakage using self-etch adhesives systems.

PubMed

Catelan, Anderson; Giorgi, Maria Cecília Caldas; Soares, Giulliana Panfiglio; Lima, Debora Alves Nunes Leite; Marchi, Giselle Maria; Aguiar, Flávio Henrique Baggio

2014-11-01

To evaluate quantitatively the marginal microleakage of restorations carried out with self-etching adhesives with or without prior phosphoric enamel acid etching of silorane or methacrylate resin-based composite restorations subjected to thermal cycling. Forty cavities were prepared at the proximal surface of bovine incisors and randomly divided according to the etching of the enamel and restorative system used. The groups were restored with methacrylate [Adper SE Plus adhesive (3M ESPE) + Filtek Z250 (3M ESPE)] or silorane [Filtek LS adhesive (3M ESPE) + Filtek LS composite (3M ESPE)] restorative systems, light-cured using a LED unit (Bluephase 16i, Vivadent). After restorative procedure and thermocycling (1000 cycles), the specimens were immersed in methylene blue for 2 h. The specimens were triturated and the powder was used for analysis in an absorbance spectrophotometer. Data were statistically analyzed by 2-way ANOVA (alpha = 0.05). No statistical difference between the restorative materials tested with or without previous acid etching of enamel in Class II marginal microleakage was observed (p > 0.05). The use of acid etching prior to self-etching adhesives did not interfere on the microleakage of methacrylate- or silorane-based restorations.

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.

The acid-base resistant zone in three dentin bonding systems.

PubMed

Inoue, Go; Nikaido, Toru; Foxton, Richard M; Tagami, Junji

2009-11-01

An acid-base resistant zone has been found to exist after acid-base challenge adjacent to the hybrid layer using SEM. The aim of this study was to examine the acid-base resistant zone using three different bonding systems. Dentin disks were applied with three different bonding systems, and then a resin composite was light-cured to make dentin disk sandwiches. After acid-base challenge, the polished surfaces were observed using SEM. For both one- and two-step self-etching primer systems, an acid-base resistant zone was clearly observed adjacent to the hybrid layer - but with differing appearances. For the wet bonding system, the presence of an acid-base resistant zone was unclear. This was because the self-etching primer systems etched the dentin surface mildly, such that the remaining mineral phase of dentin and the bonding agent yielded clear acid-base resistant zones. In conclusion, the acid-base resistant zone was clearly observed when self-etching primer systems were used, but not so for the wet bonding system.

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

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.

Process for etching mixed metal oxides

DOEpatents

Ashby, C.I.H.; Ginley, D.S.

1994-10-18

An etching process is described using dicarboxylic and tricarboxylic acids as chelating etchants for mixed metal oxide films such as high temperature superconductors and ferroelectric materials. Undesirable differential etching rates between different metal oxides are avoided by selection of the proper acid or combination of acids. Feature sizes below one micron, excellent quality vertical edges, and film thicknesses in the 100 Angstrom range may be achieved by this method. 1 fig.

Influence of implant surface topography on bone-regenerative potential and mechanical retention in the human maxilla and mandible.

PubMed

Wei, Niu; Bin, Shi; Jing, Zhou; Wei, Sun; Yingqiong, Zhao

2014-06-01

To evaluate the short- and mid-term effects of commercial pure (cp) titanium implant surface topography on osseointegration, bone-regenerative potential and mechanical retention in the human maxilla and mandible. 32 micro-implants with the same geometry but with four different surface treatments were implanted in the maxilla and mandible of eight patients. Each patient received four micro-implants, one of each type. Percentage of bone-to-implant contact analysis and histological evaluation was carried 3, 6 and 12 weeks after implantation. Furthermore, reverse removal torque tests were conducted 3 and 6 weeks after implantation to analyze functional bone attachment. Implant surfaces tested were: machined, grit-blasted, acid-etched, and grit-blasted with acid-etch. One-way ANOVA was performed using the multiple comparison Fisher's test to determine significance of observed differences among test groups. The level of significance was established at 5% (P < 0.05). Mean and standard deviations of the test groups were calculated. Surface roughness had a significant correlation with the evolution of bone regeneration. The surfaces with roughness Ra approximately 4 microim (grit-blasted and grit-blasted with acid-etch), showed rapid tissue colonization compared to machine and acid-etched surfaces. The results of reverse removal torque tests confirmed a significant correlation between surface roughness and functional bone attachment. Grit-blasted and grit-blasted with acid etched surfaces showed higher retention values compared to machine and acid-etched implants. This finding was supported by higher bone-to-implant contact observed for rougher surfaces (grit-blasted and grit-blasted with acid etching).

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.

Membrane Structure: Spin Labeling and Freeze Etching of Mycoplasma laidlawii*

PubMed Central

Tourtellotte, Mark E.; Branton, Daniel; Keith, Alec

1970-01-01

A spin-labeled fatty acid was incorporated in vivo into the polar lipids of Mycoplasma laidlawii membranes. The electron paramagnetic resonance signal from either intact cells or their extracted lipids reflected the fatty acid composition of the Mycoplasma membranes. Comparison of signals from intact cells, gramicidin-treated cells, heat-treated cells, and extracted lipids indicates that a major portion of the membrane lipids is in a semiviscous hydrocarbon environment. The results also show that the spin label in the intact membrane is slightly but significantly less mobile than it is in protein-free lipid extracts made from these membranes. Correlated electron microscope examinations using the freeze-etch technique reveal particulate components in the hydrophobic region of the membrane. The mobility of the lipids in the intact cell membrane may be influenced by their association with these particles. Images PMID:4316683

Ultra-Shallow Depth Profiling of Arsenic Implants in Silicon by Hydride Generation-Inductively Coupled Plasma Atomic Emission Spectrometry

NASA Astrophysics Data System (ADS)

Matsubara, Atsuko; Kojima, Hisao; Itoga, Toshihiko; Kanehori, Keiichi

1995-08-01

High resolution depth profiling of arsenic (As) implanted into silicon wafers by a chemical technique is described. Silicon wafers are precisely etched through repeated oxidation by hydrogen peroxide solution and dissolution of the oxide by hydrofluoric acid solution. The etched silicon thickness is determined by inductively-coupled plasma atomic emission spectrometry (ICP-AES). Arsenic concentration is determined by hydride generation ICP-AES (HG-ICP-AES) with prereduction using potassium iodide. The detection limit of As in a 4-inch silicon wafer is 2.4×1018 atoms/cm3. The etched silicon thickness is controlled to less than 4±2 atomic layers. Depth profiling of an ultra-shallow As diffusion layer with the proposed method shows good agreement with profiling using the four-probe method or secondary ion mass spectrometry.

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.

Enamel resistance to demineralization following Er:YAG laser etching for bonding orthodontic brackets

PubMed Central

Ahrari, Farzaneh; Poosti, Maryam; Motahari, Pourya

2012-01-01

Background: Several studies have shown that laser-etching of enamel for bonding orthodontic brackets could be an appropriate alternative for acid conditioning, since a potential advantage of laser could or might be caries prevention. This study compared enamel resistance to demineralization following etching with acid phosphoric or Er:YAG laser for bonding orthodontic brackets. Materials and Methods: Fifty sound human premolars were divided into two equal groups. In the first group, enamel was etched with 37% phosphoric acid for 15 seconds. In the second group, Er:YAG laser (wavelength, 2 940 nm; 300 mJ/pulse, 10 pulses per second, 10 seconds) was used for tooth conditioning. The teeth were subjected to 4-day PH-cycling process to induce caries-like lesions. The teeth were then sectioned and the surface area of the lesion was calculated in each microphotographs and expressed in pixel. The total surface of each specimen was 196 608 pixels. Results: Mean lesion areas were 7 171 and 7532 pixels for Laser-etched and Acid-etched groups, respectively. The two sample t-test showed that there was no significant difference in lesion area between the two groups (P = 0.914). Conclusion: Although Er:YAG laser seems promising for etching enamel before bonding orthodontic brackets, it does not reduce enamel demineralization when exposed to acid challenge. PMID:23162591

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.

The immediate and long-term effects of invasive and noninvasive pit and fissure sealing techniques on the microflora in occlusal fissures of human teeth.

PubMed

Kramer, P F; Zelante, F; Simionato, M R

1993-01-01

The purpose of this study was to evaluate the effect of acid conditioning and occlusal sealant on microbial colonization of pit and fissures submitted to ameloplasty or left intact. Human enamel blocks containing fissures prepared from the occlusal surfaces of unerupted third molars were implanted in occlusal fillings in molars of 12 patients for seven, 30, 60, and 120 days. After seven days of exposure to the oral environment, the pit and fissure blocks were removed and found to be colonized, mainly with gram-positive coccal flora. The acid-etching procedure itself reduced the number of cultivable microorganisms by about 95%. Subsequent application of occlusal sealant caused a gradual decrease of the remaining viable microorganism throughout the experiment. Despite the decrease of 100% after acid etching in most of the fissures submitted to ameloplasty, the occlusal sealant did not lead to a subsequent significant reduction.

Morphological and chemical characterization of the dentin/resin cement interface produced with a self-etching primer.

PubMed

Walker, Mary P; Wang, Yong; Spencer, Paulette

2002-01-01

The purpose of this study was to analyze a resin cement/dentin interface by comparing the diffusion of a resin cement into dentin surfaces pretreated with a self-etching primer with or without pretreatment by conventional acid etching. Dentin surfaces of 8 unerupted human third molars were treated with a self-etch primer (Panavia 21) with or without conventional phosphoric acid pretreatment. Panavia 21 resin cement was applied according to manufacturer's instructions. Dentin/resin cement interface sections from each tooth were examined with scanning electron microscopy and micro-Raman spectroscopy. When the self-etch primer was used following conventional acid pretreatment, the resin cement did not penetrate to the depth of the zone of demineralized dentin, leaving a substantial area of exposed dentin matrix at the dentin/cement interface. In contrast, there was substantial resin cement diffusion throughout the demineralized dentin when the self-etch primer was used without acid etching pretreatment. The in vitro evaluation of resin cement penetration throughout the zone of demineralized dentin is an important step in identifying sites of exposed dentin matrix that may promote postoperative sensitivity and may leave the dentin/resin cement interface vulnerable to premature degradation under clinical conditions. In this study, the self-etch primer used alone produced substantial resin cement penetration and left no exposed dentin matrix at the dentin/resin cement interface.

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.

Controlled core removal from a D-shaped optical fiber.

PubMed

Markos, Douglas J; Ipson, Benjamin L; Smith, Kevin H; Schultz, Stephen M; Selfridge, Richard H; Monte, Thomas D; Dyott, Richard B; Miller, Gregory

2003-12-20

The partial removal of a section of the core from a continuous D-shaped optical fiber is presented. In the core removal process, selective chemical etching is used with hydrofluoric (HF) acid. A 25% HF acid solution removes the cladding material above the core, and a 5% HF acid solution removes the core. A red laser with a wavelength of 670 nm is transmitted through the optical fiber during the etching. The power transmitted through the optical fiber is correlated to the etch depth by scanning electron microscope imaging. The developed process provides a repeatable method to produce an optical fiber with a specific etch depth.

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.

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.

Evaluating EDTA as a substitute for phosphoric acid-etching of enamel and dentin.

PubMed

Imbery, Terence A; Kennedy, Matthew; Janus, Charles; Moon, Peter C

2012-01-01

Matrix metalloproteinases (MMPs) are proteolytic enzymes released when dentin is acid-etched. The enzymes are capable of destroying unprotected collagen fibrils that are not encapsulated by the dentin adhesive. Chlorhexidine applied after etching inhibits the activation of released MMPs, whereas neutral ethylenediamine tetra-acetic acid (EDTA) prevents the release of MMPs. The purpose of this study was to determine if conditioning enamel and dentin with EDTA can be a substitute for treating acid-etching enamel and dentin with chlorhexidine. A column of composite resin was bonded to enamel and dentin after conditioning. Shear bond strengths were evaluated after 48 hours and after accelerated aging for three hours in 12% sodium hypochlorite. Shear bond strengths ranged from 15.6 MP a for accelerated aged EDTA enamel specimens to 26.8 MPa for dentin conditioned with EDTA and tested after 48 hours. A three-way ANOVA and a Tukey HSD test found statistically significant differences among the eight groups and the three independent variables (P < 0.05). EDTA was successfully substituted for phosphoric acid-etched enamel and dentin treated with chlorhexidine. Interactions of conditioning agent and aging were significant for dentin but not for enamel. In an effort to reduce the detrimental effects of MMPs, conditioning enamel and dentin with EDTA is an alternative to treating acid-etched dentin and enamel with chlorhexidine.

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.

Effects of a non-rinse conditioner on the enamel of primary teeth.

PubMed

Fava, Marcelo; Myaki, Silvio Issáo; Arana-Chavez, Victor Elias; Fava-de-Moraes, Flavio

2003-01-01

The aim of this in vitro study was to evaluate by scanning electron microscopy the morphological aspects of the enamel of primary teeth after etching with 36% phosphoric acid or a non-rinse conditioner. Ten naturally exfoliated anterior primary teeth were selected. The samples were subjected to prophylaxis with pumice paste and water using a low-speed hand piece. Etching was done on the buccal surface. Specimens were divided into 2 groups: G1 (n=10): etching with 36% phosphoric acid gel - Conditioner 36 (Dentsply) for 20 s, followed by water rinse for 15 s; G2 (n=10): etching with NRC - Non Rinse Conditioner (Dentsply) for 20 s, followed by air drying for 15 s. The samples were dehydrated, mounted on metal stubs, coated with gold and observed with Jeol JSM-6100 scanning electron microscope. Electron-micrographic analysis showed that both etching agents were effective for etching the enamel of primary teeth causing the formation of microporosities on the enamel surface, although the etching pattern was more effective with the use of 36% phosphoric acid gel.

Acid Etching and Plasma Sterilization Fail to Improve Osseointegration of Grit Blasted Titanium Implants

PubMed Central

Saksø, Mikkel; Jakobsen, Stig S; Saksø, Henrik; Baas, Jørgen; Jakobsen, Thomas; Søballe, Kjeld

2012-01-01

Interaction between implant surface and surrounding bone influences implant fixation. We attempted to improve the bone-implant interaction by 1) adding surface micro scale topography by acid etching, and 2) removing surface-adherent pro-inflammatory agents by plasma cleaning. Implant fixation was evaluated by implant osseointegration and biomechanical fixation. The study consisted of two paired animal sub-studies where 10 skeletally mature Labrador dogs were used. Grit blasted titanium alloy implants were inserted press fit in each proximal tibia. In the first study grit blasted implants were compared with acid etched grit blasted implants. In the second study grit blasted implants were compared with acid etched grit blasted implants that were further treated with plasma sterilization. Implant performance was evaluated by histomorphometrical investigation (tissue-to-implant contact, peri-implant tissue density) and mechanical push-out testing after four weeks observation time. Neither acid etching nor plasma sterilization of the grit blasted implants enhanced osseointegration or mechanical fixation in this press-fit canine implant model in a statistically significant manner. PMID:22962567

Effect of phosphate treatment of Acid-etched implants on mineral apposition rates near implants in a dog model.

PubMed

Foley, Christine Hyon; Kerns, David G; Hallmon, William W; Rivera-Hidalgo, Francisco; Nelson, Carl J; Spears, Robert; Dechow, Paul C; Opperman, Lynne A

2010-01-01

This study evaluated the effects of phosphate coating of acid-etched titanium on the mineral apposition rate (MAR) and new bone-to-implant contact (BIC) in a canine model. Titanium implants (2.2 3 4 mm) with acid-etched surfaces that were electrolytically phosphated or not were placed in 48 mandibular sites in six foxhounds. Tetracycline and calcein dyes were administered 1 week after implant placement and 1 week before sacrifice. At 12 weeks after implant placement, the animals were sacrificed. MAR and BIC were evaluated using fluorescence microscopy. Light microscopic and histologic evaluations were performed on undecalcified sections. Microscopic evaluation showed the presence of healthy osteoblasts lining bone surfaces near implants. Similar BIC was observed in phosphated and nonphosphated titanium implant sites. MAR was significantly higher around the nonphosphated titanium implant surfaces than around the phosphated titanium samples. No significant differences were found between dogs or implant sites. Acid-etched implants showed significantly higher MARs compared to acid-etched, phosphate-coated implants. Int J Maxillofac Implants 2010;25:278-286.

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.

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

Liquid droplet sensing using twisted optical fiber couplers fabricated by hydrofluoric acid flow etching

NASA Astrophysics Data System (ADS)

Son, Gyeongho; Jung, Youngho; Yu, Kyoungsik

2017-04-01

We report a directional-coupler-based refractive index sensor and its cost-effective fabrication method using hydrofluoric acid droplet wet-etching and surface-tension-driven liquid flows. The proposed fiber sensor consists of a pair of twisted tapered optical fibers with low excess losses. The fiber cores in the etched microfiber region are exposed to the surrounding medium for efficient interaction with the guided light. We observe that the etching-based low-loss fiber-optic sensors can measure the water droplet volume by detecting the refractive index changes of the surrounding medium around the etched fiber core region.

Evaluation of the bond strength of resin cements used to lute ceramics on laser-etched dentin.

PubMed

Giray, Figen Eren; Duzdar, Lale; Oksuz, Mustafa; Tanboga, Ilknur

2014-07-01

The purpose of this study was to investigate the shear bond strength (SBS) of two different adhesive resin cements used to lute ceramics on laser-etched dentin. Erbium, chromium: yttrium, scandium, gallium, garnet (Er,Cr:YSGG) laser irradiation has been claimed to improve the adhesive properties of dentin, but results to date have been controversial, and its compatibility with existing adhesive resin cements has not been conclusively determined. Two adhesive cements, one "etch-and-rinse" [Variolink II (V)] and one "self-etch" [Clearfil Esthetic Cement (C)] luting cement, were used to lute ceramic blocks (Vita Celay Blanks, Vita) onto dentin surfaces. In total, 80 dentin specimens were distributed randomly into eight experimental groups according to the dentin surface-etching technique used Er,Cr:YSGG laser and Er:YAG laser: (1) 37% orthophosphoric acid+V (control group), (2) Er,Cr:YSGG laser+V, (3) Er,Cr:YSGG laser+acid+V, (4) Er:YAG laser+V, (5) Er:YAG laser+acid+V, (6) C, (7) Er,Cr:YSGG laser+C, and (8) Er:YAG laser+C. Following these applications, the ceramic discs were bonded to prepared surfaces and were shear loaded in a universal testing machine until fracture. SBS was recorded for each group in MPa. Shear test values were evaluated statistically using the Mann-Whitney U test. No statistically significant differences were evident between the control group and the other groups (p>0.05). The Er,Cr:YSGG laser+A+V group demonstrated significantly higher SBS than did the Er,Cr:YSGG laser+V group (p=0.034). The Er,Cr:YSGG laser+C and Er:YAG laser+C groups demonstrated significantly lower SBS than did the C group (p<0.05). Dentin surfaces prepared with lasers may provide comparable ceramic bond strengths, depending upon the adhesive cement used.

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

Adhesion of resin composite core materials to dentin.

PubMed

O'Keefe, K L; Powers, J M

2001-01-01

This study determined (1) the effect of polymerization mode of resin composite core materials and dental adhesives on the bond strength to dentin, and (2) if dental adhesives perform as well to dentin etched with phosphoric acid as to dentin etched with self-etching primer. Human third molars were sectioned 2 mm from the highest pulp horn and polished. Three core materials (Fluorocore [dual cured], Core Paste [self-cured], and Clearfil Photo Core [light cured]) and two adhesives (Prime & Bond NT Dual Cure and Clearfil SE Bond [light cured]) were bonded to dentin using two dentin etching conditions. After storage, specimens were debonded in microtension and bond strengths were calculated. Scanning electron micrographs of representative bonding interfaces were analyzed. Analysis showed differences among core materials, adhesives, and etching conditions. Among core materials, dual-cured Fluorocore had the highest bond strengths. There were incompatibilities between self-cured Core Paste and Prime & Bond NT in both etched (0 MPa) and nonetched (3.0 MPa) dentin. Among adhesives, in most cases Clearfil SE Bond had higher bond strengths than Prime & Bond NT and bond strengths were higher to self-etched than to phosphoric acid-etched dentin. Scanning electron micrographs did not show a relationship between resin tags and bond strengths. There were incompatibilities between a self-cured core material and a dual-cured adhesive. All other combinations of core materials and adhesives produced strong in vitro bond strengths both in the self-etched and phosphoric acid-etched conditions.

AFM and SEM study of the effects of etching on IPS-Empress 2 TM dental ceramic

NASA Astrophysics Data System (ADS)

Luo, X.-P.; Silikas, N.; Allaf, M.; Wilson, N. H. F.; Watts, D. C.

2001-10-01

The aim of this study was to investigate the effects of increasing etching time on the surface of the new dental material, IPS-Empress 2 TM glass ceramic. Twenty one IPS-Empress 2 TM glass ceramic samples were made from IPS-Empress 2 TM ingots through lost-wax, hot-pressed ceramic fabrication technology. All samples were highly polished and cleaned ultrasonically for 5 min in acetone before and after etching with 9.6% hydrofluoric acid gel. The etching times were 0, 10, 20, 30, 60, 90 and 120 s respectively. Microstructure was analysed by scanning electron microscopy (SEM) and atomic force microscopy (AFM) was used to evaluate the surface roughness and topography. Observations with SEM showed that etching with hydrofluoric acid resulted in preferential dissolution of glass matrix, and that partially supported crystals within the glass matrix were lost with increasing etching time. AFM measurements indicated that etching increased the surface roughness of the glass-ceramic. A simple least-squares linear regression was used to establish a relationship between surface roughness parameters ( Ra, RMS), and etching time, for which r2>0.94. This study demonstrates the benefits of combining two microscopic methods for a better understanding of the surface. SEM showed the mode of action of hydrofluoric acid on the ceramic and AFM provided valuable data regarding the extent of surface degradation relative to etching time.

Assessment of microleakage of class V restored by resin composite and resin-modified glass ionomer and pit and fissure resin-based sealants following Er:YAG laser conditioning and acid etching: in vitro study

PubMed Central

Luong, Emilie; Shayegan, Amir

2018-01-01

Aim The aim of this study was to make a comparison between microleakage of conventionally restored class V cavities using acid etchant and the ones conditioned by erbium-doped yttrium aluminum garnet (Er:YAG) laser, and also to assess and compare the effectiveness of enamel surface treatments of occlusal pits and fissures by acid etching and conditioned by Er:YAG laser-etch. Materials and methods Seventy-two extracted third molars were used in this study. The samples were divided into two major groups: class V cavities and pit and fissure sealants. Each subgroup was divided into conventional acid etching, Er:YAG laser conditioning and conventional acid etching, and combination with Er:YAG laser conditioning (n=12). The teeth were placed in 2% methylene blue dye solution, were sectioned, and were evaluated according to the dye penetration criteria. Two samples per subgroup were chosen for scanning electron microscopic (SEM) analysis. Results There was a significant difference between occlusal and cervical margin groups. Laser conventional composite cementum group showed more microleakage values compared to other groups. There was no significant difference between occlusal margin groups. However, there was a significant difference between cervical margin groups in terms of microleakage. In sealant groups, there was a significant difference between laser and conventional with/without laser treatment groups in terms of microleakage. Conclusion Based on the results reported in this study, it can be concluded that the application of the Er:YAG laser beneath the resin composite, the resin-modified glass ionomers (GIs), and the fissure sealant placement may be an alternative enamel and dentin etching method to acid etching. PMID:29881311

Microleakage of self-etching sealant on noncontaminated and saliva-contaminated enamel.

PubMed

2011-01-01

The purpose of this study was to compare the microleakage of a self-etching sealant with a traditional phosphoric acid-etched sealant under noncontaminated and saliva-contaminated conditions. Fifty-two sound extracted human molars were randomly divided into 4 groups (N=13). Teeth in Groups 1 and 2 were cleaned with pumice, etched with phosphoric acid, rinsed, coated with a drying agent, placed with sealants (UltraSeal XT Plus), and light cured. Teeth in Groups 3 and 4 were cleaned with a proprietary flour pumice and rinsed prior to being sealed with a self-etching sealant (Enamel Loc). Teeth in Groups 2 and 4 were contaminated with saliva and thoroughly air-dried prior to the sealant placement. All teeth were subjected to a thermocycling process, stained with silver nitrate, and sectioned, and images of the sealant on the occlusal surface were recorded. Microleakage distance was measured in millimeters and subjected to a 2-way analysis of variance. Significantly larger microleakage distances were found for the self-etching sealant vs the traditional sealant (P<.001). Saliva contamination did not significantly affect the microleakage distance (P<.17). Under the conditions used in this in vitro study, the self-etching sealant, regardless of contamination condition, had extensive microleakage distances vs. little microleakage in the traditional phosphoric acid-etched sealant.

Active application of primer acid on acid-treated enamel: Influence on the bond effectiveness of self-etch adhesives systems.

PubMed

Araújo, Cíntia Tereza Pimenta; Prieto, Lúcia Trazzi; Costa, Daiane Cristianismo; Bosso, Mariana Avalone; Coppini, Erick Kamiya; Dias, Carlos Tadeu Santos; Paulillo, Luis Alexandre Maffei Sartini

2017-08-01

Evaluate the composite-to-enamel bond after passive or active application of self-etching primer systems on polished or pre-etched enamel with phosphoric acid. Two self-etch adhesives systems (SEAS) were used: Clearfil SE Bond and Easy Bond. Third human molars were divided into 8 groups (N = 10). The crown of each tooth was sectioned into halves and the mesial/distal surfaces were used. The adhesives were actively or passively applied on enamel with or without prior phosphoric-acid etching. Resin composite cylinders were built after adhesive application. After stored in relative humidity for 24 hr/37°C the specimens were subjected to microshear test in universal testing a machine at a crosshead speed of 0.5 mm/minute. The results were analyzed with three-way ANOVA and the Tukey test. The enamel-etching pattern was evaluated under SEM. The 2-step SEAS system presented significantly higher adhesive bond strength means (47.37 MPa) than the 1-step (36.87 MPa). A poor enamel- etching pattern was observed in active mode showing irregular and short resin tags, however there was not compromised the bond strength. Active or passive application produced similar values of bond strength to enamel regardless of enamel pretreatment and type of SEAS. © 2017 Wiley Periodicals, Inc.

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.

Anodic etching of GaN based film with a strong phase-separated InGaN/GaN layer: Mechanism and properties

NASA Astrophysics Data System (ADS)

Gao, Qingxue; Liu, Rong; Xiao, Hongdi; Cao, Dezhong; Liu, Jianqiang; Ma, Jin

2016-11-01

A strong phase-separated InGaN/GaN layer, which consists of multiple quantum wells (MQW) and superlattices (SL) layers and can produce a blue wavelength spectrum, has been grown on n-GaN thin film, and then fabricated into nanoporous structures by electrochemical etching method in oxalic acid. Scanning electron microscopy (SEM) technique reveals that the etching voltage of 8 V leads to a vertically aligned nanoporous structure, whereas the films etched at 15 V show branching pores within the n-GaN layer. Due to the low doping concentration of barriers (GaN layers) in the InGaN/GaN layer, we observed a record-low rate of etching (<100 nm/min) and nanopores which are mainly originated from the V-pits in the phase-separated layer. In addition, there exists a horizontal nanoporous structure at the interface between the phase-separated layer and the n-GaN layer, presumably resulting from the high transition of electrons between the barrier and the well (InGaN layer) at the interface. As compared to the as-grown MQW structure, the etched MQW structure exhibits a photoluminescence (PL) enhancement with a partial relaxation of compressive stress due to the increased light-extracting surface area and light-guiding effect. Such a compressive stress relaxation can be further confirmed by Raman spectra.

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.

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.

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.

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.

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

Contact Whiskers for Millimeter Wave Diodes

NASA Technical Reports Server (NTRS)

Kerr, A. R.; Grange, J. A.; Lichtenberger, J. A.

1978-01-01

Several techniques are investigated for making short conical tips on wires (whiskers) used for contacting millimeter-wave Schottky diodes. One procedure, using a phosphoric and chromic acid etching solution (PCE), is found to give good results on 12 microns phosphor-bronze wires. Full cone angles of 60 degrees-80 degrees are consistently obtained, compared with the 15 degrees-20 degrees angles obtained with the widely used sodium hydroxide etch. Methods are also described for cleaning, increasing the tip diameter (i.e. blunting), gold plating, and testing the contact resistance of the whiskers. The effects of the whisker tip shape on the electrical resistance, inductance, and capacitance of the whiskers are studied, and examples given for typical sets of parameters.

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.

[Influence of different porcelain surface treatment method on the bonding of metal brackets to porcelain].

PubMed

Fan, Cun-Hui; Chen, Jie; Liu, Xin-Qiang; Ma, Xin

2005-08-01

To investigate the influence of different porcelain surface treatment methods on the shear bond strength of metal brackets bonded to porcelain. 80 porcelain facets were divided randomly into two groups according to different adhesive material that was used to bond metal brackets. Adhesive material were Jing-Jin enamel adhesive and light-cured composite resin. Each group was further divided into 4 subgroups according to different surface treatment methods, which were acid etching with 37% phosphoric acid (H3PO4), acid etching with 9.6% hydrofluoric acid (HF), deglazing by grinding and silanating the porcelain surface. All specimens were stored in 37 degrees C water for 24 hours and then the shear bond strength and the porcelain fracture after debonding was determined. The porcelain surfaces after HF etching, H3PO4 etching and deglazing by grinding were examined by scanning electron microscopy respectively. The shear bond strengths in the HF etching groups, the deglazing groups and the silanating groups were much greater than that in the phosphoric etching groups (P < 0.01). Adequate orthodontic bonding strength was achieved both when bonded with light-cured composite resin after deglazing by grinding and when bonded with either of these adhesives after HF etching or surface silanating. There were no differences in the rates of porcelain fractures among groups (P > 0.05). HF etching, deglazing by grinding and silanating can all increase the shear bond strength between metal bracket and porcelain. Surface silanating of porcelain is a better surface treatment when metal brackets bonded to porcelain.

On the sensitivity of some common metallographic reagents to restoring obliterated marks on medium carbon (0.31% C) steel surfaces.

PubMed

Yin, Siaw Hui; Kuppuswamy, R

2009-01-10

Chemical etching, which is the most sensitive method to recover obliterated serial numbers on metal surfaces, has been practised quite successfully in forensic science laboratories all over the world. A large number of etchants suitable for particular metal surfaces based on empirical studies is available in the literature. This article reviews the sensitivity and efficacy of some popular etchants for recovering obliterated marks on medium carbon steel (0.31% C with ferrite-pearlite microstructure) used in automobile parts. The experiments involved engraving these carbon steel plates with some alphanumeric characters using a computer controlled machine "Gravograph" and erasing them to several depths below the bottom of their engraving depth. Seven metallographic reagents of which most of them were copper containing compounds were chosen for etching. The erased plates were etched with every one of these etchants using swabbing method. The results have revealed that Fry's reagent comprising cupric chloride 90 g, hydrochloric acid 120 mL and water 100mL provided the necessary contrast and was concluded to be the most sensitive. The same reagent was recommended by earlier workers for revealing strain lines in steel surfaces. Earlier, another reagent containing 5 g copper sulphate, 60 mL water, 30 mL (conc.) ammonium hydroxide, and 60 mL (conc.) hydrochloric acid was proved to be more sensitive to restore erased marks on low carbon steel (0.1% C with ferrite-pearlite structure) [M.A.M. Zaili, R. Kuppuswamy, H. Harun, Restoration of engraved marks on steel surfaces by etching technique, Forensic Sci. Int. 171 (2007) 27-32]. Thus the sensitivity of the etching reagent on steel surfaces appeared to be dependent on the content of carbon in the steel.

Acid etching of titanium for bonding with veneering composite resins.

PubMed

Ban, Seiji; Taniki, Toshio; Sato, Hideo; Kono, Hiroshi; Iwaya, Yukari; Miyamoto, Motoharu

2006-06-01

Commercially pure titanium (cpTi) was etched using three concentrated acids: 18% HCl, 43% H3PO4, and 48% H2SO4. The bond strengths between five types of veneering composite resin and eight cpTi treatments (involving combinations of sandblasting, acid etching in 48% H2SO4, and vacuum firing) were determined before and after 10,000 and 20,000 thermal cycles. There were no significant differences in the bond strength of resin to cpTi after etching in 48% H2SO4 at 90 degrees C for 15 minutes, at 60 degrees C for 15, 30, or 60 minutes, and after sandblasting with and without vacuum firing (p > 0.05); moreover, these treatments yielded the highest values. As for vacuum firing, it had no significant effect on resin bond strength to cpTi before or after 10,000 and 20,000 thermal cycles. We therefore concluded that acid etching in concentrated H2SO4 is a simple and effective surface modification method of titanium for bonding to veneering composite resins.

Biomechanical properties of jaw periosteum-derived mineralized culture on different titanium topography.

PubMed

Att, Wael; Kubo, Katsutoshi; Yamada, Masahiro; Maeda, Hatsuhiko; Ogawa, Takahiro

2009-01-01

This study evaluated the biomechanical properties of periosteum-derived mineralized culture on different surface topographies of titanium. Titanium surfaces modified by machining or by acid etching were analyzed using scanning electron microscopy (SEM). Rat mandibular periosteum-derived cells were cultured on either of the titanium surfaces. Cell proliferation was evaluated by cell counts, and gene expression was analyzed using a reverse-transcriptase polymerase chain reaction. Alkaline phosphatase (ALP) stain assay was employed to evaluate osteoblastic activity. Matrix mineralization was examined via von Kossa stain assay, total calcium deposition, and SEM. The hardness and elastic modulus of mineralized cultures were measured using a nano-indenter. The machined surface demonstrated a flat topographic configuration, while the acid-etched surface revealed a uniform micron-scale roughness. Both cell density and ALP activity were significantly higher on the machined surface than on the acid-etched surface. The expression of bone-related genes was up-regulated or enhanced on the acid-etched surface compared to the machined surface. Von Kossa stain showed significantly greater positive areas for the machined surface compared to the acid-etched surface, while total calcium deposition was statistically similar. Mineralized culture on the acid-etched surface was characterized by denser calcium deposition, more mature collagen deposition on the superficial layer, and larger and denser globular matrices inside the matrix than the culture on the machined surface. The mineralized matrix on the acid-etched surface was two times harder than on the machined surface, whereas the elastic modulus was comparable between the two surfaces. The design of this study can be used as a model to evaluate the effect of implant surface topography on the biomechanical properties of periosteum-derived mineralized culture. The results suggest that mandibular periosteal cells respond to different titanium surface topographies differently enough to produce mineralized matrices with different biomechanical qualities.

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.

Factors affecting the shear bond strength of metal and ceramic brackets bonded to different ceramic surfaces.

PubMed

Abu Alhaija, Elham S J; Abu AlReesh, Issam A; AlWahadni, Ahed M S

2010-06-01

The aims of this study were to evaluate the shear bond strength (SBS) of metal and ceramic brackets bonded to two different all-ceramic crowns, IPS Empress 2 and In-Ceram Alumina, to compare the SBS between hydrofluoric acid (HFA), phosphoric acid etched, and sandblasted, non-etched all-ceramic surfaces. Ninety-six all-ceramic crowns were fabricated resembling a maxillary left first premolar. The crowns were divided into eight groups: (1) metal brackets bonded to sandblasted 9.6 per cent HFA-etched IPS Empress 2 crowns; (2) metal brackets bonded to sandblasted 9.6 per cent HFA-etched In-Ceram crowns; (3) ceramic brackets bonded to sandblasted 9.6 per cent HFA-etched IPS Empress 2 crowns; (4) ceramic brackets bonded to sandblasted 9.6 per cent HFA-etched In-Ceram crowns; (5) metal brackets bonded to sandblasted 37 per cent phosphoric acid-etched IPS Empress 2 crowns; (6) metal brackets bonded to sandblasted 37 per cent phosphoric acid-etched In-Ceram crowns; (7) metal brackets bonded to sandblasted, non-etched IPS Empress 2 crowns; and (8) metal brackets bonded to sandblasted, non-etched In-Ceram crowns. Metal and ceramic orthodontic brackets were bonded using a conventional light polymerizing adhesive resin. An Instron universal testing machine was used to determine the SBS at a crosshead speed of 0.1 mm/minute. Comparison between groups was performed using a univariate general linear model and chi-squared tests. The highest mean SBS was found in group 3 (120.15 +/- 45.05 N) and the lowest in group 8 (57.86 +/- 26.20 N). Of all the variables studied, surface treatment was the only factor that significantly affected SBS (P < 0.001). Acid etch application to sandblasted surfaces significantly increased the SBS in groups 1, 2, 5, and 6. The SBS of metal brackets debonded from groups 1, 3, and 5 were not significantly different from those of groups 2, 4, and 6. All debonded metal brackets revealed a similar pattern of bond failure at the adhesive-restorative interface. However, ceramic brackets had a significantly different adhesive failure pattern with dominant failure at the adhesive-bracket interface. Ceramic fractures after bracket removal were found more often in groups 1-4. No significant difference in ceramic fracture was observed between the IPS Empress 2 and In-Ceram groups.

Nd:YAG laser ablation and acid resistance of enamel.

PubMed

Kwon, Yong Hoon; Kwon, Oh-Won; Kim, Hyung-Il; Kim, Kyo-Han

2003-09-01

The acid resistance of Nd:YAG laser-ablated enamel surfaces was studied by evaluating crystal structure, mineral distribution, and fluorescence radiance and image in the present study. For comparison, 37% phosphoric acid etching was performed. The formation of beta-tricalcium phosphate (beta-TCP) was confirmed in the laser-ablated surface. The Ca/P ratio increased after ablation due to mineral re-distribution. In contrast, the Ca/P ratio decreased after acid etching due to mineral loss. The laser-ablated enamels showed a smaller increase of fluorescence radiances and less clear laser confocal scanning microscope images than those observed in the acid-etched enamels. The former suggests a minimized mineral loss. The Nd:YAG laser irradiation will enhance the acid resistance and retard the carious progression in enamel.

Adhesive performance of a multi-mode adhesive system: 1-year in vitro study.

PubMed

Marchesi, Giulio; Frassetto, Andrea; Mazzoni, Annalisa; Apolonio, Fabianni; Diolosà, Marina; Cadenaro, Milena; Di Lenarda, Roberto; Pashley, David H; Tay, Franklin; Breschi, Lorenzo

2014-05-01

The aim of this study was to investigate the adhesive stability over time of a multi-mode one-step adhesive applied using different bonding techniques on human coronal dentine. The hypotheses tested were that microtensile bond strength (μTBS), interfacial nanoleakage expression and matrix metalloproteinases (MMPs) activation are not affected by the adhesive application mode (following the use of self-etch technique or with the etch-and-rinse technique on dry or wet dentine) or by ageing for 24h, 6 months and 1year in artificial saliva. Human molars were cut to expose middle/deep dentine and assigned to one of the following bonding systems (N=15): (1) Scotchbond Universal (3M ESPE) self-etch mode, (2) Scotchbond Universal etch-and-rinse technique on wet dentine, (3) Scotchbond Universal etch-and-rinse technique on dry dentine, and (4) Prime&Bond NT (Dentsply De Trey) etch-and-rinse technique on wet dentine (control). Specimens were processed for μTBS test in accordance with the non-trimming technique and stressed to failure after 24h, 6 months or 1 year. Additional specimens were processed and examined to assay interfacial nanoleakage and MMP expression. At baseline, no differences between groups were found. After 1 year of storage, Scotchbond Universal applied in the self-etch mode and Prime&Bond NT showed higher μTBS compared to the other groups. The lowest nanoleakage expression was found for Scotchbond Universal applied in the self-etch mode, both at baseline and after storage. MMPs activation was found after application of each tested adhesive. The results of this study support the use of the self-etch approach for bonding the tested multi-mode adhesive system to dentine due to improved stability over time. Improved bonding effectiveness of the tested universal adhesive system on dentine may be obtained if the adhesive is applied with the self-etch approach. Copyright © 2014 Elsevier Ltd. All rights reserved.

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.

The effect of storage conditions, contamination modes and cleaning procedures on the resin bond strength to lithium disilicate ceramic.

PubMed

Klosa, Karsten; Wolfart, Stefan; Lehmann, Frank; Wenz, Hans-Jürgen; Kern, Matthias

2009-04-01

The purpose of this in-vitro study was to evaluate the resin bond strength to pre-etched lithium disilicate ceramic using different cleaning methods after two contamination modes (saliva or saliva and silicone). Plexiglas tubes filled with composite resin (MultiCore Flow) were bonded to etched and silanized ceramic disks made of lithium disilicate ceramic (IPS e.max Press) using a luting resin (Multilink Automix). Either etched or unetched ceramic surfaces were contaminated with saliva or with saliva followed by a disclosing silicone. Groups of 16 specimens each were bonded after pretreatment using 4 surface cleaning agents (37% phosphoric acid, 5% hydrofluoric acid, 96% isopropanol, air polishing device with sodium bicarbonate) in different combinations. Before measuring tensile bond strength, specimens were stored for 3 or 150 days with thermocycling. After 150 days of storage, etching of saliva-contaminated surfaces with 5% hydrofluoric acid and/or 37% phosphoric acid provided statistically significantly higher bond strengths (37.9 to 49.5 MPa) than the other cleaning methods (1.7 to 15.5 MPa). After saliva and silicone contamination, etching with 5% hydrofluoric acid provided statistically significantly higher bond strengths (44.5 to 50.3 MPa) than all other cleaning methods (0.3 to 13.5 MPa). Ceramic cleaning methods after try-in procedures have a significant influence on the resin bond strength and are dependent on the type of contamination. Re-etching lithium disilicate ceramic with 5% hydrofluoric acid is most effective in removing contamination with saliva and/or a silicone disclosing medium.

Effect of sulfuric acid etching of polyetheretherketone on the shear bond strength to resin cements.

PubMed

Sproesser, Oliver; Schmidlin, Patrick R; Uhrenbacher, Julia; Roos, Malgorzata; Gernet, Wolfgang; Stawarczyk, Bogna

2014-10-01

To examine the influence of etching duration on the bond strength of PEEK substrate in combination with different resin composite cements. In total, 448 PEEK specimens were fabricated, etched with sulfuric acid for 5, 15, 30, 60, 90, 120, and 300 s and then luted with two conventional resin cements (RelyX ARC and Variolink II) and one self-adhesive resin cement (Clearfil SA Cement) (n = 18/subgroup). Non-etched specimens served as the control group. Specimens were stored in distilled water for 28 days at 37°C and shear bond strengths were measured. Data were analyzed nonparametrically using Kruskal-Wallis-H (p < 0.05). Non-etched PEEK demonstrated no bond strength to resin composite cements. The optimal etching duration varied with the type of resin composite: 60 s for RelyX ARC (15.3 ± 7.2 MPa), 90 s for Variolink II (15.2 ± 7.2 MPa), and 120 s for Clearfil SA Cement (6.4 ± 5.9 MPa). Regardless of etching duration, however, the self-etching resin composite cement showed significantly lower shear bond strength values when compared to groups luted with the conventional resin composites. Although sulfuric acid seems to be suitable and effective for PEEK surface pre-treatment, further investigations are required to examine the effect of other adhesive systems and cements.

Low-temperature oxidizing plasma surface modification and composite polymer thin-film fabrication techniques for tailoring the composition and behavior of polymer surfaces

NASA Astrophysics Data System (ADS)

Tompkins, Brendan D.

This dissertation examines methods for modifying the composition and behavior of polymer material surfaces. This is accomplished using (1) low-temperature low-density oxidizing plasmas to etch and implant new functionality on polymers, and (2) plasma enhanced chemical vapor deposition (PECVD) techniques to fabricate composite polymer materials. Emphases are placed on the structure of modified polymer surfaces, the evolution of polymer surfaces after treatment, and the species responsible for modifying polymers during plasma processing. H2O vapor plasma modification of high-density polyethylene (HDPE), low-density polyethylene (LDPE), polypropylene (PP), polystyrene (PS), polycarbonate (PC), and 75A polyurethane (PU) was examined to further our understanding of polymer surface reorganization leading to hydrophobic recovery. Water contact angles (wCA) measurements showed that PP and PS were the most susceptible to hydrophobic recovery, while PC and HDPE were the most stable. X-ray photoelectron spectroscopy (XPS) revealed a significant quantity of polar functional groups on the surface of all treated polymer samples. Shifts in the C1s binding energies (BE) with sample age were measured on PP and PS, revealing that surface reorganization was responsible for hydrophobic recovery on these materials. Differential scanning calorimetry (DSC) was used to rule out the intrinsic thermal properties as the cause of reorganization and hydrophobic recovery on HDPE, LDPE, and PP. The different contributions that polymer cross-linking and chain scission mechanisms make to polymer aging effects are considered. The H2O plasma treatment technique was extended to the modification of 0.2 microm and 3.0 microm track-etched polycarbonate (PC-TE) and track-etched polyethylene terephthalate (PET-TE) membranes with the goal of permanently increasing the hydrophilicity of the membrane surfaces. Contact angle measurements on freshly treated and aged samples confirmed the wettability of the membrane surfaces was significantly improved by plasma treatment. XPS and SEM analyses revealed increased oxygen incorporation onto the surface of the membranes, without any damage to the surface or pore structure. Contact angle measurements on a membrane treated in a stacked assembly suggest the plasma effectively modified the entire pore cross section. Plasma treatment also increased water flux through the membranes, with results from plasma modified membranes matching those from commercially available hydrophilic membranes (treated with wetting agent). Mechanisms for the observed modification are discussed in terms of OH and O radicals implanting oxygen functionality into the polymers. Oxidizing plasma systems (O2, CO2, H2O vapor, and formic acid vapor) were used to modify track-etched polycarbonate membranes and explore the mechanisms and species responsible for etching polycarbonate during plasma processing. Etch rates were measured using scanning electron microscopy; modified polycarbonate surfaces were further characterized using x-ray photoelectron spectroscopy and water contact angles. Etch rates and surface characterization results were combined with optical emission spectroscopy data used to identify gas-phase species and their relative densities. Although the oxide functionalities implanted by each plasma system were similar, the H2O vapor and formic acid vapor plasmas yielded the lowest contact angles after treatment. The CO2, H2O vapor, and formic acid vapor plasma-modified surfaces were, however, found to be similarly stable one month after treatment. Overall, etch rate correlated directly to the relative gas-phase density of atomic oxygen and, to a lesser extent, hydroxyl radicals. PECVD of acetic acid vapor (CH3COOH) was used to deposit films on PC-TE and silicon wafer substrates. The CH3COOH films were characterized using XPS, wCA, and SEM. This modification technique resulted in continuous deposition and self-limiting deposition of a-CxO yHz films on Si wafers and PC-TE, respectively. The self-limiting deposition on PC-TE revealed that resulting films have minimal impact on 3D PC structures. This technique would allow for more precise fabrication of patterned or nano-textured PC. PECVD is used to synthesize hydrocarbon/fluorocarbon thin films with compositional gradients by continuously changing the ratio of gases in a C 3F8/H2 plasma. The films are characterized using variable angle spectroscopic ellipsometry (VASE), Fourier transform infrared spectroscopy (FTIR), XPS, wCA, and SEM. These methods revealed that shifting spectroscopic signals can be used to characterize organization in the deposited film. Using these methods, along with gas-phase diagnostics, film chemistry and the underlying deposition mechanisms are elucidated, leading to a model that accurately predicts film thickness.

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.

Caries-preventive effect of fissure sealant containing surface reaction-type pre-reacted glass ionomer filler and bonded by self-etching primer.

PubMed

Shimazu, Kisaki; Ogata, Kiyokazu; Karibe, Hiroyuki

2012-01-01

We aimed to evaluate the caries-preventive effect of a fissure sealant containing surface reaction-type pre-reacted glass ionomer (S-PRG) filler and bonded by self-etching primer versus those of 2 conventional resin-based sealants bonded by acid etching in terms of its impact on enamel demineralization and remineralization, enamel bond strength, and integrity of debonded enamel surfaces. Demineralization, remineralization, and bond strength on untreated enamel and enamel subsurface lesions of bovine incisors were assessed among the sealants by polarizing microscopy and microradiography; debonded enamel surfaces were examined by scanning electron microscopy. The conventional resin-based sealants bonded by acid etching caused surface defects on the enamel subsurface lesions and significantly increased the lesion depth (p = 0.014), indicative of enamel demineralization. However the S-PRG filler-containing sealant bonded by self-etching primer maintained the enamel surface integrity and inhibited enamel demineralization. No difference in bond strength on both untreated enamel and enamel subsurface lesions was noted among the sealants. An S-PRG filler-containing fissure sealant bonded by self-etching primer can prevent enamel demineralization, microleakage, and gaps without the tags created by acid etching regardless of the enamel condition. Such sealants are suitable for protecting the pits and fissures of immature permanent teeth.

Creation of superhydrophobic stainless steel surfaces by acid treatments and hydrophobic film deposition.

PubMed

Li, Lester; Breedveld, Victor; Hess, Dennis W

2012-09-26

In this work, we present a method to render stainless steel surfaces superhydrophobic while maintaining their corrosion resistance. Creation of surface roughness on 304 and 316 grade stainless steels was performed using a hydrofluoric acid bath. New insight into the etch process is developed through a detailed analysis of the chemical and physical changes that occur on the stainless steel surfaces. As a result of intergranular corrosion, along with metallic oxide and fluoride redeposition, surface roughness was generated on the nano- and microscales. Differences in alloy composition between 304 and 316 grades of stainless steel led to variations in etch rate and different levels of surface roughness for similar etch times. After fluorocarbon film deposition to lower the surface energy, etched samples of 304 and 316 stainless steel displayed maximum static water contact angles of 159.9 and 146.6°, respectively. However, etching in HF also caused both grades of stainless steel to be susceptible to corrosion. By passivating the HF-etched samples in a nitric acid bath, the corrosion resistant properties of stainless steels were recovered. When a three step process was used, consisting of etching, passivation and fluorocarbon deposition, 304 and 316 stainless steel samples exhibited maximum contact angles of 157.3 and 134.9°, respectively, while maintaining corrosion resistance.

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

Swain, Basudev, E-mail: swain@iae.re.kr; Mishra, Chinmayee; Hong, Hyun Seon

Sustainable valorization processes for selective recovery of pure copper nanopowder from Indium-Tin-Oxide (ITO) etching wastewater by various wet chemical reduction processes, their chemistry has been investigated and compared. After the indium recovery by solvent extraction from ITO etching wastewater, the same is also an environmental challenge, needs to be treated before disposal. After the indium recovery, ITO etching wastewater contains 6.11 kg/m{sup 3} of copper and 1.35 kg/m{sup 3} of aluminum, pH of the solution is very low converging to 0 and contain a significant amount of chlorine in the media. In this study, pure copper nanopowder was recovered usingmore » various reducing reagents by wet chemical reduction and characterized. Different reducing agents like a metallic, an inorganic acid and an organic acid were used to understand reduction behavior of copper in the presence of aluminum in a strong chloride medium of the ITO etching wastewater. The effect of a polymer surfactant Polyvinylpyrrolidone (PVP), which was included to prevent aggregation, to provide dispersion stability and control the size of copper nanopowder was investigated and compared. The developed copper nanopowder recovery techniques are techno-economical feasible processes for commercial production of copper nanopowder in the range of 100–500 nm size from the reported facilities through a one-pot synthesis. By all the process reported pure copper nanopowder can be recovered with>99% efficiency. After the copper recovery, copper concentration in the wastewater reduced to acceptable limit recommended by WHO for wastewater disposal. The process is not only beneficial for recycling of copper, but also helps to address environment challenged posed by ITO etching wastewater. From a complex wastewater, synthesis of pure copper nanopowder using various wet chemical reduction route and their comparison is the novelty of this recovery process. - Highlights: • From the Indium-Tin-Oxide etching wastewater, copper nanopowder was synthesized. • Solution chemistry of ITO etching wastewater is addressed. • A techno-economical feasible, environment friendly and occupational safe process. • Brings back the material to production stream and address the circular economy. • A cradle to cradle technology management lowers the futuristic carbon economy.« less

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

Adhesion of multimode adhesives to enamel and dentin after one year of water storage.

PubMed

Vermelho, Paulo Moreira; Reis, André Figueiredo; Ambrosano, Glaucia Maria Bovi; Giannini, Marcelo

2017-06-01

This study aimed to evaluate the ultramorphological characteristics of tooth-resin interfaces and the bond strength (BS) of multimode adhesive systems to enamel and dentin. Multimode adhesives (Scotchbond Universal (SBU) and All-Bond Universal) were tested in both self-etch and etch-and-rinse modes and compared to control groups (Optibond FL and Clearfil SE Bond (CSB)). Adhesives were applied to human molars and composite blocks were incrementally built up. Teeth were sectioned to obtain specimens for microtensile BS and TEM analysis. Specimens were tested after storage for either 24 h or 1 year. SEM analyses were performed to classify the failure pattern of beam specimens after BS testing. Etching increased the enamel BS of multimode adhesives; however, BS decreased after storage for 1 year. No significant differences in dentin BS were noted between multimode and control in either evaluation period. Storage for 1 year only reduced the dentin BS for SBU in self-etch mode. TEM analysis identified hybridization and interaction zones in dentin and enamel for all adhesives. Silver impregnation was detected on dentin-resin interfaces after storage of specimens for 1 year only with the SBU and CSB. Storage for 1 year reduced enamel BS when adhesives are applied on etched surface; however, BS of multimode adhesives did not differ from those of the control group. In dentin, no significant difference was noted between the multimode and control group adhesives, regardless of etching mode. In general, multimode adhesives showed similar behavior when compared to traditional adhesive techniques. Multimode adhesives are one-step self-etching adhesives that can also be used after enamel/dentin phosphoric acid etching, but each product may work better in specific conditions.

Shear bond strength of composite bonded with three adhesives to Er,Cr:YSGG laser-prepared enamel.

PubMed

Türkmen, Cafer; Sazak-Oveçoğlu, Hesna; Günday, Mahir; Güngör, Gülşad; Durkan, Meral; Oksüz, Mustafa

2010-06-01

To assess in vitro the shear bond strength of a nanohybrid composite resin bonded with three adhesive systems to enamel surfaces prepared with acid and Er,Cr:YSGG laser etching. Sixty extracted caries- and restoration-free human maxillary central incisors were used. The teeth were sectioned 2 mm below the cementoenamel junction. The crowns were embedded in autopolymerizing acrylic resin with the labial surfaces facing up. The labial surfaces were prepared with 0.5-mm reduction to receive composite veneers. Thirty specimens were etched with Er,Cr:YSGG laser. This group was also divided into three subgroups, and the following three bonding systems were then applied on the laser groups and the other three unlased groups: (1) 37% phosphoric acid etch + Bond 1 primer/adhesive (Pentron); (2) Nano-bond self-etch primer (Pentron) + Nano-bond adhesive (Pentron); and (3) all-in-one adhesive-single dose (Futurabond NR, Voco). All of the groups were restored with a nanohybrid composite resin (Smile, Pentron). Shear bond strength was measured with a Zwick universal test device with a knife-edge loading head. The data were analyzed with two-factor ANOVA. There were no significant differences in shear bond strength between self-etch primer + adhesive and all-in-one adhesive systems for nonetched and laser-etched enamel groups (P > .05). However, bond strength values for the laser-etched + Bond 1 primer/adhesive group (48.00 +/- 13.86 MPa) were significantly higher than the 37% phosphoric acid + Bond 1 primer/adhesive group (38.95 +/- 20.07 MPa) (P < .05). The Er,Cr:YSGG laser-powered hydrokinetic system etched the enamel surface more effectively than 37% phosphoric acid for subsequent attachment of composite material.

Enamel Deproteinization using Papacarie and 10% Papain Gel on Shear Bond Strength of Orthodontic Brackets Before and After Acid Etching.

PubMed

Agarwal, R M; Yeluri, R; Singh, C; Munshi, A K

2015-01-01

To suggest Papacarie(®) as a new deproteinizing agent in comparison with indigenously prepared 10% papain gel before and after acid etching that may enhance the quality of the bond between enamel surface and composite resin complex. One hundred and twenty five extracted human premolars were utilized and divided into five groups: In the group 1, enamel surface was etched and primer was applied. In group 2, treatment with papacarie(®) for 60 seconds followed by etching and primer application. In group 3, etching followed by treatment with papacarie(®) for 60 seconds and primer application. In group 4, treatment with 10% papain gel for 60 seconds followed by etching and primer application. In group 5, etching followed by treatment with 10% papain gel for 60 seconds and primer application . After bonding the brackets, the mechanical testing was performed using a Universal testing machine. The failure mode was analyzed using an adhesive remnant index. The etching patterns before and after application of papacarie(®) and 10% papain gel was also evaluated using SEM. The values obtained for shear bond strength were submitted to analysis of variance and Tukey test (p < 0.05). It was observed that group 2 and group 4 had the highest shear bond strength and was statistically significant from other groups (p=0.001). Regarding Adhesive remnant index no statistical difference was seen between the groups (p=0.538). Papacarie(®) or 10% papain gel can be used to deproteinize the enamel surface before acid etching to enhance the bond strength of orthodontic brackets.

Bond strength of orthodontic light-cured resin-modified glass ionomer cement.

PubMed

Cheng, Hsiang Yu; Chen, Chien Hsiu; Li, Chuan Li; Tsai, Hung Huey; Chou, Ta Hsiung; Wang, Wei Nan

2011-04-01

The purpose of this study was to compare the bond strengths and debonded interfaces achieved with light-cured resin-modified glass ionomer cement (RMGIC) and conventional light-cured composite resin. In addition, the effects of acid etching and water contamination were examined. One hundred human premolars were randomly divided into five equal groups. The mini Dyna-lock upper premolar bracket was selected for testing. The first four groups were treated with light-cured RMGIC with or without 15 per cent phosphoric acid-etching treatment and with or without water contamination preceding bracket bonding. The control samples were treated with the conventional light-cured Transbond composite resin under acid etching and without water contamination. Subsequently, the brackets were debonded by tensile force using an Instron machine. The modified adhesive remnant index (ARI) scores were assigned to the bracket base of the debonded interfaces using a scanning electron microscope. The bond strength and modified ARI scores were determined and analysed statistically by one-way analysis of variance and chi-square test. Under all four conditions, the bond strength of the light-cure RMGIC was equal to or higher than that of the conventional composite resin. The highest bond strength was achieved when using RMGIC with acid etching but without water contamination. The modified ARI scores were 2 for Fuji Ortho LC and 3 for Transbond. No enamel detachment was found in any group. Fifteen per cent phosphoric acid etching without moistening the enamel of Fuji Ortho LC provided the more favourable bond strength. Enamel surfaces, with or without water contamination and with or without acid etching, had the same or a greater bond strength than Transbond.

[Brushing abrasion of the enamel surface after erosion].

PubMed

Lipei, Chen; Xiangke, Ci; Xiaoyan, Ou

2017-08-01

Objective A study was conducted to compare the effect of different enamel remineralization periods after erosion on the depth of brushing abrasion. Methods Ten volunteers were selected for a 4-day experiment. A total of 60 enamels were randomly assigned into six groups (A-F) and placed in intraoral palatal devices. On the first day, the palatal devices were placed in oral cavity (24 h) . On the following three days, brushing experiments were performed extraorally, two times per day. The specific experimental method of brushing follows these next steps. First, the group F specimens were covered with a film of wax, and then acid etched for 2 min. Subsequently, the film of wax was detached. The groups from A to D were brushed after remineralization at the following time intervals: group A, 0 min; group B, 20 min; group C, 40 min; group D, 60 min. Erosion and remineralization were performed on group E, but without brushing. Remineralization was performed on group F, but without acid etching and brushing. The depth of enamel abrasion was determined by a mechanical profilometer. The surface morphology of the enamel blocks was observed using a scanning electron microscope. Results 1) The depth of abrasion was different in varied enamel remineralization time after acid etching. The statistical significant differences between groups were as follows. 2) When the time of enamel remineralization after acid etching was short, the surface depression in the electron microscope was deep, and the surface morphology was rough. Conclusion Brushing immediately after acid etching would cause much serious abrasion to the enamel surface. Brushing after 60 min can effectively reduce the abrasion of acid etching enamel.

Method for etching thin films of niboium and niobium-containing compounds for preparing superconductive circuits

DOEpatents

Kampwirth, R.T.; Schuller, I.K.; Falco, C.M.

1979-11-23

An improved method of preparing thin film superconducting electrical circuits of niobium or niobium compounds is provided in which a thin film of the niobium or niobium compound is applied to a nonconductive substrate and covered with a layer of photosensitive material. The sensitive material is in turn covered with a circuit pattern exposed and developed to form a mask of the circuit in photoresistive material on the surface of the film. The unmasked excess niobium film is removed by contacting the substrate with an aqueous etching solution of nitric acid, sulfuric acid, and hydrogen fluoride, which will rapidly etch the niobium compound without undercutting the photoresist. A modification of the etching solution will permit thin films to be lifted from the substrate without further etching.

Rubbing time and bonding performance of one-step adhesives to primary enamel and dentin.

PubMed

Botelho, Maria Paula Jacobucci; Isolan, Cristina Pereira; Schwantz, Júlia Kaster; Lopes, Murilo Baena; Moraes, Rafael Ratto de

2017-01-01

This study investigated whether increasing the concentration of acidic monomers in one-step adhesives would allow reducing their application time without interfering with the bonding ability to primary enamel and dentin. Experimental one-step self-etch adhesives were formulated with 5 wt% (AD5), 20 wt% (AD20), or 35 wt% (AD35) acidic monomer. The adhesives were applied using rubbing motion for 5, 10, or 20 s. Bond strengths to primary enamel and dentin were tested under shear stress. A commercial etch-and-rinse adhesive (Single Bond 2; 3M ESPE) served as reference. Scanning electron microscopy was used to observe the morphology of bonded interfaces. Data were analysed at p<0.05. In enamel, AD35 had higher bond strength when rubbed for at least 10 s, while application for 5 s generated lower bond strength. In dentin, increased acidic monomer improved bonding only for 20 s rubbing time. The etch-and-rinse adhesive yielded higher bond strength to enamel and similar bonding to dentin as compared with the self-etch adhesives. The adhesive layer was thicker and more irregular for the etch-and-rinse material, with no appreciable differences among the self-etch systems. Overall, increasing the acidic monomer concentration only led to an increase in bond strength to enamel when the rubbing time was at least 10 s. In dentin, despite the increase in bond strength with longer rubbing times, the results favoured the experimental adhesives compared to the conventional adhesive. Reduced rubbing time of self-etch adhesives should be avoided in the clinical setup.

Ethanol wet-bonding technique sensitivity assessed by AFM.

PubMed

Osorio, E; Toledano, M; Aguilera, F S; Tay, F R; Osorio, R

2010-11-01

In ethanol wet bonding, water is replaced by ethanol to maintain dehydrated collagen matrices in an extended state to facilitate resin infiltration. Since short ethanol dehydration protocols may be ineffective, this study tested the null hypothesis that there are no differences in ethanol dehydration protocols for maintaining the surface roughness, fibril diameter, and interfibrillar spaces of acid-etched dentin. Polished human dentin surfaces were etched with phosphoric acid and water-rinsed. Tested protocols were: (1) water-rinse (control); (2) 100% ethanol-rinse (1-min); (3) 100% ethanol-rinse (5-min); and (4) progressive ethanol replacement (50-100%). Surface roughness, fibril diameter, and interfibrillar spaces were determined with atomic force microscopy and analyzed by one-way analysis of variance and the Student-Newman-Keuls test (α = 0.05). Dentin roughness and fibril diameter significantly decreased when 100% ethanol (1-5 min) was used for rinsing (p < 0.001). Absolute ethanol produced collapse and shrinkage of collagen fibrils. Ascending ethanol concentrations did not collapse the matrix and shrank the fibrils less than absolute ethanol-rinses.

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).

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.

Effect of different surface treatments on roughness of IPS Empress 2 ceramic.

PubMed

Kara, Haluk Baris; Dilber, Erhan; Koc, Ozlem; Ozturk, A Nilgun; Bulbul, Mehmet

2012-03-01

The aim of this study was to evaluate the influence of different surface treatments (air abrasion, acid etching, laser irradiation) on the surface roughness of a lithium-disilicate-based core ceramic. A total of 40 discs of lithium disilicate-based core ceramic (IPS Empress 2; Ivoclar Vivadent, Schaan, Liechtenstein) were prepared (10 mm in diameter and 1 mm in thickness) according to the manufacturer's instructions. Specimens were divided into four groups (n = 10), and the following treatments were applied: air abrasion with alumina particles (50 μm), acid etching with 5% hydrofluoric acid, Nd:YAG laser irradiation (1 mm distance, 100 mJ, 20 Hz, 2 W) and Er:YAG laser irradiation (1 mm distance, 500 mJ, 20 Hz, 10 W). Following determination of surface roughness (R(a)) by profilometry, specimens were examined with atomic force microscopy. The data were analysed by one-way analysis of variance (ANOVA) and Tukey HSD test (α = 0.05). One-way ANOVA indicated that surface roughness following air abrasion was significantly different from the surface roughness following laser irradiation and acid etching (P < 0.001). The Tukey HSD test indicated that the air abrasion group had a significantly higher mean value of roughness (P < 0.05) than the other groups. No significant difference was found between the acid etching and laser irradiation (both Er:YAG and Nd:YAG) groups (P > 0.05). Air abrasion increased surface roughness of lithium disilicate-based core ceramic surfaces more effectively than acid-etching and laser irradiation.

Comparison of Self-Etch Primers with Conventional Acid Etching System on Orthodontic Brackets

PubMed Central

Zope, Amit; Zope-Khalekar, Yogita; Chitko, Shrikant S.; Kerudi, Veerendra V.; Patil, Harshal Ashok; Jaltare, Pratik; Dolas, Siddhesh G

2016-01-01

Introduction The self-etching primer system consists of etchant and primer dispersed in a single unit. The etching and priming are merged as a single step leading to fewer stages in bonding procedure and reduction in the number of steps that also reduces the chance of introduction of error, resulting in saving time for the clinician. It also results in smaller extent of enamel decalcification. Aim To compare the Shear Bond Strength (SBS) of orthodontic bracket bonded with Self-Etch Primers (SEP) and conventional acid etching system and to study the surface appearance of teeth after debonding; etching with conventional acid etch and self-etch priming, using stereomicroscope. Materials and Methods Five Groups (n=20) were created randomly from a total of 100 extracted premolars. In a control Group A, etching of enamel was done with 37% phosphoric acid and bonding of stainless steel brackets with Transbond XT (3M Unitek, Monrovia, California). Enamel conditioning in left over four Groups was done with self-etching primers and adhesives as follows: Group B-Transbond Plus (3M Unitek), Group C Xeno V+ (Dentsply), Group D-G-Bond (GC), Group E-One-Coat (Coltene). The Adhesive Remnant Index (ARI) score was also evaluated. Additionally, the surface roughness using profilometer were observed. Results Mean SBS of Group A was 18.26±7.5MPa, Group B was 10.93±4.02MPa, Group C was 6.88±2.91MPa while of Group D was 7.78±4.13MPa and Group E was 10.39±5.22MPa respectively. In conventional group ARI scores shows that over half of the adhesive was remaining on the surface of tooth (score 1 to 3). In self-etching primer groups ARI scores show that there was no or minor amount of adhesive remaining on the surface of tooth (score 4 and 5). SEP produces a lesser surface roughness on the enamel than conventional etching. However, statistical analysis shows significant correlation (p<0.001) of bond strength with surface roughness of enamel. Conclusion All groups might show clinically useful SBS values and Transbond XT can be successfully used for bracket bonding after enamel conditioning with any of the SEPs tested. The SEPs used in Groups C (Xeno V+) and D (G-Bond) have significantly lowered SBS. Although, the values might still be clinically acceptable. PMID:28208997

Microfluidic-based photocatalytic microreactor for environmental application: a review of fabrication substrates and techniques, and operating parameters.

PubMed

Das, Susmita; Srivastava, Vimal Chandra

2016-06-08

Photochemical technology with microfluidics is emerging as a new platform in environmental science. Microfluidic technology has various advantages, like better mixing and a shorter diffusion distance for the reactants and products; and uniform distribution of light on the photocatalyst. Depending on the material type and related applications, several fabrication techniques have been adopted by various researchers. Microreactors have been prepared by various techniques, such as lithography, etching, mechanical microcutting technology, etc. Lithography can be classified into photolithography, soft lithography and X-ray lithography techniques whereas the etching process is divided into wet etching (chemical etching) and dry etching (plasma etching) techniques. Several substrates, like polymers, such as polydimethyl-siloxane (PDMS), polymethyle-methacrylate (PMMA), hydrogel, etc.; metals, such as stainless steel, titanium foil, etc.; glass, such as silica capillary, glass slide, etc.; and ceramics have been used for microchannel fabrication. During degradation in a microreactor, the degradation efficiency is affected by few important parameters such as flow rate, initial concentration of the target compound, microreactor dimensions, light intensity, photocatalyst structure and catalyst support. The present paper discusses and critically reviews fabrication techniques and substrates used for microchannel fabrication and critical operating parameters for organics, especially dye degradation in the microreactor. The kinetics of degradation has also been discussed.

Influence of laser etching on enamel and dentin bond strength of Silorane System Adhesive.

PubMed

Ustunkol, Ildem; Yazici, A Ruya; Gorucu, Jale; Dayangac, Berrin

2015-02-01

The aim of this in vitro study was to evaluate the shear bond strength (SBS) of Silorane System Adhesive to enamel and dentin surfaces that had been etched with different procedures. Ninety freshly extracted human third molars were used for the study. After the teeth were embedded with buccal surfaces facing up, they were randomly divided into two groups. In group I, specimens were polished with a 600-grit silicon carbide (SiC) paper to obtain flat exposed enamel. In group II, the overlying enamel layer was removed and exposed dentin surfaces were polished with a 600-grit SiC paper. Then, the teeth in each group were randomly divided into three subgroups according to etching procedures: etched with erbium, chromium:yttrium-scandium-gallium-garnet laser (a), etched with 35% phosphoric acid (b), and non-etched (c, control). Silorane System Adhesive was used to bond silorane restorative to both enamel and dentin. After 24-h storage in distilled water at room temperature, a SBS test was performed using a universal testing machine at a crosshead speed of 1 mm/min. The data were analyzed using two-way ANOVA and Bonferroni tests (p < 0.05). The highest SBS was found after additional phosphoric acid treatment in dentin groups (p < 0.05). There were no statistically significant differences between the laser-etched and non-etched groups in enamel and dentin (p > 0.05). The SBS of self-etch adhesive to dentin was not statistically different from enamel (p > 0.05). Phosphoric acid treatment seems the most promising surface treatment for increasing the enamel and dentin bond strength of Silorane System Adhesive.

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.

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.

Optical and electrical characterization methods of plasma-induced damage in silicon nitride films

NASA Astrophysics Data System (ADS)

Kuyama, Tomohiro; Eriguchi, Koji

2018-06-01

We proposed evaluation methods of plasma-induced damage (PID) in silicon nitride (SiN) films. The formation of an oxide layer by air exposure was identified for damaged SiN films by X-ray photoelectron spectroscopy (XPS). Bruggeman’s effective medium approximation was employed for an optical model consisting of damaged and undamaged layers, which is applicable to an in-line monitoring by spectroscopic ellipsometry (SE). The optical thickness of the damaged layer — an oxidized layer — extended after plasma exposure, which was consistent with the results obtained by a diluted hydrofluoric acid (DHF) wet etching. The change in the conduction band edge of the damaged SiN films was presumed from two electrical techniques, i.e., current–voltage (I–V) measurement and time-dependent dielectric breakdown (TDDB) test with a constant voltage stress. The proposed techniques can be used for assigning the plasma-induced structural change in an SiN film widely used as an etch-protecting layer.

Shear Bond Strength of Self-etching Adhesives to Cavities Prepared by Diamond Bur or Er,Cr:YSGG Laser and Effect of Prior Acid Etching.

PubMed

Jhingan, Pulkit; Sachdev, Vinod; Sandhu, Meera; Sharma, Karan

2015-12-01

To compare and evaluate shear bond strength of self-etching adhesives bonded to cavities prepared by diamond bur or Er,Cr:YSGG laser and the effect of prior acid etching on shear bond strength. Ninety-six caries-free human premolars were selected and divided into 2 groups depending on mode of cavity preparation (48 teeth each). Cavities were prepared with Er,Cr:YSGG laser in group 1 and diamond burs in an air-turbine handpiece in group 2. Groups 1 and 2 were further subdivided into three subgroups of 8 teeth each, which were bonded with sixth- or seventh-generation adhesives with or without prior acid etching, followed by restoration of all samples with APX Flow. These samples were subjected to shear bond strength testing. In addition, the surface morphology of 24 samples each from groups 1 and 2 was evaluated using SEM. Data were analyzed using the Shapiro-Wilk test, one- and two-way ANOVA, the t-test, and the least significant difference test, which showed that the data were normally distributed (p > 0.05). The shear bond strength of adhesives in cavities prepared by Er,Cr:YSGG laser was significantly higher than in diamond bur-prepared cavities (p < 0.05). SEM analysis showed a smear-layer-free anfractuous surface on laser-ablated teeth, in contrast to conventional bur-prepared teeth. The Er,Cr:YSGG laser-ablated surface proved to be more receptive for adhesion than those prepared by diamond bur irrespective of the bonding agent used. Seventh-generation adhesives yielded higher shear bond strength than did sixth-generation adhesives. Prior acid etching decreased the shear bond strength of self-etching adhesives.

Rubbing time and bonding performance of one-step adhesives to primary enamel and dentin

PubMed Central

Botelho, Maria Paula Jacobucci; Isolan, Cristina Pereira; Schwantz, Júlia Kaster; Lopes, Murilo Baena; de Moraes, Rafael Ratto

2017-01-01

Abstract Objectives: This study investigated whether increasing the concentration of acidic monomers in one-step adhesives would allow reducing their application time without interfering with the bonding ability to primary enamel and dentin. Material and methods: Experimental one-step self-etch adhesives were formulated with 5 wt% (AD5), 20 wt% (AD20), or 35 wt% (AD35) acidic monomer. The adhesives were applied using rubbing motion for 5, 10, or 20 s. Bond strengths to primary enamel and dentin were tested under shear stress. A commercial etch-and-rinse adhesive (Single Bond 2; 3M ESPE) served as reference. Scanning electron microscopy was used to observe the morphology of bonded interfaces. Data were analysed at p<0.05. Results: In enamel, AD35 had higher bond strength when rubbed for at least 10 s, while application for 5 s generated lower bond strength. In dentin, increased acidic monomer improved bonding only for 20 s rubbing time. The etch-and-rinse adhesive yielded higher bond strength to enamel and similar bonding to dentin as compared with the self-etch adhesives. The adhesive layer was thicker and more irregular for the etch-and-rinse material, with no appreciable differences among the self-etch systems. Conclusion: Overall, increasing the acidic monomer concentration only led to an increase in bond strength to enamel when the rubbing time was at least 10 s. In dentin, despite the increase in bond strength with longer rubbing times, the results favoured the experimental adhesives compared to the conventional adhesive. Reduced rubbing time of self-etch adhesives should be avoided in the clinical setup. PMID:29069150

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.

Effects of potassium oxalate on knoop hardness of etch-and-rinse adhesives.

PubMed

Silva, S M A; Malacarne-Zanon, J; Carvalho, R M; Alves, M C; De Goes, M F; Anido-Anido, A; Carrilho, M R

2012-01-01

The objective of this study was to determine whether the hardness of etch-and-rinse adhesives may be affected by the pretreatment of acid-etched dentin with potassium oxalate desensitizer. Unerupted human third molars were cut into crown segments by removing the occlusal enamel and roots. The pulp chamber of these crown segments was connected to a syringe barrel filled with phosphate-buffered saline so that the moisture of dentin was maintained during the bonding procedures. Three etch-and-rinse adhesives-two two-step systems (Adper Single Bond 2 [SB], One-Step [OS]) and one three-step system (Adper Scotchbond Multi-Purpose [MP])-were applied to acid-etched dentin that had been treated (experimental groups) or not (control groups) with potassium oxalate (BisBlock). The Knoop hardness (KHN) of adhesives was taken at different sites of the outer surface of the adhesive-bonded dentin. The KHN of the three tested adhesives applied to acid-etched dentin treated with potassium oxalate was significantly lower than that exhibited by the respective controls (not treated with oxalate; p<0.05). Regardless of the adhesive, the treatment with potassium oxalate reduced the adhesives' KHN (p<0.05), with the OS system exhibiting the lowest KHN compared with the MP and SB systems.

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.

Shear bond strength of one-step self-etch adhesives to enamel: effect of acid pretreatment.

PubMed

Poggio, Claudio; Scribante, Andrea; Della Zoppa, Federica; Colombo, Marco; Beltrami, Riccardo; Chiesa, Marco

2014-02-01

The purposes of this study were to evaluate the effect of surface pretreatment with phosphoric acid on the enamel bond strength of four-one-step self-etch adhesives with different pH values. One hundred bovine permanent mandibular incisors were used. The materials used in this study included four-one-step self-etch adhesives with different pH values: Adper(™) Easy Bond Self-Etch Adhesive (ph = 0,8-1), Futurabond NR (ph = 1,4), G-aenial Bond (ph = 1,5), Clearfil(3) S Bond (ph = 2,7). One two-step self-etch adhesive (Clearfil SE Bond/ph = 0,8-1) was used as control. The teeth were assigned into two subgroups according to bonding procedure. In the first subgroup (n = 50), no pretreatment agent was applied. In the second subgroup (n = 50), etching was performed using 37% phosphoric acid for 30 s. After adhesive systems application, a nanohybrid composite resin was inserted into the enamel surface. The specimens were placed in a universal testing machine (Model 3343, Instron Corp., Canton, Mass., USA). After the testing procedure, the fractured surfaces were examined with an optical microscope at a magnification of 10× to determine failure modes. The adhesive remnant index (ARI) was used to assess the amount of adhesive left on the enamel surface. Descriptive statistics of the shear bond strength and frequency distribution of ARI scores were calculated. Enamel pretreatment with phosphoric acid significantly increased bond strength values of all the adhesives tested. No significant differences in bond strength were detected among the four different one-step self-etch adhesives with different pH. Two-step self-etch adhesive showed the highest bond strength. © 2013 John Wiley & Sons A/S.

Transient and residual stresses in a pressable glass-ceramic before and after resin-cement coating determined using profilometry.

PubMed

Isgró, G; Addison, O; Fleming, G J P

2011-05-01

The effect of heat-pressing and subsequent pre-cementation (acid-etching) and resin-cementation operative techniques on the development of transient and residual stresses in different thicknesses of a lithium disilicate glass-ceramic were characterised using profilometry prior to biaxial flexure strength (BFS) determination. 60 IPS e.max Press discs were pressed and divested under controlled conditions. The discs were polished on one surface to thicknesses of 0.61±0.05, 0.84±0.08, and 1.06±0.07 mm (Groups A-C, respectively). The mean of the maximum deflection (acid-etching and resin-coating was determined using high resolution profilometery prior to BFS testing. Paired sample t-tests were performed (p<0.05) on the 20 individual samples in each group (Groups A-C) for each comparison. Differences between the baseline quantification and resin-cement coating deflection values and BFS values for Groups A-C were determined using a one-way ANOVA with post hoc Tukey tests (p<0.05). Baseline quantification for Groups A-C identified no significant differences between the group means of the maximum deflection values (p=0.341). Following HF acid-etching, a significant increase in deflection for all groups (p<0.001) was identified compared with the baseline quantification. Additionally, resin-cement coating significantly increased deflection for Group A (p<0.001), Group B (p<0.001) and Group C (p=0.001) specimens for the individual groups. The increased deflection from baseline quantification to resin-cement coating was significantly different (p<0.001) for the three specimen thicknesses, although the BFS values were not. The lower reported baseline quantification range of the mean of the maximum deflection for the IPS e.max(®) Press specimens was predominantly the result of specimen polishing regime inducing a tensile stress state across the surface defect integral which accounted for the observed surface convexity. Acid-etching and resin-cementation had a significant impact on the development and magnitude of the transient and residual stresses in the lithium disilicate glass-ceramic investigated. Copyright © 2011 Elsevier Ltd. All rights reserved.

Shear bond strength of a new self-adhering flowable composite resin for lithium disilicate-reinforced CAD/CAM ceramic material

PubMed Central

Sancakli, Hande Sar; Sancakli, Erkan; Eren, Meltem Mert; Ozel, Sevda; Yucel, Taner; Yildiz, Esra

2014-01-01

PURPOSE The purpose of this study was to evaluate and compare the effects of different surface pretreatment techniques on the surface roughness and shear bond strength of a new self-adhering flowable composite resin for use with lithium disilicate-reinforced CAD/CAM ceramic material. MATERIALS AND METHODS A total of one hundred thirty lithium disilicate CAD/CAM ceramic plates with dimensions of 6 mm × 4 mm and 3 mm thick were prepared. Specimens were then assigned into five groups (n=26) as follows: untreated control, coating with 30 µm silica oxide particles (Cojet™ Sand), 9.6% hydrofluoric acid etching, Er:YAG laser irradiation, and grinding with a high-speed fine diamond bur. A self-adhering flowable composite resin (Vertise Flow) was applied onto the pre-treated ceramic plates using the Ultradent shear bond Teflon mold system. Surface roughness was measured by atomic force microscopy. Shear bond strength test were performed using a universal testing machine at a crosshead speed of 1 mm/min. Surface roughness data were analyzed by one-way ANOVA and the Tukey HSD tests. Shear bond strength test values were analyzed by Kruskal-Wallis and Mann-Whitney U tests at α=.05. RESULTS Hydrofluoric acid etching and grinding with high-speed fine diamond bur produced significantly higher surface roughness than the other pretreatment groups (P<.05). Hydrofluoric acid etching and silica coating yielded the highest shear bond strength values (P<.001). CONCLUSION Self-adhering flowable composite resin used as repair composite resin exhibited very low bond strength irrespective of the surface pretreatments used. PMID:25551002

Four chemical methods of porcelain conditioning and their influence over bond strength and surface integrity

PubMed Central

Stella, João Paulo Fragomeni; Oliveira, Andrea Becker; Nojima, Lincoln Issamu; Marquezan, Mariana

2015-01-01

OBJECTIVE: To assess four different chemical surface conditioning methods for ceramic material before bracket bonding, and their impact on shear bond strength and surface integrity at debonding. METHODS: Four experimental groups (n = 13) were set up according to the ceramic conditioning method: G1 = 37% phosphoric acid etching followed by silane application; G2 = 37% liquid phosphoric acid etching, no rinsing, followed by silane application; G3 = 10% hydrofluoric acid etching alone; and G4 = 10% hydrofluoric acid etching followed by silane application. After surface conditioning, metal brackets were bonded to porcelain by means of the Transbond XP system (3M Unitek). Samples were submitted to shear bond strength tests in a universal testing machine and the surfaces were later assessed with a microscope under 8 X magnification. ANOVA/Tukey tests were performed to establish the difference between groups (α= 5%). RESULTS: The highest shear bond strength values were found in groups G3 and G4 (22.01 ± 2.15 MPa and 22.83 ± 3.32 Mpa, respectively), followed by G1 (16.42 ± 3.61 MPa) and G2 (9.29 ± 1.95 MPa). As regards surface evaluation after bracket debonding, the use of liquid phosphoric acid followed by silane application (G2) produced the least damage to porcelain. When hydrofluoric acid and silane were applied, the risk of ceramic fracture increased. CONCLUSIONS: Acceptable levels of bond strength for clinical use were reached by all methods tested; however, liquid phosphoric acid etching followed by silane application (G2) resulted in the least damage to the ceramic surface. PMID:26352845

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

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

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.

Selective etchant for oxide sacrificial material in semiconductor device fabrication

DOEpatents

Clews, Peggy J.; Mani, Seethambal S.

2005-05-17

An etching composition and method is disclosed for removing an oxide sacrificial material during manufacture of semiconductor devices including micromechanical, microelectromechanical or microfluidic devices. The etching composition and method are based on the combination of hydrofluoric acid (HF) and sulfuric acid (H.sub.2 SO.sub.4). These acids can be used in the ratio of 1:3 to 3:1 HF:H.sub.2 SO.sub.4 to remove all or part of the oxide sacrificial material while providing a high etch selectivity for non-oxide materials including polysilicon, silicon nitride and metals comprising aluminum. Both the HF and H.sub.2 SO.sub.4 can be provided as "semiconductor grade" acids in concentrations of generally 40-50% by weight HF, and at least 90% by weight H.sub.2 SO.sub.4.

In vivo effect of a self-etching primer on dentin.

PubMed

Milia, E; Lallai, M R; García-Godoy, F

1999-08-01

To determine the ultrastructural aspects of the dentin collagen area in the cavity preparation floor produced in vivo after phosphoric acid acid-etching or after using Clearfil Liner Bond 2 self-etching primer (LB2 Primer). Twenty-four non-carious third molars scheduled for extraction from young adult patients (16-30 years old) were used. Conventional Class I cavities (+/- 2 mm deep) were prepared on the occlusal surfaces of all teeth using a cylindrical diamond bur on a high-speed handpiece with copious water spray. To avoid dehydration of the dentin, the smear layer-covered dentin was briefly air-dried for 2 seconds. Cavities were assigned at random to the following groups: Group A: Dentin etched for 15 seconds with 34% phosphoric acid, rinsed for 20 seconds and then briefly air-dried for 2 seconds with oil-free compressed air leaving the surfaces slightly moist. Group B: LB2 Primer was applied to the cavity surfaces for 30 seconds and then briefly air-dried to remove the solvent. Group C: The untreated dentin smear layer was used as a control. In all three groups, the cavities were filled incrementally with a resin-based composite (APX), light curing every increment for 40 seconds. After 30 minutes, the teeth were extracted atraumatically and the samples immediately prepared for evaluation with the transmission electron microscope. The use of a self-etching primer did not produce significant morphological changes in the moist dentin substrate. Adverse morphological conditions where observed when there was an excess water on the dentin surface. Phosphoric acid altered the collagen more severely than the self-etching primer.

Closed System Step Etching of CI chondrite Ivuna reveals primordial noble gases in the HF-solubles

NASA Astrophysics Data System (ADS)

Riebe, My E. I.; Busemann, Henner; Wieler, Rainer; Maden, Colin

2017-05-01

We analyzed all the noble gases in HF-soluble phases in the CI chondrite Ivuna by in-vacuum gas release using the "Closed System Step Etching" (CSSE) technique, which allows for direct noble gas measurements of acid-soluble phases. The main motivation was to investigate if there are primordial noble gases in HF-soluble phases in Ivuna, something that has not been done before in CI chondrites, as most primordial noble gases are known to reside in HF-resistant phases. The first steps under mild etching released He, Ne, and Ar with solar-like elemental and isotopic compositions, confirming that Ivuna contains implanted solar wind (SW) noble gases acquired in the parent body regolith. The SW component released in some etch steps was elementally unfractionated. This is unusual as trapped SW noble gases are elementally fractionated in most meteoritic material. In the intermediate etch steps under slightly harsher etching, cosmogenic noble gases were more prominent than SW noble gases. The HF-soluble portion of Ivuna contained primordial Ne and Xe, that was most visible in the last etch steps after all cosmogenic and most SW gases had been released. The primordial Ne and Xe in the HF-solubles have isotopic and elemental ratios readily explained as a mixture of the two most abundant primordial noble gas components in Ivuna bulk samples: HL and Q. Only small fractions of the total HL and Q in Ivuna were released during CSSE analysis; ∼3% of 20NeHL and ∼4% of 132XeQ. HL is known to reside in nanodiamond-rich separates and Q-gases are most likely carried by a carbonaceous phase known as phase Q. Q-gases were likely released from an HF-soluble portion of phase Q. However, nanodiamonds might not be the source of the HL-gases released upon etching, since nanodiamond-rich separates are very HF-resistant and the less tightly bound nanodiamond component P3 was not detected.

Development of Superhydrophobic Material SS 17-4 PH for Bracket Orthodontic Application by Metal Injection Molding

NASA Astrophysics Data System (ADS)

Supriadi, S.; Suharno, B.; Widjaya, T.; Ayuningtyas, S. T.; Baek, E. R.

2018-01-01

Dental’s plaque is a common problem that encountered during orthodontic treatment using bracket. It is caused by demineralization of enamel due to the activity of bacteria. The bacteria increase with remaining excess food which trapped in teeth and bracket. A hydrophobic surface could reduce food attachment on the bracket because of extremely low wettability properties that make it easy to clean with water. There are several methods to obtain hydrophobic surfaces, which are sol-gel, template replica and also etching. The propose of this work is to compare etching treatment and surface modification on sintered SS 17-4 PH as bracket material using CuCl2 and HCl as an etchant while stearic acid was used for surface modification. Hydrophobic surfaces were produced under various etching time i.e 15, 30, 45 and 60 seconds for CuCl2 and 40, 50, 60 and 70 minutes for HCl and also HCl concentration i.e 1,2 and 3 mol/L at room temperature. The hydrophobicity is observed using contact angle measurement while the microstructures observed by Scanning Electron Microscope. The result shows the contact angle could be achieved up to 60% higher than the as-sintered material. Hydrophobic structure has successfully fabricated using etching technique that might be applied to the orthodontic bracket.

Low-Temperature Aging of Delta-Ferrite in 316L SS Welds; Changes in Mechanical Properties and Etching Properties

NASA Astrophysics Data System (ADS)

Abe, Hiroshi; Shimizu, Keita; Watanabe, Yutaka

Thermal aging embrittlement of LWR components made of stainless cast (e.g. CF-8 and CF-8M) is a potential degradation issue, and careful attention has been paid on it. Although welds of austenitic stainless steels (SSs) have γ-δ duplex microstructure, which is similar to that of the stainless cast, examination on thermal aging characteristics of the SS welds is very limited. In order to evaluate thermal aging behavior of weld metal of austenitic stainless steel, the 316L SS weld metal has been prepared and changes in mechanical properties and in etching properties at isothermal aging at 335°C have been investigated. The hardness of the ferrite phase has increased with aging, while the hardness of austenite phase has stayed same. It has been suggested that spinodal decomposition has occurred in δ-ferrite by the 335°C aging. The etching rates of δ-ferrite at immersion test in 5wt% hydrochloric acid solution have been also investigated using an AFM technique. The etching rate of ferrite phase has decreased consistently with the increase in hardness of ferrite phase. It has been thought that this characteristic is also caused by spinodal decomposition of ferrite into chromium-rich (α') and iron-rich (α).

Hydroxyapatite Effect on Photopolymerization of Self-etching Adhesives with Different Aggressiveness

PubMed Central

Zhang, Ying; Wang, Yong

2012-01-01

Objective To understand the correlation of the acidic monomer/hydroxyapatite (HAp) reaction with the photopolymerization behavior of self-etching adhesives with different aggressiveness. Methods Two commercial self-etching adhesives the strong Adper Prompt L-Pop (APLP, pH~0.8) and the mild Adper Easy Bond (AEB, pH~2.5) were used. HAp powders were incorporated into both adhesives to acquire solutions with concentrations of 0, 1, 3, 5, 7 wt%. The attenuated total reflectance Fourier transform infrared (ATR/FT-IR) technique was employed to collect the in-situ spectra during light-curing, from which the degree of conversion (DC) and polymerization rate (PR) were calculated. The pH of each tested solution was also measured. Results Without HAp incorporation, the DC and PR of the strong APLP (7.8% and 0.12%/s, respectively) were much lower than those of the mild AEB (85.5% and 5.7%/s, respectively). The DC and PR of APLP displayed an apparent increasing trend with the HAp content. For example, the DC increased from 7.8% to 58.4% and the PR increased from 0.12 to 3.8%/s when the HAp content increased from 0 to 7 wt%. In contrast, the DC and PR of AEB were much less affected by the HAp content. The observations were correlated well with the spectral and pH changes, which indicated that APLP underwent a higher extent of chemical reaction with HAp than AEB. Conclusions The results disclosed the important role of the acidic monomer/HAp chemical reaction in improving the photopolymerization of the strong (low-pH) self-etching adhesives such as APLP. The phenomenon of polymerization improvement strongly depended on the adhesive aggressiveness. PMID:22445789

Fiberoptic microneedles: novel optical diffusers for interstitial delivery of therapeutic light.

PubMed

Kosoglu, Mehmet A; Hood, Robert L; Rossmeisl, John H; Grant, David C; Xu, Yong; Robertson, John L; Rylander, Marissa Nichole; Rylander, Christopher G

2011-11-01

Photothermal therapies have limited efficacy and application due to the poor penetration depth of light inside tissue. In earlier work, we described the development of novel fiberoptic microneedles to provide a means to mechanically penetrate dermal tissue and deliver light directly into a localized target area.This paper presents an alternate fiberoptic microneedle design with the capability of delivering more diffuse, but therapeutically useful photothermal energy. Laser lipolysis is envisioned as a future clinical application for this design. A novel fiberoptic microneedle was developed using hydrofluoric acid etching of optical fiber to permit diffuse optical delivery. Microneedles etched for 10, 30, and 50 minutes, and an optical fiber control were compared with three techniques. First, red light delivery from the microneedles was evaluated by imaging the reflectance of the light from a white paper.Second, spatial temperature distribution of the paper in response to near-IR light (1,064 nm, 1 W CW) was recorded using infrared thermography. Third, ex vivo adipose tissue response during 1,064 nm, (5 W CW)irradiation was recorded with bright field microscopy. Acid etching exposed a 3 mm length of the fiber core, allowing circumferential delivery of light along this length. Increasing etching time decreased microneedle diameter, resulting in increased uniformity of red and 1,064 nm light delivery along the microneedle axis. For equivalent total energy delivery, thinner microneedles reduced carbonization in the adipose tissue experiments. We developed novel microscale optical diffusers that provided a more homogeneous light distribution from their surfaces, and compared performance to a flat-cleaved fiber, a device currently utilized in clinical practice. These fiberoptic microneedles can potentially enhance clinical laser procedures by providing direct delivery of diffuse light to target chromophores, while minimizing undesirable photothermal damage in adjacent, non-target tissue. Copyright © 2011 Wiley Periodicals, Inc.

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.

Effects of different etching methods and bonding procedures on shear bond strength of orthodontic metal brackets applied to different CAD/CAM ceramic materials.

PubMed

Buyuk, S Kutalmış; Kucukekenci, Ahmet Serkan

2018-03-01

To investigate the shear bond strength (SBS) of orthodontic metal brackets applied to different types of ceramic surfaces treated with different etching procedures and bonding agents. Monolithic CAD/CAM ceramic specimens (N = 120; n = 40 each group) of feldspathic ceramic Vita Mark II, resin nanoceramic Lava Ultimate, and hybrid ceramic Vita Enamic were fabricated (14 × 12 × 3 mm). Ceramic specimens were separated into four subgroups (n = 10) according to type of surface treatment and bonding onto the ceramic surface. Within each group, four subgroups were prepared by phosphoric acid, hydrofluoric acid, Transbond XT primer, and Clearfill Ceramic primer. Mandibular central incisor metal brackets were bonded with light-cure composite. The SBS data were analyzed using three-way analysis of variance (ANOVA) and Tukey HSD tests. The highest SBS was found in the Vita Enamic group, which is a hybrid ceramic, etched with hydrofluoric acid and applied Transbond XT Adhesive primer (7.28 ± 2.49 MPa). The lowest SBS was found in the Lava Ultimate group, which is a resin nano-ceramic etched with hydrofluoric acid and applied Clearfill ceramic primer (2.20 ± 1.21 MPa). CAD/CAM material types and bonding procedures affected bond strength ( P < .05), but the etching procedure did not ( P > .05). The use of Transbond XT as a primer bonding agent resulted in higher SBS.

An Easy to Manufacture Micro Gas Preconcentrator for Chemical Sensing Applications.

PubMed

McCartney, Mitchell M; Zrodnikov, Yuriy; Fung, Alexander G; LeVasseur, Michael K; Pedersen, Josephine M; Zamuruyev, Konstantin O; Aksenov, Alexander A; Kenyon, Nicholas J; Davis, Cristina E

2017-08-25

We have developed a simple-to-manufacture microfabricated gas preconcentrator for MEMS-based chemical sensing applications. Cavities and microfluidic channels were created using a wet etch process with hydrofluoric acid, portions of which can be performed outside of a cleanroom, instead of the more common deep reactive ion etch process. The integrated heater and resistance temperature detectors (RTDs) were created with a photolithography-free technique enabled by laser etching. With only 28 V DC (0.1 A), a maximum heating rate of 17.6 °C/s was observed. Adsorption and desorption flow parameters were optimized to be 90 SCCM and 25 SCCM, respectively, for a multicomponent gas mixture. Under testing conditions using Tenax TA sorbent, the device was capable of measuring analytes down to 22 ppb with only a 2 min sample loading time using a gas chromatograph with a flame ionization detector. Two separate devices were compared by measuring the same chemical mixture; both devices yielded similar peak areas and widths (fwhm: 0.032-0.033 min), suggesting reproducibility between devices.

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).

Radiation induced deposition of copper nanoparticles inside the nanochannels of poly(acrylic acid)-grafted poly(ethylene terephthalate) track-etched membranes

NASA Astrophysics Data System (ADS)

Korolkov, Ilya V.; Güven, Olgun; Mashentseva, Anastassiya A.; Atıcı, Ayse Bakar; Gorin, Yevgeniy G.; Zdorovets, Maxim V.; Taltenov, Abzal A.

2017-01-01

Poly(ethylene terephthalate) PET, track-etched membranes (TeMs) with 400 nm average pore size were UV-grafted with poly(acrylic acid) (PAA) after oxidation of inner surfaces by H2O2/UV system. Carboxylate groups of grafted PAA chains were easily complexed with Cu2+ ions in aqueous solutions. These ions were converted into metallic copper nanoparticles (NPs) by radiation-induced reduction of copper ions in aqueous-alcohol solution by gamma rays in the dose range of 46-250 kGy. Copper ions chelating with -COOH groups of PAA chains grafted on PET TeMs form polymer-metal ion complex that prevent the formation of agglomerates during reduction of copper ions to metallic nanoparticles. The detailed analysis by X-Ray diffraction technique (XRD), transmission electron microscopy (TEM), scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed the deposition of copper nanoparticles with the average size of 70 nm on the inner surface of nanochannels of PET TeMs. Samples were also investigated by FTIR, ESR spectroscopies to follow copper ion reduction.

Image processing analysis of nuclear track parameters for CR-39 detector irradiated by thermal neutron

NASA Astrophysics Data System (ADS)

Al-Jobouri, Hussain A.; Rajab, Mustafa Y.

2016-03-01

CR-39 detector which covered with boric acid (H3Bo3) pellet was irradiated by thermal neutrons from (241Am - 9Be) source with activity 12Ci and neutron flux 105 n. cm-2. s-1. The irradiation times -TD for detector were 4h, 8h, 16h and 24h. Chemical etching solution for detector was sodium hydroxide NaOH, 6.25N with 45 min etching time and 60 C˚ temperature. Images of CR-39 detector after chemical etching were taken from digital camera which connected from optical microscope. MATLAB software version 7.0 was used to image processing. The outputs of image processing of MATLAB software were analyzed and found the following relationships: (a) The irradiation time -TD has behavior linear relationships with following nuclear track parameters: i) total track number - NT ii) maximum track number - MRD (relative to track diameter - DT) at response region range 2.5 µm to 4 µm iii) maximum track number - MD (without depending on track diameter - DT). (b) The irradiation time -TD has behavior logarithmic relationship with maximum track number - MA (without depending on track area - AT). The image processing technique principally track diameter - DT can be take into account to classification of α-particle emitters, In addition to the contribution of these technique in preparation of nano- filters and nano-membrane in nanotechnology fields.

Surface Modification of Ti-35Nb-10Ta-1.5Fe by the Double Acid-Etching Process

PubMed Central

Amigó, Angélica

2018-01-01

Surface topography and composition influence the osteoblastic proliferation and osseointegration rates, which favor the biomechanical stability of bone anchoring and implants. In recent years, beta titanium alloys have been developed, and are composed of biocompatible elements, have low elastic modulus, high corrosion resistance, and mechanical properties to improve the long performance behavior of biomaterials. In the present research, the influence of the acid-etching process was studied in Ti6Al4V ELI and Ti35Nb10Ta1.5Fe. Samples were etched in a two-step acid treatment. Surface roughness parameters were quantified under a confocal microscope, topography was studied by scanning electron microscopy, and surface composition was analyzed with energy dispersive X-ray spectroscopy. The results revealed that the two-step acid treatment changes the topography of the β alloy, increases the surface area, and changes the chemical composition of the surface. Two differentiated regions were identified in the Ti35Nb10Ta1.5Fe alloy after the acid-etching process: The α + β region with higher values of mean roughness due to the lower chemical resistance of this region; and the β region with lower values of roughness parameters. PMID:29587427

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.

METHOD OF APPLYING COPPER COATINGS TO URANIUM

DOEpatents

Gray, A.G.

1959-07-14

A method is presented for protecting metallic uranium, which comprises anodic etching of the uranium in an aqueous phosphoric acid solution containing chloride ions, cleaning the etched uranium in aqueous nitric acid solution, promptly electro-plating the cleaned uranium in a copper electro-plating bath, and then electro-plating thereupon lead, tin, zinc, cadmium, chromium or nickel from an aqueous electro-plating bath.

IRON COATED URANIUM AND ITS PRODUCTION

DOEpatents

Gray, A.G.

1960-03-15

A method of applying a protective coating to a metallic uranium article is given. The method comprises etching the surface of the article with an etchant solution containlng chloride ions, such as a solution of phosphoric acid and hydrochloric acid, cleaning the etched surface, electroplating iron thereon from a ferrous ammonium sulfate electroplating bath, and soldering an aluminum sheath to the resultant iron layer.

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.

Solvothermal synthesis of selenium nano and microspheres deposited on silicon surface by microwave-assisted method

NASA Astrophysics Data System (ADS)

Ahmad, Muthanna

2016-10-01

This work describes a new application of the solvothermal method, based on the microwave heating, for the synthesis of nano and microparticles of selenium. The reaction of selenium with hydrofluoric acid on the silicon surface is induced by microwave irradiation under high pressure and temperature of 60 bar and 160 °C, respectively. This method allows the deposition of spherical-like particles on the in situ etched silicon surface. The size of deposited selenium spheres scales from tens of nanometers up to tens of micrometers. The morphology and composition of the deposited selenium were analyzed by various analytical techniques. The formation dynamic of spherical structure is explained on the base of reduction of selenium species by hydrogen inside gas bubbles which are generated on the silicon surface by the etching process.

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.

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.

Epoxy bond and stop etch fabrication method

DOEpatents

Simmons, Jerry A.; Weckwerth, Mark V.; Baca, Wes E.

2000-01-01

A class of epoxy bond and stop etch (EBASE) microelectronic fabrication techniques is disclosed. The essence of such techniques is to grow circuit components on top of a stop etch layer grown on a first substrate. The first substrate and a host substrate are then bonded together so that the circuit components are attached to the host substrate by the bonding agent. The first substrate is then removed, e.g., by a chemical or physical etching process to which the stop etch layer is resistant. EBASE fabrication methods allow access to regions of a device structure which are usually blocked by the presence of a substrate, and are of particular utility in the fabrication of ultrafast electronic and optoelectronic devices and circuits.

Change in surface properties of zirconia and initial attachment of osteoblastlike cells with hydrophilic treatment.

PubMed

Watanabe, Hiroaki; Saito, Kensuke; Kokubun, Katsutoshi; Sasaki, Hodaka; Yoshinari, Masao

2012-01-01

The objectives of this study were to characterize change in surface properties of tetragonal zirconia polycrystals (TZP) after hydrophilic treatment, and to determine the effect of such changes on initial attachment of osteoblast-like cells. Roughened surfaces were produced by alumina-blasting and acid-etching. Hydrophilic treatment comprised application of immediately after blasting and acid-etching (Blast/Etch), oxygen plasma (O2-Plasma), ultraviolet light (UV). Specimens stored in air were used as a control. The water contact angle was determined and surface analysis was performed using an X-ray photoelectron spectroscopy. Blast/Etch, O2-Plasma and UV specimens showed superhydrophilicity, and these hydrophilic treatments to TZP elicited a marked decrease in carbon content and an increase in hydroxyl groups. Hydrophilic treatments enhanced initial attachment of osteoblast-like cells and a change in cell morphologies. These results indicate that Blast/Etch, O2-Plasma, or UV treatment has potential in the creation and maintenance of superhydrophilic surfaces and enhancing initial attachment of osteoblast-like cells.

Tensile bond strength of an aged resin composite repaired with different protocols.

PubMed

Celik, Esra Uzer; Ergücü, Zeynep; Türkün, L Sebnem; Ercan, Utku Kürșat

2011-08-01

To evaluate the effect of different surface treatments and bonding procedures on the tensile bond strength (TBS) of resin composites repaired 6 months after polymerization. Resin composite sticks were aged in distilled water at 37°C for 6 months. They were divided into 12 groups (n = 10) according to the combination of surface treatment/bonding procedures [none, only bur treatment, XP Bond (XPB/Dentsply/DeTrey) with/without bur, AdheSE (A-SE/Ivoclar/Vivadent) with/without bur, Composite Primer (CP/GC) with/without bur, CP after bur and acid-etching, XPB after acid etching and CP with bur, A-SE after bur and CP]. The ultimate tensile bond strength (UTS) of the resin composites was tested in intact but aged specimens. Tensile bond strengths were tested with a universal testing machine (Shimadzu). Data were analyzed using one-way ANOVA and Duncan Multiple Comparisons tests (p < 0.05). All repaired groups showed significantly higher TBS than the group without any sureface treatment (p < 0.05). Four groups resulted in TBS similar to those of intact resin composite UTS: A-SE, A-SE with bur, A-SE after CP with bur, and XPB after acid etching+CP with bur. Bur treatment, silane primer or etch-and-rinse adhesive application alone were not successful in the repair process of aged resin composite, whereas self-etching adhesive alone showed similar performance to the intact specimens. Combined procedures generally showed better performance: A-SE with bur, A-SE after CP with bur, and XPB after acid etching +CP with bur showed TBS similar to those of the intact specimens. It was concluded that bur roughening of the surfaces and rebonding procedures were essential for repairing aged resin composites.

Comparison of Shear Bond Strength of Orthodontic Brackets Bonded to Enamel Prepared By Er:YAG Laser and Conventional Acid-Etching

PubMed Central

Hosseini, M.H.; Namvar, F.; Chalipa, J.; Saber, K.; Chiniforush, N.; Sarmadi, S.; Mirhashemi, A.H.

2012-01-01

Introduction: The purpose of this study was to compare shear bond strength (SBS) of orthodontic brackets bonded to enamel prepared by Er:YAG laser with two different powers and conventional acid-etching. Materials and Methods: Forty-five human premolars extracted for orthodontic purposes were randomly assigned to three groups based on conditioning method: Group 1- conventional etching with 37% phosphoric acid; Group 2- irradiation with Er:YAG laser at 1 W; and Group 3- irradiation with Er:YAG laser at 1.5 W. Metal brackets were bonded on prepared enamel using a light-cured composite. All groups were subjected to thermocycling process. Then, the specimens mounted in auto-cure acryle and shear bond strength were measured using a universal testing machine with a crosshead speed of 0.5 mm per second. After debonding, the amount of resin remaining on the teeth was determined using the adhesive remnant index (ARI) scored 1 to 5. One-way analysis of variance was used to compare shear bond strengths and the Kruskal-Wallis test was performed to evaluate differences in the ARI for different etching types. Results: The mean and standard deviation of conventional acid-etch group, 1W laser group and 1.5W laser group was 3.82 ± 1.16, 6.97 ± 3.64 and 6.93 ± 4.87, respectively. Conclusion: The mean SBS obtained with an Er:YAG laser operated at 1W or 1.5W is approximately similar to that of conventional etching. However, the high variability of values in bond strength of irradiated enamel should be considered to find the appropriate parameters for applying Er:YAG laser as a favorable alternative for surface conditioning. PMID:22924098

Comparative evaluation of self-etching primers and phosphoric acid effectiveness on composite to enamel bond: an in vitro study.

PubMed

Patil, Basanagouda S; Rao, Bk Raghavendra; Sharathchandra, Sm; Hegde, Reshma; Kumar, G Vinay

2013-09-01

The aim of the present study was to investigate the effectiveness of the one total-etch self-priming adhesive, one two-step self-etching primer adhesive, and one 'all-in-one' self-etching adhesive system on the adhesion of a resin composite to enamel. Thirty-six freshly extracted human mandibular molars were selected for this study. A fat area about 5 mm in diameter was created on the exposed mesial surface of enamel of each tooth by moist grinding with 320, 420 and 600 grit silicon carbide paper. Twelve teeth were randomly assigned into three groups. In group 1, Adper Easy One (3M ESPE), a one step self-etching primer adhesive was applied and light curing unit for 10 seconds. In group 2, Adper SE Plus, a two-step self-etching primer with bottle A containing the aqueous primer and bottle B containing the acidic adhesive was applied and light cured for 10 seconds. Group 3 (control)-etchant 37% phosphoric acid is applied to the surface for 15 seconds and rinsed with water and air dried and adhesive (single bond 2) is applied to the surface and tube is placed and light cured for 20 seconds. Composite material (Z350) was placed in the tube and light cured for 40 seconds in all the groups. Bond strength testing was done using universal testing machine at the enamel-composite interface. The debonded enamel surface was evaluated in stereomicroscope to assess the cohesive, adhesive or mixed fracture. Data was statistically analyzed by one way analysis of variance (ANOVA). Group 1 performed least among all groups with a mean score of 19.46 MPa. Group 2 had a mean score of 25.67 MPa. Group 3 had a mean score of 27.16 MPa. Under the conditions of this in vitro study, the bond strength values of the two-step self-etching primer systems tested were similar to the total-etch. And, one step self-etching primers have lower bond strength compared to the total-etch.

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.

Cleaning carbon steel

NASA Technical Reports Server (NTRS)

Maynard, V.

1976-01-01

Increased etch rate using 8% citric acid actually reduces total amount of material etched away by eliminating reprocessing that was frequently required. Time required in citrosolve solution is reduced and more protective passive coating is provided.

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

[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.

Formation of nanogaps in InAs nanowires by selectively etching embedded InP segments.

PubMed

Schukfeh, M I; Storm, K; Hansen, A; Thelander, C; Hinze, P; Beyer, A; Weimann, T; Samuelson, L; Tornow, M

2014-11-21

We present a method to fabricate nanometer scale gaps within InAs nanowires by selectively etching InAs/InP heterostructure nanowires. We used vapor-liquid-solid grown InAs nanowires with embedded InP segments of 10-60 nm length and developed an etching recipe to selectively remove the InP segment. A photo-assisted wet etching process in a mixture of acetic acid and hydrobromic acid gave high selectivity, with accurate removal of InP segments down to 20 nm, leaving the InAs wire largely unattacked, as verified using scanning electron and transmission electron microscopy. The obtained nanogaps in InAs wires have potential as semiconducting electrodes to investigate electronic transport in nanoscale objects. We demonstrate this functionality by dielectrophoretically trapping 30 nm diameter gold nanoparticles into the gap.

Effect of two fiber post types and two luting cement systems on regional post retention using the push-out test.

PubMed

Wang, Vivian J-J; Chen, Ya-Ming; Yip, Kevin H-K; Smales, Roger J; Meng, Qing-Fei; Chen, Lijuan

2008-03-01

To investigate regional root canal push-out bond strengths for two fiber-reinforced post types using two adhesive systems. The crowns of 24 recently extracted sound maxillary central incisors were sectioned transversely 2 mm coronal to the labial cemento-enamel junction, and the roots treated endodontically. Following standardized post space preparations, fiber-reinforced posts (C-POST; AESTHETI-PLUS) were placed using two adhesive systems (acid-etch ONE-STEP PLUS/C&B CEMENT; self-adhesive RelyX Unicem), in four equal groups. Push-out bond strength tests were performed at four sites in each root. Results were analyzed using split-plot ANOVA, with a=0.05 for statistical significance. AESTHETI-PLUS quartz fiber-reinforced posts showed significantly higher push-out strengths than C-POST carbon fiber-reinforced posts (P<0.0001). The separate acid-etch adhesive system resulted in significantly higher bond strengths than the self-etch self-adhesive system (P<0.0001). Bond strengths decreased significantly from coronal to apical root canal regions (P<0.0001). The quartz fiber-reinforced post placed using the separate acid-etch adhesive system provided significantly better post retention than the carbon fiber-reinforced post placed using the self-etch self-adhesive system.

Laser investigation of the non-uniformity of fluorescent species in dental enamel

NASA Astrophysics Data System (ADS)

Tran, Stephanie U.; Ridge, Jeremy S.; Nelson, Leonard Y.; Seibel, Eric J.

In the present study, artificial type I and type II erosions were created on dental specimen using acetic acid and EDTA respectively. Specimens were prepared by etching extracted teeth samples in acid to varying degrees, after which the absolute fluorescence intensity ratio of the etched enamel relative to sound enamel was recorded for each specimen using 405 and 532 nm laser excitation. Results showed differences in the fluorescence ratio of etched to sound enamel for type I and II erosions. These findings suggest a non-uniform distribution of fluorescent species in the interprismatic region as compared to the prismatic region.

Redox buffered hydrofluoric acid etchant for the reduction of galvanic attack during release etching of MEMS devices having noble material films

DOEpatents

Hankins, Matthew G [Albuquerque, NM

2009-10-06

Etchant solutions comprising a redox buffer can be used during the release etch step to reduce damage to the structural layers of a MEMS device that has noble material films. A preferred redox buffer comprises a soluble thiophosphoric acid, ester, or salt that maintains the electrochemical potential of the etchant solution at a level that prevents oxidation of the structural material. Therefore, the redox buffer preferentially oxidizes in place of the structural material. The sacrificial redox buffer thereby protects the exposed structural layers while permitting the dissolution of sacrificial oxide layers during the release etch.

COATING METHOD

DOEpatents

Townsend, R.G.

1959-08-25

A method is described for protectively coating beryllium metal by etching the metal in an acid bath, immersing the etched beryllium in a solution of sodium zincate for a brief period of time, immersing the beryllium in concentrated nitric acid, immersing the beryhlium in a second solution of sodium zincate, electroplating a thin layer of copper over the beryllium, and finally electroplating a layer of chromium over the copper layer.

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.

Self-etching ceramic primer versus hydrofluoric acid etching: Etching efficacy and bonding performance.

PubMed

El-Damanhoury, Hatem M; Gaintantzopoulou, Maria D

2018-01-01

This study assessed the effect of pretreatment of hybrid and glass ceramics using a self-etching primer on the shear bond strength (SBS) and surface topography, in comparison to pretreatment with hydrofluoric acid and silane. 40 rectangular discs from each ceramic material (IPS e.max CAD;EM, Vita Mark II;VM, Vita Enamic;VE), were equally divided (n=10) and assigned to one of four surface pretreatment methods; etching with 4.8% hydrofluoric acid followed by Monobond plus (HFMP), Monobond etch & prime (Ivoclar Vivadent) (MEP), No treatment (NT) as negative control and Monobond plus (Ivoclar Vivadent) with no etching (MP) as positive control. SBS of resin cement (Multilink-N, Ivoclar Vivadent) to ceramic surfaces was tested following a standard protocol. Surface roughness was evaluated using an Atomic force microscope (AFM). Surface topography and elemental analysis were analyzed using SEM/EDX. Data were analyzed with two-way analysis of variance (ANOVA) and post-hoc Bonferroni test at a significance level of α=0.05. Pretreatment with HFMP resulted in higher SBS and increased surface roughness in comparison to MEP and MP. Regardless the method of surface pretreatment, the mean SBS values of EM ceramic was significantly higher (p<0.05) than those recorded for VM and VE, except when VE was treated with MEP, where the difference was statistically insignificant. Traces of fluoride ion were detected when MEP was used with VE and VM. Under limited conditions, using MEP resulted in comparable SBS results to HFMP; meanwhile HFMP remains the gold standard for pretreatment of glass ceramics for resin-luting cementation. Copyright © 2017 Japan Prosthodontic Society. Published by Elsevier Ltd. All rights reserved.

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

A novel 2D silicon nano-mold fabrication technique for linear nanochannels over a 4 inch diameter substrate

PubMed Central

Yin, Zhifu; Qi, Liping; Zou, Helin; Sun, Lei

2016-01-01

A novel low-cost 2D silicon nano-mold fabrication technique was developed based on Cu inclined-deposition and Ar+ (argon ion) etching. With this technique, sub-100 nm 2D (two dimensional) nano-channels can be etched economically over the whole area of a 4 inch n-type <100> silicon wafer. The fabricating process consists of only 4 steps, UV (Ultraviolet) lithography, inclined Cu deposition, Ar+ sputter etching, and photoresist & Cu removing. During this nano-mold fabrication process, we investigated the influence of the deposition angle on the width of the nano-channels and the effect of Ar+ etching time on their depth. Post-etching measurements showed the accuracy of the nanochannels over the whole area: the variation in width is 10%, in depth it is 11%. However, post-etching measurements also showed the accuracy of the nanochannels between chips: the variation in width is 2%, in depth it is 5%. With this newly developed technology, low-cost and large scale 2D nano-molds can be fabricated, which allows commercial manufacturing of nano-components over large areas. PMID:26752559

Laser micro-etching of metal prostheses for personal identification

PubMed Central

Ganapathy, Dhanraj; Sivaswamy, Vinay; Sekhar, Prathap

2017-01-01

Denture marking techniques play a vital role in establishing personal identification in suitable clinical and forensic situations. The denture marking techniques are categorized broadly into additive and ablative methods. Additive methods involve embedding or impregnation of markers for establishing personal identity. Ablative methods involve partial removal of the denture surface thereby providing a marking for identification. Engraving and etching methods are the commonly used ablative methods. Ablative methods can be of contact and noncontact subtypes. Laser micro-etching is a precise noncontact ablative denture marking technique that could be used for prostheses-guided personal identification. PMID:28584473

Laser micro-etching of metal prostheses for personal identification.

PubMed

Ganapathy, Dhanraj; Sivaswamy, Vinay; Sekhar, Prathap

2017-01-01

Denture marking techniques play a vital role in establishing personal identification in suitable clinical and forensic situations. The denture marking techniques are categorized broadly into additive and ablative methods. Additive methods involve embedding or impregnation of markers for establishing personal identity. Ablative methods involve partial removal of the denture surface thereby providing a marking for identification. Engraving and etching methods are the commonly used ablative methods. Ablative methods can be of contact and noncontact subtypes. Laser micro-etching is a precise noncontact ablative denture marking technique that could be used for prostheses-guided personal identification.

Bioactive Surface Modification of Hydroxyapatite

PubMed Central

Okazaki, Yohei; Hiasa, Kyou; Yasuda, Keisuke; Nogami, Keisuke; Mizumachi, Wataru; Hirata, Isao

2013-01-01

The purpose of this study was to establish an acid-etching procedure for altering the Ca/P ratio of the nanostructured surface of hydroxyapatite (HAP) by using surface chemical and morphological analyses (XPS, XRD, SEM, surface roughness, and wettability) and to evaluate the in vitro response of osteoblast-like cells (MC3T3-E1 cells) to the modified surfaces. This study utilized HAP and HAP treated with 10%, 20%, 30%, 40%, 50%, or 60% phosphoric acid solution for 10 minutes at 25°C, followed by rinsing 3 times with ultrapure water. The 30% phosphoric acid etching process that provided a Ca/P ratio of 1.50, without destruction of the grain boundary of HAP, was selected as a surface-modification procedure. Additionally, HAP treated by the 30% phosphoric acid etching process was stored under dry conditions at 25°C for 12 hours, and the Ca/P ratio approximated to 1.00 accidentally. The initial adhesion, proliferation, and differentiation (alkaline phosphatase (ALP) activity and relative mRNA level for ALP) of MC3T3-E1 cells on the modified surfaces were significantly promoted (P < 0.05 and 0.01). These findings show that the 30% phosphoric acid etching process for the nanostructured HAP surface can alter the Ca/P ratio effectively and may accelerate the initial adhesion, proliferation, and differentiation of MC3T3-E1 cells. PMID:23862150

Shear bond strength and SEM morphology evaluation of different dental adhesives to enamel prepared with ER:YAG laser

PubMed Central

Pires, Patrícia T.; Ferreira, João C.; Oliveira, Sofia A.; Azevedo, Álvaro F.; Dias, Walter R.; Melo, Paulo R.

2013-01-01

Context: Early observations of enamel surfaces prepared by erbium lasers motivated clinicians to use laser as an alternative to chemical etching. Aims: Evaluate shear bond strength (SBS) values of different dental adhesives on Erbium:Yttrium Aluminum Garnet (Er:YAG) laser prepared enamel and to evaluate possible etching patterns correlations between dental adhesives and SBS values. Subjects and Methods: One hundred bovine incisors were randomly assigned to SBS tests on enamel (n = 15) and to enamel morphology analysis (n = 5) after Er:YAG laser preparation as follows: Group I – 37% phosphoric acid (PA)+ ExciTE®; Group II – ExciTE®; Group III – AdheSE® self-etching; Group IV – FuturaBond® no-rinse. NR; Group V – Xeno® V. Teeth were treated with the adhesive systems and subjected to thermal cycling. SBS were performed in a universal testing machine at 5 mm/min. Statistical Analysis Used: One-way ANOVA and post-hoc tests (P < 0.05). For the morphology evaluation, specimens were immersed in Ethylenediamine tetraacetic acid (EDTA) and the etching pattern analyzed under Scanning Electron Microscope (SEM). Results: Mean bond strengths were Group I – 47.17 ± 1.61 MPa (type I etching pattern); Group II – 32.56 ± 1.64 MPa, Group III – 29.10 ± 1.34 MPa, Group IV – 23.32 ± 1.53 MPa (type III etching pattern); Group V – 24.43 MPa ± 1.55 (type II etching pattern). Conclusions: Different adhesive systems yielded significantly different SBSs. Acid etching significantly increased the adhesion in laser treated enamel. No differences in SBS values were obtained between AdheSE® and ExciTE® without condition with PA. FuturaBond® NR and Xeno® V showed similar SBS, which was lower in comparison to the others adhesives. No correlation between enamel surface morphology and SBS values was observed, except when PA was used. PMID:23853447

Shear bond strength and SEM morphology evaluation of different dental adhesives to enamel prepared with ER:YAG laser.

PubMed

Pires, Patrícia T; Ferreira, João C; Oliveira, Sofia A; Azevedo, Alvaro F; Dias, Walter R; Melo, Paulo R

2013-01-01

Early observations of enamel surfaces prepared by erbium lasers motivated clinicians to use laser as an alternative to chemical etching. Evaluate shear bond strength (SBS) values of different dental adhesives on Erbium:Yttrium Aluminum Garnet (Er:YAG) laser prepared enamel and to evaluate possible etching patterns correlations between dental adhesives and SBS values. One hundred bovine incisors were randomly assigned to SBS tests on enamel (n = 15) and to enamel morphology analysis (n = 5) after Er:YAG laser preparation as follows: Group I - 37% phosphoric acid (PA)+ ExciTE(®); Group II - ExciTE(®); Group III - AdheSE(®) self-etching; Group IV - FuturaBond(®) no-rinse. NR; Group V - Xeno(®) V. Teeth were treated with the adhesive systems and subjected to thermal cycling. SBS were performed in a universal testing machine at 5 mm/min. One-way ANOVA and post-hoc tests (P < 0.05). For the morphology evaluation, specimens were immersed in Ethylenediamine tetraacetic acid (EDTA) and the etching pattern analyzed under Scanning Electron Microscope (SEM). Mean bond strengths were Group I - 47.17 ± 1.61 MPa (type I etching pattern); Group II - 32.56 ± 1.64 MPa, Group III - 29.10 ± 1.34 MPa, Group IV - 23.32 ± 1.53 MPa (type III etching pattern); Group V - 24.43 MPa ± 1.55 (type II etching pattern). Different adhesive systems yielded significantly different SBSs. Acid etching significantly increased the adhesion in laser treated enamel. No differences in SBS values were obtained between AdheSE(®) and ExciTE(®) without condition with PA. FuturaBond(®) NR and Xeno(®) V showed similar SBS, which was lower in comparison to the others adhesives. No correlation between enamel surface morphology and SBS values was observed, except when PA was used.

Effects of different orthodontic primers on enamel demineralization around orthodontic brackets.

PubMed

Baysal, Asli; Yasa, Asli; Sogut, Ozlem; Ozturk, Mehmet Ali; Uysal, Tancan

2015-09-01

The purpose of this work is to evaluate the effectiveness of one self-etching and two filled orthodontic primers on enamel demineralization around orthodontic brackets. Brackets were bonded to 84 bovine teeth and the vestibular enamel surfaces covered with acid-resistant nail varnish exposing 1 mm of space on each side of the bracket base. The teeth were allocated to four groups, using either Transbond XT conventional primer on etched enamel (group 1), Transbond Plus Self-Etching Primer on untreated enamel (group 2), Pro Seal filled resin primer on etched enamel (group 3), or Opal Seal filled resin primer on etched enamel (group 4). Each tooth was subjected to 15,000 strokes of brushing followed by exposure to an acid challenge. Calcium-ion release from each sample was calculated using atomic absorption spectrophotometry. Data were analyzed using one-way ANOVA and a post hoc Tukey test. Differences were considered statistically significant at p ≤ 0.05. Statistically significant differences were observed between the four groups (p < 0.001). No significant difference was found between the controls (group 1) and the Opal Seal group. Higher calcium release was observed in the Pro Seal group and the self-etching primer group compared to the controls. The highest calcium release was recorded in the self-etching primer group. Filled sealants may not have a protective effect against enamel demineralization. Transbond Plus Self-Etching Primer should be used cautiously, considering the risk of demineralization involved in its application.

Toward a durable superhydrophobic aluminum surface by etching and ZnO nanoparticle deposition.

PubMed

Rezayi, Toktam; Entezari, Mohammad H

2016-02-01

Fabrication of suitable roughness is a fundamental step for acquiring superhydrophobic surfaces. For this purpose, a deposition of ZnO nanoparticles on Al surface was carried out by simple immersion and ultrasound approaches. Then, surface energy reduction was performed using stearic acid (STA) ethanol solution for both methods. The results demonstrated that ultrasound would lead to more stable superhydrophobic Al surfaces (STA-ZnO-Al-U) in comparison with simple immersion method (STA-ZnO-Al-I). Besides, etching in HCl solution in another sample was carried out before ZnO deposition for acquiring more mechanically stable superhydrophobic surface. The potentiodynamic measurements demonstrate that etching in HCl solution under ultrasound leads to superhydrophobic surface (STA-ZnO-Al(E)-U). This sample shows remarkable decrease in corrosion current density (icorr) and long-term stability improvement versus immersion in NaCl solution (3.5%) in comparison with the sample prepared without etching (STA-ZnO-Al-U). Scanning electron micrograph (SEM) and energy-dispersive X-ray spectroscopy (EDX) confirmed a more condense and further particle deposition on Al substrate when ultrasound was applied in the system. The crystallite evaluation of deposited ZnO nanoparticles was carried out using X-ray diffractometer (XRD). Finally, for STA grafting verification on Al surface, Fourier transform infrared in conjunction with attenuated total reflection (FTIR-ATR) was used as a proper technique. Copyright © 2015 Elsevier Inc. All rights reserved.

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.

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.

High-quality fiber fabrication in buffered hydrofluoric acid solution with ultrasonic agitation.

PubMed

Zhong, Nianbing; Liao, Qiang; Zhu, Xun; Wang, Yongzhong; Chen, Rong

2013-03-01

An etching method for preparing high-quality fiber-optic sensors using a buffered etchant with ultrasonic agitation is proposed. The effects of etching conditions on the etch rate and surface morphology of the etched fibers are investigated. The effect of surface roughness is discussed on the fibers' optical properties. Linear etching behavior and a smooth fiber surface can be repeatedly obtained by adjusting the ultrasonic power and etchant pH. The fibers' spectral quality is improved as the ratio of the pit depth to size decreases, and the fibers with smooth surfaces are more sensitive to a bacterial suspension than those with rough surfaces.

SURFACE TREATMENT OF METALLIC URANIUM

DOEpatents

Gray, A.G.; Schweikher, E.W.

1958-05-27

The treatment of metallic uranium to provide a surface to which adherent electroplates can be applied is described. Metallic uranium is subjected to an etchant treatment in aqueous concentrated hydrochloric acid, and the etched metal is then treated to dissolve the resulting black oxide and/or chloride film without destroying the etched metal surface. The oxide or chloride removal is effected by means of moderately concentrated nitric acid in 3 to 20 seconds.

Structural evolution of self-ordered alumina tapered nanopores with 100 nm interpore distance

NASA Astrophysics Data System (ADS)

Li, Juan; Li, Congshan; Gao, Xuefeng

2011-10-01

We in-detail investigated the profile evolution processes of highly ordered alumina under the cyclic treatment of mild anodizing of aluminum foils in oxalic acid followed by etching in phosphoric acid. With the cyclic times increasing, the profiles of nanopores were gradually evolved into the parabola-like, trumpet-like and conical shape. Although the inserted etching itself nearly had no impact on the growth rate of the nanopores due to the rapid recovering of thinned barrier layer at the initial stage of next anodizing, overmuch etching could bring apparent side effects such as wall-breaking, thinning and taper-removing from the top down. The anodizing and etching kinetics and their synergetic effects in modulating different aspect ratios and open sizes of conical pores were studied systematically. These findings are helpful to tailor high-quality anodic alumina taper-pores with tunable profiles.

Microdroplet-etched highly birefringent low-loss fiber tapers.

PubMed

Mikkelsen, Jared C; Poon, Joyce K S

2012-07-01

We use hydrofluoric acid microdroplets to directly etch highly birefringent biconical fiber tapers from standard single-mode fibers. The fiber tapers have micrometer-sized cross sections, which are controlled by the etching condition. The characteristic teardrop cross section leads to a high group birefringence of B(G)≈0.017 and insertion losses <0.7 dB over waist lengths of about 2.1 mm.

Selective Acid Etching Improves the Bond Strength of Universal Adhesive to Sound and Demineralized Enamel of Primary Teeth.

PubMed

Antoniazzi, Bruna Feltrin; Nicoloso, Gabriel Ferreira; Lenzi, Tathiane Larissa; Soares, Fabio Zovico Maxnuck; Rocha, Rachel de Oliveira

To evaluate the influence of enamel condition and etching strategy on bond strength of a universal adhesive in primary teeth. Thirty-six primary molars were randomly assigned to six groups (n = 6) according to the enamel condition (sound [S] and demineralized [DEM]/cariogenic challenge by pH cycling prior to restorative procedures) and adhesive system (Scotchbond Universal Adhesive [SBU]) used in either etch-and-rinse (ER) or selfetching (SE) mode, with Clearfil SE Bond as the self-etching control. The adhesives were applied to flat enamel surfaces and composite cylinders (0.72 mm2) were built up. After 24-h storage in water, specimens were subjected to the microshear test. Bond strength (MPa) data were analyzed using two-way ANOVA and Tukey's post-hoc tests (α = 0.05). Significant differences were found considering the factors adhesive system (p = 0.003) and enamel condition (p = 0.001). Demineralized enamel negatively affected the bond strength, with μSBS values approximately 50% lower than those obtained for sound enamel. SBU performed better in etch-and-rinse mode, and the bond strength found for SBU applied in self-etching mode was similar to that of CSE. Enamel etching with phosphoric acid improves the bond strength of a universal adhesive system to primary enamel. Demineralized primary enamel results in lower bond strength.

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.

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).

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.

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.

Multi-Step Deep Reactive Ion Etching Fabrication Process for Silicon-Based Terahertz Components

NASA Technical Reports Server (NTRS)

Reck, Theodore (Inventor); Perez, Jose Vicente Siles (Inventor); Lee, Choonsup (Inventor); Cooper, Ken B. (Inventor); Jung-Kubiak, Cecile (Inventor); Mehdi, Imran (Inventor); Chattopadhyay, Goutam (Inventor); Lin, Robert H. (Inventor); Peralta, Alejandro (Inventor)

2016-01-01

A multi-step silicon etching process has been developed to fabricate silicon-based terahertz (THz) waveguide components. This technique provides precise dimensional control across multiple etch depths with batch processing capabilities. Nonlinear and passive components such as mixers and multipliers waveguides, hybrids, OMTs and twists have been fabricated and integrated into a small silicon package. This fabrication technique enables a wafer-stacking architecture to provide ultra-compact multi-pixel receiver front-ends in the THz range.

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.

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.

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.

Microstructural characterization of Ti-6Al-4V alloy subjected to the duplex SMAT/plasma nitriding.

PubMed

Pi, Y; Faure, J; Agoda-Tandjawa, G; Andreazza, C; Potiron, S; Levesque, A; Demangel, C; Retraint, D; Benhayoune, H

2013-09-01

In this study, microstructural characterization of Ti-6Al-4V alloy, subjected to the duplex surface mechanical attrition treatment (SMAT)/nitriding treatment, leading to improve its mechanical properties, was carried out through novel and original samples preparation methods. Instead of acid etching which is limited for morphological characterization by scanning electron microscopy (SEM), an original ion polishing method was developed. Moreover, for structural characterization by transmission electron microscopy (TEM), an ion milling method based with the use of two ions guns was also carried out for cross-section preparation. To demonstrate the efficiency of the two developed methods, morphological investigations were done by traditional SEM and field emission gun SEM. This was followed by structural investigations through selected area electron diffraction (SAED) coupled with TEM and X-ray diffraction techniques. The results demonstrated that ionic polishing allowed to reveal a variation of the microstructure according to the surface treatment that could not be observed by acid etching preparation. TEM associated to SAED and X-ray diffraction provided information regarding the nanostructure compositional changes induced by the duplex SMAT/nitriding process. Copyright © 2013 Wiley Periodicals, Inc.

Bonding of universal adhesives to dentine--Old wine in new bottles?

PubMed

Chen, C; Niu, L-N; Xie, H; Zhang, Z-Y; Zhou, L-Q; Jiao, K; Chen, J-H; Pashley, D H; Tay, F R

2015-05-01

Multi-mode universal adhesives offer clinicians the choice of using the etch-and-rinse technique, selective enamel etch technique or self-etch technique to bond to tooth substrates. The present study examined the short-term in vitro performance of five universal adhesives bonded to human coronal dentine. Two hundred non-carious human third molars were assigned to five groups based on the type of the universal adhesives (Prime&Bond Elect, Scotchbond Universal, All-Bond Universal, Clearfil Universal Bond and Futurabond U). Two bonding modes (etch-and-rinse and self-etch) were employed for each adhesive group. Bonded specimens were stored in deionized water for 24h or underwent a 10,000-cycle thermocycling ageing process prior to testing (N=10). Microtensile bond testing (μTBS), transmission electron microscopy (TEM) of resin-dentine interfaces in non-thermocycled specimens and scanning electron microscopy (SEM) of tracer-infused water-rich zones within hybrid layers of thermocycled specimens were performed. Both adhesive type and testing condition (with/without thermocycling) have significant influences on μTBS. The use of each adhesive in either the etch-and-rinse or self-etch application mode did not result in significantly different μTBS to dentine. Hybrid layers created by these adhesives in the etch-and-rinse bonding mode and self-etch bonding mode were ∼5μm and ≤0.5μm thick respectively. Tracer-infused regions could be identified within the resin-dentine interface from all the specimens prepared. The increase in versatility of universal adhesives is not accompanied by technological advances for overcoming the challenges associated with previous generations of adhesives. Therapeutic adhesives with bio-protective and bio-promoting effects are still lacking in commercialized adhesives. Universal adhesives represent manufacturers' attempt to introduce versatility in product design via adaptation of a single-bottle self-etch adhesive for other application modes without compromising its bonding effectiveness. Published by Elsevier Ltd.

No-waiting dentine self-etch concept-Merit or hype.

PubMed

Huang, Xue-Qing; Pucci, César R; Luo, Tao; Breschi, Lorenzo; Pashley, David H; Niu, Li-Na; Tay, Franklin R

2017-07-01

A recently-launched universal adhesive, G-Premio Bond, provides clinicians with the alternative to use the self-etch technique for bonding to dentine without waiting for the adhesive to interact with the bonding substrate (no-waiting self-etch; Japanese brochure), or after leaving the adhesive undisturbed for 10s (10-s self-etch; international brochure). The present study was performed to examine in vitro performance of this new universal adhesive bonded to human coronal dentine using the two alternative self-etch modes. One hundred and ten specimens were bonded using two self-etch application modes and examined with or without thermomechanical cycling (10,000 thermal cycles and 240,000 mechanical cycles) to simulate one year of intraoral functioning. The bonded specimens were sectioned for microtensile bond testing, ultrastructural and nanoleakage examination using transmission electron microscopy. Changes in the composition of mineralised dentine after adhesive application were examined using Fourier transform infrared spectroscopy. Both reduced application time and thermomechanical cycling resulted in significantly lower bond strengths, thinner hybrid layers, and significantly more extensive nanoleakage after thermomechanical cycling. Using the conventional 10-s application time improved bonding performance when compared with the no-waiting self-etch technique. Nevertheless, nanoleakage was generally extensive under all testing parameters employed for examining the adhesive. Although sufficient bond strength to dentine may be achieved using the present universal adhesive in the no-waiting self-etch mode that does not require clinicians to wait prior to polymerisation of the adhesive, this self-etch concept requires further technological refinement before it can be recommended as a clinical technique. Although the surge for cutting application time to increase user friendliness remains the most frequently sought conduit for advancement of dentine bonding technology, the use of the present universal adhesive in the no-waiting self-etch mode may not represent the best use of the adhesive. Published by Elsevier Ltd.

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.

Atomic-scale etching of hexagonal boron nitride for device integration based on two-dimensional materials.

PubMed

Park, Hamin; Shin, Gwang Hyuk; Lee, Khang June; Choi, Sung-Yool

2018-05-29

Hexagonal boron nitride (h-BN) is considered an ideal template for electronics based on two-dimensional (2D) materials, owing to its unique properties as a dielectric film. Most studies involving h-BN and its application to electronics have focused on its synthesis using techniques such as chemical vapor deposition, the electrical analysis of its surface state, and the evaluation of its performance. Meanwhile, processing techniques including etching methods have not been widely studied despite their necessity for device fabrication processes. In this study, we propose the atomic-scale etching of h-BN for integration into devices based on 2D materials, using Ar plasma at room temperature. A controllable etching rate, less than 1 nm min-1, was achieved and the low reactivity of the Ar plasma enabled the atomic-scale etching of h-BN down to a monolayer in this top-down approach. Based on the h-BN etching technique for achieving electrical contact with the underlying molybdenum disulfide (MoS2) layer of an h-BN/MoS2 heterostructure, a top-gate MoS2 field-effect transistor (FET) with h-BN gate dielectric was fabricated and characterized by high electrical performance based on the on/off current ratio and carrier mobility.

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.

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.

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.

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.

Effect of various de-anodizing techniques on the surface stability of non-colored and colored nanoporous AAO films in acidic solution

NASA Astrophysics Data System (ADS)

Awad, Ahmed M.; Shehata, Omnia S.; Heakal, Fakiha El-Taib

2015-12-01

Anodic aluminum oxide (AAO) is well known as an important nanostructured material, and a useful template in the fabrication of nanostructures. Nanoporous anodic alumina (PAA) with high open porosity was prepared by adopting three de-anodizing regimes following the first anodizing step and preceding the second one. The de-anodizing methods include electrolytic etching (EE) and chemical etching using either phosphoric acid (PE) or sodium hydroxide (HE) solutions. Three of the obtained AAO samples were black colored by electrodeposition of copper nanoparticles in their pores. Electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization techniques were used to characterize the electrochemical performance of the two sets of the prepared samples. In general, the data obtained in aggressive aerated 0.5 M HCl solution demonstrated dissimilar behavior for the three prepared samples despite that the second anodizing step was the same for all of them. The data indicated that the resistance and thickness of the inner barrier part of nano-PAA film, are the main controlling factors determining its stability. On the other hand, coloring the film decreased its stability due to the galvanic effect. The difference in the electrochemical behavior of the three colored samples was discussed based on the difference in both the pore size and thickness of the outer porous part of PAA film as supported by SEM, TEM and cross-sectional micrographs. These results can thus contribute for better engineering applications of nanoporous AAO.

High quality self-separated GaN crystal grown on a novel nanoporous template by HVPE.

PubMed

Huo, Qin; Shao, Yongliang; Wu, Yongzhong; Zhang, Baoguo; Hu, Haixiao; Hao, Xiaopeng

2018-02-16

In this study, a novel nanoporous template was obtained by a two-step etching process from MOCVD-GaN/Al 2 O 3 (MGA) with electrochemical etching sequentially followed by chemical wet etching. The twice-etched MOCVD-GaN/Al 2 O 3 (TEMGA) templates were utilized to grow GaN crystals by hydride vapor phase epitaxy (HVPE) method. The GaN crystals were separated spontaneously from the TEMGA template with the assistance of voids formed by the etched nanopores. Several techniques were utilized to characterize the quality of the free-standing GaN crystals obtained from the TEMGA template. Results showed that the quality of the as-obtained GaN crystals was improved obviously compared with those grown on the MGA. This convenient technique can be applied to grow high-quality free-standing GaN crystals.

III-Nitride Blue Laser Diode with Photoelectrochemically Etched Current Aperture

NASA Astrophysics Data System (ADS)

Megalini, Ludovico

Group III-nitride is a remarkable material system to make highly efficient and high-power optoelectronics and electronic devices because of the unique electrical, physical, chemical and structural properties it offers. In particular, InGaN-based blue Laser Diodes (LDs) have been successfully employed in a variety of applications ranging from biomedical and military devices to scientific instrumentation and consumer electronics. Recently their use in highly efficient Solid State Lighting (SSL) has been proposed because of their superior beam quality and higher efficiency at high input power density. Tremendous advances in research of GaN semi-polar and non-polar crystallographic planes have led both LEDs and LDs grown on these non-basal planes to rival with, and with the promise to outperform, their equivalent c-plane counterparts. However, still many issues need to be addressed, both related to material growth and device fabrication, including a lack of conventional wet etching techniques. GaN and its alloys with InN and AlN have proven resistant essentially to all known standard wet etching techniques, and the predominant etching methods rely on chlorine-based dry etching (RIE). These introduce sub-surface damage which can degrade the electrical properties of the epitaxial structure and reduce the reliability and lifetime of the final device. Such reasons and the limited effectiveness of passivation techniques have so far suggested to etch the LD ridges before the active region, although it is well-known that this can badly affect the device performance, especially in narrow stripe width LDs, because the gain guiding obtained in the planar configuration is weak and the low index step and high lateral current leakage result in devices with threshold current density higher than devices whose ridge is etched beyond the active region. Moreover, undercut etching of III-nitride layers has proven even more challenging, with limitations in control of the lateral etch distance. In this dissertation it is presented the first nitride blue edge emitting LD with a photoelectrochemical etched current aperture (CA-LD) into the device active region. Photoelectrochemical etching (PECE) has emerged as a powerful wet etching technique for III-nitride compounds. Beyond the advantages of wet etching technique, PECE offers bandgap selectivity, which is particularly desirable because it allows more freedom in designing new and advanced devices with higher performances. In the first part of this thesis a review of PECE is presented, and it is shown how it can be used to achieve a selective and controllable deep undercut of the active region of LEDs and LDs, in particular the selective PECE of MQW active region of (10-10) m-plane and (20-2-1) plane structures is reported. In the second part of this thesis, the fabrication flow process of the CA-LD is described. The performance of these devices is compared with that of shallow etched ridge LDs with a nominally identical epitaxial structure and active region width and it is experimentally shown that the CA-LD design has superior performance. CW operation of a (20-2-1) CA-LD with a 1.5 microm wide active region is demonstrated. Finally, in the third and last part of this thesis, the CA-LD performance is discussed in more details, in particular, an analysis of optical scattering losses caused by the rough edges of the remnant PEC etched active region is presented.

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.

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.

BOND STRENGTH AND MORPHOLOGY OF ENAMEL USING SELF-ETCHING ADHESIVE SYSTEMS WITH DIFFERENT ACIDITIES

PubMed Central

Moura, Sandra Kiss; Reis, Alessandra; Pelizzaro, Arlete; Dal-Bianco, Karen; Loguercio, Alessandro Dourado; Arana-Chavez, Victor Elias; Grande, Rosa Helena Miranda

2009-01-01

Objectives: To assess the bond strength and the morphology of enamel after application of self-etching adhesive systems with different acidities. The tested hypothesis was that the performance of the self-etching adhesive systems does not vary for the studied parameters. Material and methods: Composite resin (Filtek Z250) buildups were bonded to untreated (prophylaxis) and treated (burcut or SiC-paper) enamel surfaces of third molars after application of four self-etching and two etch-and-rinse adhesive systems (n=6/condition): Clearfil SE Bond (CSE); OptiBond Solo Plus Self-Etch (OP); AdheSe (AD); Tyrian Self Priming Etching (TY), Adper Scotchbond Multi-Purpose Plus (SBMP) and Adper Single Bond (SB). After storage in water (24 h/37°C), the bonded specimens were sectioned into sticks with 0.8 mm2 cross-sectional area and the microtensile bond strength was tested at a crosshead speed of 0.5 mm/min. The mean bond strength values (MPa) were subjected to two-way ANOVA and Tukey's test (α=0.05). The etching patterns of the adhesive systems were also observed with a scanning electron microscope. Results: The main factor adhesive system was statistically significant (p<0.05). The mean bond strength values (MPa) and standard deviations were: CSE (20.5±3.5), OP (11.3±2.3), AD (11.2±2.8), TY (11.1±3.0), SBMP (21.9±4.0) and SB (24.9±3.0). Different etching patterns were observed for the self-etching primers depending on the enamel treatment and the pH of the adhesive system. Conclusion: Although there is a tendency towards using adhesive systems with simplified application procedures, this may compromise the bonding performance of some systems to enamel, even when the prismless enamel is removed. PMID:19668991

Micro/nanofabrication of poly({sub L}-lactic acid) using focused ion beam direct etching

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

Oyama, Tomoko Gowa; Nagasawa, Naotsugu; Taguchi, Mitsumasa

2013-10-14

Micro/nanofabrication of biocompatible and biodegradable poly({sub L}-lactic acid) (PLLA) using focused Ga ion beam direct etching was evaluated for future bio-device applications. The fabrication performance was determined with different ion fluences and fluxes (beam currents), and it was found that the etching speed and fabrication accuracy were affected by irradiation-induced heat. Focused ion beam (FIB)-irradiated surfaces were analyzed using micro-area X-ray photoelectron spectroscopy. Owing to reactions such as the physical sputtering of atoms and radiation-induced decomposition, PLLA was gradually carbonized with increasing C=C bonds. Controlled micro/nanostructures of PLLA were fabricated with C=C bond-rich surfaces expected to have good cell attachmentmore » properties.« less

No positive effect of Acid etching or plasma cleaning on osseointegration of titanium implants in a canine femoral condyle press-fit model.

PubMed

Saksø, H; Jakobsen, T; Saksø, M; Baas, J; Jakobsen, Ss; Soballe, K

2013-01-01

Implant surface treatments that improve early osseointegration may prove useful in long-term survival of uncemented implants. We investigated Acid Etching and Plasma Cleaning on titanium implants. In a randomized, paired animal study, four porous coated Ti implants were inserted into the femurs of each of ten dogs. PC (Porous Coating; control)PC+PSHA (Plasma Sprayed Hydroxyapatite; positive control)PC+ET (Acid Etch)PC+ET+PLCN (Plasma Cleaning) After four weeks mechanical fixation was evaluated by push-out test and osseointegration by histomorphometry. The PSHA-coated implants were better osseointegrated than the three other groups on outer surface implant porosity (p<0.05) while there was no statistical difference in deep surface implant porosity when compared with nontreated implant. Within the deep surface implant porosity, there was more newly formed bone in the control group compared to the ET and ET+PCLN groups (p<0.05). In all compared groups, there was no statistical difference in any biomechanical parameter. In terms of osseointegration on outer surface implant porosity PC+PSHA was superior to the other three groups. Neither the acid etching nor the plasma cleaning offered any advantage in terms of implant osseointegration. There was no statistical difference in any of the biomechanical parameters among all groups in the press-fit model at 4 weeks of evaluation time.

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.

Ultra-sensitive EUV resists based on acid-catalyzed polymer backbone breaking

NASA Astrophysics Data System (ADS)

Manouras, Theodoros; Kazazis, Dimitrios; Koufakis, Eleftherios; Ekinci, Yasin; Vamvakaki, Maria; Argitis, Panagiotis

2018-03-01

The main target of the current work was to develop new sensitive polymeric materials for lithographic applications, focusing in particular to EUV lithography, the main chain of which is cleaved under the influence of photogenerated acid. Resist materials based on the cleavage of polymer main chain are in principle capable to create very small structures, to the dimensions of the monomers that they consist of. Nevertheless, in the case of the commonly used nonchemically amplified materials of this type issues like sensitivity and poor etch resistance limit their areas of application, whereas inadequate etch resistance and non- satisfactory process reliability are the usual problems encountered in acid catalysed materials based on main chain scission. In our material design the acid catalyzed chain cleavable polymers contain very sensitive moieties in their backbone while they remain intact in alkaline ambient. These newly synthesized polymers bear in addition suitable functional groups for the achievement of desirable lithographic characteristics (thermal stability, acceptable glass transition temperature, etch resistance, proper dissolution behavior, adhesion to the substrate). Our approach for achieving acceptable etch resistance, a main drawback in other main chain cleavable resists, is based on the introduction of polyaromatic hydrocarbons in the polymeric backbone, whereas the incorporation of an inorganic component further enhances the etch resistance. Single component systems can also be designed following the proposed approach by the incorporation of suitable PAGs and base quencher molecules in the main chain. Resist formulations based on a random copolymer designed according to the described rules evaluated in EUV exhibit ultrahigh sensitivity, capability for high resolution patterning and overall processing characteristics that make them strong candidates for industrial use upon further optimization.

Comparing the shear bond strength of direct and indirect composite inlays in relation to different surface conditioning and curing techniques

PubMed Central

Zorba, Yahya Orcun; Ilday, Nurcan Ozakar; Bayındır, Yusuf Ziya; Demirbuga, Sezer

2013-01-01

Objective: The aim of this study was to test the null hypothesis that different surface conditioning (etch and rinse and self-etch) and curing techniques (light cure/dual cure) had no effect on the shear bond strength of direct and indirect composite inlays. Materials and Methods: A total of 112 extracted human molar teeth were horizontally sectioned and randomly divided into two groups according to restoration technique (direct and indirect restorations). Each group was further subdivided into seven subgroups (n = 8) according to bonding agent (etch and rinse adhesives Scotchbond multi-purpose plus, All-Bond 3, Adper Single Bond and Prime Bond NT; and self-etch adhesives Clearfil Liner Bond, Futurabond DC and G bond). Indirect composites were cemented to dentin surfaces using dual-curing luting cement. Shear bond strength of specimens was tested using a Universal Testing Machine. Two samples from each subgroup were evaluated under Scanning electron microscopy to see the failing modes. Data was analyzed using independent sample t-tests and Tukey's tests. Results: Surface conditioning and curing of bonding agents were all found to have significant effects on shear bond strength (P < 0.05) of both direct and indirect composite inlays. With direct restoration, etch and rinse systems and dual-cured bonding agents yielded higher bond strengths than indirect restoration, self-etch systems and light-cured bonding agents. Conclusions: The results of the present study indicated that direct restoration to be a more reliable method than indirect restoration. Although etch and rinse bonding systems showed higher shear bond strength to dentin than self-etch systems, both systems can be safely used for the adhesion of direct as well as indirect restorations. PMID:24932118

Comparing the shear bond strength of direct and indirect composite inlays in relation to different surface conditioning and curing techniques.

PubMed

Zorba, Yahya Orcun; Ilday, Nurcan Ozakar; Bayındır, Yusuf Ziya; Demirbuga, Sezer

2013-10-01

The aim of this study was to test the null hypothesis that different surface conditioning (etch and rinse and self-etch) and curing techniques (light cure/dual cure) had no effect on the shear bond strength of direct and indirect composite inlays. A total of 112 extracted human molar teeth were horizontally sectioned and randomly divided into two groups according to restoration technique (direct and indirect restorations). Each group was further subdivided into seven subgroups (n = 8) according to bonding agent (etch and rinse adhesives Scotchbond multi-purpose plus, All-Bond 3, Adper Single Bond and Prime Bond NT; and self-etch adhesives Clearfil Liner Bond, Futurabond DC and G bond). Indirect composites were cemented to dentin surfaces using dual-curing luting cement. Shear bond strength of specimens was tested using a Universal Testing Machine. Two samples from each subgroup were evaluated under Scanning electron microscopy to see the failing modes. Data was analyzed using independent sample t-tests and Tukey's tests. Surface conditioning and curing of bonding agents were all found to have significant effects on shear bond strength (P < 0.05) of both direct and indirect composite inlays. With direct restoration, etch and rinse systems and dual-cured bonding agents yielded higher bond strengths than indirect restoration, self-etch systems and light-cured bonding agents. The results of the present study indicated that direct restoration to be a more reliable method than indirect restoration. Although etch and rinse bonding systems showed higher shear bond strength to dentin than self-etch systems, both systems can be safely used for the adhesion of direct as well as indirect restorations.

Effect of acid etching on bond strength of nanoionomer as an orthodontic bonding adhesive

PubMed Central

Khan, Saba; Verma, Sanjeev K.; Maheshwari, Sandhya

2015-01-01

Aims: A new Resin Modified Glass Ionomer Cement known as nanoionomer containing nanofillers of fluoroaluminosilicate glass and nanofiller 'clusters' has been introduced. An in-vitro study aimed at evaluating shear bond strength (SBS) and adhesive remnant index (ARI) of nanoionomer under etching/unetched condition for use as an orthodontic bonding agent. Material and Methods: A total of 75 extracted premolars were used, which were divided into three equal groups of 25 each: 1-Conventional adhesive (Enlight Light Cure, SDS, Ormco, CA, USA) was used after and etching with 37% phosphoric acid for 30 s, followed by Ortho Solo application 2-nanoionomer (Ketac™ N100, 3M, ESPE, St. Paul, MN, USA) was used after etching with 37% phosphoric acid for 30 s 3-nanoionomer was used without etching. The SBS testing was performed using a digital universal testing machine (UTM-G-410B, Shanta Engineering). Evaluation of ARI was done using scanning electron microscopy. The SBS were compared using ANOVA with post-hoc Tukey test for intergroup comparisons and ARI scores were compared with Chi-square test. Results: ANOVA (SBS, F = 104.75) and Chi-square (ARI, Chi-square = 30.71) tests revealed significant differences between groups (P < 0.01). The mean (SD) SBS achieved with conventional light cure adhesive was significantly higher (P < 0.05) (10.59 ± 2.03 Mpa, 95% CI, 9.74-11.41) than the nanoionomer groups (unetched 4.13 ± 0.88 Mpa, 95% CI, 3.79-4.47 and etched 9.32 ± 1.87 Mpa, 95% CI, 8.58-10.06). However, nanoionomer with etching, registered SBS in the clinically acceptable range of 5.9–7.8 MPa, as suggested by Reynolds (1975). The nanoionomer groups gave significantly lower ARI values than the conventional adhesive group. Conclusion: Based on this in-vitro study, nanoionomer with etching can be successfully used as an orthodontic bonding agent leaving less adhesive remnant on enamel surface, making cleaning easier. However, in-vivo studies are needed to confirm the validity of present findings. PMID:26955629

The influence of H{sub 2}O{sub 2} concentration to the structure of silicon nanowire growth by metal-assisted chemical etching

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

Omar, Hafsa, E-mail: mrshafsaomar@gmail.com; Jani, Abdul Mutalib Md., E-mail: abdmutalib@perlis.uitm.edu.my; Abdullah, Saifollah, E-mail: saifollah@salam.utm.edu.my

2016-07-06

A simple and low cost method to produce well aligned silicon nanowires at large areas using Ag-assisted chemical etching at room temperature were presented. The structure of silicon nanowires growth by metal-assisted chemical etching was observed. Prior to the etching, the silicon nanowires were prepared by electroless metal deposited (EMD) in solution containing hydrofluoric acid and hydrogen peroxide in Teflon vessel. The silver particle was deposited on substrate by immersion in hydrofluoric acid and silver nitrate solution for sixty second. The silicon nanowires were growth in different hydrogen peroxide concentration which are 0.3M, 0.4M, 0.5M and 0.6M and 0.7M.The influencemore » of hydrogen peroxide concentration to the formation of silicon nanowires was studied. The morphological properties of silicon nanowires were investigated using field emission scanning electron microscopy (FESEM) and Energy Dispersive X-Ray Spectroscopy (EDS).« less

EFFECT OF AN ADDITIONAL HYDROPHILIC VERSUS HYDROPHOBIC COAT ON THE QUALITY OF DENTINAL SEALING PROVIDED BY TWO-STEP ETCH-AND-RINSE ADHESIVES

PubMed Central

Silva, Safira Marques de Andrade; Carrilho, Marcela Rocha de Oliveira; Marquezini, Luiz; Garcia, Fernanda Cristina Pimentel; Manso, Adriana Pigozzo; Alves, Marcelo Corrêa; de Carvalho, Ricardo Marins

2009-01-01

Objective: To test the hypothesis that the quality of the dentinal sealing provided by two-step etch-and-rinse adhesives cannot be altered by the addition of an extra layer of the respective adhesive or the application of a more hydrophobic, non-solvated resin. Material and Methods: full-crown preparations were acid-etched with phosphoric acid for 15 s and bonded with Adper Single Bond (3M ESPE), Excite DSC (Ivoclar/Vivadent) or Prime & Bond NT (Dentsply). The adhesives were used according to the manufacturers' instructions (control groups) or after application to dentin they were a) covered with an extra coat of each respective system or b) coated with a non-solvated bonding agent (Adper Scotchbond Multi-Purpose Adhesive, 3M ESPE). Fluid flow rate was measured before and after dentin surfaces were acid-etched and bonded with adhesives. Results: None of the adhesives or experimental treatments was capable to block completely the fluid transudation across the treated dentin. Application of an extra coat of the adhesive did not reduce the fluid flow rate of adhesive-bonded dentin (p>0.05). Conversely, the application of a more hydrophobic non-solvated resin resulted in significant reductions in the fluid flow rate (p<0.05) for all tested adhesives. Conclusions: The quality of the dentinal sealing provided by etch-and-rinse adhesives can be significantly improved by the application of a more hydrophobic, non-solvated bonding agent. PMID:19466248

Wide angle near-field optical probes by reverse tube etching.

PubMed

Patanè, S; Cefalì, E; Arena, A; Gucciardi, P G; Allegrini, M

2006-04-01

We present a simple modification of the tube etching process for the fabrication of fiber probes for near-field optical microscopy. It increases the taper angle of the probe by a factor of two. The novelty is that the fiber is immersed in hydrofluoric acid and chemically etched in an upside-down geometry. The tip formation occurs inside the micrometer tube cavity formed by the polymeric jacket. By applying this approach, called reverse tube etching, to multimode fibers with 200/250 microm core/cladding diameter, we have fabricated tapered regions featuring high surface smoothness and average cone angles of approximately 30 degrees . A simple model based on the crucial role of the gravity in removing the etching products, explains the tip formation process.

Effect of helium ion beam treatment on wet etching of silicon dioxide

NASA Astrophysics Data System (ADS)

Petrov, Yu. V.; Grigoryev, E. A.; Sharov, T. V.; Baraban, A. P.

2018-03-01

We investigated the effect of helium ion beam treatment on the etching rate of silicon dioxide in a water based solution of hydrofluoric acid. A 460-nm-thick silicon dioxide film on silicon was irradiated with helium ions having energies of 20 keV and 30 keV with ion fluences ranging from 1014 cm-2 to 1017 cm-2. The dependence of the etching rate on depth was obtained and compared with the depth distribution of ion-induced defects, which was obtained from numerical simulation. Irradiation with helium ions results in an increase of the etching rate of silicon dioxide. The dependence of the etching rate on the calculated concentration of ion-induced defects is described.

Ion-beam nanopatterning: experimental results with chemically-assisted beam

NASA Astrophysics Data System (ADS)

Pochon, Sebastien C. R.

2018-03-01

The need for forming gratings (for example used in VR headsets) in materials such as SiO2 has seen a recent surge in the use of Ion beam etching techniques. However, when using an argon-only beam, the selectivity is limited as it is a physical process. Typically, gases such as CHF3, SF6, O2 and Cl2 can be added to argon in order to increase selectivity; depending on where the gas is injected, the process is known as Reactive Ion Beam Etching (RIBE) or Chemically Assisted Ion Beam Etching (CAIBE). The substrate holder can rotate in order to provide an axisymmetric etch rate profile. It can also be tilted over a range of angles to the beam direction. This enables control over the sidewall profile as well as radial uniformity optimisation. Ion beam directionality in conjunction with variable incident beam angle via platen angle setting enables profile control and feature shaping during nanopatterning. These hardware features unique to the Ion Beam etching methods can be used to create angled etch features. The CAIBE technique is also well suited to laser diode facet etch (for optoelectronic devices); these typically use III-V materials like InP. Here, we report on materials such as SiO2 etched without rotation and at a fixed platen angle allowing the formation of gratings and InP etched at a fixed angle with rotation allowing the formation of nanopillars and laser facets.

Dicalcium phosphate (CaHPO4·2H2O) precipitation through ortho- or meta-phosphoric acid-etching: effects on the durability and nanoleakage/ultra-morphology of resin-dentine interfaces.

PubMed

Feitosa, Victor Pinheiro; Bazzocchi, Maria Giulia; Putignano, Angelo; Orsini, Giovanna; Luzi, Arlinda Luzi; Sinhoreti, Mário Alexandre Coelho; Watson, Timothy F; Sauro, Salvatore

2013-11-01

To compare the effects of two etching procedures using meta-phosphoric (MPA) or ortho-phosphoric acid (OPA) on dentine demineralisation, resin-dentine bonds durability and interface nanoleakage/ultra-morphology. Middle-dentine specimens were etched using 37% OPA (15s) or 40% MPA (60s) and submitted to infrared spectroscopy (FTIR) or ultra-morphology dye-assisted (calcium-staining) confocal microscopy (Ca-CLSM). A three-step etch-and-rinse adhesive was formulated, applied onto dentine and light-cured for 30s before composite build-up. After 24h, the dentine-bonded specimens were cut into 1mm(2) beams; half were immediately submitted to microtensile bond strength (μTBS) and half stored in DW for six months. The μTBS results were analysed with repeated-measures ANOVA and Tukey's test (p<0.05). Further teeth were bonded and prepared for interface nanoleakage/ultra-morphology confocal evaluation. FTIR and Ca-CLSM analyses showed dicalcium phosphate dihydrate (Brushite) precipitation in MPA-etched dentine and on the bottom (front of demineralisation) of the OPA-etched dentine. Statistical analysis showed similar μTBS for both etching procedures after 24h. The μTBS of specimens in OPA-group dropped significantly (p<0.05) after six month; the specimens in the MPA group showed no statistically difference (p>0.05). CLSM depicted no evident sign of nanoleakage within the resin-dentine interface of the MPA-treated specimens, while the specimens in OPA-group presented intense nanoleakage and interface degradation. The use of MPA (60s) as an alternative dentine conditioning agent in etch-and-rinse bonding procedures may be a suitable strategy to create more durable resin-dentine bonds. Copyright © 2013 Elsevier Ltd. All rights reserved.

Effect of a New Surface Treatment Solution on the Bond Strength of Composite to Enamel

DTIC Science & Technology

2016-06-01

enamel ( Erickson et al., 2005). More significantly, clinical studies have shown significantly less marginal defects and staining with selective...using phosphoric acid. Erickson et al., (2009) also found improved bond strengths with a selective-etch step and attributed this to the degree of...cut enamel and dentin. Oper Dent 2005;30(1):39-49. Erickson RL, Barkmeier WW, Kimmes NS. Bond strength of self-etch adhesives to pre-etched

Fundamental Studies on High Temperature Deformation, Recrystallization, and Grain Growth of Two-Phase Materials

DTIC Science & Technology

1990-09-26

50 ml. Glycerine R -etch 17 ml. Benzalkonium Chloride 35 ml. Ethanol Kroll - etch 2 ml. Hydrofluoric Acid ( 50 %) 4 ml. Nitric Acid Conc. 100 ml...The amount of work given ( 60 % reduction in area ) in this last step was found to be sufficient to recrystallize all of the alloys within 12 hours at...formed at the center of thedisc with the following solution: 10 gins. Zinc Chloride 5 gms. Aluminum Chloride 300 ml. Methanol 50 ml. N - Butanol A JEOL

Ion beam sputter etching and deposition of fluoropolymers

NASA Technical Reports Server (NTRS)

Banks, B. A.; Sovey, J. S.; Miller, T. B.; Crandall, K. S.

1978-01-01

Fluoropolymer etching and deposition techniques including thermal evaporation, RF sputtering, plasma polymerization, and ion beam sputtering are reviewed. Etching and deposition mechanism and material characteristics are discussed. Ion beam sputter etch rates for polytetrafluoroethylene (PTFE) were determined as a function of ion energy, current density and ion beam power density. Peel strengths were measured for epoxy bonds to various ion beam sputtered fluoropolymers. Coefficients of static and dynamic friction were measured for fluoropolymers deposited from ion bombarded PTFE.

[Effect of hydrofluoric acid etching time on the resin bond durability of glass ceramic].

PubMed

Meng, Xiang-feng; Zhou, Xiao-lu; Luo, Xiao-ping

2010-05-01

To analyze the effect of hydrofluoric acid (HFA) etching time on the resin bond durability of glass ceramic. Three groups of samples of machinable glass ceramic (ProCAD) were etched by 4.8% HFA for 0, 30 and 60 s respectively. The roughness parameters (Ra, Sm, S) and surface area of the samples, were measured with a 3D-laser scanning microscope. Then the ceramic surfaces were bonded with four resin cements (silane coupler/resin cement), which were Monobond S/Variolink II, Clearfil Ceramic Primer/Clearfil Esthetic Cement, GC Ceramic Primer/Linkmax HV, and Porcelain Liner M/SuperBond. The micro-bond strengths between the ceramic and the resin were tested at baseline and after the samples had been treated in 30000 thermal cycles. The Ra [(3.89+/-1.94), (12.53+/-0.80), (13.58+/-1.10) microm] and surface area [(7.81+/-2.96), (30.18+/-2.05), (34.16+/-1.97) mm2] of ceramic increased with the increase of HFA etching time. The thermal cycling test reduced the bond strength of all test groups. The bond strength of Monobond S/Variolink II group [(3.59+/-3.51), (16.18+/-2.62), (20.33+/-2.45) MPa] and Clearfil Ceramic Primer/Clearfil Esthetic Cement group [(4.74+/-2.08), (7.77+/-1.55), (13.45+/-3.75) MPa] increased with the increase of HFA etching time; 30 s HFA etching group of Porcelain Liner M/SuperBond had higher bond strength [(22.00+/-1.64) MPa] than its 0 s HFA etching group [(12.96+/-4.17) MPa], and no significant difference was found between the 30 s and 60 s HFA etching groups of Porcelain Liner M/SuperBond [(20.42+/-3.01) MPa]. HFA etching time had no effect on the bond strength of GC Ceramic Primer/Linkmax HV. HFA etching can improve the resin bond durability of glass ceramic, and the etching time is not only related to the change of ceramic surface roughness and area, but also to the characteristics of resins.

Enamel and dentin bond strengths of a new self-etch adhesive system.

PubMed

Walter, Ricardo; Swift, Edward J; Boushell, Lee W; Braswell, Krista

2011-12-01

statement of problem:  Self-etch adhesives typically are mildly acidic and therefore less effective than etch-and-rinse adhesives for bonding to enamel.   The purpose of this study was to evaluate the enamel and dentin shear bond strengths of a new two-step self-etch adhesive system, OptiBond XTR (Kerr Corporation, Orange, CA, USA).   The labial surfaces of 80 bovine teeth were ground to create flat, 600-grit enamel or dentin surfaces. Composite was bonded to enamel or dentin using the new two-step self-etch system or a three-step etch-and-rinse (OptiBond FL, Kerr), two-step self-etch (Clearfil SE Bond, Kuraray America, Houston, TX, USA), or one-step self-etch adhesive (Xeno IV, Dentsply Caulk, Milford, DE, USA). Following storage in water for 24 hours, shear bond strengths were determined using a universal testing machine. The enamel and dentin data sets were subjected to separate analysis of variance and Tukey's tests. Scanning electron microscopy was used to evaluate the effects of each system on enamel.   Mean shear bond strengths to enamel ranged from 18.1 MPa for Xeno IV to 41.0 MPa for OptiBond FL. On dentin, the means ranged from 33.3 MPa for OptiBond FL to 47.1 MPa for Clearfil SE Bond. OptiBond XTR performed as well as Clearfil SE Bond on dentin and as well as OptiBond FL on enamel. Field emission scanning electron microscope revealed that OptiBond XTR produced an enamel etch pattern that was less defined than that of OptiBond FL (37.5% phosphoric acid) but more defined than that of Clearfil SE Bond or Xeno IV.   The new two-step self-etch adhesive system formed excellent bonds to enamel and dentin in vitro. OptiBond XTR, a new two-step self-etch adhesive system, is a promising material for bonding to enamel as well as to dentin. © 2011 Wiley Periodicals, Inc.

Evaluation of Mineral Content and Photon Interaction Parameters of Dental Enamel After Phosphoric Acid and Er:YAG Laser Treatment.

PubMed

Simsek, Huseyin; Gurbuz, Taskın; Buyuk, Suleyman Kutalmış; Ozdemir, Yuksel

2017-05-01

The purpose of this study was to evaluate the effects of laser and acid etching on the mineral content and photon interaction parameters of dental enamel in human teeth. The composition of dental enamel may vary, especially at the surface, depending on the reactions that occur during dental treatment. Forty maxillary premolars were divided randomly into 2 groups of 20 teeth. In the first group, half of teeth crowns were etched by using 37% phosphoric acid; in the second group, half of teeth crowns were etched by using an erbium:yttrium-aluminum-garnet (Er:YAG) laser. The remaining half crowns in each group were used as untreated controls. We characterized the calcium (Ca), phosphorus (P), magnesium (Mg), sodium (Na), and potassium (K) contents in each specimen by using wavelength dispersive X-ray fluorescence spectrometry. The total atomic cross-section ([Formula: see text]), effective atomic number ([Formula: see text]), and electron density (N e ) of the tooth samples were determined at photon energies of 22.1, 25, 59.5, and 88 keV by using a narrow beam transmission method. Data were analyzed statistically by using the Mann-Whitney U test. The mineral contents after Er:YAG laser and phosphoric acid etching did not differ significantly (p > 0.05), and no significant variation in [Formula: see text], [Formula: see text], or N e was observed. Therefore, we conclude that the Er:YAG laser and phosphoric acid systems used in this study did not affect mineral composition or photon interaction parameters of dental enamel.

Comparison of shear bond strength of self-etch and self-adhesive cements bonded to lithium disilicate, enamel and dentin.

PubMed

Naranjo, Jennifer; Ali, Mohsin; Belles, Donald

2015-11-01

Comparison of shear bond strength of self-etch and self-adhesive cements bonded to lithium disilicate, enamel and dentin. With several self-adhesive resin cements currently available, there is confusion about which product and technique is optimal for bonding ceramic restorations to teeth. The objective of this study was to compare the shear bond strength of lithium disilicate cemented to enamel and dentin using 5 adhesive cements. 100 lithium disilicate rods were pretreated with 5% hydrofluoric acid, silane, and cemented to 50 enamel and 50 dentin surfaces using five test cements: Variolink II (etch-and-rinse) control group, Clearfil Esthetic (two step self-etch), RelyX Unicem, SpeedCEM, and BifixSE (self-adhesive). All specimens were stored (37 degrees C, 100% humidity) for 24 hours before testing their shear bond strength using a universal testing machine (Instron). Debonded surfaces were observed under a low-power microscope to assess the location and type of failure. The highest bond strength for both enamel and dentin were recorded for Variolink II, 15.1MPa and 20.4MPa respectively, and the lowest were recorded for BifixSE, 0.6MPa and 0.9MPa respectively. Generally, higher bond strengths were found for dentin (7.4MPa) than enamel (5.3MPa). Tukey's post hoc test showed no significant difference between Clearfil Esthetic and SpeedCem (p = 0.059), Unicem and SpeedCem (p = 0.88), and Unicem and BifixSE (p = 0.092). All cements bonded better to lithium disilicate than to enamel or dentin, as all bond failures occurred at the tooth/adhesive interface except for Variolink II. Bond strengths recorded for self-adhesive cements were very low compared to the control "etch and rinse" and self-etch systems. Further improvements are apparently needed in self-adhesive cements for them to replace multistep adhesive systems. The use of conventional etch and rinse cements such as Veriolink II should be preferred for cementing all ceramic restorations over self-adhesive cements until the bond strengths are improved.

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.

Image processing analysis of nuclear track parameters for CR-39 detector irradiated by thermal neutron

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

Al-Jobouri, Hussain A., E-mail: hahmed54@gmail.com; Rajab, Mustafa Y., E-mail: mostafaheete@gmail.com

CR-39 detector which covered with boric acid (H{sub 3}Bo{sub 3}) pellet was irradiated by thermal neutrons from ({sup 241}Am - {sup 9}Be) source with activity 12Ci and neutron flux 10{sup 5} n. cm{sup −2}. s{sup −1}. The irradiation times -T{sub D} for detector were 4h, 8h, 16h and 24h. Chemical etching solution for detector was sodium hydroxide NaOH, 6.25N with 45 min etching time and 60 C° temperature. Images of CR-39 detector after chemical etching were taken from digital camera which connected from optical microscope. MATLAB software version 7.0 was used to image processing. The outputs of image processing of MATLABmore » software were analyzed and found the following relationships: (a) The irradiation time -T{sub D} has behavior linear relationships with following nuclear track parameters: i) total track number - N{sub T} ii) maximum track number - MRD (relative to track diameter - D{sub T}) at response region range 2.5 µm to 4 µm iii) maximum track number - M{sub D} (without depending on track diameter - D{sub T}). (b) The irradiation time -T{sub D} has behavior logarithmic relationship with maximum track number - M{sub A} (without depending on track area - A{sub T}). The image processing technique principally track diameter - D{sub T} can be take into account to classification of α-particle emitters, In addition to the contribution of these technique in preparation of nano- filters and nano-membrane in nanotechnology fields.« less

Six-month evaluation of adhesives interface created by a hydrophobic adhesive to acid-etched ethanol-wet bonded dentine with simplified dehydration protocols.

PubMed

Sadek, Fernanda T; Mazzoni, Annalisa; Breschi, Lorenzo; Tay, Franklin R; Braga, Roberto R

2010-04-01

To evaluate the efficacy of simplified dehydration protocols, in the absence of tubular occlusion, on bond strength and interfacial nanoleakage of a hydrophobic experimental adhesive blend to acid-etched, ethanol-dehydrated dentine immediately and after 6 months. Molars were randomly assigned to 6 treatment groups (n=5). Under pulpal pressure simulation, dentine crowns were acid-etched with 35% H(3)PO(4) and rinsed with water. Adper Scotchbond Multi-Purpose was used for the control group. The remaining groups had their dentine surface dehydrated with ethanol solutions: group 1=50%, 70%, 80%, 95% and 3x100%, 30s for each application; group 2 the same ethanol sequence with 15s for each solution; groups 3, 4 and 5 used 100% ethanol only, applied in seven, three or one 30s step, respectively. After dehydration, a primer (50% BisGMA+TEGDMA, 50% ethanol) was used, followed by the neat comonomer adhesive application. Resin composite build-ups were then prepared using an incremental technique. Specimens were stored for 24h, sectioned into beams and stressed to failure after 24h or after 6 months of artificial ageing. Interfacial silver leakage evaluation was performed for both storage periods (n=5 per subgroup). Group 1 showed higher bond strengths at 24h or after 6 months of ageing (45.6+/-5.9(a)/43.1+/-3.2(a)MPa) and lower silver impregnation. Bond strength results were statistically similar to control group (41.2+/-3.3(ab)/38.3+/-4.0(ab)MPa), group 2 (40.0+/-3.1(ab)/38.6+/-3.2(ab)MPa), and group 3 at 24h (35.5+/-4.3(ab)MPa). Groups 4 (34.6+/-5.7(bc)/25.9+/-4.1(c)MPa) and 5 (24.7+/-4.9(c)/18.2+/-4.2(c)MPa) resulted in lower bond strengths, extensive interfacial nanoleakage and more prominent reductions (up to 25%) in bond strengths after 6 months of ageing. Simplified dehydration protocols using one or three 100% ethanol applications should be avoided for the ethanol-wet bonding technique in the absence of tubular occlusion, as they showed decreased bond strength, more severe nanoleakage and reduced bond stability over time. Copyright 2009 Elsevier Ltd. All rights reserved.

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

Enzyme-enhanced fluorescence detection of DNA on etched optical fibers.

PubMed

Niu, Shu-yan; Li, Quan-yi; Ren, Rui; Zhang, Shu-sheng

2009-05-15

A novel DNA biosensor based on enzyme-enhanced fluorescence detection on etched optical fibers was developed. The hybridization complex of DNA probe and biotinylated target was formed on the etched optical fiber, and was then bound with streptavidin labeled horseradish peroxidase (streptavidin-HRP). The target DNA was quantified through the fluorescent detection of bi-p,p'-4-hydroxyphenylacetic acid (DBDA) generated from the substrate 4-hydroxyphenylacetic acid (p-HPA) under the catalysis of HRP, with a detection limit of 1 pM and a linear range from 1.69 pM to 169 pM. It is facile to regenerate this sensor through surface treatment with concentrated urea solution. It was discovered that the sensor can retain 70% of its original activity after three detection-regeneration cycles.

Low-loss slot waveguides with silicon (111) surfaces realized using anisotropic wet etching

NASA Astrophysics Data System (ADS)

Debnath, Kapil; Khokhar, Ali; Boden, Stuart; Arimoto, Hideo; Oo, Swe; Chong, Harold; Reed, Graham; Saito, Shinichi

2016-11-01

We demonstrate low-loss slot waveguides on silicon-on-insulator (SOI) platform. Waveguides oriented along the (11-2) direction on the Si (110) plane were first fabricated by a standard e-beam lithography and dry etching process. A TMAH based anisotropic wet etching technique was then used to remove any residual side wall roughness. Using this fabrication technique propagation loss as low as 3.7dB/cm was realized in silicon slot waveguide for wavelengths near 1550nm. We also realized low propagation loss of 1dB/cm for silicon strip waveguides.

The development of a method of producing etch resistant wax patterns on solar cells

NASA Technical Reports Server (NTRS)

Pastirik, E.

1980-01-01

A potentially attractive technique for wax masking of solar cells prior to etching processes was studied. This technique made use of a reuseable wax composition which was applied to the solar cell in patterned form by means of a letterpress printing method. After standard wet etching was performed, wax removal by means of hot water was investigated. Application of the letterpress wax printing process to silicon was met with a number of difficulties. The most serious shortcoming of the process was its inability to produce consistently well-defined printed patterns on the hard silicon cell surface.

Figuring of plano-elliptical neutron focusing mirror by local wet etching.

PubMed

Yamamura, Kazuya; Nagano, Mikinori; Takai, Hiroyuki; Zettsu, Nobuyuki; Yamazaki, Dai; Maruyama, Ryuji; Soyama, Kazuhiko; Shimada, Shoichi

2009-04-13

Local wet etching technique was proposed to fabricate high-performance aspherical mirrors. In this process, only the limited area facing to the small nozzle is removed by etching on objective surface. The desired objective shape is deterministically fabricated by performing the numerically controlled scanning of the nozzle head. Using the technique, a plano-elliptical mirror to focus the neutron beam was successfully fabricated with the figure accuracy of less than 0.5 microm and the focusing gain of 6. The strong and thin focused neutron beam is expected to be a useful tool for the analyses of various material properties.

In vitro remineralization of acid-etched human enamel with Ca 3SiO 5

NASA Astrophysics Data System (ADS)

Dong, Zhihong; Chang, Jiang; Deng, Yan; Joiner, Andrew

2010-02-01

Bioactive and inductive silicate-based bioceramics play an important role in hard tissue prosthetics such as bone and teeth. In the present study, a model was established to study the acid-etched enamel remineralization with tricalcium silicate (Ca 3SiO 5, C 3S) paste in vitro. After soaking in simulated oral fluid (SOF), Ca-P precipitation layer was formed on the enamel surface, with the prolonged soaking time, apatite layer turned into density and uniformity and thickness increasingly from 250 to 350 nm for 1 day to 1.7-1.9 μm for 7 days. Structure of apatite crystals was similar to that of hydroxyapatite (HAp). At the same time, surface smoothness of the remineralized layer is favorable for the oral hygiene. These results suggested that C 3S treated the acid-etched enamel can induce apatite formation, indicating the biomimic mineralization ability, and C 3S could be used as an agent of inductive biomineralization for the enamel prosthesis and protection.

Effect of Minocycline on the Durability of Dentin Bonding Produced with Etch-and-Rinse Adhesives.

PubMed

Loguercio, A D; Stanislawczuk, R; Malaquias, P; Gutierrez, M F; Bauer, J; Reis, A

2016-01-01

To evaluate the effect of minocycline and chlorhexidine pretreatment of acid-etched dentin on the longevity of resin-dentin bond strength (μTBS) and nanoleakage of two-step etch-and-rinse adhesives. Before application of Prime & Bond NT and Adper Single Bond 2 in occlusal dentin, the dentin surfaces were treated with 37% phosphoric acid, rinsed, air-dried, and rewetted with water (control group), 2% minocycline, or 2% chlorexidine digluconate. Composite buildups were constructed incrementally, and specimens were longitudinally sectioned to obtain bonded sticks (0.8 mm 2 ) to be tested in tension (0.5 mm/min) immediately or after 24 months of water storage. For nanoleakage, two specimens of each tooth/period were immersed in the silver nitrate solution, photo-developed, and polished with SiC paper for analysis under energy-dispersive X-ray spectroscopy/scanning electron microscopy. Reductions of the μTBS and increases in the nanoleakage were observed for both adhesives when the rewetting procedure was performed with water. Stable bonds were observed for the 2% minocycline and 2% chlorexidine digluconate groups after 24 months. The use of 2% minocycline as pretreatment of acid-etched dentin is one alternative to retard the degradation of resin-dentin interfaces over a 24-month period as well as 2% chlorexidine digluconate.

Technique for etching monolayer and multilayer materials

DOEpatents

Bouet, Nathalie C. D.; Conley, Raymond P.; Divan, Ralu; Macrander, Albert

2015-10-06

A process is disclosed for sectioning by etching of monolayers and multilayers using an RIE technique with fluorine-based chemistry. In one embodiment, the process uses Reactive Ion Etching (RIE) alone or in combination with Inductively Coupled Plasma (ICP) using fluorine-based chemistry alone and using sufficient power to provide high ion energy to increase the etching rate and to obtain deeper anisotropic etching. In a second embodiment, a process is provided for sectioning of WSi.sub.2/Si multilayers using RIE in combination with ICP using a combination of fluorine-based and chlorine-based chemistries and using RF power and ICP power. According to the second embodiment, a high level of vertical anisotropy is achieved by a ratio of three gases; namely, CHF.sub.3, Cl.sub.2, and O.sub.2 with RF and ICP. Additionally, in conjunction with the second embodiment, a passivation layer can be formed on the surface of the multilayer which aids in anisotropic profile generation.

Tactical Video Display.

DTIC Science & Technology

1981-02-01

steady state. A substrate temperatue during the deposition of the ZnS phosphor of about 220-240 0 C seems very compatible to maximize all the physio...create a severe problem for the etching characteristics of the back elec- trode (Al). Zn and Al can both be etched by alkaline and acidic solution. Few

Light Enhanced Hydrofluoric Acid Passivation: A Sensitive Technique for Detecting Bulk Silicon Defects

PubMed Central

Grant, Nicholas E.

2016-01-01

A procedure to measure the bulk lifetime (>100 µsec) of silicon wafers by temporarily attaining a very high level of surface passivation when immersing the wafers in hydrofluoric acid (HF) is presented. By this procedure three critical steps are required to attain the bulk lifetime. Firstly, prior to immersing silicon wafers into HF, they are chemically cleaned and subsequently etched in 25% tetramethylammonium hydroxide. Secondly, the chemically treated wafers are then placed into a large plastic container filled with a mixture of HF and hydrochloric acid, and then centered over an inductive coil for photoconductance (PC) measurements. Thirdly, to inhibit surface recombination and measure the bulk lifetime, the wafers are illuminated at 0.2 suns for 1 min using a halogen lamp, the illumination is switched off, and a PC measurement is immediately taken. By this procedure, the characteristics of bulk silicon defects can be accurately determined. Furthermore, it is anticipated that a sensitive RT surface passivation technique will be imperative for examining bulk silicon defects when their concentration is low (<1012 cm-3). PMID:26779939

Effect of etching with distinct hydrofluoric acid concentrations on the flexural strength of a lithium disilicate-based glass ceramic.

PubMed

Prochnow, Catina; Venturini, Andressa B; Grasel, Rafaella; Bottino, Marco C; Valandro, Luiz Felipe

2017-05-01

This study examined the effects of distinct hydrofluoric acid concentrations on the mechanical behavior of a lithium disilicate-based glass ceramic. Bar-shaped specimens were produced from ceramic blocks (e.max CAD, Ivoclar Vivadent). The specimens were polished, chamfered, and sonically cleaned in distilled water. The specimens were randomly divided into five groups (n = 23). The HF1, HF3, HF5, and HF10 specimens were etched for 20 s with acid concentrations of 1%, 3%, 5%, and 10%, respectively, while the SC (control) sample was untreated. The etched surfaces were evaluated using a scanning electron microscope and an atomic force microscope. Finally, the roughness was measured, and 3-point bending flexural tests were performed. The data were analyzed using one-way analysis of variance (ANOVA) and Tukey's test (α = 0.05). The Weibull modulus and characteristic strength were also determined. No statistical difference in the roughness and flexural strength was determined among the groups. The structural reliabilities (Weilbull moduli) were similar for the tested groups; however, the characteristic strength of the HF1 specimen was greater than that of the HF10 specimen. Compared with the untreated ceramic, the surface roughness and flexural strength of the ceramic were unaffected upon etching, regardless of the acid concentration. © 2016 Wiley Periodicals, Inc. J Biomed Mater Res Part B: Appl Biomater, 105B: 885-891, 2017. © 2016 Wiley Periodicals, Inc.

Effect of zirconia surface treatment using nitric acid-hydrofluoric acid on the shear bond strengths of resin cements

PubMed Central

Kim, Sun Jai; Shim, June Sung

2017-01-01

PURPOSE The aim of this study was to compare the surface roughness of zirconia when using Zircos E etching system (ZSAT), applying a nitric acid-hydrofluoric acid compound as a pretreatment agent, and also to compare the shear bonding strength according to different resin cements. MATERIALS AND METHODS ZSAT, air abrasion, and tribochemical silicacoating were applied on prepared 120 zirconia specimens (10 mm in diameter, 7 mm in height) using CAD/CAM. Each 12 specimens with 4 different resin cements (Panavia F 2.0, Rely X Unicem, Superbond C&B, and Hot bond) were applied to test interfacial bond strength. The statistical analysis was performed using SAS 9.1 (SAS Institute Inc., Cary, NC, USA). The results are as follows: after application of the ZSAT on the zirconia specimens, surface roughness value after 2-hour etching was higher than those after 1- and 3-hour etching on SEM images. RESULTS For Superbond C&B and Rely X Unicem, the specimens treated with ZSAT showed higher shear bond strength values than those treated with air abrasion and tribochemical silicacoating system. Regarding the failure mode of interface over cement and zirconia surface, Rely X Unicem and Hot bond showed cohesive failures and Panavia F 2.0 and Superbond C&B showed mixed failures. CONCLUSION Zircos E etching system in zirconia restoration could increase its shear bond strength. However, its long term success rate and clinical application should be further evaluated. PMID:28435615

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.

Simultaneous fabrication of very high aspect ratio positive nano- to milliscale structures.

PubMed

Chen, Long Qing; Chan-Park, Mary B; Zhang, Qing; Chen, Peng; Li, Chang Ming; Li, Sai

2009-05-01

A simple and inexpensive technique for the simultaneous fabrication of positive (i.e., protruding), very high aspect (>10) ratio nanostructures together with micro- or millistructures is developed. The method involves using residual patterns of thin-film over-etching (RPTO) to produce sub-micro-/nanoscale features. The residual thin-film nanopattern is used as an etching mask for Si deep reactive ion etching. The etched Si structures are further reduced in size by Si thermal oxidation to produce amorphous SiO(2), which is subsequently etched away by HF. Two arrays of positive Si nanowalls are demonstrated with this combined RPTO-SiO(2)-HF technique. One array has a feature size of 150 nm and an aspect ratio of 26.7 and another has a feature size of 50 nm and an aspect ratio of 15. No other parallel reduction technique can achieve such a very high aspect ratio for 50-nm-wide nanowalls. As a demonstration of the technique to simultaneously achieve nano- and milliscale features, a simple Si nanofluidic master mold with positive features with dimensions varying continuously from 1 mm to 200 nm and a highest aspect ratio of 6.75 is fabricated; the narrow 200-nm section is 4.5 mm long. This Si master mold is then used as a mold for UV embossing. The embossed open channels are then closed by a cover with glue bonding. A high aspect ratio is necessary to produce unblocked closed channels after the cover bonding process of the nanofluidic chip. The combined method of RPTO, Si thermal oxidation, and HF etching can be used to make complex nanofluidic systems and nano-/micro-/millistructures for diverse applications.

Consideration of correlativity between litho and etching shape

NASA Astrophysics Data System (ADS)

Matsuoka, Ryoichi; Mito, Hiroaki; Shinoda, Shinichi; Toyoda, Yasutaka

2012-03-01

We developed an effective method for evaluating the correlation of shape of Litho and Etching pattern. The purpose of this method, makes the relations of the shape after that is the etching pattern an index in wafer same as a pattern shape on wafer made by a lithography process. Therefore, this method measures the characteristic of the shape of the wafer pattern by the lithography process and can predict the hotspot pattern shape by the etching process. The method adopts a metrology management system based on DBM (Design Based Metrology). This is the high accurate contouring created by an edge detection algorithm used wafer CD-SEM. Currently, as semiconductor manufacture moves towards even smaller feature size, this necessitates more aggressive optical proximity correction (OPC) to drive the super-resolution technology (RET). In other words, there is a trade-off between highly precise RET and lithography management, and this has a big impact on the semiconductor market that centers on the semiconductor business. 2-dimensional shape of wafer quantification is important as optimal solution over these problems. Although 1-dimensional shape measurement has been performed by the conventional technique, 2-dimensional shape management is needed in the mass production line under the influence of RET. We developed the technique of analyzing distribution of shape edge performance as the shape management technique. In this study, we conducted experiments for correlation method of the pattern (Measurement Based Contouring) as two-dimensional litho and etch evaluation technique. That is, observation of the identical position of a litho and etch was considered. It is possible to analyze variability of the edge of the same position with high precision.

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.

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

Monolithic Laser.

DTIC Science & Technology

1977-09-01

procedures that could be effectively used . Neither chemical nor in situ vapor etch techniques alleviated these problems. The presence of M in the top...mask consisting of rectangles 300 um x 200 urn. The crystal is then chemically etched in two steps. First, a calibrated Na0H:H.0. 39 etch ^ is used ... fabricated (including optical cavity formation) monolithically using conventional photolithographic fabrication technology. This development is a

Effect of the calcium silicate-based sealer removal protocols and time-point of acid etching on the dentin adhesive interface.

PubMed

Morais, Jéssika Mayhara Pereira; Victorino, Keli Regina; Escalante-Otárola, Wilfredo Gustavo; Jordão-Basso, Keren Cristina Fagundes; Palma-Dibb, Regina Guenka; Kuga, Milton Carlos

2018-06-15

The aim of the study was to evaluate the effects when acid etching on the dentin surface was immediately performed (I) or 7 days (D) after calcium silicate-based sealer (MTA Fillapex) removal, using 95% ethanol (E) or xylol (X). First study, 60 bovine incisor dentin specimens were impregnated with sealer and divided into six groups (n = 10): (EI), E + I; (XI), X + I; (ED), E + D; (XD), X + D, (UN), untreated and (MR), mechanical removal of sealer. Scanning electron microscopy (SEM) images (500×) were obtained from each specimen and scores assessed the sealer residues persistence. Second study, 60 specimens were similarly treated; however, the specimens were restored with composite resin after the removal protocols. Hybrid layer formation was evaluated using confocal laser microscopy (1,024×). Third study, 60 specimens were similarly obtained and subjected to micro-shear test to evaluate the effects of removal protocols on the bond strength of etch-and- rinse adhesive system to dentin. XI showed the highest persistence of sealer residues (p < .05), similar to MR (p > .05). EI showed the greatest hybrid layer extension, except in relation to UN (p < .05). XI and MR presented the lowest bond strength adhesive system to dentin (p < .05). Acid etching immediately after calcium silicate-based endodontic sealer removal using xylol presented the highest residues persistence and negatively affected the adhesive interface between dentin and etch-and-rinse adhesive system. © 2018 Wiley Periodicals, Inc.

Plasma etching a ceramic composite. [evaluating microstructure

NASA Technical Reports Server (NTRS)

Hull, David R.; Leonhardt, Todd A.; Sanders, William A.

1992-01-01

Plasma etching is found to be a superior metallographic technique for evaluating the microstructure of a ceramic matrix composite. The ceramic composite studied is composed of silicon carbide whiskers (SiC(sub W)) in a matrix of silicon nitride (Si3N4), glass, and pores. All four constituents are important in evaluating the microstructure of the composite. Conventionally prepared samples, both as-polished or polished and etched with molten salt, do not allow all four constituents to be observed in one specimen. As-polished specimens allow examination of the glass phase and porosity, while molten salt etching reveals the Si3N4 grain size by removing the glass phase. However, the latter obscures the porosity. Neither technique allows the SiC(sub W) to be distinguished from the Si3N4. Plasma etching with CF4 + 4 percent O2 selectively attacks the Si3N4 grains, leaving SiC(sub W) and glass in relief, while not disturbing the pores. An artifact of the plasma etching reaction is the deposition of a thin layer of carbon on Si3N4, allowing Si3N4 grains to be distinguished from SiC(sub W) by back scattered electron imaging.

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.

The use of a 'bleach-etch-seal' deproteinization technique on MIH affected enamel.

PubMed

Gandhi, Shan; Crawford, Peter; Shellis, Peter

2012-11-01

To ascertain whether deproteinization pretreatment of molar-incisor hypomineralization (MIH) enamel affects resin sealant infiltration. Thirty one extracted MIH teeth were divided into three sections and randomly allocated into the Control (etch and FS), Treatment 1 (5% NaOCl, etched and fissure sealed), and Treatment 2 (5% NaOCl and fissure sealed with no etch) groups. Two hundred seventy nine sealant tag/enamel grade observations were recorded by scanning electron microscopy. Control and Treatment 1 were similar in their outcomes, and Treatment 2 was markedly different. There was no statistical evidence to suggest that there was any difference between Treatment 1 and the Control Treatment (95% CI, 0.52, 1.51; P = 0.6). There was a marked difference between Treatment 2 and the Control Treatment (95% CI, 0.07, 0.25; P < 0.001). All treatments also demonstrated a high-predicted probability of obtaining 'poor' sealant tags (Control = 47%, Treatment 1 = 49%, and Treatment 2 = 40%). The findings suggest that there was no significant difference in the tag quality between the conventional technique (Control) and the 'bleach-etch-seal' technique (Treatment 1). There was no benefit in pre-treating with NaOCl alone (without etch) before sealing. This research also showed that there was a high-predicted probability of obtaining 'poor' sealant tags in MIH enamel, regardless of which of the three treatments was used. © 2012 The Authors. International Journal of Paediatric Dentistry © 2012 BSPD, IAPD and Blackwell Publishing Ltd.

Hafnium Oxide Film Etching Using Hydrogen Chloride Gas

NASA Astrophysics Data System (ADS)

Habuka, Hitoshi; Yamaji, Masahiko; Kobori, Yoshitsugu; Horii, Sadayoshi; Kunii, Yasuo

2009-12-01

Hydrogen chloride gas removes the hafnium oxide film formed by atomic layer deposition at the etch rate of about 1 nm/min. A 100 nm-thick hafnium oxide film was perfectly etched off at 1173 K for 60 min by 100% hydrogen chloride gas at 100 sccm. A weight decrease in the hafnium oxide film was observed at temperatures higher than ca. 600 K, which corresponds to the sublimation point of hafnium tetrachloride. The etching by-product is considered to be hafnium tetrachloride. The etching technique developed in this study is expected to be applicable to various processes, such as the cleaning of a hafnium oxide film deposition reactor.

Electrochemical etching technique of platinum-iridium tips for scanning tunneling microscopy

NASA Astrophysics Data System (ADS)

Herrera, Oscar

The scanning tunneling microscope (STM) allows researchers to investigate atomic and molecular structures and properties of nanomaterials. Through the quantum tunneling effect a charge is transferred between the surface of the material and a Platinum-Iridium (Pt-Ir) tip. The production of Pt-Ir tips by electrochemical etching (ECE) has been developed as an alternative technique, to achieve enhanced scanned images of samples, in contrast to the standard mechanical method (SMM). The sharpness apex structure is an essential feature during scanning in order to provide reliable data. We generated a control group of tips by the SMM technique and another group by the ECE technique to investigate the resolution effectiveness in scanning of graphite. The etching of the tips was produced using an auto-variable transformer running a 30 V AC in a 1.5 and 4.0 M CaCl2 solution. The scanning of the graphite surface was conducted at 7x7 nm image width, 0.2 seconds time/line, 256 points/line and 0.05 V for tip voltage. ECE etched tips displayed consistent image resolution, and the sharpness of the tip apex was generally uniform.

Mechanical Stress in InP Structures Etched in an Inductively Coupled Plasma Reactor with Ar/Cl2/CH4 Plasma Chemistry

NASA Astrophysics Data System (ADS)

Landesman, Jean-Pierre; Cassidy, Daniel T.; Fouchier, Marc; Pargon, Erwine; Levallois, Christophe; Mokhtari, Merwan; Jimenez, Juan; Torres, Alfredo

2018-02-01

We investigated the crystal lattice deformation that can occur during the etching of structures in bulk InP using SiNx hard masks with Ar/Cl2/CH4 chemistries in an inductively coupled plasma reactor. Two techniques were used: degree of polarization (DOP) of the photo-luminescence, which gives information on the state of mechanical stress present in the structures, and spectrally resolved cathodo-luminescence (CL) mapping. This second technique also provides elements on the mechanical stress in the samples through analysis of the spectral shift of the CL intrinsic emission lines. Preliminary DOP mapping experiments have been conducted on the SiNx hard mask patterns without etching the underlying InP. This preliminary study demonstrated the potential of DOP to map mechanical stress quantitatively in the structures. In a second step, InP patterns with various widths between 1 μm and 20 μm, and various depths between 1 μm and 6 μm, were analyzed by the 2 techniques. DOP measurements were made both on the (100) top surface of the samples and on the (110) cleaved cross section. CL measurements were made only from the (100) surface. We observed that inside the etched features, close to the vertical etched walls, there is always some compressive deformation, while it is tensile just outside the etched features. The magnitude of these effects depends on the lateral and depth dimensions of the etched structures, and on the separation between them (the tensile deformation increases between them due to some kind of proximity effect when separation decreases).

Etchant for incoloy-903 welds

NASA Technical Reports Server (NTRS)

Gerstmeyer, J. A.

1980-01-01

Special reagent consists of 1 part 90% lactic acid, 1 part 70% nitric acid, and 4 part, 37% hydrochloric acid. Solution etches parent and weld metals at same rate, without overetching. Underlying grain structure of both metals is revealed.

Determination of total fluoride in HF/HNO3/H2SiF6 etch solutions by new potentiometric titration methods.

PubMed

Weinreich, Wenke; Acker, Jörg; Gräber, Iris

2007-03-30

In the photovoltaic industry the etching of silicon in HF/HNO(3) solutions is a decisive process for cleaning wafer surfaces or to produce certain surface morphologies like polishing or texturization. With regard to cost efficiency, a maximal utilisation of etch baths in combination with highest quality and accuracy is strived. To provide an etch bath control realised by a replenishment with concentrated acids the main constituents of these HF/HNO(3) etch solutions including the reaction product H(2)SiF(6) have to be analysed. Two new methods for the determination of the total fluoride content in an acidic etch solution based on the precipitation titration with La(NO(3))(3) are presented within this paper. The first method bases on the proper choice of the reaction conditions, since free fluoride ions have to be liberated from HF and H(2)SiF(6) at the same time to be detected by a fluoride ion-selective electrode (F-ISE). Therefore, the sample is adjusted to a pH of 8 for total cleavage of the SiF(6)(2-) anion and titrated in absence of buffers. In a second method, the titration with La(NO(3))(3) is followed by a change of the pH-value using a HF resistant glass-electrode. Both methods provide consistent values, whereas the analysis is fast and accurate, and thus, applicable for industrial process control.

Fundamental Studies on Ambient Temperature Creep Deformation Behavior of Alpha and Alpha-Beta Titanium Alloys

DTIC Science & Technology

1994-02-15

Solutions [49] A-Etch 25 (mL) Hydrofluoric Acid (HF 50%) 25 Nitric Acid Cone (HN03) 50 Glycerine R-Etch 18.5 gm (17 mL) Benzalkonium Chloride 35 (mL... Reduction Project (0704-0188) Washington, DC 20503. 1. AGENCY USE ONLY (Leave Blank) 2. REPORT DATE 1994 3. REPORT TYPE AND DATES COVERED Final 4...K and a 60% reduction in area was given for all of the alloys. This work was found to be sufficient to recrystallize all of the alloys within 12

Acid Solutions for Etching Corrosion-Resistant Metals

NASA Technical Reports Server (NTRS)

Simmons, J. R.

1982-01-01

New study characterized solutions for etching austenitic stainless steels, nickel-base alloys, and titanium alloys (annealed). Solutions recommended for use remove at least 0.4 mil of metal from surface in less than an hour. Solutions do not cause intergranular attack on metals for which they are effective, when used under specified conditions.

Size-focusing synthesis of gold nanoclusters with p-mercaptobenzoic acid.

PubMed

Tvedte, Laura M; Ackerson, Christopher J

2014-09-18

Etching or size-focusing methods are now widespread for preparation of atomically monodisperse thiolate-protected gold nanoparticles. Size-focusing methods are not widespread, however, in the production of water-soluble gold nanoparticles. Reported here is a new method for size-focusing of large gold nanoparticles utilizing p-mercaptobenzoic acid. We observe preferential formation of three large gold nanoparticles with approximate masses of 23, 51, and 88 kDa. On the basis of the stability of these masses against further etching or growth, they appear to be especially stable sizes. These sizes are not prominent after etching challenges with organosoluble ligands, and the 51 and 88 kDa sizes appear to be novel stable thiolate-protected gold cluster sizes. The overall trend in particle size distribution over time is also unusual, with larger sizes dominating at longer time points.

Evaluation of Different Types of Lasers in Surface Conditioning of Porcelains: A Review Article

PubMed Central

Mirhashemi, Amirhossin; Sharifi, Nastaran; Moharrami, Mohammad; Chiniforush, Nasim

2017-01-01

To achieve proper bond strength for porcelains, adequate surface roughness is essential, which is traditionally gained by sandblasting or acid etching with hydrofluoric (HF) acid. Nowadays with the development of laser systems, serious efforts were made to apply this new instrument for surface etching of porcelains due to easy usage, safety, and more efficiency. There are different kinds of lasers and porcelains, so choosing the ones which will be good match for each other is crucial. Besides that, changing the irradiation setting can be beneficial as well. This article reviewed 33 related studies and summarized results of etching accomplished by Nd:YAG, Er:YAG, Er,Cr:YSGG and CO2 lasers on different types of porcelains considering different laser settings and evaluation methods to bring a comprehensive insight. PMID:29123628

Influence of previous acid etching on bond strength of universal adhesives to enamel and dentin.

PubMed

Torres, Carlos Rocha Gomes; Zanatta, Rayssa Ferreira; Silva, Tatiane Josefa; Huhtala, Maria Filomena Rocha Lima; Borges, Alessandra Bühler

2017-01-01

The objective of this study was to evaluate the effect of acid pretreatment on the bond strength of composite resin bonded to enamel and dentin with 2 different universal self-etching adhesives. The null hypothesis was that the acid treatment performed prior to adhesive application would not significantly change the bond strength to enamel or dentin for either universal adhesive tested. A sample of 112 bovine incisors were selected and embedded in acrylic resin. Half were ground until a flat enamel surface was obtained, and the other half were polished until a 6 × 6-mm area of dentin was exposed, resulting into 2 groups (n = 56). The enamel and dentin groups were divided into 2 subgroups according to the adhesive system applied: Futurabond U or Scotchbond Universal. Each of these subgroups was divided into 2 additional subgroups (n = 14); 1 subgroup received phosphoric acid pretreatment, and 1 subgroup did not. The bond strength was assessed with a microtensile test. Data from enamel and dentin specimens were analyzed separately using 1-way analysis of variance. The acid pretreatment did not significantly change the bond strength of the adhesives tested, either to enamel (P = 0.4161) or to dentin (P = 0.4857). The acid etching pretreatment did not affect the bond strength to dentin and enamel when the tested universal multipurpose adhesive systems were used.

High power cladding light stripper using segmented corrosion method: theoretical and experimental studies.

PubMed

Yin, Lu; Yan, Mingjian; Han, Zhigang; Wang, Hailin; Shen, Hua; Zhu, Rihong

2017-04-17

We present the segmented corrosion method that uses hydrofluoric acid to etch the fiber of a fiber laser for removing high-power cladding light to improve stripping uniformity and power handling capability. For theoretical guidelines, we propose a simulation model of etched-fiber stripping to evaluate the relationship between the etched-fiber parameters and cladding light attenuation and to analyze the stripping uniformity achieved with segmented corrosion. A two-segment etched fiber is fabricated with cladding light attenuation of 19.8 dB and power handling capability up to 670 W. We find that the cladding light is stripped uniformly and the temperature distribution is uniform without the formation of hot spots.

Optical-diffraction method for determining crystal orientation

DOEpatents

Sopori, B.L.

1982-05-07

Disclosed is an optical diffraction technique for characterizing the three-dimensional orientation of a crystal sample. An arbitrary surface of the crystal sample is texture etched so as to generate a pseudo-periodic diffraction grating on the surface. A laser light beam is then directed onto the etched surface, and the reflected light forms a farfield diffraction pattern in reflection. Parameters of the diffraction pattern, such as the geometry and angular dispersion of the diffracted beam are then related to grating shape of the etched surface which is in turn related to crystal orientation. This technique may be used for examining polycrystalline silicon for use in solar cells.

An application of stereoscopy and image processing in forensics: recovering obliterated firearms serial number

NASA Astrophysics Data System (ADS)

da Silva Nunes, L. C.; dos Santos, Paulo Acioly M.

2004-10-01

We present an application of the use of stereoscope to recovering obliterated firearms serial number. We investigate a promising new combined cheap method using both non-destructive and destructive techniques. With the use of a stereomicroscope coupled with a digital camera and a flexible cold light source, we can capture the image of the damaged area, and with continuous polishing and sometimes with the help of image processing techniques we could enhance the observed images and they can also be recorded as evidence. This method has already proven to be useful, in certain cases, in aluminum dotted pistol frames, whose serial number is printed with a laser, when etching techniques are not successful. We can also observe acid treated steel surfaces and enhance the images of recovered serial numbers, which sometimes lack of definition.

[Evaluation of the effect of one-step self etching adhesives applied in pit and fissure sealing].

PubMed

Su, Hong-Ru; Xu, Pei-Cheng; Qian, Wen-Hao

2016-06-01

To observe the effect of three one-step self etching adhesive systems used in fit and fissure sealant and explore the feasibility of application in caries prevention in school. Seven hundred and twenty completely erupted mandibular first molars in 360 children aged 7 to 9 years old were chosen. The split-mouth design was used to select one side as the experimental group, divided into A1(Easy One Adper), B1(Adper Easy One), and C1(iBond SE).The contra lateral teeth served as A2,B2 and C2 groups (phosphoric acid). The retention and caries status were regularly reviewed .The clinical effect of the two groups was compared using SPSS19.0 software package for Chi - square test. At 3 and 6 months, pit and fissure sealant retention rate in A1 and A2, B1 and B2,C1 and C2 group had no significant difference. At 12 months, sealant retention in A1 and B1 group was significantly lower than A2 and B2 group (P<0.05). No significant difference was found between C1 and C2 groups (P>0.05). At 24 months, sealant retention rate in A1, B1 and C1 group was significantly lower than A2, B2 and C2 group (P<0.05). The caries rate in A1and A2, B1 and B2, C1 and C2 group had no significant difference during different follow-up time (P>0.05). The clinical anticariogenic effect of three kinds of one-step etching adhesives and phosphoric acid etching sealant was similar .One-step self etching adhesive system was recommended for pit and fissure sealant to improve the students' oral health. The long-term retention rate of one-step self etching adhesive system was lower than the phosphoric acid method to long term observation is needed.

The effect of silver nanoparticles on composite shear bond strength to dentin with different adhesion protocols.

PubMed

Fatemeh, Koohpeima; Mohammad Javad, Mokhtari; Samaneh, Khalafi

2017-01-01

The purpose of this study was to investigate the effect of silver nanoparticles on composite shear bond strength using one etch and rinse and one self-etch adhesive systems. Silver nanoparticles were prepared. Transmission electron microscope and X-ray diffraction were used to characterize the structure of the particles. Nanoparticles were applied on exposed dentin and then different adhesives and composites were applied. All samples were tested by universal testing machine and shear bond strength was assesed. Particles with average diameter of about 20 nm and spherical shape were found. Moreover, it was shown that pretreatment by silver nanoparticles enhanced shear bond strength in both etch and rinse, and in self-etch adhesive systems (p≤0.05). Considering the positive antibacterial effects of silver nanoparticles, using them is recommended in restorative dentistry. It seems that silver nanoparticles could have positive effects on bond strength of both etch-and-rinse and self-etch adhesive systems. The best results of silver nanoparticles have been achieved with Adper Single Bond and before acid etching.

Temperature compensated sleeve type mirror mount

NASA Technical Reports Server (NTRS)

1973-01-01

The primary mirror of a large (26-inch diameter aperture) solar telescope was made of glass ceramic and designed with an integral hub on the back of the center of the mirror. This permits heat from the mirror to radiate off its back to a nearby cold plate. To permit mounting without high stresses, the hub was ground down to a smooth cylindrical surface 3.5 inch in diameter. The ground surface was then acid-etched to remove 0.007 inch (on the diameter) by immersion for five minutes in a mixture of four parts 92% sulfuric acid and three parts 50% hydrofluoric acid. The acid etching removes microcracks from the ground Cer-Vit surface. An Invar sleeve was fabricated to fit over the hub with about 0.010 inch radial (0.020 inch diametral) clearance.

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.

Effect of Metal Ion Etching on the Tribological, Mechanical and Microstructural Properties of TiN-COATED d2 Tool Steel Using Cae Pvd Technique

NASA Astrophysics Data System (ADS)

Ali, Mubarak; Hamzah, Esah Binti; Hj. Mohd Toff, Mohd Radzi

A study has been made on TiN coatings deposited on D2 tool steel substrates by using commercially available cathodic arc evaporation, physical vapor deposition technique. The goal of this work is to determine the usefulness of TiN coatings in order to improve the micro-Vickers hardness, coefficient of friction and surface roughness of TiN coating deposited on tool steel, which is vastly use in tool industry for various applications. A pin-on-disc test was carried out to study the coefficient of friction versus sliding distance of TiN coating at various ion etching rates. The tribo-test showed that the minimum value recorded for friction coefficient was 0.386 and 0.472 with standard deviation of 0.056 and 0.036 for the coatings deposited at zero and 16 min ion etching. The differences in friction coefficient and surface roughness was mainly associated with the macrodroplets, which was produced during etching stage. The coating deposited for 16 min metal ion etching showed the maximum hardness, i.e., about five times higher than uncoated one and 1.24 times to the coating deposited at zero ion etching. After friction test, the wear track was observed by using field emission scanning electron microscope. The coating deposited for zero ion etching showed small amounts of macrodroplets as compared to the coating deposited for 16 min ion etching. The elemental composition on the wear scar were investigated by means of energy dispersive X-ray, indicate no further TiN coating on wear track. A considerable improvement in TiN coatings was recorded as a function of various ion etching rates.

Method for the preparation of inorganic single crystal and polycrystalline electronic materials

NASA Technical Reports Server (NTRS)

Groves, W. O. (Inventor)

1969-01-01

Large area, semiconductor crystals selected from group 3-5 compounds and alloys are provided for semiconductor device fabrication by the use of a selective etching operation which completely removes the substrate on which the desired crystal was deposited. The substrate, selected from the same group as the single crystal, has a higher solution rate than the epitaxial single crystal which is essentially unaffected by the etching solution. The preparation of gallium phosphide single crystals using a gallium arsenide substrate and a concentrated nitric acid etching solution is described.

Silicon vertical microstructure fabrication by catalytic etching

NASA Astrophysics Data System (ADS)

Huang, Mao-Jung; Yang, Chii-Rong; Chang, Chun-Ming; Chu, Nien-Nan; Shiao, Ming-Hua

2012-08-01

This study presents an effective, simple and inexpensive process for forming micro-scale vertical structures on a (1 0 0) silicon wafer. Several modified etchants and micro-patterns including rectangular, snake-like, circular and comb patterns were employed to determine the optimum etching process. We found that an etchant solution consisting of 4.6 M hydrofluoric acid, 0.44 M hydrogen peroxide and isopropyl alcohol produces microstructures at an etching rate of 0.47 µm min-1 and surface roughness of 17.4 nm. All the patterns were transferred faithfully to the silicon substrate.

Maskless micro/nanofabrication on GaAs surface by friction-induced selective etching

PubMed Central

2014-01-01

In the present study, a friction-induced selective etching method was developed to produce nanostructures on GaAs surface. Without any resist mask, the nanofabrication can be achieved by scratching and post-etching in sulfuric acid solution. The effects of the applied normal load and etching period on the formation of the nanostructure were studied. Results showed that the height of the nanostructure increased with the normal load or the etching period. XPS and Raman detection demonstrated that residual compressive stress and lattice densification were probably the main reason for selective etching, which eventually led to the protrusive nanostructures from the scratched area on the GaAs surface. Through a homemade multi-probe instrument, the capability of this fabrication method was demonstrated by producing various nanostructures on the GaAs surface, such as linear array, intersecting parallel, surface mesas, and special letters. In summary, the proposed method provided a straightforward and more maneuverable micro/nanofabrication method on the GaAs surface. PMID:24495647

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 enamel etching time on roughness and bond strength.

PubMed

Barkmeier, Wayne W; Erickson, Robert L; Kimmes, Nicole S; Latta, Mark A; Wilwerding, Terry M

2009-01-01

The current study examined the effect of different enamel conditioning times on surface roughness and bond strength using an etch-and-rinse system and four self-etch adhesives. Surface roughness (Ra) and composite to enamel shear bond strengths (SBS) were determined following the treatment of flat ground human enamel (4000 grit) with five adhesive systems: (1) Adper Single Bond Plus (SBP), (2) Adper Prompt L-Pop (PLP), (3) Clearfil SE Bond (CSE), (4) Clearfil S3 Bond (CS3) and (5) Xeno IV (X4), using recommended treatment times and an extended treatment time of 60 seconds (n = 10/group). Control groups were also included for Ra (4000 grit surface) and SBS (no enamel treatment and Adper Scotchbond Multi-Purpose Adhesive). For surface roughness measurements, the phosphoric acid conditioner of the SBP etch-and-rinse system was rinsed from the surface with an air-water spray, and the other four self-etch adhesive agents were removed with alternating rinses of water and acetone. A Proscan 2000 non-contact profilometer was used to determine Ra values. Composite (Z100) to enamel bond strengths (24 hours) were determined using Ultradent fixtures and they were debonded with a crosshead speed of 1 mm/minute. The data were analyzed with ANOVA and Fisher's LSD post-hoc test. The etch-and- rinse system (SBP) produced the highest Ra (microm) and SBS (MPa) using both the recommended treatment time (0.352 +/- 0.028 microm and 40.5 +/- 6.1 MPa) and the extended treatment time (0.733 +/- 0.122 microm and 44.2 +/- 8.2 MPa). The Ra and SBS of the etch-and-rinse system were significantly greater (p < 0.05) than all the self-etch systems and controls. Increasing the treatment time with phosphoric acid (SBP) and PLP produced greater surface roughness (p < 0.05) but did not result in significantly higher bond strengths (p > 0.05).

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.

Fabrication mechanism of friction-induced selective etching on Si(100) surface

PubMed Central

2012-01-01

As a maskless nanofabrication technique, friction-induced selective etching can easily produce nanopatterns on a Si(100) surface. Experimental results indicated that the height of the nanopatterns increased with the KOH etching time, while their width increased with the scratching load. It has also found that a contact pressure of 6.3 GPa is enough to fabricate a mask layer on the Si(100) surface. To understand the mechanism involved, the cross-sectional microstructure of a scratched area was examined, and the mask ability of the tip-disturbed silicon layer was studied. Transmission electron microscope observation and scanning Auger nanoprobe analysis suggested that the scratched area was covered by a thin superficial oxidation layer followed by a thick distorted (amorphous and deformed) layer in the subsurface. After the surface oxidation layer was removed by HF etching, the residual amorphous and deformed silicon layer on the scratched area can still serve as an etching mask in KOH solution. The results may help to develop a low-destructive, low-cost, and flexible nanofabrication technique suitable for machining of micro-mold and prototype fabrication in micro-systems. PMID:22356699

Fabrication mechanism of friction-induced selective etching on Si(100) surface.

PubMed

Guo, Jian; Song, Chenfei; Li, Xiaoying; Yu, Bingjun; Dong, Hanshan; Qian, Linmao; Zhou, Zhongrong

2012-02-23

As a maskless nanofabrication technique, friction-induced selective etching can easily produce nanopatterns on a Si(100) surface. Experimental results indicated that the height of the nanopatterns increased with the KOH etching time, while their width increased with the scratching load. It has also found that a contact pressure of 6.3 GPa is enough to fabricate a mask layer on the Si(100) surface. To understand the mechanism involved, the cross-sectional microstructure of a scratched area was examined, and the mask ability of the tip-disturbed silicon layer was studied. Transmission electron microscope observation and scanning Auger nanoprobe analysis suggested that the scratched area was covered by a thin superficial oxidation layer followed by a thick distorted (amorphous and deformed) layer in the subsurface. After the surface oxidation layer was removed by HF etching, the residual amorphous and deformed silicon layer on the scratched area can still serve as an etching mask in KOH solution. The results may help to develop a low-destructive, low-cost, and flexible nanofabrication technique suitable for machining of micro-mold and prototype fabrication in micro-systems.

Documentation concerning KKP development work

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

Dixit, S.; Thomas, I.; Rushford, M.

1994-12-22

Fabrication has been completed on a 16 level KPP on a 5-inch diameter aperture fused silica using lithographic techniques and wet etching of fused silica in a buffered hydrofluoric acid solution. The experimentally measured far-field intensity pattern displays the desired top-hat envelope and has a superimposed speckle on it. The far-field contains 90% of the incident energy inside the 640 {mu}m region. This is a significant improvement over the binary RPP`s in terms of the far-field profile control and energy concentration. Sources contributing to the energy loss are identified and efforts are underway to overcome these limitations.

Infrared Photodiodes Made by Low Energy Ion Etching of Molecular Beam Epitaxy Grown Mercury-Cadmium Alloy

NASA Astrophysics Data System (ADS)

Yoo, Sung-Shik

Ion etching was used to form junctions on the p-type (111)B Hg_{1-x}Cd_ {x}Te grown by Molecular Beam Epitaxy(MBE). When Hg_{1-x}Cd_{x}Te layers are etched by Ar ions at energies ranging between 300 and 450eV, the top Hg_{1 -x}Cd_{x}Te layer is converted to n-type. The converted region is electrically characterized as a defective n^+-region near the surface, and a low doped n^--region exist below the damaged region. The total thickness of the converted n-type layer was found to be considerable. These results suggest that the creation of the n-type layer is due to the filling of mercury vacancies by mercury atoms displaced by the Ar ion irradiation on the surface. For the performance of the resulting photodiodes on MBE grown (111)B Hg_{1-x}Cd _{x}Te using this technique, the dynamic resistances at 80K are one order of magnitude less than those of junctions made on Liquid Phase Epitaxially and Bulk grown Hg_{1 -x}Cd_{x}Te. The ion etching technique was compared with ion implantation technique by fabricating diodes on the same MBE grown (111)B Hg _{1-x}Cd_{x}Te layers. The result of the comparison illustrates that ion etching technique is as good as ion implantation technique for the fabrication of Hg_{1-x}Cd _{x}Te photodiodes. Also it is believed that the performance of the diodes is limited by a relatively large density of twin defects usually found in MBE grown (111)B Hg_{1-x}Cd _{x}Te.

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.

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.

Bond strengths of brackets bonded to enamel surfaces conditioned with femtosecond and Er:YAG laser systems.

PubMed

Aglarci, Cahide; Demir, Necla; Aksakalli, Sertac; Dilber, Erhan; Sozer, Ozlem Akinci; Kilic, Hamdi Sukur

2016-08-01

The aim of this study was to compare femtosecond and Er:YAG laser systems with regard to enamel demineralization and bracket bond strength. Human-extracted premolars were randomized to three groups (n = 17) depending on the conditioning treatment used for the buccal surfaces: 37 % orthophosphoric acid, Er:YAG laser etching (MSP mode 120 mJ, 10 Hz, 1.2 W), and femtosecond laser etching (0.4 W, 800 nm, 90 fs/pulse, 1 kHz). Metal brackets were bonded with Transbond XT to the conditioned surfaces and light cured for 20 s. The samples were thermocycled (5000 cycles, 5-55 °C) and subjected to shear bond strength (SBS) testing using a universal testing machine. Failure types were analyzed under an optical stereomicroscope and SEM. The adhesive remnant index (ARI) was evaluated to assess residual adhesive on the enamel surface. The results revealed no significant differences in SBS between the Er:YAG laser (7.2 ± 3.3 MPa) and acid etching groups (7.3 ± 2.7 MPa; p < 0.05), whereas a significant difference was observed between the femtosecond laser etching group (3.3 ± 1.2 MPa) and the other two groups (p < 0.01). ARI scores were significantly different among the three groups. The results of our study suggest that laser conditioning with an Er:YAG system results in successful etching, similar to that obtained with acid. The sole use of a femtosecond laser system may not provide an adequate bond strength at the bracket-enamel interface.

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.

Effects of dextrose and lipopolysaccharide on the corrosion behavior of a Ti-6Al-4V alloy with a smooth surface or treated with double-acid-etching.

PubMed

Faverani, Leonardo P; Assunção, Wirley G; de Carvalho, Paulo Sérgio P; Yuan, Judy Chia-Chun; Sukotjo, Cortino; Mathew, Mathew T; Barao, Valentim A

2014-01-01

Diabetes and infections are associated with a high risk of implant failure. However, the effects of such conditions on the electrochemical stability of titanium materials remain unclear. This study evaluated the corrosion behavior of a Ti-6Al-4V alloy, with a smooth surface or conditioned by double-acid-etching, in simulated body fluid with different concentrations of dextrose and lipopolysaccharide. For the electrochemical assay, the open-circuit-potential, electrochemical impedance spectroscopy, and potentiodynamic test were used. The disc surfaces were characterized by scanning electron microscopy and atomic force microscopy. Their surface roughness and Vickers microhardness were also tested. The quantitative data were analyzed by Pearson's correlation and independent t-tests (α = 0.05). In the corrosion parameters, there was a strong lipopolysaccharide correlation with the Ipass (passivation current density), Cdl (double-layer capacitance), and Rp (polarization resistance) values (p<0.05) for the Ti-6Al-4V alloy with surface treatment by double-acid-etching. The combination of dextrose and lipopolysaccharide was correlated with the Icorr (corrosion current density) and Ipass (p<0.05). The acid-treated groups showed a significant increase in Cdl values and reduced Rp values (p<0.05, t-test). According to the topography, there was an increase in surface roughness (R2 = 0.726, p<0.0001 for the smooth surface; R2 = 0.405, p = 0.036 for the double-acid-etching-treated surface). The microhardness of the smooth Ti-6Al-4V alloy decreased (p<0.05) and that of the treated Ti-6Al-4V alloy increased (p<0.0001). Atomic force microscopy showed changes in the microstructure of the Ti-6Al-4V alloy by increasing the surface thickness mainly in the group associated with dextrose and lipopolysaccharide. The combination of dextrose and lipopolysaccharide affected the corrosion behavior of the Ti-6Al-4V alloy surface treated with double-acid-etching. However, no dose-response corrosion behavior could be observed. These results suggest a greater susceptibility to corrosion of titanium implants in diabetic patients with associated infections.

Effects of Dextrose and Lipopolysaccharide on the Corrosion Behavior of a Ti-6Al-4V Alloy with a Smooth Surface or Treated with Double-Acid-Etching

PubMed Central

Faverani, Leonardo P.; Assunção, Wirley G.; de Carvalho, Paulo Sérgio P.; Yuan, Judy Chia-Chun; Sukotjo, Cortino; Mathew, Mathew T.; Barao, Valentim A.

2014-01-01

Diabetes and infections are associated with a high risk of implant failure. However, the effects of such conditions on the electrochemical stability of titanium materials remain unclear. This study evaluated the corrosion behavior of a Ti-6Al-4V alloy, with a smooth surface or conditioned by double-acid-etching, in simulated body fluid with different concentrations of dextrose and lipopolysaccharide. For the electrochemical assay, the open-circuit-potential, electrochemical impedance spectroscopy, and potentiodynamic test were used. The disc surfaces were characterized by scanning electron microscopy and atomic force microscopy. Their surface roughness and Vickers microhardness were also tested. The quantitative data were analyzed by Pearson's correlation and independent t-tests (α = 0.05). In the corrosion parameters, there was a strong lipopolysaccharide correlation with the Ipass (passivation current density), Cdl (double-layer capacitance), and Rp (polarization resistance) values (p<0.05) for the Ti-6Al-4V alloy with surface treatment by double-acid-etching. The combination of dextrose and lipopolysaccharide was correlated with the Icorr (corrosion current density) and Ipass (p<0.05). The acid-treated groups showed a significant increase in Cdl values and reduced Rp values (p<0.05, t-test). According to the topography, there was an increase in surface roughness (R2 = 0.726, p<0.0001 for the smooth surface; R2 = 0.405, p = 0.036 for the double-acid-etching-treated surface). The microhardness of the smooth Ti-6Al-4V alloy decreased (p<0.05) and that of the treated Ti-6Al-4V alloy increased (p<0.0001). Atomic force microscopy showed changes in the microstructure of the Ti-6Al-4V alloy by increasing the surface thickness mainly in the group associated with dextrose and lipopolysaccharide. The combination of dextrose and lipopolysaccharide affected the corrosion behavior of the Ti-6Al-4V alloy surface treated with double-acid-etching. However, no dose-response corrosion behavior could be observed. These results suggest a greater susceptibility to corrosion of titanium implants in diabetic patients with associated infections. PMID:24671257

Fabrication and analysis of single-crystal KTiOPO₄ films with thicknesses in the micrometer range.

PubMed

Ma, Changdong; Lu, Fei; Xu, Bo; Fan, Ranran

2016-02-01

Single-crystal potassium titanyl phosphate (KTiOPO4, KTP) films with thicknesses less than 5 μm are obtained by using helium (He) implantation combined with ion-beam-enhanced etching. A heavily damaged layer created by a 4×10(16)  cm(-2) fluence of 2 MeV He implantation is removed by means of wet chemical etching in hydrofluoric acid (HF). Thus, free-standing films of KTP with thicknesses in the range of 3-5 μm are obtained. The etching rate can be adjusted over a wide range by choosing temperature and HF concentration, as well as annealing conditions. Sharp etching edges and the smooth surface of the film indicate that a high selective-etching rate is achieved in the damaged layer, and the remaining part of the crystal is undamaged. X-ray and Raman-scattering results prove that KTP films have good single-crystal properties.

Formation of Micro- and Nanostructures on the Nanotitanium Surface by Chemical Etching and Deposition of Titania Films by Atomic Layer Deposition (ALD)

PubMed Central

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

2015-01-01

In this study, an integrated approach was used for the preparation of a nanotitanium-based bioactive material. The integrated approach included three methods: severe plastic deformation (SPD), chemical etching and atomic layer deposition (ALD). For the first time, it was experimentally shown that the nature of the etching medium (acidic or basic Piranha solutions) and the etching time have a significant qualitative impact on the nanotitanium surface structure both at the nano- and microscale. The etched samples were coated with crystalline biocompatible TiO2 films with a thickness of 20 nm by Atomic Layer Deposition (ALD). Comparative study of the adhesive and spreading properties of human osteoblasts MG-63 has demonstrated that presence of nano- and microscale structures and crystalline titanium oxide on the surface of nanotitanium improve bioactive properties of the material. PMID:28793716

Wet-chemical dissolution of TRISO-coated simulated high-temperature-reactor fuel particles

NASA Astrophysics Data System (ADS)

Skolo, K. P.; Jacobs, P.; Venter, J. H.; Klopper, W.; Crouse, P. L.

2012-01-01

Chemical etching with different mixtures of acidic solutions has been investigated to disintegrate the two outermost coatings from tri-structural isotropic coated particles containing zirconia kernels, which are used in simulated particles instead of uranium dioxide. A scanning electron microscope (SEM) was used to study the morphology of the particles after the first etching step as well as at different stages of the second etching step. SEM examination shows that the outer carbon layer can be readily removed with a CrO 3-HNO 3/H 2SO 4 solution. This finding was verified by energy dispersive spectroscopy (EDS) analysis. Etching of the silicon carbide layer in a hydrofluoric-nitric solution yielded partial removal of the coating and localized attack of the underlying coating layers. The SEM results provide evidence that the etching of the silicon carbide layer is strongly influenced by its microstructure.

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

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.

Adiabatic tapered optical fiber fabrication in two step etching

NASA Astrophysics Data System (ADS)

Chenari, Z.; Latifi, H.; Ghamari, S.; Hashemi, R. S.; Doroodmand, F.

2016-01-01

A two-step etching method using HF acid and Buffered HF is proposed to fabricate adiabatic biconical optical fiber tapers. Due to the fact that the etching rate in second step is almost 3 times slower than the previous droplet etching method, terminating the fabrication process is controllable enough to achieve a desirable fiber diameter. By monitoring transmitted spectrum, final diameter and adiabaticity of tapers are deduced. Tapers with losses about 0.3 dB in air and 4.2 dB in water are produced. The biconical fiber taper fabricated using this method is used to excite whispering gallery modes (WGMs) on a microsphere surface in an aquatic environment. So that they are suitable to be used in applications like WGM biosensors.

Chemically etched fiber tips for near-field optical microscopy: a process for smoother tips.

PubMed

Lambelet, P; Sayah, A; Pfeffer, M; Philipona, C; Marquis-Weible, F

1998-11-01

An improved method for producing fiber tips for scanning near-field optical microscopy is presented. The improvement consists of chemically etching quartz optical fibers through their acrylate jacket. This new method is compared with the previous one in which bare fibers were etched. With the new process the meniscus formed by the acid along the fiber does not move during etching, leading to a much smoother surface of the tip cone. Subsequent metallization is thus improved, resulting in better coverage of the tip with an aluminum opaque layer. Our results show that leakage can be avoided along the cone, and light transmission through the tip is spatially limited to an optical aperture of a 100-nm dimension.

Influence of laboratory degradation methods and bonding application parameters on microTBS of self-etch adhesives to dentin.

PubMed

Erhardt, Maria Carolina G; Pisani-Proença, Jatyr; Osorio, Estrella; Aguilera, Fátima S; Toledano, Manuel; Osorio, Raquel

2011-04-01

To evaluate the laboratory resistance to degradation and the use of different bonding treatments on resin-dentin bonds formed with three self-etching adhesive systems. Flat, mid-coronal dentin surfaces from extracted human molars were bonded according to manufacturer's directions and submitted to two challenging regimens: (A) chemical degradation with 10% NaOC1 immersion for 5 hours; and (B) fatigue loading at 90 N using 50,000 cycles at 3.0 Hz. Additional dentin surfaces were bonded following four different bonding application protocols: (1) according to manufacturer's directions; (2) acid-etched with 36% phosphoric acid (H3PO4) for 15 seconds; (3) 10% sodium hypochlorite (NaOClaq) treated for 2 minutes, after H3PO4-etching; and (4) doubling the application time of the adhesives. Two one-step self-etch adhesives (an acetone-based: Futurabond/FUT and an ethanol-based: Futurabond NR/FNR) and a two-step self-etch primer system (Clearfil SE Bond/CSE) were examined. Specimens were sectioned into beams and tested for microtensile bond strength (microTBS). Selected debonded specimens were observed under scanning electron microscopy (SEM). Data (MPa) were analyzed by ANOVA and multiple comparisons tests (alpha= 0.05). microTBS significantly decreased after chemical and mechanical challenges (P< 0.05). CSE showed higher microTBS than the other adhesive systems, regardless the bonding protocol. FUT attained the highest microTBS after doubling the application time. H3PO4 and H3PO4 + NaOCl pretreatments significantly decreased bonding efficacy of the adhesives.

Tailored Height Gradients in Vertical Nanowire Arrays via Mechanical and Electronic Modulation of Metal-Assisted Chemical Etching.

PubMed

Otte, M A; Solis-Tinoco, V; Prieto, P; Borrisé, X; Lechuga, L M; González, M U; Sepulveda, B

2015-09-02

In current top-down nanofabrication methodologies the design freedom is generally constrained to the two lateral dimensions, and is only limited by the resolution of the employed nanolithographic technique. However, nanostructure height, which relies on certain mask-dependent material deposition or etching techniques, is usually uniform, and on-chip variation of this parameter is difficult and generally limited to very simple patterns. Herein, a novel nanofabrication methodology is presented, which enables the generation of high aspect-ratio nanostructure arrays with height gradients in arbitrary directions by a single and fast etching process. Based on metal-assisted chemical etching using a catalytic gold layer perforated with nanoholes, it is demonstrated how nanostructure arrays with directional height gradients can be accurately tailored by: (i) the control of the mass transport through the nanohole array, (ii) the mechanical properties of the perforated metal layer, and (iii) the conductive coupling to the surrounding gold film to accelerate the local electrochemical etching process. The proposed technique, enabling 20-fold on-chip variation of nanostructure height in a spatial range of a few micrometers, offers a new tool for the creation of novel types of nano-assemblies and metamaterials with interesting technological applications in fields such as nanophotonics, nanophononics, microfluidics or biomechanics. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

Nanoscale silver-assisted wet etching of crystalline silicon for anti-reflection surface textures.

PubMed

Li, Rui; Wang, Shuling; Chuwongin, Santhad; Zhou, Weidong

2013-01-01

We report here an electro-less metal-assisted chemical etching (MacEtch) process as light management surface-texturing technique for single crystalline Si photovoltaics. Random Silver nanostructures were formed on top of the Si surface based on the thin film evaporation and annealing process. Significant reflection reduction was obtained from the fabricated Si sample, with approximately 2% reflection over a wide spectra range (300 to 1050 nm). The work demonstrates the potential of MacEtch process for anti-reflection surface texture fabrication of large area, high efficiency, and low cost thin film solar cell.

Fabrication of 3D surface structures using grayscale lithography

NASA Astrophysics Data System (ADS)

Stilson, Christopher; Pal, Rajan; Coutu, Ronald A.

2014-03-01

The ability to design and develop 3D microstructures is important for microelectromechanical systems (MEMS) fabrication. Previous techniques used to create 3D devices included tedious steps in direct writing and aligning patterns onto a substrate followed by multiple photolithography steps using expensive, customized equipment. Additionally, these techniques restricted batch processing and placed limits on achievable shapes. Gray-scale lithography enables the fabrication of a variety of shapes using a single photolithography step followed by reactive ion etching (RIE). Micromachining 3D silicon structures for MEMS can be accomplished using gray-scale lithography along with dry anisotropic etching. In this study, we investigated: using MATLAB for mask designs; feasibility of using 1 μm Heidelberg mask maker to direct write patterns onto photoresist; using RIE processing to etch patterns into a silicon substrate; and the ability to tailor etch selectivity for precise fabrication. To determine etch rates and to obtain desired etch selectivity, parameters such as gas mixture, gas flow, and electrode power were studied. This process successfully demonstrates the ability to use gray-scale lithography and RIE for use in the study of micro-contacts. These results were used to produce a known engineered non-planer surface for testing micro-contacts. Surface structures are between 5 μm and 20 μm wide with varying depths and slopes based on mask design and etch rate selectivity. The engineered surfaces will provide more insight into contact geometries and failure modes of fixed-fixed micro-contacts.

Impact of pH and application time of meta-phosphoric acid on resin-enamel and resin-dentin bonding.

PubMed

Cardenas, A F M; Siqueira, F S F; Bandeca, M C; Costa, S O; Lemos, M V S; Feitora, V P; Reis, A; Loguercio, A D; Gomes, J C

2018-02-01

To evaluate the immediate microshear resin-enamel bond strength (μSBS) and the immediate and 6-month microtensile bond strength (μTBS) and nanoleakage (NL) of the adhesive interface performed by different pHs of 40% meta-phosphoric acid (MPA) were compared with conventional 37% ortho-phosphoric acid (OPA) under different application times. Additionally, the enamel etching patterns were evaluated and the chemical/morphological changes induced by these differents groups were evaluated. One hundred and ninety-eight extracted human molars were randomly assigned into experimental groups according to the combination of independent variables: Acid [37% ortho-phosphoric acid (OPA), 40% meta-phosphoric acid (MPA) at pHs of: 0.5, 1 and 2] and Application Time [7, 15 and 30s]. Enamel-bond specimens were prepared and tested under μSBS. Resin-dentin beams were tested under μTBS tested immediately or after 6-months of water storage. Nanoleakage was evaluated using bonded-beams of each tooth/time-period. Enamel etching pattern and chemical and ultra-morphology analyses were also performed. The μSBS (MPa) data were subjected to a two-way repeated measures ANOVA (Acid vs. Application time). For μTBS, Acid vs application time vs storage time data were subjected to three-way ANOVA and Tukey's test (α = 0.05). MPA pH 0.5 showed μTBS similar to OPA, independently of the application time on enamel (p>0.05) or dentin (p>0.05). OPA provided higher nanoleakage values than MPA (p = 0.003). Significant decreases in TBS and increases in NL were only observed for OPA after 6 months (p = 0.001). An increase in the application time resulted in a more pronounced etching pattern for MPA. Chemical analysis showed that dentin demineralized by MPA depicted peaks of brushite and octacalcium phosphate. MPA exposed less collagen than OPA. However, optimal results for MPA were dependent on pH/application time. The use of 40% meta-phosphoric acid with a pH of 0.5 is an alternative acid-etching agent for dentin and enamel bonding. Furthermore, the use of MPA preserves the resin-dentin interface over a 6-months period, due to presence of brushite and octacalcium phosphate and a reduced demineralization pattern. Copyright © 2017 Elsevier Ltd. All rights reserved.

Stabilizing platinum in phosphoric acid fuel cells

NASA Technical Reports Server (NTRS)

Remick, R. J.

1981-01-01

The cathode of the phosphoric acid fuel cell uses a high surface area platinum catalyst supported on a carbon substrate. During operation, the small platinum crystallites sinter, causing loss in cell performance. A support was developed that stabilizes platinum in the high surface area condition by retarding or preventing the sintering process. The approach is to form etch pits in the carbon by oxidizing the carbon in the presence of a metal oxide catalyst, remove the metal oxide by an acid wash, and then deposit platinum in these pits. Results confirm the formation of etch pits in each of the three supports chosen for investigation: Vulcan XC-72R, Vulcan XC-72 that was graphized at 2500 C, and Shawinigan Acetylene Black.

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.

Effect of laser and air abrasion pretreatment on the microleakage of a fissure sealant applied with conventional and self etch adhesives.

PubMed

Tirali, R E; Celik, C; Arhun, N; Berk, G; Cehreli, S B

2013-01-01

The purpose of this study was to investigate the effects of different pretreatment protocols along with different bonding agents on the microleakage of a fissure sealant material. A total of 144 freshly extracted noncarious human third molars were used The teeth were randomly assigned into three groups with respect to the pretreatment protocol employed: A. Air Abrasion B. Er,Cr:YSGG laser C. No pretreatment (Control). In each group specimens were further subjected to one of the following procedures before application of the sealant: 1. %36 Phosphoric acid-etch (AE) (DeTrey Conditioner 36/Denstply, UK) 2.AE+Prime&Bond NT (Dentsply, UK) 3. Clearfil S3 Bond (Kuraray, Japan) 4. Clearfil SE Bond (Kuraray, Japan). All teeth were sealed with the same fissure sealant material (Conseal F/SDI, Australia). Sealed teeth were further subjected to thermocycling, dye penetration test, sectioning and quantitative image analysis. Statistical evaluation of the microleakage data was performed with two way independent ANOVA and multiple comparisons test at p = 0.05. For qualitative evaluation 2 samples from each group were examined under Scanning Electron Microscopy. Microleakage was affected by both the type of pretreatment and the subsequent bonding protocols employed (p < 0.05). Overall, the highest (Mean = 0.36 mm) and lowest (Mean = 0.06 mm) microleakage values were observed in samples with unpretreated enamel sealed by S3+Conseal F and samples with laser pretreated enamel sealed by Acid Etch+Prime&-Bond+Conseal F protocols, respectively (p < 0.05). In the acid-etch group samples pretreated with laser yielded in slightly lower microleakage scores when compared with unpretreated samples and samples pretreated with air abrasion but the statistical significance was not important (p = 0,179). Similarly, when bonding agent is applied following acid-etching procedure, microleakage scores were not affected from pretreatment protocol (p = 0,615) (intact enamel/laser or air-abrasion). For both all-in one and two step self etch adhesive systems, unpretreated samples demonstrated the highest microleakage scores. For the groups in which bonding agent was utilized, pretreatments did not effected microleakage. Both the tested pretreatment protocols and adhesive procedures had different effects on the sealing properties of Conseal F in permanent tooth enamel.

Classification review of dental adhesive systems: from the IV generation to the universal type

PubMed Central

Sofan, Eshrak; Sofan, Afrah; Palaia, Gaspare; Tenore, Gianluca; Romeo, Umberto; Migliau, Guido

2017-01-01

Summary Adhesive dentistry has undergone great progress in the last decades. In light of minimal-invasive dentistry, this new approach promotes a more conservative cavity design, which relies on the effectiveness of current enamel-dentine adhesives. Adhesive dentistry began in 1955 by Buonocore on the benefits of acid etching. With changing technologies, dental adhesives have evolved from no-etch to total-etch (4th and 5th generation) to self-etch (6th, 7th and 8th generation) systems. Currently, bonding to dental substrates is based on three different strategies: 1) etch-and-rinse, 2) self-etch and 3) resin-modified glass-ionomer approach as possessing the unique properties of self-adherence to the tooth tissue. More recently, a new family of dentin adhesives has been introduced (universal or multi-mode adhesives), which may be used either as etch-and-rinse or as self-etch adhesives. The purpose of this article is to review the literature on the current knowledge for each adhesive system according to their classification that have been advocated by many authorities in most operative/restorative procedures. As noted by several valuable studies that have contributed to understanding of bonding to various substrates helps clinicians to choose the appropriate dentin bonding agents for optimal clinical outcomes. PMID:28736601

Seebeck Coefficient of Thermocouples from Nickel-Coated Carbon Fibers: Theory and Experiment.

PubMed

Hardianto, Hardianto; De Mey, Gilbert; Ciesielska-Wrόbel, Izabela; Hertleer, Carla; Van Langenhove, Lieva

2018-05-30

Thermocouples made of etched and non-etched nickel-coated carbon yarn (NiCCY) were investigated. Theoretic Seebeck coefficients were compared to experimental results from measurements of generated electric voltage by these thermocouples. The etching process for making thermocouples was performed by immersion of NiCCY in the solution containing a mixture of hydrochloric acid (HCl) (37% of concentration), and hydrogen peroxide (H₂O₂) in three different concentrations-3%, 6%, and 10%. Thirty minutes of etching to remove Ni from NiCCY was followed by washing and drying. Next, the ability to generate electrical voltage by the thermocouples (being a junction of the etched and the non-etched NiCCY) was measured in different ranges of temperatures, both a cold junction (291.15⁻293.15 K) and a hot junction (293.15⁻325.15 K). A formula predicting the Seebeck coefficient of this thermocouple was elaborated, taking into consideration resistance values of the tested samples. It was proven that there is a good agreement between the theoretical and experimental data, especially for the yarns etched with 6% and 10% peroxide (both were mixed with HCl). The electrical resistance of non-fully etched nickel remaining on the carbon fiber surface ( R 1 ) can have a significant effect on the thermocouples' characteristics.

SEMICONDUCTOR TECHNOLOGY: Wet etching characteristics of a HfSiON high-k dielectric in HF-based solutions

NASA Astrophysics Data System (ADS)

Yongliang, Li; Qiuxia, Xu

2010-03-01

The wet etching properties of a HfSiON high-k dielectric in HF-based solutions are investigated. HF-based solutions are the most promising wet chemistries for the removal of HfSiON, and etch selectivity of HF-based solutions can be improved by the addition of an acid and/or an alcohol to the HF solution. Due to densification during annealing, the etch rate of HfSiON annealed at 900 °C for 30 s is significantly reduced compared with as-deposited HfSiON in HF-based solutions. After the HfSiON film has been completely removed by HF-based solutions, it is not possible to etch the interfacial layer and the etched surface does not have a hydrophobic nature, since N diffuses to the interface layer or Si substrate formation of Si-N bonds that dissolves very slowly in HF-based solutions. Existing Si-N bonds at the interface between the new high-k dielectric deposit and the Si substrate may degrade the carrier mobility due to Coulomb scattering. In addition, we show that N2 plasma treatment before wet etching is not very effective in increasing the wet etch rate for a thin HfSiON film in our case.

What's new in dentine bonding? Self-etch adhesives.

PubMed

Burke, F J Trevor

2004-12-01

Bonding to dentine is an integral part of contemporary restorative dentistry, but early systems were not user-friendly. The introduction of new systems which have a reduced number of steps--the self-etch adhesives--could therefore be an advantage to clinicians, provided that they are as effective as previous adhesives. These new self-etch materials appear to form hybrid layers as did the previous generation of materials. However, there is a need for further clinical research on these new materials. Advantages of self-etch systems include, no need to etch and rinse, reduced post-operative sensitivity and low technique sensitivity. Disadvantages include, the inhibition of set of self- or dual-cure resin materials and the need to roughen untreated enamel surfaces prior to bonding.

Semiconductor structure and recess formation etch technique

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

Lu, Bin; Sun, Min; Palacios, Tomas Apostol

2017-02-14

A semiconductor structure has a first layer that includes a first semiconductor material and a second layer that includes a second semiconductor material. The first semiconductor material is selectively etchable over the second semiconductor material using a first etching process. The first layer is disposed over the second layer. A recess is disposed at least in the first layer. Also described is a method of forming a semiconductor structure that includes a recess. The method includes etching a region in a first layer using a first etching process. The first layer includes a first semiconductor material. The first etching processmore » stops at a second layer beneath the first layer. The second layer includes a second semiconductor material.« less

Method for providing an arbitrary three-dimensional microstructure in silicon using an anisotropic deep etch

DOEpatents

Morales, Alfredo M.; Gonzales, Marcela

2004-06-15

The present invention describes a method for fabricating an embossing tool or an x-ray mask tool, providing microstructures that smoothly vary in height from point-to-point in etched substrates, i.e., structure which can vary in all three dimensions. The process uses a lithographic technique to transfer an image pattern in the surface of a silicon wafer by exposing and developing the resist and then etching the silicon substrate. Importantly, the photoresist is variably exposed so that when developed some of the resist layer remains. The remaining undeveloped resist acts as an etchant barrier to the reactive plasma used to etch the silicon substrate and therefore provides the ability etch structures of variable depths.

Examination of the laser-induced variations in the chemical etch rate of a photosensitive glass ceramic

NASA Astrophysics Data System (ADS)

Voges, Melanie; Beversdorff, Manfred; Willert, Chris; Krain, Hartmut

2007-10-01

Previous studies in our laboratory have reported that the chemical etch rate of a commercial photosensitive glass ceramic (FoturanTM, Schott Corp., Germany) in dilute hydrofluoric acid is strongly dependent on the incident laser irradiance during patterning at λ=266 nm and λ=355 nm. To help elucidate the underlying chemical and physical processes associated with the laser-induced variations in the chemical etch rate, several complimentary techniques were employed at various stages of the UV laser exposure and thermal treatment. X-ray diffraction (XRD) was used to identify the crystalline phases that are formed in Foturan following laser irradiation and annealing, and monitor the crystalline content as a function of laser irradiance at λ=266 nm and λ=355 nm. The XRD results indicate the nucleation of lithium metasilicate (Li2SiO3) crystals as the exclusive phase following laser irradiation and thermal treatment at temperatures not exceeding 605 °C. The XRD studies also show that the Li2SiO3 density increases with increasing laser irradiance and saturates at high laser irradiance. For our thermal treatment protocol, the average Li2SiO3 crystal diameters are 117.0±10.0 nm and 91.2±5.8 nm for λ=266 nm and λ=355 nm, respectively. Transmission electron microscopy (TEM) was utilized to examine the microscopic structural features of the lithium metasilicate crystals. The TEM results reveal that the growth of lithium metasilicate crystals proceeds dendritically, and produces Li2SiO3 crystals that are ˜700 1000 nm in length for saturation exposures. Optical transmission spectroscopy (OTS) was used to study the growth of metallic silver clusters that act as nucleation sites for the Li2SiO3 crystalline phase. The OTS results show that the (Ag0)x cluster concentration has a dependence on incident laser irradiance that is similar to the etch rate ratios and Li2SiO3 concentration. A comparison between the XRD and optical transmission results and our prior etch rate results show that the etch rate contrast and absolute etch rates are dictated by the Li2SiO3 concentration, which is in turn governed by the (Ag0)x cluster concentration. These results characterize the relationship between the laser exposure and chemical etch rate for Foturan, and permit a more detailed understanding of the photophysical processes that occur in the general class of photostructurable glass ceramic materials. Consequently, these results may also influence the laser processing of other photoactive materials.

Nanoleakage in Hybrid Layer and Acid-Base Resistant Zone at the Adhesive/Dentin Interface.

PubMed

Nikaido, Toru; Nurrohman, Hamid; Takagaki, Tomohiro; Sadr, Alireza; Ichinose, Shizuko; Tagami, Junji

2015-10-01

The aim of interfacial nanoleakage evaluation is to gain a better understanding of degradation of the adhesive-dentin interface. The acid-base resistant zone (ABRZ) is recognized at the bonded interface under the hybrid layer (HL) in self-etch adhesive systems after an acid-base challenge. The purpose of this study was to evaluate nanoleakage in HL and ABRZ using three self-etch adhesives; Clearfil SE Bond (SEB), Clearfil SE One (SEO), and G-Bond Plus (GBP). One of the three adhesives was applied on the ground dentin surface and light cured. The specimens were longitudinally divided into two halves. One half remained as the control group. The others were immersed in ammoniacal silver nitrate solution, followed by photo developing solution under fluorescent light. Following this, the specimens were subjected to acid-base challenges with an artificial demineralization solution (pH4.5) and sodium hypochlorite, and prepared in accordance with common procedures for transmission electron microscopy (TEM) examination. The TEM images revealed silver depositions in HL and ABRZ due to nanoleakage in all the adhesives; however, the extent of nanoleakage was material dependent. Funnel-shaped erosion beneath the ABRZ was observed only in the all-in-one adhesive systems; SEO and GBP, but not in the two-step self-etch adhesive system; SEB.

Design of a new bottom antireflective coating composition for KrF resist

NASA Astrophysics Data System (ADS)

Mizutani, Kazuyoshi; Momota, Makoto; Aoai, Toshiaki; Yagihara, Morio

1999-06-01

A study for a new organic bottom antireflective coating (BARC) composition is described. A structural design of a light-absorbing dye was most important because dye structure not only plays a role in eliminating reflection from a substrate but also shows influence on dry etch rate of BARC material to a considerable extent. For example, an anthracene moiety with large absorption at 248 nm had undesirable dry etch resistance. 3-Hydroxy-2-naphthoic acid moiety was found to be one of suitable dyes for KrF BARC compositions, and the polymer bearing the dye showed enough absorbance and good erodability in dry etch. The BARC polymer was eroded as one and a half times faster than a novolak resin, and a little faster than an anthracene incorporated polymer. The result was discussed from the concepts of Ohnishi parameter and the ring parameter for dry etch durability of resist materials. BARC polymer should be thermoset by hard bake to eliminate intermixing with resist compositions. The BARC polymer bearing hydroxy group which is useful for a crosslinking reaction was thermoset in the presence of melamine-formaldehyde crosslinker and an acid catalyst after baking over 200 degrees C.

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.

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.

Fabrication of lithographically defined optical coupling facets for silicon-on-insulator waveguides by inductively coupled plasma etching

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

Yap, K.P.; Lamontagne, B.; Delage, A.

2006-05-15

We present a technique to lithographically define and fabricate all required optical facets on a silicon-on-insulator photonic integrated circuit by an inductively coupled plasma etch process. This technique offers 1 {mu}m positioning accuracy of the facets at any location within the chip and eliminates the need of polishing. Facet fabrication consists of two separate steps to ensure sidewall verticality and minimize attack on the end surfaces of the waveguides. Protection of the waveguides by a thermally evaporated aluminum layer before the 40-70 {mu}m deep optical facet etching has been proven essential in assuring the facet smoothness and integrity. Both scanningmore » electron microscopy analysis and optical measurement results show that the quality of the facets prepared by this technique is comparable to the conventional facets prepared by polishing.« less

[Fiber reinforced composite posts: literature review].

PubMed

Frydman, G; Levatovsky, S; Pilo, R

2013-07-01

FRC (Fiber-reinforced composite) posts have been used since the beginning of the 90s with the introduction of carbon fiber posts. Fiber posts are widely used to restore endodontically treated teeth that have insufficient coronal tooth structure. Many in vitro and in vivo studies have shown the advantage of using FRC over prefabricated and cast metal post especially indicated in narrow root canals which are prone to vertically root fracture. The most frequent failure of FRC is debonding of a post at the resin cement/dentin interface. Bonding to dentin may be achieved by using etch-and-rinse and self-etch adhesives. The bond strength formed by self-adhesive cements is noticeably lower in comparison to the bond strength formed with resin cements applied in combination with etch-and-rinse adhesives. In an attempt to maximize resin bonding to fiber posts, several surface treatments have been suggested. Sandblasting with alumina particles results in an increased surface roughness and surface area without affecting the integrity of the post as long as it is applied by 50 microm alumina particles at 2.5 bars for maximally 5 seconds at a distance of 30 mm. The efficiency of post salinization is controversial and its contribution to the retention is of minor importance. Hydrofluoric acid has recently been proposed for etching glass fiber posts but this technique produced substantial damage to the glass fibers and affected the integrity of the post. Delayed cementation of fiber post (at least 24h post endodontic treatment) resulted in higher retentive strengths in comparison to immediate cementation and the best results were obtained when the luting agent was brought into the post space with lentulo spirals or specific syringes. The resin cement film thickness also influences the pullout strengths of fiber-reinforced posts .The highest bond strength values were obtained when the cement layer oversized the post spaces but not larger than 0.3 mm. The use of core build-up materials as post luting cements is not recommended. The use of FRC post, combined with proper adhesive cementation technique can give an excellent solution when restoring endodontically treated teeth that are prone to fracture.

Effect of oxalic acid pre-treatment in restorations of non-carious cervical lesions: A randomized clinical trial.

PubMed

de Souza, André Mattos Brito; Colares, Regina Claudia Ramos; Mendonça, Juliano Satori; Rodrigues, Lidiany Karla Azevedo; Santiago, Sérgio Lima

2014-09-01

Non-carious cervical lesions are usually associated with dentin hypersensitivity. The use of oxalic acid in restorations of these lesions could be beneficial in relieving pain. To evaluate the use of oxalic acid in restorations of non-carious cervical lesions. A randomized clinical trial. One operator placed 90 restorations in 20 volunteers of both sexes, with at least two lesions to be restored with the techniques: Control - Restoration with total-etch technique and Experimental - Restoration with pretreatment with oxalic acid followed by application of adhesive system. The restorative adhesive system used was XP Bond/Durafill. The restorations were directly assessed by two independent examiners using a modified United States Public Health Service (USPHS) method at baseline, 6 and 12 months, taking into account the following criteria: Retention (R), marginal integrity (MI), marginal discoloration (MD), postoperative sensitivity (S), caries (C), and anatomic form (AF). The data were statistically analyzed using the Fisher exact and McNemar tests. The level of significance was set at 5%. After 1 year, the results of restorations clinically satisfactory obtained for the control and experimental group respectively were: R (97% / 89%), MI (100% / 100%), MD (100% / 100%), S (100% / 100%), C (100% / 100%), and AF (100% / 100%). The use of oxalic acid as an agent of dentin pretreatment did not influence the clinical performance of restorations in non-carious cervical lesions after 1 year.

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.

Effect of Er:YAG laser pulse duration on the shear bond strength of bleached dentin

NASA Astrophysics Data System (ADS)

Yu, Ping; Yu, Dandan; Zhao, Peng; Xu, Zhou; Gao, Shanshan

2017-11-01

The influence of different Er:YAG laser pulse durations on the shear bond strength (SBS) of bleached dentin was investigated in this study. In total, 176 crowns of extracted human premolars were cut horizontally, embedded and ground to expose the sound dentin. Of these, 132 specimens were bleached with 12% hydrogen peroxide (HP) and divided into three groups, irradiated by an Er:YAG laser with different pulse lengths of 50 µs super short pulse (SSP), 100 µs moderate short pulse (MSP) and 300 µs short pulse (SP), respectively. The energy density of the three groups was the same at about 15.73 J cm-2 for each. Then, each group was further divided into two subgroups according to whether it had been etched with 37% phosphoric acid or not. The control group (N  =  22) was bleached and etched with acid while the blank group (N  =  22) was just etched with acid. The surface morphology of the dentin was observed using scanning electron microscopy (SEM). The SBS of the composite resin to the conditioned dentin was tested with a universal testing machine. It was found that the SBS of the dentin significantly decreased after bleaching treatment, while it was possible to restore it using Er:YAG laser irradiation. Lasers with various pulse durations led to different surface morphologies but had no effect on the SBS. The SSP laser was more suitable on account of it resulting in less thermal damage, and additional acid etching was not necessary for the irradiated bleached dentin in the clinic because it could not further improve the SBS value.

Effect of Hydrofluoric Acid Concentration on Resin Adhesion to a Feldspathic Ceramic.

PubMed

Venturini, Andressa Borin; Prochnow, Catina; Rambo, Dagma; Gundel, Andre; Valandro, Luiz Felipe

2015-08-01

To evaluate the effect of different concentrations of hydrofluoric acid (HF) on the contact angle and the resin bond strength durability to feldspathic ceramic. To evaluate the contact angles of distilled water on etched feldspathic ceramic, 25 specimens (12×10×2.4 mm) of VitaBlocks Mark II were used, divided into 5 groups (n=5): one unconditioned control (UC) group with no ceramic surface treatment, and 4 other groups that were etched for 60 s with different concentrations of HF: 1% (HF1), 3% (HF3), 5% (HF5) and 10% (HF10). The bond testing utilized 40 ceramic blocks (12×10×4 mm) that were fabricated and subjected to the same surface treatments as previously mentioned (excluding the control). The etched surfaces were silanized and resin cement was applied. After 24 h, the blocks were sectioned to produce bar specimens that were divided into two groups, non-aged (immediate testing) and aged (storage for 230 days+12,000 thermocycles at 5°C and 55°C), and subjected to microtensile testing (μTBS). Micromorphogical analysis of the treated surfaces was also performed (atomic force and scanning electron microscopy). One-way ANOVA and Tukey's tests were applied for data analysis. UC had the highest contact angle (61.4°), whereas HF10 showed the lowest contact angle (17.5°). In non-aged conditions, different acids promoted statistically similar bond strengths (14.2 to 15.7 MPa) (p>0.05); in terms of bond durability, only the bond strength of the HF1 group presented a statistically significant decrease comparing before and after aging (14.5 to 10.2 MPa). When etched with 3%, 5%, or 10% hydrofluoric acid, the ceramic tested showed stable resin adhesion after long-term aging.

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.

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.

Consideration of VT5 etch-based OPC modeling

NASA Astrophysics Data System (ADS)

Lim, ChinTeong; Temchenko, Vlad; Kaiser, Dieter; Meusel, Ingo; Schmidt, Sebastian; Schneider, Jens; Niehoff, Martin

2008-03-01

Including etch-based empirical data during OPC model calibration is a desired yet controversial decision for OPC modeling, especially for process with a large litho to etch biasing. While many OPC software tools are capable of providing this functionality nowadays; yet few were implemented in manufacturing due to various risks considerations such as compromises in resist and optical effects prediction, etch model accuracy or even runtime concern. Conventional method of applying rule-based alongside resist model is popular but requires a lot of lengthy code generation to provide a leaner OPC input. This work discusses risk factors and their considerations, together with introduction of techniques used within Mentor Calibre VT5 etch-based modeling at sub 90nm technology node. Various strategies are discussed with the aim of better handling of large etch bias offset without adding complexity into final OPC package. Finally, results were presented to assess the advantages and limitations of the final method chosen.

Optical-fiber strain sensors with asymmetric etched structures.

PubMed

Vaziri, M; Chen, C L

1993-11-01

Optical-fiber strain gauges with asymmetric etched structures have been analyzed, fabricated, and tested. These sensors are very sensitive with a gauge factor as high as 170 and a flat frequency response to at least 2.7 kHz. The gauge factor depends on the asymmetry of the etched structures and the number of etched sections. To understand the physical principles involved, researchers have used structural analysis programs based on a finite-element method to analyze fibers with asymmetric etched structures under tensile stress. The results show that lateral bends are induced on the etched fibers when they are stretched axially. To relate the lateral bending to the optical attenuation, we have also employed a ray-tracing technique to investigate the dependence of the attenuation on the structural deformation. Based on the structural analysis and the ray-tracing study parameters affecting the sensitivity have been studied. These results agree with the results of experimental investigations.

Microfluidic etching and oxime-based tailoring of biodegradable polyketoesters.

PubMed

Barrett, Devin G; Lamb, Brian M; Yousaf, Muhammad N

2008-09-02

A straightforward, flexible, and inexpensive method to etch biodegradable poly(1,2,6-hexanetriol alpha-ketoglutarate) films is reported. Microfluidic delivery of the etchant, a solution of NaOH, can create micron-scale channels through local hydrolysis of the polyester film. In addition, the presence of a ketone in the repeat unit allows for prior or post chemoselective modifications, enabling the design of functionalized microchannels. Delivery of oxyamine tethered ligands react with ketone groups on the polyketoester to generate covalent oxime linkages. By thermally sealing an etched film to a second flat surface, poly(1,2,6-hexanetriol alpha-ketoglutarate) can be used to create biodegradable microfluidic devices. In order to determine the versatility of the microfluidic etch technique, poly(epsilon-caprolactone) was etched with acetone. This strategy provides a facile method for the direct patterning of biodegradable materials, both through etching and chemoselective ligand immobilization.

Large-scale and highly efficient synthesis of micro- and nano-fibers with controlled fiber morphology by centrifugal jet spinning for tissue regeneration

NASA Astrophysics Data System (ADS)

Ren, Liyun; Pandit, Vaibhav; Elkin, Joshua; Denman, Tyler; Cooper, James A.; Kotha, Shiva P.

2013-02-01

PLLA fibrous tissue scaffolds with controlled fiber nanoscale surface roughness are fabricated with a novel centrifugal jet spinning process. The centrifugal jet spinning technique is a highly efficient synthesis method for micron- to nano-sized fibers with a production rate up to 0.5 g min-1. During the centrifugal jet spinning process, a polymer solution jet is stretched by the centrifugal force of a rotating chamber. By engineering the rheological properties of the polymer solution, solvent evaporation rate and centrifugal force that are applied on the solution jet, polyvinylpyrrolidone (PVP) and poly(l-lactic acid) (PLLA) composite fibers with various diameters are fabricated. Viscosity measurements of polymer solutions allowed us to determine critical polymer chain entanglement limits that allow the generation of continuous fiber as opposed to beads or beaded fibers. Above a critical concentration at which polymer chains are partially or fully entangled, lower polymer concentrations and higher centrifugal forces resulted in thinner fibers. Etching of PVP from the PLLA-PVP composite fibers doped with increasing PVP concentrations yielded PLLA fibers with increasing nano-scale surface roughness and porosity, which increased the fiber hydrophilicity dramatically. Scanning electron micrographs of the etched composite fibers suggest that PVP and PLLA were co-contiguously phase separated within the composite fibers during spinning and nano-scale roughness features were created after the partial etching of PVP. To study the tissue regeneration efficacy of the engineered PLLA fiber matrix, human dermal fibroblasts are used to simulate partial skin graft. Fibers with increased PLLA surface roughness and porosity demonstrated a trend towards higher cell attachment and proliferation.PLLA fibrous tissue scaffolds with controlled fiber nanoscale surface roughness are fabricated with a novel centrifugal jet spinning process. The centrifugal jet spinning technique is a highly efficient synthesis method for micron- to nano-sized fibers with a production rate up to 0.5 g min-1. During the centrifugal jet spinning process, a polymer solution jet is stretched by the centrifugal force of a rotating chamber. By engineering the rheological properties of the polymer solution, solvent evaporation rate and centrifugal force that are applied on the solution jet, polyvinylpyrrolidone (PVP) and poly(l-lactic acid) (PLLA) composite fibers with various diameters are fabricated. Viscosity measurements of polymer solutions allowed us to determine critical polymer chain entanglement limits that allow the generation of continuous fiber as opposed to beads or beaded fibers. Above a critical concentration at which polymer chains are partially or fully entangled, lower polymer concentrations and higher centrifugal forces resulted in thinner fibers. Etching of PVP from the PLLA-PVP composite fibers doped with increasing PVP concentrations yielded PLLA fibers with increasing nano-scale surface roughness and porosity, which increased the fiber hydrophilicity dramatically. Scanning electron micrographs of the etched composite fibers suggest that PVP and PLLA were co-contiguously phase separated within the composite fibers during spinning and nano-scale roughness features were created after the partial etching of PVP. To study the tissue regeneration efficacy of the engineered PLLA fiber matrix, human dermal fibroblasts are used to simulate partial skin graft. Fibers with increased PLLA surface roughness and porosity demonstrated a trend towards higher cell attachment and proliferation. Electronic supplementary information (ESI) available. See DOI: 10.1039/c3nr33423f

Bond strength of composites on Er:YAG and Er,Cr:YSGG laser-irradiated enamel

NASA Astrophysics Data System (ADS)

Apel, Christian; Gutknecht, Norbert

1999-02-01

In an in vitro study the bond strength of composite materials on Er:YAG and Er,Cr:YSGG laser-radiated enamel was examined. The results achieved on enamel surfaces conditioned conventionally using the acid etching method served as a control. On 80 extracted cariesfree third molars an enamel area of 4 X 4 mm was conditioned with three different systems. The Er:YAG laser was used at pulse frequencies of 8 Hz, 10 Hz, 12 Hz and 15 Hz using an energy of 120 mJ at each setting. The Er,Cr:YSGG laser was used at the settings of 20 Hz/50 mJ, 20 Hz/100 mJ and 20 Hz/150 mJ. The repetition rate for this device is constantly 20 Hz. In the reference group 10 teeth were etched with 37% phosphoric acid. In order to be able to perform the tensile tests under standard conditions metal brackets were placed on the conditioned surfaces. The 'Orthodontic-Bonding-System' was used as an adhesive system. The brackets were pulled off from the etched surfaces vertically to the tooth using a tensile testing machine. The results confirmed the highest bond strengths in the group of enamel surfaces which have been conditioned with acid etching gel. The bond strength of the Er:YAG laser (8, 10 and 12 Hz)- and Er,Cr:YSGG laser (20 Hz/150 mJ)-conditioned enamel surfaces was not significantly lower.

The processing of enriched germanium for the Majorana Demonstrator and R&D for a next generation double-beta decay experiment

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

Abgrall, N.; Arnquist, I. J.; Avignone III, F. T.

The Majorana Demonstrator is an array of point-contact Ge detectors fabricated from Ge isotopically enriched to 88% in 76Ge to search for neutrinoless double beta decay. The processing of Ge for germanium detectors is a well-known technology. However, because of the high cost of Ge enriched in 76Ge special procedures were required to maximize the yield of detector mass and to minimize exposure to cosmic rays. These procedures include careful accounting for the material; shielding it to reduce cosmogenic generation of radioactive isotopes; and development of special reprocessing techniques for contaminated solid germanium, shavings, grindings, acid etchant and cutting fluidsmore » from detector fabrication. Processing procedures were developed that resulted in a total yield in detector mass of 70%. However, none of the acid-etch solution and only 50% of the cutting fluids from detector fabrication were reprocessed. Had they been processed, the projections for the recovery yield would be between 80% and 85%. Maximizing yield is critical to justify a possible future ton-scale experiment. A process for recovery of germanium from the acid-etch solution was developed with yield of about 90%. All material was shielded or stored underground whenever possible to minimize the formation of 68Ge by cosmic rays, which contributes background in the double-beta decay region of interest and cannot be removed by zone refinement and crystal growth. Formation of 68Ge was reduced by a significant factor over that in natural abundance detectors not protected from cosmic rays.« less

A comparative study of different bleaching agents on the morphology of human enamel: an in vitro SEM study.

PubMed

Uthappa, Roshan; Suprith, M L; Bhandary, Shreetha; Dash, Sumit

2012-11-01

The purpose of the study was to compare two different commercial bleaching agents, Opalescence with Colgate Platinum, and 30% phosphoric acid used as aggressive agent on the morphology of human enamel. Ten freshly extracted, noncarious, human maxillary central incisors extracted for periodontal reasons were used in this study. The labial surface of the disinfected teeth were polished using a polishing paste with the help of rubber cup and a slow speed handpiece. Each tooth was sectioned at cement-enamel junction and the crown was separated into four specimens, all taken from labial surface. Group 1 was treated with Colgate Platinum for 7 hours, group 2 with Opalescence for 7 hours, group 3 was treated with 30% phosphoric acid for 30 seconds and group 4 was untreated and used as control. After the treatment period, the specimens were washed with normal saline and stored in sterile bottle and sealed. Photomicrographs obtained from the scanning electron microscopy (SEM) after surface treatments were examined for no alteration, slight alteration, moderate alteration and severe alterations. The specimens treated with commercial bleaching agents revealed no enamel surface morphologic alterations compared to control group. The specimen treated with phosphoric acid showed severe alterations. Ten percent carbamide peroxide evaluated in this study does not etch tooth enamel or alter enamel surface morphology as do conventional etching techniques. Carbamine peroxide is a safe and effective tooth whitening agent even when used for extended period of time. The enamel surface remains smooth which reduces caries due to plaque collection.

The processing of enriched germanium for the Majorana   Demonstrator  and R&D for a next generation double-beta decay experiment

DOE PAGES

Abgrall, N.; Arnquist, I. J.; Avignone III, F. T.; ...

2017-10-07

The Majorana Demonstrator is an array of point-contact Ge detectors fabricated from Ge isotopically enriched to 88% in 76Ge to search for neutrinoless double beta decay. The processing of Ge for germanium detectors is a well-known technology. However, because of the high cost of Ge enriched in 76Ge special procedures were required to maximize the yield of detector mass and to minimize exposure to cosmic rays. These procedures include careful accounting for the material; shielding it to reduce cosmogenic generation of radioactive isotopes; and development of special reprocessing techniques for contaminated solid germanium, shavings, grindings, acid etchant and cutting fluidsmore » from detector fabrication. Processing procedures were developed that resulted in a total yield in detector mass of 70%. However, none of the acid-etch solution and only 50% of the cutting fluids from detector fabrication were reprocessed. Had they been processed, the projections for the recovery yield would be between 80% and 85%. Maximizing yield is critical to justify a possible future ton-scale experiment. A process for recovery of germanium from the acid-etch solution was developed with yield of about 90%. All material was shielded or stored underground whenever possible to minimize the formation of 68Ge by cosmic rays, which contributes background in the double-beta decay region of interest and cannot be removed by zone refinement and crystal growth. Formation of 68Ge was reduced by a significant factor over that in natural abundance detectors not protected from cosmic rays.« less

The processing of enriched germanium for the MAJORANA DEMONSTRATOR and R&D for a next generation double-beta decay experiment

NASA Astrophysics Data System (ADS)

Abgrall, N.; Arnquist, I. J.; Avignone, F. T., III; Barabash, A. S.; Bertrand, F. E.; Bradley, A. W.; Brudanin, V.; Busch, M.; Buuck, M.; Caja, J.; Caja, M.; Caldwell, T. S.; Christofferson, C. D.; Chu, P.-H.; Cuesta, C.; Detwiler, J. A.; Dunagan, C.; Dunstan, D. T.; Efremenko, Yu.; Ejiri, H.; Elliott, S. R.; Gilliss, T.; Giovanetti, G. K.; Goett, J.; Green, M. P.; Gruszko, J.; Guinn, I. S.; Guiseppe, V. E.; Haufe, C. R. S.; Henning, R.; Hoppe, E. W.; Jasinski, B. R.; Kidd, M. F.; Konovalov, S. I.; Kouzes, R. T.; Lopez, A. M.; MacMullin, J.; Martin, R. D.; Massarczyk, R.; Meijer, S. J.; Mertens, S.; Meyer, J. H.; Myslik, J.; O'Shaughnessy, C.; Poon, A. W. P.; Radford, D. C.; Rager, J.; Reine, A. L.; Reising, J. A.; Rielage, K.; Robertson, R. G. H.; Shanks, B.; Shirchenko, M.; Suriano, A. M.; Tedeschi, D.; Toth, L. M.; Trimble, J. E.; Varner, R. L.; Vasilyev, S.; Vetter, K.; Vorren, K.; White, B. R.; Wilkerson, J. F.; Wiseman, C.; Xu, W.; Yakushev, E.; Yu, C.-H.; Yumatov, V.; Zhitnikov, I.; Zhu, B. X.

2018-01-01

The MAJORANA DEMONSTRATOR is an array of point-contact Ge detectors fabricated from Ge isotopically enriched to 88% in 76 Ge to search for neutrinoless double beta decay. The processing of Ge for germanium detectors is a well-known technology. However, because of the high cost of Ge enriched in 76 Ge special procedures were required to maximize the yield of detector mass and to minimize exposure to cosmic rays. These procedures include careful accounting for the material; shielding it to reduce cosmogenic generation of radioactive isotopes; and development of special reprocessing techniques for contaminated solid germanium, shavings, grindings, acid etchant and cutting fluids from detector fabrication. Processing procedures were developed that resulted in a total yield in detector mass of 70%. However, none of the acid-etch solution and only 50% of the cutting fluids from detector fabrication were reprocessed. Had they been processed, the projections for the recovery yield would be between 80% and 85%. Maximizing yield is critical to justify a possible future ton-scale experiment. A process for recovery of germanium from the acid-etch solution was developed with yield of about 90%. All material was shielded or stored underground whenever possible to minimize the formation of 68Ge by cosmic rays, which contributes background in the double-beta decay region of interest and cannot be removed by zone refinement and crystal growth. Formation of 68Ge was reduced by a significant factor over that in natural abundance detectors not protected from cosmic rays.

TOPICAL REVIEW: Black silicon method X: a review on high speed and selective plasma etching of silicon with profile control: an in-depth comparison between Bosch and cryostat DRIE processes as a roadmap to next generation equipment

NASA Astrophysics Data System (ADS)

Jansen, H V; de Boer, M J; Unnikrishnan, S; Louwerse, M C; Elwenspoek, M C

2009-03-01

An intensive study has been performed to understand and tune deep reactive ion etch (DRIE) processes for optimum results with respect to the silicon etch rate, etch profile and mask etch selectivity (in order of priority) using state-of-the-art dual power source DRIE equipment. The research compares pulsed-mode DRIE processes (e.g. Bosch technique) and mixed-mode DRIE processes (e.g. cryostat technique). In both techniques, an inhibitor is added to fluorine-based plasma to achieve directional etching, which is formed out of an oxide-forming (O2) or a fluorocarbon (FC) gas (C4F8 or CHF3). The inhibitor can be introduced together with the etch gas, which is named a mixed-mode DRIE process, or the inhibitor can be added in a time-multiplexed manner, which will be termed a pulsed-mode DRIE process. Next, the most convenient mode of operation found in this study is highlighted including some remarks to ensure proper etching (i.e. step synchronization in pulsed-mode operation and heat control of the wafer). First of all, for the fabrication of directional profiles, pulsed-mode DRIE is far easier to handle, is more robust with respect to the pattern layout and has the potential of achieving much higher mask etch selectivity, whereas in a mixed-mode the etch rate is higher and sidewall scalloping is prohibited. It is found that both pulsed-mode CHF3 and C4F8 are perfectly suited to perform high speed directional etching, although they have the drawback of leaving the FC residue at the sidewalls of etched structures. They show an identical result when the flow of CHF3 is roughly 30 times the flow of C4F8, and the amount of gas needed for a comparable result decreases rapidly while lowering the temperature from room down to cryogenic (and increasing the etch rate). Moreover, lowering the temperature lowers the mask erosion rate substantially (and so the mask selectivity improves). The pulsed-mode O2 is FC-free but shows only tolerable anisotropic results at -120 °C. The downside of needing liquid nitrogen to perform cryogenic etching can be improved by using a new approach in which both the pulsed and mixed modes are combined into the so-called puffed mode. Alternatively, the use of tetra-ethyl-ortho-silicate (TEOS) as a silicon oxide precursor is proposed to enable sufficient inhibiting strength and improved profile control up to room temperature. Pulsed-mode processing, the second important aspect, is commonly performed in a cycle using two separate steps: etch and deposition. Sometimes, a three-step cycle is adopted using a separate step to clean the bottom of etching features. This study highlights an issue, known by the authors but not discussed before in the literature: the need for proper synchronization between gas and bias pulses to explore the benefit of three steps. The transport of gas from the mass flow controller towards the wafer takes time, whereas the application of bias to the wafer is relatively instantaneous. This delay causes a problem with respect to synchronization when decreasing the step time towards a value close to the gas residence time. It is proposed to upgrade the software with a delay time module for the bias pulses to be in pace with the gas pulses. If properly designed, the delay module makes it possible to switch on the bias exactly during the arrival of the gas for the bottom removal step and so it will minimize the ionic impact because now etch and deposition steps can be performed virtually without bias. This will increase the mask etch selectivity and lower the heat impact significantly. Moreover, the extra bottom removal step can be performed at (also synchronized!) low pressure and therefore opens a window for improved aspect ratios. The temperature control of the wafer, a third aspect of this study, at a higher etch rate and longer etch time, needs critical attention, because it drastically limits the DRIE performance. It is stressed that the exothermic reaction (high silicon loading) and ionic impact (due to metallic masks and/or exposed silicon) are the main sources of heat that might raise the wafer temperature uncontrollably, and they show the weakness of the helium backside technique using mechanical clamping. Electrostatic clamping, an alternative technique, should minimize this problem because it is less susceptible to heat transfer when its thermal resistance and the gap of the helium backside cavity are minimized; however, it is not a subject of the current study. Because oxygen-growth-based etch processes (due to their ultra thin inhibiting layer) rely more heavily on a constant wafer temperature than fluorocarbon-based processes, oxygen etches are more affected by temperature fluctuations and drifts during the etching. The fourth outcome of this review is a phenomenological model, which explains and predicts many features with respect to loading, flow and pressure behaviour in DRIE equipment including a diffusion zone. The model is a reshape of the flow model constructed by Mogab, who studied the loading effect in plasma etching. Despite the downside of needing a cryostat, it is shown that—when selecting proper conditions—a cryogenic two-step pulsed mode can be used as a successful technique to achieve high speed and selective plasma etching with an etch rate around 25 µm min-1 (<1% silicon load) with nearly vertical walls and resist etch selectivity beyond 1000. With the model in hand, it can be predicted that the etch rate can be doubled (50 µm min-1 at an efficiency of 33% for the fluorine generation from the SF6 feed gas) by minimizing the time the free radicals need to pass the diffusion zone. It is anticipated that this residence time can be reduced sufficiently by a proper inductive coupled plasma (ICP) source design (e.g. plasma shower head and concentrator). In order to preserve the correct profile at such high etch rates, the pressure during the bottom removal step should be minimized and, therefore, the synchronized three-step pulsed mode is believed to be essential to reach such high etch rates with sufficient profile control. In order to improve the etch rate even further, the ICP power should be enhanced; the upgrading of the turbopump seems not yet to be relevant because the throttle valve in the current study had to be used to restrict the turbo efficiency. In order to have a versatile list of state-of-the-art references, it has been decided to arrange it in subjects. The categories concerning plasma physics and applications are, for example, books, reviews, general topics, fluorine-based plasmas, plasma mixtures with oxygen at room temperature, wafer heat transfer and high aspect ratio trench (HART) etching. For readers 'new' to this field, it is advisable to study at least one (but rather more than one) of the reviews concerning plasma as found in the first 30 references. In many cases, a paper can be classified into more than one category. In such cases, the paper is directed to the subject most suited for the discussion of the current review. For example, many papers on heat transfer also treat cryogenic conditions and all the references dealing with highly anisotropic behaviour have been directed to the category HARTs. Additional pointers could get around this problem but have the disadvantage of creating a kind of written spaghetti. I hope that the adapted organization structure will help to have a quick look at and understanding of current developments in high aspect ratio plasma etching. Enjoy reading... Henri Jansen 18 June 2008

The processing of enriched germanium for the Majorana Demonstrator and R&D for a next generation double-beta decay experiment

DOE PAGES

Abgrall, N.; Arnquist, I. J.; Avignone III, F. T.; ...

2017-10-07

The Majorana Demonstrator is an array of point-contact Ge detectors fabricated from Ge isotopically enriched to 88% in 76Ge to search for neutrinoless double beta decay. The processing of Ge for germanium detectors is a well-known technology. However, because of the high cost of Ge enriched in 76Ge special procedures were required to maximize the yield of detector mass and to minimize exposure to cosmic rays. These procedures include careful accounting for the material; shielding it to reduce cosmogenic generation of radioactive isotopes; and development of special reprocessing techniques for contaminated solid germanium, shavings, grindings, acid etchant and cutting fluidsmore » from detector fabrication. Processing procedures were developed that resulted in a total yield in detector mass of 70%. However, none of the acid-etch solution and only 50% of the cutting fluids from detector fabrication were reprocessed. Had they been processed, the projections for the recovery yield would be between 80% and 85%. Maximizing yield is critical to justify a possible future ton-scale experiment. A process for recovery of germanium from the acid-etch solution was developed with yield of about 90%. All material was shielded or stored underground whenever possible to minimize the formation of 68Ge by cosmic rays, which contributes background in the double-beta decay region of interest and cannot be removed by zone refinement and crystal growth. Formation of 68Ge was reduced by a significant factor over that in natural abundance detectors not protected from cosmic rays.« less

Enamel Thickness before and after Orthodontic Treatment Analysed in Optical Coherence Tomography

PubMed Central

Koprowski, Robert; Safranow, Krzysztof; Woźniak, Krzysztof

2017-01-01

Despite the continuous development of materials and techniques of adhesive bonding, the basic procedure remains relatively constant. The technique is based on three components: etching substance, adhesive system, and composite material. The use of etchants during bonding orthodontic brackets carries the risk of damage to the enamel. Therefore, the article examines the effect of the manner of enamel etching on its thickness before and after orthodontic treatment. The study was carried out in vitro on a group of 80 teeth. It was divided into two subgroups of 40 teeth each. The procedure of enamel etching was performed under laboratory conditions. In the first subgroup, the classic method of enamel etching and the fifth-generation bonding system were used. In the second subgroup, the seventh-generation (self-etching) bonding system was used. In both groups, metal orthodontic brackets were fixed and the enamel was cleaned with a cutter fixed on the micromotor after their removal. Before and after the treatment, two-dimensional optical coherence tomography scans were performed. The enamel thickness was assessed on the two-dimensional scans. The average enamel thickness in both subgroups was not statistically significant. PMID:28243604

Photocatalytic Active Bismuth Fluoride/Oxyfluoride Surface Crystallized 2Bi2O3-B2O3 Glass-Ceramics

NASA Astrophysics Data System (ADS)

Sharma, Sumeet Kumar; Singh, V. P.; Chauhan, Vishal S.; Kushwaha, H. S.; Vaish, Rahul

2018-03-01

The present article deals with 2Bi2O3-B2O3 (BBO) glass whose photocatalytic activity has been enhanced by the method of wet etching using an aqueous solution of hydrofluoric acid (HF). X-ray diffraction of the samples reveals that etching with an aqueous solution of HF leads to the formation of BiF3 and BiO0.1F2.8 phases. Surface morphology obtained from scanning electron microscopy show granular and plate-like morphology on the etched glass samples. Rhodamine 6G (Rh 6G) has been used to investigate the photocatalytic activity of the as-quenched and etched glasses. Enhanced visible light-driven photocatalytic activity was observed in HF etched glass-ceramics compared to the as-quenched BBO glass. Contact angle of the as-quenched glass was 90.2°, which decreases up to 20.02° with an increase in concentration of HF in the etching solution. Enhanced photocatalytic activity and increase in the hydrophilic nature suggests the efficient treatment of water pollutants by using the prepared surface crystallized glass-ceramics.

Methods of increasing the harshness of texture of old concrete pavements--acid etching.

DOT National Transportation Integrated Search

1975-01-01

Of the four acids tested in the laboratory, the nitric and hydrochloric types were selected for field experiments. These two acids performed about equally well, the choice as to which to use is dictated by price and availability. In the field experim...

Influence of laser structuring of PEEK, PEEK-GF30 and PEEK-CF30 surfaces on the shear bond strength to a resin cement.

PubMed

Henriques, Bruno; Fabris, Douglas; Mesquita-Guimarães, Joana; Sousa, Anne C; Hammes, Nathalia; Souza, Júlio C M; Silva, Filipe S; Fredel, Márcio C

2018-08-01

The aim of this study was to evaluate the influence of a surface conditioning technique using laser ablation and acid etching on PEEK substrate on its bonding strength to a resin cement. Cylindrical specimens of unfilled PEEK, 30% glass fiber reinforced PEEK and 30% carbon fiber reinforced PEEK were separated in four groups according to the following surface treatments: acid etching with H 2 SO 4 , laser ablation with 200 µm holes spaced 400 µm apart (D2E4), laser ablation with 200 µm holes spaced 600 µm apart (D2E6), and laser ablation (D2E4) followed by acid etching. A dual-curing resin cement (Allcem CORE) was then applied to the PEEK surface. Specimens were aged in distilled water at 37 °C for 24 h. Shear bond strength tests were performed to the fracture of the samples. Two-way ANOVA statistical analysis was performed with a significance level of 0.05. Scanning electron microscopy analysis was performed to analyse the conditioned and fracture surfaces. SEM images of the test interfaces showed that the resin cement could not flow in the holes designed by the laser ablation on the PEEK surface. The shear bond strength of PEEK to resin cement was not improved by the surface modification of the PEEK. Also, there was a statistically significant decrease in shear bond strength for unfilled PEEK specimens. On carbon or glass reinforced PEEK, the change was not significant. SEM images of the fracture surfaces revealed that the failure mode was mainly adhesive. Although laser ablation promoted the PEEK surface modification by the formation of retentive holes, the test resin cement could not thoroughly flow on the rough modified surfaces to establish an effective mechanical interlocking. That negatively affected the shear bonding strength of PEEK to the resin cement. Further studies should be carried out to increase the bonding between PEEK and resin cements. Copyright © 2018 Elsevier Ltd. All rights reserved.

Heavily Boron-Doped Silicon Layer for the Fabrication of Nanoscale Thermoelectric Devices

PubMed Central

Liu, Yang; Deng, Lingxiao; Zhang, Mingliang; Zhang, Shuyuan; Ma, Jing; Song, Peishuai; Liu, Qing; Ji, An; Yang, Fuhua; Wang, Xiaodong

2018-01-01

Heavily boron-doped silicon layers and boron etch-stop techniques have been widely used in the fabrication of microelectromechanical systems (MEMS). This paper provides an introduction to the fabrication process of nanoscale silicon thermoelectric devices. Low-dimensional structures such as silicon nanowire (SiNW) have been considered as a promising alternative for thermoelectric applications in order to achieve a higher thermoelectric figure of merit (ZT) than bulk silicon. Here, heavily boron-doped silicon layers and boron etch-stop processes for the fabrication of suspended SiNWs will be discussed in detail, including boron diffusion, electron beam lithography, inductively coupled plasma (ICP) etching and tetramethylammonium hydroxide (TMAH) etch-stop processes. A 7 μm long nanowire structure with a height of 280 nm and a width of 55 nm was achieved, indicating that the proposed technique is useful for nanoscale fabrication. Furthermore, a SiNW thermoelectric device has also been demonstrated, and its performance shows an obvious reduction in thermal conductivity. PMID:29385759

Effect of double-layer application on dentin bond durability of one-step self-etch adhesives.

PubMed

Taschner, M; Kümmerling, M; Lohbauer, U; Breschi, L; Petschelt, A; Frankenberger, R

2014-01-01

The aim of this in vitro study was 1) to analyze the influence of a double-layer application technique of four one-step self-etch adhesive systems on dentin and 2) to determine its effect on the stability of the adhesive interfaces stored under different conditions. Four different one-step self-etch adhesives were selected for the study (iBondSE, Clearfil S(3) Bond, XenoV(+), and Scotchbond Universal). Adhesives were applied according to manufacturers' instructions or with a double-layer application technique (without light curing of the first layer). After bonding, resin-dentin specimens were sectioned for microtensile bond strength testing in accordance with the nontrimming technique and divided into 3 subgroups of storage: a) 24 hours (immediate bond strength, T0), b) six months (T6) in artificial saliva at 37°C, or c) five hours in 10 % NaOCl at room temperature. After storage, specimens were stressed to failure. Fracture mode was assessed under a light microscope. At T0, iBond SE showed a significant increase in microtensile bond strength when the double-application technique was applied. All adhesive systems showed reduced bond strengths after six months of storage in artificial saliva and after storage in 10% NaOCl for five hours; however at T6, iBond SE, Clearfil S(3) Bond, and XenoV(+) showed significantly higher microtensile bond strength results for the double-application technique compared with the single-application technique. Scotchbond Universal showed no difference between single- or double-application, irrespective of the storage conditions. The results of this study show that improvements in bond strength of one-step self-etch adhesives by using the double-application technique are adhesive dependent.

In-Situ Atomic Force Microscope Imaging of Calcite Etch Pit Morphology Changes in Undersaturated and 1-Hydroxyethylidene-1,1-diphosphonic Acid Poisoned Solutions

PubMed Central

Britt, David W.

2012-01-01

Morphology changes in etch pits formed on the (1014) cleavage plane of calcite were induced by varying the ratio of [Ca2+] to [CO32−] in the bulk solution as well as through the addition of the crystal poison 1-hydroxyethylidene-1,1-diphosphonic acid (HEDP). Three distinct morphologies were noted: symmetric rhombic, asymmetric rhombic, and triangular with a rough curved hypotenuse. The latter represents a transient morphology which is only observed during the actual dissolution process, while the former morphologies persist after dissolution is halted. PMID:25125794

Etching process for improving the strength of a laser-machined silicon-based ceramic article

DOEpatents

Copley, Stephen M.; Tao, Hongyi; Todd-Copley, Judith A.

1991-01-01

A process for improving the strength of laser-machined articles formed of a silicon-based ceramic material such as silicon nitride, in which the laser-machined surface is immersed in an etching solution of hydrofluoric acid and nitric acid for a duration sufficient to remove substantially all of a silicon film residue on the surface but insufficient to allow the solution to unduly attack the grain boundaries of the underlying silicon nitride substrate. This effectively removes the silicon film as a source of cracks that otherwise could propagate downwardly into the silicon nitride substrate and significantly reduce its strength.

Etching process for improving the strength of a laser-machined silicon-based ceramic article

DOEpatents

Copley, S.M.; Tao, H.; Todd-Copley, J.A.

1991-06-11

A process is disclosed for improving the strength of laser-machined articles formed of a silicon-based ceramic material such as silicon nitride, in which the laser-machined surface is immersed in an etching solution of hydrofluoric acid and nitric acid for a duration sufficient to remove substantially all of a silicon film residue on the surface but insufficient to allow the solution to unduly attack the grain boundaries of the underlying silicon nitride substrate. This effectively removes the silicon film as a source of cracks that otherwise could propagate downwardly into the silicon nitride substrate and significantly reduce its strength. 1 figure.

Ultrathin Compound Semiconductor on Insulator Layers for High-Performance Nanoscale Transistors

DTIC Science & Technology

2010-11-11

patterned on the sur- face of the source substrate. The InAs layer was then pattern etched into nano- ribbons using a mixture of citric acid (1 g per ml of...Electron. Dev. 55, 547–556 (2008). 27. DeSalvo, G. C., Kaspi, R. & Bozada, C. A. Citric acid etching of GaAs1-xSbx, Al0.5Ga0.5Sb, and InAs for...interfacial layer formed by thermal oxidation and used for surface passivation is clearly evident. LETTER RESEARCH 1 1 N O V E M B E R 2 0 1 0 | V O L

Novel Development of Phosphate Treated Porous Hydroxyapatite.

PubMed

Doi, Kazuya; Abe, Yasuhiko; Kobatake, Reiko; Okazaki, Yohei; Oki, Yoshifumi; Naito, Yoshihito; Prananingrum, Widyasri; Tsuga, Kazuhiro

2017-12-08

Phosphoric acid-etching treatment to the hydroxyapatite (HA) surface can modify the solubility calcium structure. The aim of the present study was to develop phosphate treated porous HA, and the characteristic structures and stimulation abilities of bone formation were evaluated to determine its suitability as a new type of bone graft material. Although the phosphoric acid-etching treatment did not alter the three-dimensional structure, a micrometer-scale rough surface topography was created on the porous HA surface. Compared to porous HA, the porosity of phosphate treated porous HA was slightly higher and the mechanical strength was lower. Two weeks after placement of the cylindrical porous or phosphate treated porous HA in a rabbit femur, newly formed bone was detected in both groups. At the central portion of the bone defect area, substantial bone formation was detected in the phosphate treated porous HA group, with a significantly higher bone formation ratio than detected in the porous HA group. These results indicate that phosphate treated porous HA has a superior surface topography and bone formation abilities in vivo owing to the capacity for both osteoconduction and stimulation abilities of bone formation conferred by phosphoric acid etching.

Novel Development of Phosphate Treated Porous Hydroxyapatite

PubMed Central

Doi, Kazuya; Abe, Yasuhiko; Kobatake, Reiko; Okazaki, Yohei; Oki, Yoshifumi; Naito, Yoshihito; Prananingrum, Widyasri; Tsuga, Kazuhiro

2017-01-01

Phosphoric acid-etching treatment to the hydroxyapatite (HA) surface can modify the solubility calcium structure. The aim of the present study was to develop phosphate treated porous HA, and the characteristic structures and stimulation abilities of bone formation were evaluated to determine its suitability as a new type of bone graft material. Although the phosphoric acid-etching treatment did not alter the three-dimensional structure, a micrometer-scale rough surface topography was created on the porous HA surface. Compared to porous HA, the porosity of phosphate treated porous HA was slightly higher and the mechanical strength was lower. Two weeks after placement of the cylindrical porous or phosphate treated porous HA in a rabbit femur, newly formed bone was detected in both groups. At the central portion of the bone defect area, substantial bone formation was detected in the phosphate treated porous HA group, with a significantly higher bone formation ratio than detected in the porous HA group. These results indicate that phosphate treated porous HA has a superior surface topography and bone formation abilities in vivo owing to the capacity for both osteoconduction and stimulation abilities of bone formation conferred by phosphoric acid etching. PMID:29292788

Effect of post-space treatment on retention of fiber posts in different root regions using two self-etching systems.

PubMed

Zhang, Ling; Huang, Li; Xiong, Yu; Fang, Ming; Chen, Ji-Hua; Ferrari, Marco

2008-06-01

The effect of post-space treatment on the retention of fiber posts in different root regions was evaluated using two self-etching systems. Post spaces were prepared in extracted premolars and then the root canals were subjected to one of the following post-space treatments: (i) water irrigation (control); (ii) etching with 35% phosphoric acid for 30 s; (iii) irrigation with 17% EDTA followed by 5.25% sodium hypochlorite (NaOCl); and (iv) ultrasonic agitation associated with 17% EDTA and 5.25% NaOCl irrigating solutions. The dentin surfaces were examined under scanning electron microscopy (SEM) after different post-space treatments. Fiber posts were then luted in the treated roots using resin cement with either Clearfil SE Bond or Clearfil DC Bond, and the thin-slice push-out test was performed. Scanning electron microscopy showed that all the post-space treatments tested were effective in removal of the smear layer of debris, or sealer/gutta-percha remnants, on the root canal. The apical push-out strength was affected by post-space treatment. Both 35% phosphoric acid etching and ultrasonic agitation in combination with EDTA/NaOCl irrigation improved the apical push-out strength of the fiber post, regardless of the type of self-etching system. A solo irrigation with an EDTA/NaOCl solution resulted in a lower apical push-out strength compared with the other two experimental groups.

Effect of Time and Deposition Method on Quality of Phosphonic Acid Modifier Self-Assembled Monolayers on Indium Zinc Oxide

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

Sang, Lingzi; Knesting, Kristina M.; Bulusu, Anuradha

Phosphonic acid (PA) self-assembled monolayers (SAMs) are utilized at critical interfaces between transparent conductive oxides (TCO) and organic active layers in organic photovoltaic devices (OPVs). The effects of PA deposition method and time on the formation of close-packed, high-quality monolayers is investigated here for SAMs fabricated by solution deposition, micro-contact printing, and spray coating. The solution deposition isotherm for pentafluorinated benzylphosphonic acid (F5BnPA) on indium-doped zinc oxide (IZO) is studied using polarization modulation-infrared reflection-absorption spectroscopy (PM-IRRAS) at room temperature as a model PA/IZO system. Fast surface adsorption occurs within the first min; however, well-oriented high-quality SAMs are reached only aftermore » -48 h, presumably through a continual process of molecular adsorption/desorption and monolayer filling accompanied by molecular reorientation. Two other rapid, soak-free deposition techniques, micro-contact printing and spray coating, are also explored. SAM quality is compared for deposition of phenyl phosphonic acid (PPA), F13-octylphosphonic acid (F13OPA), and pentafluorinated benzyl phosphonic acid (F5BnPA) by solution deposition, micro-contact printing and spray coating using PM-IRRAS. In contrast to micro-contact printing and spray coating techniques, 48-168 h solution deposition at both room temperature and 70 degrees C result in contamination- and surface etch-free close-packed monolayers with good reproducibility. SAMs fabricated by micro-contact printing and spray coating are much less well ordered.« less

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 Different Composite Restorations on the Cuspal Deflection of Premolars Restored with Different Insertion Techniques- An In vitro Study.

PubMed

Singhal, Sakshi; Gurtu, Anuraag; Singhal, Anurag; Bansal, Rashmi; Mohan, Sumit

2017-08-01

This study was conducted to assess the effect of different composite materials on the cuspal deflection of premolars restored with bulk placement of resin composite in comparison to horizontal incremental placement and modified tangential incremental placement. The aim of this study was to evaluate the cuspal deflection caused by different composite materials when different insertion techniques were used. Two different composite materials were used that is Tetric N Ceram (Ivoclar Vivadent marketing, India) and SonicFill TM (Kerr Sybron Dental). Forty standardized Mesio-Occluso-Distal (MOD) preparations were prepared on maxillary first premolars. Each group was divided according to composite insertion technique (n=10), as follows: Group I - bulk insertion using Tetric N Ceram, Group II - Horizontal incremental insertion technique using Tetric N Ceram, Group III- Modified tangential incremental technique using Tetric N Ceram, and Group IV- bulk insertion using SonicFill TM . Preparations were acid-etched, and bonded with adhesive resin to provide micro mechanical attachment before restoration using a uniform etching and bonding protocol in all the groups. All groups received the same total photo-polymerization time. Cuspal deflection was measured during the restorative procedure using customized digital micrometer assembly. One-way ANOVA test was applied for the analysis of significant difference between the groups, p-value less than 0.05 was considered statistically significant. The average cuspal deflections for the different groups were as follows: Group I 0.045±0.018, Group II 0.029±0.009, Group III 0.018±0.005 and Group IV 0.017±0.004. The intergroup comparison revealed statistically significant difference. A measurable amount of cuspal deflection was present in all the four studied groups. In general, bulkfill restoration technique with conventional composite showed significantly highest cusp deflection. There were no significant differences in cuspal deflection among sonicFill TM and modified tangential incremental insertion techniques.

Relationship between enamel bond fatigue durability and surface free-energy characteristics with universal adhesives.

PubMed

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

2018-04-01

The relationship between enamel bond fatigue durability and surface free-energy characteristics with universal adhesives was investigated. The initial shear bond strengths and shear fatigue strengths of five universal adhesives to enamel were determined with and without phosphoric acid pre-etching. The surface free-energy characteristics of adhesive-treated enamel with and without pre-etching were also determined. The initial shear bond strength and shear fatigue strength of universal adhesive to pre-etched enamel were higher than those to ground enamel. The initial shear bond strength and shear fatigue strength of universal adhesive to pre-etched enamel were material dependent, unlike those to ground enamel. The surface free-energy of the solid (γ S ) and the hydrogen-bonding force (γSh) of universal adhesive-treated enamel were different depending on the adhesive, regardless of the presence or absence of pre-etching. The bond fatigue durability of universal adhesives was higher to pre-etched enamel than to ground enamel. In addition, the bond fatigue durability to pre-etched enamel was material dependent, unlike that to ground enamel. The surface free-energy characteristics of universal adhesive-treated enamel were influenced by the adhesive type, regardless of the presence or absence of pre-etching. The surface free-energy characteristics of universal adhesive-treated enamel were related to the results of the bond fatigue durability. © 2018 Eur J Oral Sci.

Bend measurement using an etched fiber incorporating a fiber Bragg grating.

PubMed

Rauf, Abdul; Zhao, Jianlin; Jiang, Biqiang; Jiang, Yajun; Jiang, Wei

2013-01-15

A fiber Bragg grating (FBG) based bend measurement method using an etched fiber is proposed that utilizes the coupling of the core mode to the cladding and radiation modes at the bending region. An etching region of 99 µm diameter that serves as bend sensing head is achieved at 10 mm upstream the FBG through processing in 40% hydrofluoric acid, while the FBG acts as a narrowband reflector to enhance the sensitivity. The power variation curves are obtained for a wide range of bend angles, but the performance is limited due to the presence of the loss peaks. The sensing response is improved by immersing the etching region in a refractive index matching gel. The results are analyzed by using curve fitting formulas and are in good agreement. A large dynamic range of -27° to +27° and sensitivity of 0.43 dBm/deg is achieved, which can be enhanced by reducing the etched diameter.

Process For Patterning Dispenser-Cathode Surfaces

NASA Technical Reports Server (NTRS)

Garner, Charles E.; Deininger, William D.

1989-01-01

Several microfabrication techniques combined into process cutting slots 100 micrometer long and 1 to 5 micrometer wide into tungsten dispenser cathodes for traveling-wave tubes. Patterned photoresist serves as mask for etching underlying aluminum. Chemically-assisted ion-beam etching with chlorine removes exposed parts of aluminum layer. Etching with fluorine or chlorine trifluoride removes tungsten not masked by aluminum layer. Slots enable more-uniform low-work function coating dispensed to electron-emitting surface. Emission of electrons therefore becomes more uniform over cathode surface.

Fabrication of nano-structured super-hydrophobic film on aluminum by controllable immersing method

NASA Astrophysics Data System (ADS)

Wu, Ruomei; Liang, Shuquan; Pan, Anqiang; Yuan, Zhiqing; Tang, Yan; Tan, Xiaoping; Guan, Dikai; Yu, Ya

2012-06-01

Aluminum alloy surface can be etched easily in acid environment, but the microstructure of alloy surface hardly meets the customers' demand. In this work, a facile acidic-assistant surface oxidation technique has been employed to form reproducible super-hydrophobic surfaces on aluminum alloy plates. The samples immersed in three different acid solutions at ambient temperatures are studied and the results demonstrated that the aqueous mixture solution of oxalic acid and hydrochloric is easier to produce better faces and better stability. Scanning electron microscopy (SEM), X-ray diffraction (XRD), Raman spectrometer, X-ray photoelectron spectroscopy (XPS) and water contact angle measurement are used to investigate the morphologies, microstructures, chemical compositions and hydrophobicity of the produced films on aluminum substrates. The surfaces, configured of a labyrinth structure with convexity and concavity, are in different roughness and gloss because of the different recipe acid solutions used. Better roughness of the surface can be obtained by adjusting the concentration of Clˉ and oxalate ions in acid solutions. The present research work provides a new strategy for the controllable preparation super-hydrophobic films of general materials on aluminum alloy for practical industrial applications.

Facile method for preparing superoleophobic surfaces with hierarchical microcubic/nanowire structures

NASA Astrophysics Data System (ADS)

Kwak, Wonshik; Hwang, Woonbong

2016-02-01

To facilitate the fabrication of superoleophobic surfaces having hierarchical microcubic/nanowire structures (HMNS), even for low surface tension liquids including octane (surface tension = 21.1 mN m-1), and to understand the influences of surface structures on the oleophobicity, we developed a convenient method to achieve superoleophobic surfaces on aluminum substrates using chemical acid etching, anodization and fluorination treatment. The liquid repellency of the structured surface was validated through observable experimental results the contact and sliding angle measurements. The etching condition required to ensure high surface roughness was established, and an optimal anodizing condition was determined, as a critical parameter in building the superoleophobicity. The microcubic structures formed by acid etching are essential for achieving the formation of the hierarchical structure, and therefore, the nanowire structures formed by anodization lead to an enhancement of the superoleophobicity for low surface tension liquids. Under optimized morphology by microcubic/nanowire structures with fluorination treatment, the contact angle over 150° and the sliding angle less than 10° are achieved even for octane.

Mechanical Properties of Mineralized Collagen Fibrils As Influenced By Demineralization

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

Balooch, M.; Habelitz, S.; Kinney, J.H.

2009-05-11

Dentin and bone derive their mechanical properties from a complex arrangement of collagen type-I fibrils reinforced with nanocrystalline apatite mineral in extra- and intrafibrillar compartments. While mechanical properties have been determined for the bulk of the mineralized tissue, information on the mechanics of the individual fibril is limited. Here, atomic force microscopy was used on individual collagen fibrils to study structural and mechanical changes during acid etching. The characteristic 67 nm periodicity of gap zones was not observed on the mineralized fibril, but became apparent and increasingly pronounced with continuous demineralization. AFM-nanoindentation showed a decrease in modulus from 1.5 GPamore » to 50 MPa during acid etching of individual collagen fibrils and revealed that the modulus profile followed the axial periodicity. The nanomechanical data, Raman spectroscopy and SAXS support the hypothesis that intrafibrillar mineral etches at a substantially slower rate than the extrafibrillar mineral. These findings are relevant for understanding the biomechanics and design principles of calcified tissues derived from collagen matrices.« less

Surface modification with alumina blasting and H2SO4-HCl etching for bonding two resin-composite veneers to titanium.

PubMed

Taira, Yohsuke; Egoshi, Takafumi; Kamada, Kohji; Sawase, Takashi

2014-02-01

The purpose of this study was to investigate the effect of an experimental surface treatment with alumina blasting and acid etching on the bond strengths between each of two resin composites and commercially pure titanium. The titanium surface was blasted with alumina and then etched with 45wt% H2SO4 and 15wt% HCl (H2SO4-HCl). A light- and heat-curing resin composite (Estenia) and a light-curing resin composite (Ceramage) were used with adjunctive metal primers. Veneered specimens were subjected to thermal cycling between 4 and 60°C for 50,000 cycles, and the shear bond strengths were determined. The highest bond strengths were obtained for Blasting/H2SO4-HCl/Estenia (30.2 ± 4.5 MPa) and Blasting/Etching/Ceramage (26.0 ± 4.5 MPa), the values of which were not statistically different, followed by Blasting/No etching/Estenia (20.4 ± 2.4 MPa) and Blasting/No etching/Ceramage (0.8 ± 0.3 MPa). Scanning electron microscopy observations revealed that alumina blasting and H2SO4-HCl etching creates a number of micro- and nanoscale cavities on the titanium surface, which contribute to adhesive bonding. © 2013 Eur J Oral Sci.

Effect of a functional monomer (MDP) on the enamel bond durability of single-step self-etch adhesives.

PubMed

Tsuchiya, Kenji; Takamizawa, Toshiki; Barkmeier, Wayne W; Tsubota, Keishi; Tsujimoto, Akimasa; Berry, Thomas P; Erickson, Robert L; Latta, Mark A; Miyazaki, Masashi

2016-02-01

The present study aimed to determine the effect of the functional monomer, 10-methacryloxydecyl dihydrogen phosphate (MDP), on the enamel bond durability of single-step self-etch adhesives through integrating fatigue testing and long-term water storage. An MDP-containing self-etch adhesive, Clearfil Bond SE ONE (SE), and an experimental adhesive, MDP-free (MF), which comprised the same ingredients as SE apart from MDP, were used. Shear bond strength (SBS) and shear fatigue strength (SFS) were measured with or without phosphoric acid pre-etching. The specimens were stored in distilled water for 24 h, 6 months, or 1 yr. Although similar SBS and SFS values were obtained for SE with pre-etching and for MF after 24 h of storage in distilled water, SE with pre-etching showed higher SBS and SFS values than MF after storage in water for 6 months or 1 yr. Regardless of the pre-etching procedure, SE showed higher SBS and SFS values after 6 months of storage in distilled water than after 24 h or 1 yr. To conclude, MDP might play an important role in enhancing not only bond strength but also bond durability with respect to repeated subcritical loading after long-term water storage. © 2015 Eur J Oral Sci.

Reaction rates of graphite with ozone measured by etch decoration

NASA Technical Reports Server (NTRS)

Hennig, G. R.; Montet, G. L.

1968-01-01

Etch-decoration technique of detecting vacancies in graphite has been used to determine the reaction rates of graphite with ozone in the directions parallel and perpendicular to the layer planes. It consists essentially of peeling single atom layers off graphite crystals without affecting the remainder of the crystal.

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

Banerjee, D.; Sankaranarayanan, S.; Khachariya, D.

We demonstrate a method for nanowire formation by natural selection during wet anisotropic chemical etching in boiling phosphoric acid. Nanowires of sub-10 nm lateral dimensions and lengths of 700 nm or more are naturally formed during the wet etching due to the convergence of the nearby crystallographic hexagonal etch pits. These nanowires are site controlled when formed in augmentation with dry etching. Temperature and power dependent photoluminescence characterizations confirm excitonic transitions up to room temperature. The exciton confinement is enhanced by using two-dimensional confinement whereby enforcing greater overlap of the electron-hole wave-functions. The surviving nanowires have less defects and a small temperaturemore » variation of the output electroluminescent light. We have observed superluminescent behaviour of the light emitting diodes formed on these nanowires. There is no observable efficiency roll off for current densities up to 400 A/cm{sup 2}.« less

Total elemental composition analysis of soil samples using the PIXE technique

NASA Astrophysics Data System (ADS)

Bolormaa, Oyuntsetseg; Baasansuren, Jamsranjav; Kawasaki, Katsunori; Watanabe, Makiko; Hattroi, Toshiyuki

2007-09-01

The determination of major and trace element contents in soils was developed by acid digestion method combined with particle-induced X-ray emission spectrometry (PIXE). The digestion of soils was achieved by using nitric acid (HNO3), hydrochloric acid HCl and hydrogen peroxide (H2O2) with repeated additions. A 20 μL aliquot from the digested samples was evaporated on the Nuclepore Track-Etch Membrane and irradiated by the 2.5 MeV proton beam from the single-end type Van de Graaff accelerator. The accuracy of this methodology was estimated based on series of measurements done for a reference material of soil CRM 023-050. The proposed experimental procedure was shown to have good reproducibility of the experimental results. The corresponding limits of detection (LODs) for Na, Mg, Al, P, S, Cl, K, Cr, Mn, Fe, Ni, Cu, Zn, As, Sr, Mo and Cd were estimated. Other soil characteristics such as total carbon (TC) and nitrogen (TN) content, pH and electrical conductivity (EC) were also measured.

Controllable Fabrication of Non-Close-Packed Colloidal Nanoparticle Arrays by Ion Beam Etching

NASA Astrophysics Data System (ADS)

Yang, Jie; Zhang, Mingling; Lan, Xu; Weng, Xiaokang; Shu, Qijiang; Wang, Rongfei; Qiu, Feng; Wang, Chong; Yang, Yu

2018-06-01

Polystyrene (PS) nanoparticle films with non-close-packed arrays were prepared by using ion beam etching technology. The effects of etching time, beam current, and voltage on the size reduction of PS particles were well investigated. A slow etching rate, about 9.2 nm/min, is obtained for the nanospheres with the diameter of 100 nm. The rate does not maintain constant with increasing the etching time. This may result from the thermal energy accumulated gradually in a long-time bombardment of ion beam. The etching rate increases nonlinearly with the increase of beam current, while it increases firstly then reach its saturation with the increase of beam voltage. The diameter of PS nanoparticles can be controlled in the range from 34 to 88 nm. Based on the non-close-packed arrays of PS nanoparticles, the ordered silicon (Si) nanopillars with their average diameter of 54 nm are fabricated by employing metal-assisted chemical etching technique. Our results pave an effective way to fabricate the ordered nanostructures with the size less than 100 nm.

Self-terminated etching of GaN with a high selectivity over AlGaN under inductively coupled Cl2/N2/O2 plasma with a low-energy ion bombardment

NASA Astrophysics Data System (ADS)

Zhong, Yaozong; Zhou, Yu; Gao, Hongwei; Dai, Shujun; He, Junlei; Feng, Meixin; Sun, Qian; Zhang, Jijun; Zhao, Yanfei; DingSun, An; Yang, Hui

2017-10-01

Etching of GaN/AlGaN heterostructure by O-containing inductively coupled Cl2/N2 plasma with a low-energy ion bombardment can be self-terminated at the surface of the AlGaN layer. The estimated etching rates of GaN and AlGaN were 42 and 0.6 nm/min, respectively, giving a selective etching ratio of 70:1. To study the mechanism of the etching self-termination, detailed characterization and analyses were carried out, including X-ray photoelectron spectroscopy (XPS) and time-of-flight secondary ion mass spectroscopy (TOF-SIMS). It was found that in the presence of oxygen, the top surface of the AlGaN layer was converted into a thin film of (Al,Ga)Ox with a high bonding energy, which effectively prevented the underlying atoms from a further etching, resulting in a nearly self-terminated etching. This technique enables a uniform and reproducible fabrication process for enhancement-mode high electron mobility transistors with a p-GaN gate.

CoPt/TiN films nanopatterned by RF plasma etching towards dot-patterned magnetic media

NASA Astrophysics Data System (ADS)

Szívós, János; Pothorszky, Szilárd; Soltys, Jan; Serényi, Miklós; An, Hongyu; Gao, Tenghua; Deák, András; Shi, Ji; Sáfrán, György

2018-03-01

CoPt thin films as possible candidates for Bit Patterned magnetic Media (BPM) were prepared and investigated by electron microscopy techniques and magnetic measurements. The structure and morphology of the Direct Current (DC) sputtered films with N incorporation were revealed in both as-prepared and annealed state. Nanopatterning of the samples was carried out by means of Radio Frequency (RF) plasma etching through a Langmuir-Blodgett film of silica nanospheres that is a fast and high throughput technique. As a result, the samples with hexagonally arranged 100 nm size separated dots of fct-phase CoPt were obtained. The influence of the order of nanopatterning and anneling on the nanostructure formation was revealed. The magnetic properties of the nanopatterned fct CoPt films were investigated by Vibrating Sample Magnetometer (VSM) and Magnetic Force Microscopy (MFM). The results show that CoPt thin film nanopatterned by means of the RF plasma etching technique is promising candidate to a possible realization of BPM. Furthermore, this technique is versatile and suitable for scaling up to technological and industrial applications.

Comparison of shear bond strength of universal adhesives on etched and nonetched enamel.

PubMed

Beltrami, Riccardo; Chiesa, Marco; Scribante, Andrea; Allegretti, Jessica; Poggio, Claudio

2016-04-06

The purpose of this study was to evaluate the effect of surface pretreatment with 37% phosphoric acid on the enamel bond strength of different universal adhesives. One hundred and sixty bovine permanent mandibular incisors freshly extracted were used as a substitute for human teeth. The materials tested in this study included 6 universal adhesives, and 2 self-etch adhesives as control. The teeth were assigned into 2 groups: In the first group, etching was performed using 37% phosphoric acid for 30 seconds. In the second group, no pretreatment agent was applied. After adhesive application, a nanohybrid composite resin was inserted into the enamel surface by packing the material into cylindrical-shaped plastic matrices. After storing, the specimens were placed in a universal testing machine. The normality of the data was calculated using the Kolmogorov-Smirnov test. Analysis of variance (ANOVA) was applied to determine whether significant differences in debond strength values existed among the various groups. Groups with phosphoric acid pretreatment showed significantly higher shear bond strength values than groups with no enamel pretreatment (p<0.001). No significant variation in shear strength values was detected when comparing the different adhesive systems applied onto enamel after orthophosphoric acid application (p>0.05). All adhesives provide similar bond strength values when enamel pretreatment is applied even if compositions are different. Bond strength values are lower than promised by manufacturers.

The effect of different chemical agents on human enamel: an atomic force and scanning electron microscopy study

NASA Astrophysics Data System (ADS)

Rominu, Roxana O.; Rominu, Mihai; Negrutiu, Meda Lavinia; Sinescu, Cosmin; Pop, Daniela; Petrescu, Emanuela

2010-12-01

PURPOSE: The goal of our study was to investigate the changes in enamel surface roughess induced by the application of different chemical substances by atomic force microscopy and scanning electron microscopy. METHOD: Five sound human first upper premolar teeth were chosen for the study. The buccal surface of each tooth was treated with a different chemical agent as follows: Sample 1 - 38% phosphoric acid etching (30s) , sample 2 - no surface treatment (control sample), 3 - bleaching with 37.5 % hydrogen peroxide (according to the manufacturer's instructions), 4 - conditioning with a self-etching primer (15 s), 5 - 9.6 % hydrofluoric acid etching (30s). All samples were investigated by atomic force microscopy in a non-contact mode and by scanning electron microscopy. Several images were obtained for each sample, showing evident differences regarding enamel surface morphology. The mean surface roughness and the mean square roughness were calculated and compared. RESULTS: All chemical substances led to an increased surface roughness. Phosphoric acid led to the highest roughness while the control sample showed the lowest. Hydrofluoric acid also led to an increase in surface roughness but its effects have yet to be investigated due to its potential toxicity. CONCLUSIONS: By treating the human enamel with the above mentioned chemical compounds a negative microretentive surface is obtained, with a morphology depending on the applied substance.

A survey of some metallographic etching reagents for restoration of obliterated engraved marks on aluminium-silicon alloy surfaces.

PubMed

Uli, Norjaidi; Kuppuswamy, R; Amran, Mohd Firdaus Che

2011-05-20

A brief survey to assess the sensitivity and efficacy of some common etching reagents for revealing obliterated engraved marks on Al-Si alloy surfaces is presented. Experimental observations have recommended use of alternate swabbing of 10% NaOH and 10% HNO(3) on the obliterated surfaces for obtaining the desired results. The NaOH etchant responsible for bringing back the original marks resulted in the deposition of some dark coating that has masked the recovered marks. The coating had been well removed by dissolving it in HNO(3) containing 10-20% acid. However, the above etching procedure was not effective on aluminium (99% purity) and Al-Zn-Mg-Cu alloy surfaces. Also the two reagents (i) immersion in 10% aq. phosphoric acid and (ii) alternate swabbing of 60% HCl and 40% NaOH suggested earlier for high strength Al-Zn-Mg-Cu alloys [23] were quite ineffective on Al-Si alloys. Thus different aluminium alloys needed different etching treatments for successfully restoring the obliterated marks. Al-Si alloys used in casting find wide applications especially in the manufacture of engine blocks of motor vehicles. Hence, the results presented in this paper are of much relevance in serial number restoration problems involving this alloy. Copyright © 2010 Elsevier Ireland Ltd. All rights reserved.

Ceramic Surface Treatment with a Single-component Primer: Resin Adhesion to Glass Ceramics.

PubMed

Prado, Mayara; Prochnow, Catina; Marchionatti, Ana Maria Estivalete; Baldissara, Paolo; Valandro, Luiz Felipe; Wandscher, Vinicius Felipe

2018-04-19

To evaluate the microshear bond strength (μSBS) of composite cement bonded to two machined glass ceramics and its durability, comparing conventional surface conditioning (hydrofluoric acid + silane) to a one-step primer (Monobond Etch & Prime). Machined slices of lithium disilicate ceramic (LDC) (IPS e.max CAD) and feldspathic ceramic (FC) (VITA Mark II) glass ceramics were divided into two groups (n = 10) according to two factors: 1. surface treatment: HF+S (ca 5% hydrofluoric acid [IPS Ceramic Etching GEL] + silane coupling agent [SIL; Monobond Plus]) or MEP (single-component ceramic conditioner; Monobond Etch & Prime); 2. storage condition: baseline (without aging; tested 24 h after cementing) or aged (70 days of water storage + 12,000 thermal cycles). Composite cement (Multilink Automix, Ivoclar Vivadent) was applied to starch matrices on the treated ceramic surfaces and photoactivated. A μSBS test was performed (0.5 mm/min) and the failure pattern was determined. Contact angle and micromorphological analyses were also performed. Data were analyzed with Student's t-test (α = 5%). For both ceramic materials, HF+S resulted in higher mean μSBS (MPa) at baseline (LDC: HF+S 21.2 ± 2.2 > MEP 10.4 ± 2.4; FC: HF+S 19.6 ± 4.3 > MEP 13.5 ± 5.4) and after aging (LDC: HF+S 14.64 ± 2.31 > MEP 9 ± 3.4; FC HF+S: 14.73 ± 3.33 > MEP 11.1 ± 3.3). HF+S resulted in a statistically significant decrease in mean μSBS after aging (p = 0.0001), while MEP yielded no significant reduction. The main failure type was adhesive between composite cement and ceramic. HF+S resuted in the lowest contact angle. Hydrofluoric acid + silane resulted in higher mean μSBS than Monobond Etch & Prime for both ceramics; however, Monobond Etch & Prime had stable bonding after aging.

Overview of several applications of chemical downstream etching (CDE) for IC manufacturing: advantages and drawbacks versus WET processes

NASA Astrophysics Data System (ADS)

de Buttet, Côme; Prevost, Emilie; Campo, Alain; Garnier, Philippe; Zoll, Stephane; Vallier, Laurent; Cunge, Gilles; Maury, Patrick; Massin, Thomas; Chhun, Sonarith

2017-03-01

Today the IC manufacturing faces lots of problematics linked to the continuous down scaling of printed structures. Some of those issues are related to wet processing, which are often used in the IC manufacturing flow for wafer cleaning, material etching and surface preparation. In the current work we summarize the limitations for the next nodes of wet processing such as metallic contaminations, wafer charging, corrosion and pattern collapse. As a replacement, we promoted the isotropic chemical dry etching (CDE) which is supposed to fix all the above drawbacks. Etching steps of SI3N4 layers were evaluated in order to prove the interest of such technique.

Gray scale x-ray mask

DOEpatents

Morales, Alfredo M [Livermore, CA; Gonzales, Marcela [Seattle, WA

2006-03-07

The present invention describes a method for fabricating an embossing tool or an x-ray mask tool, providing microstructures that smoothly vary in height from point-to-point in etched substrates, i.e., structure which can vary in all three dimensions. The process uses a lithographic technique to transfer an image pattern in the surface of a silicon wafer by exposing and developing the resist and then etching the silicon substrate. Importantly, the photoresist is variably exposed so that when developed some of the resist layer remains. The remaining undeveloped resist acts as an etchant barrier to the reactive plasma used to etch the silicon substrate and therefore provides the ability etch structures of variable depths.

Longevity of Self-etch Dentin Bonding Adhesives Compared to Etch-and-rinse Dentin Bonding Adhesives: A Systematic Review.

PubMed

Masarwa, Nader; Mohamed, Ahmed; Abou-Rabii, Iyad; Abu Zaghlan, Rawan; Steier, Liviu

2016-06-01

A systematic review and meta-analysis were performed to compare longevity of Self-Etch Dentin Bonding Adhesives to Etch-and-Rinse Dentin Bonding Adhesives. The following databases were searched for PubMed, MEDLINE, Web of Science, CINAHL, the Cochrane Library complemented by a manual search of the Journal of Adhesive Dentistry. The MESH keywords used were: "etch and rinse," "total etch," "self-etch," "dentin bonding agent," "bond durability," and "bond degradation." Included were in-vitro experimental studies performed on human dental tissues of sound tooth structure origin. The examined Self-Etch Bonds were of two subtypes; Two Steps and One Step Self-Etch Bonds, while Etch-and-Rinse Bonds were of two subtypes; Two Steps and Three Steps. The included studies measured micro tensile bond strength (μTBs) to evaluate bond strength and possible longevity of both types of dental adhesives at different times. The selected studies depended on water storage as the aging technique. Statistical analysis was performed for outcome measurements compared at 24 h, 3 months, 6 months and 12 months of water storage. After 24 hours (p-value = 0.051), 3 months (p-value = 0.756), 6 months (p-value=0.267), 12 months (p-value=0.785) of water storage self-etch adhesives showed lower μTBs when compared to the etch-and-rinse adhesives, but the comparisons were statistically insignificant. In this study, longevity of Dentin Bonds was related to the measured μTBs. Although Etch-and-Rinse bonds showed higher values at all times, the meta-analysis found no difference in longevity of the two types of bonds at the examined aging times. Copyright © 2016 Elsevier Inc. All rights reserved.

Reinforcement of dentin in self-etch adhesive technology: a new concept.

PubMed

Waidyasekera, Kanchana; Nikaido, Toru; Weerasinghe, Dinesh S; Ichinose, Shizuko; Tagami, Junji

2009-08-01

Characterize the ultramorphology and secondary caries inhibition potential of different dentin adhesive systems in order to find a satisfactory explanation resist to recurrent caries. Human premolar dentin was treated with one of the two self-etching adhesive systems, Clearfil SE Bond, Clearfil Protect Bond or an acid-etching adhesive system, Single Bond. The bonded interface was exposed to an artificial demineralizing solution (pH 4.5) for 90 min and then 5% sodium hypochlorite for 20 min. Transmission electron microscopic observation was performed at the adhesive-dentin interface. The width of the reinforced zone was measured and data were analyzed with univariate analysis of variance under general linear model. In order to identify type of crystallites in the reinforced zone selected area electron diffraction was performed. An acid-base resistant zone (ABRZ) was found adjacent to the hybrid layer in the outer lesion front with only Clearfil SE Bond and Clearfil Protect Bond, while Single Bond was devoid of this protective zone. Crystallite arrangement and the ultramorphology were almost similar in the corresponding regions of Clearfil SE Bond and Clearfil Protect Bond. However, thickness of the ABRZ at the mid portion was 1159(+/-41.91)nm in Clearfil protect Bond, which was significantly thicker than that of Clearfil SE Bond (F=514.84, p<0.001). Selected area electron diffraction confirmed the crystallites in the zone as apatite. The self-etching adhesive systems created a new reinforced acid resistant dentin under the hybrid layer. Difference in the thickness of the zone expressed a different potential for demineralization inhibition.

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

Donnelly, Vincent M.; Kornblit, Avinoam

The field of plasma etching is reviewed. Plasma etching, a revolutionary extension of the technique of physical sputtering, was introduced to integrated circuit manufacturing as early as the mid 1960s and more widely in the early 1970s, in an effort to reduce liquid waste disposal in manufacturing and achieve selectivities that were difficult to obtain with wet chemistry. Quickly, the ability to anisotropically etch silicon, aluminum, and silicon dioxide in plasmas became the breakthrough that allowed the features in integrated circuits to continue to shrink over the next 40 years. Some of this early history is reviewed, and a discussionmore » of the evolution in plasma reactor design is included. Some basic principles related to plasma etching such as evaporation rates and Langmuir–Hinshelwood adsorption are introduced. Etching mechanisms of selected materials, silicon, silicon dioxide, and low dielectric-constant materials are discussed in detail. A detailed treatment is presented of applications in current silicon integrated circuit fabrication. Finally, some predictions are offered for future needs and advances in plasma etching for silicon and nonsilicon-based devices.« less

Defect-selective dry etching for quick and easy probing of hexagonal boron nitride domains.

PubMed

Wu, Qinke; Lee, Joohyun; Park, Sangwoo; Woo, Hwi Je; Lee, Sungjoo; Song, Young Jae

2018-03-23

In this study, we demonstrate a new method to selectively etch the point defects or the boundaries of as-grown hexagonal boron nitride (hBN) films and flakes in situ on copper substrates using hydrogen and argon gases. The initial quality of the chemical vapor deposition-grown hBN films and flakes was confirmed by UV-vis absorption spectroscopy, atomic force microscopy, and transmission electron microscopy. Different gas flow ratios of Ar/H 2 were then employed to etch the same quality of samples and it was found that etching with hydrogen starts from the point defects and grows epitaxially, which helps in confirming crystalline orientations. However, etching with argon is sensitive to line defects (boundaries) and helps in visualizing the domain size. Finally, based on this defect-selective dry etching technique, it could be visualized that the domains of a polycrystalline hBN monolayer merged together with many parts, even with those that grew from a single nucleation seed.

Defect-selective dry etching for quick and easy probing of hexagonal boron nitride domains

NASA Astrophysics Data System (ADS)

Wu, Qinke; Lee, Joohyun; Park, Sangwoo; Woo, Hwi Je; Lee, Sungjoo; Song, Young Jae

2018-03-01

In this study, we demonstrate a new method to selectively etch the point defects or the boundaries of as-grown hexagonal boron nitride (hBN) films and flakes in situ on copper substrates using hydrogen and argon gases. The initial quality of the chemical vapor deposition-grown hBN films and flakes was confirmed by UV-vis absorption spectroscopy, atomic force microscopy, and transmission electron microscopy. Different gas flow ratios of Ar/H2 were then employed to etch the same quality of samples and it was found that etching with hydrogen starts from the point defects and grows epitaxially, which helps in confirming crystalline orientations. However, etching with argon is sensitive to line defects (boundaries) and helps in visualizing the domain size. Finally, based on this defect-selective dry etching technique, it could be visualized that the domains of a polycrystalline hBN monolayer merged together with many parts, even with those that grew from a single nucleation seed.

Impact of Parameter Variation in Fabrication of Nanostructure by Atomic Force Microscopy Nanolithography

PubMed Central

Dehzangi, Arash; Larki, Farhad; Hutagalung, Sabar D.; Goodarz Naseri, Mahmood; Majlis, Burhanuddin Y.; Navasery, Manizheh; Hamid, Norihan Abdul; Noor, Mimiwaty Mohd

2013-01-01

In this letter, we investigate the fabrication of Silicon nanostructure patterned on lightly doped (1015 cm−3) p-type silicon-on-insulator by atomic force microscope nanolithography technique. The local anodic oxidation followed by two wet etching steps, potassium hydroxide etching for silicon removal and hydrofluoric etching for oxide removal, are implemented to reach the structures. The impact of contributing parameters in oxidation such as tip materials, applying voltage on the tip, relative humidity and exposure time are studied. The effect of the etchant concentration (10% to 30% wt) of potassium hydroxide and its mixture with isopropyl alcohol (10%vol. IPA ) at different temperatures on silicon surface are expressed. For different KOH concentrations, the effect of etching with the IPA admixture and the effect of the immersing time in the etching process on the structure are investigated. The etching processes are accurately optimized by 30%wt. KOH +10%vol. IPA in appropriate time, temperature, and humidity. PMID:23776479

Effect of oxygen plasma etching on pore size-controlled 3D polycaprolactone scaffolds for enhancing the early new bone formation in rabbit calvaria.

PubMed

Kook, Min-Suk; Roh, Hee-Sang; Kim, Byung-Hoon

2018-05-02

This study was to investigate the effects of O 2 plasma-etching of the 3D polycaprolactone (PCL) scaffold surface on preosteoblast cell proliferation and differentiation, and early new bone formation. The PCL scaffolds were fabricated by 3D printing technique. After O 2 plasma treatment, surface characterizations were examined by scanning electron microscopy, atomic force microscopy, and contact angle. MTT assay was used to determine cell proliferation. To investigate the early new bone formation, rabbits were sacrificed at 2 weeks for histological analyses. As the O 2 plasma etching time is increased, roughness and hydrophilicity of the PCL scaffold surface increased. The cell proliferation and differentiation on plasma-etched samples was significantly increased than on untreated samples. At 2 weeks, early new bone formation in O 2 plasma-etched PCL scaffolds was the higher than that of untreated scaffolds. The O 2 plasma-etched PCL scaffolds showed increased preosteoblast differentiation as well as increased new bone formation.

Micro/nano hierarchical structured titanium treated by NH4OH/H2O2 for enhancing cell response

PubMed Central

Yuan, Xin; Kang, Yi; Zuo, Jun; Xie, Youneng; Ma, Li; Ren, Xuelei; Bian, Zeyu; Zhou, Kechao; Wang, Xiyang; Yu, Zhiming

2018-01-01

In this paper, two kinds of titanium surfaces with novel micro/nano hierarchical structures, namely Etched (E) surface and Sandblast and etched (SE) surface, were successfully fabricated by NH4OH and H2O2 mixture. And their cellular responses of MG63 were investigated compared with Sandblast and acid-etching (SLA) surface. Scanning electron microscope (SEM), Surface profiler, X-ray photoelectron spectroscopy (XPS), and Contact angle instrument were employed to assess the surface morphologies, roughness, chemistry and wettability respectively. Hierarchical structures with micro holes of 10–30 μm in diameter and nano pits of tens of nanometers in diameter formed on both E and SE surfaces. The size of micro holes is very close to osteoblast cell, which makes them wonderful beds for osteoblast. Moreover, these two kinds of surfaces possess similar roughness and superior hydrophilicity to SLA. Reactive oxygen species were detected on E and SE surface, and thus considerable antimicrobial performance and well fixation can be speculated on them. The cell experiments also demonstrated a boost in cell attachment, and that proliferation and osteogenic differentiation were achieved on them, especially on SE surface. The results indicate that the treatment of pure titanium with H2O2/NH4OH is an effective technique to improve the initial stability of implants and enhance the osseointegration, which may be a promising surface treatment to titanium implant. PMID:29723214

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.

Design and grayscale fabrication of beamfanners in a silicon substrate

NASA Astrophysics Data System (ADS)

Ellis, Arthur Cecil

2001-11-01

This dissertation addresses important first steps in the development of a grayscale fabrication process for multiple phase diffractive optical elements (DOS's) in silicon. Specifically, this process was developed through the design, fabrication, and testing of 1-2 and 1-4 beamfanner arrays for 5-micron illumination. The 1-2 beamfanner arrays serve as a test-of- concept and basic developmental step toward the construction of the 1-4 beamfanners. The beamfanners are 50 microns wide, and have features with dimensions of between 2 and 10 microns. The Iterative Annular Spectrum Approach (IASA) method, developed by Steve Mellin of UAH, and the Boundary Element Method (BEM) are the design and testing tools used to create the beamfanner profiles and predict their performance. Fabrication of the beamfanners required the techniques of grayscale photolithography and reactive ion etching (RIE). A 2-3micron feature size 1-4 silicon beamfanner array was fabricated, but the small features and contact photolithographic techniques available prevented its construction to specifications. A second and more successful attempt was made in which both 1-4 and 1-2 beamfanner arrays were fabricated with a 5-micron minimum feature size. Photolithography for the UAH array was contracted to MEMS-Optical of Huntsville, Alabama. A repeatability study was performed, using statistical techniques, of 14 photoresist arrays and the subsequent RIE process used to etch the arrays in silicon. The variance in selectivity between the 14 processes was far greater than the variance between the individual etched features within each process. Specifically, the ratio of the variance of the selectivities averaged over each of the 14 etch processes to the variance of individual feature selectivities within the processes yielded a significance level below 0.1% by F-test, indicating that good etch-to-etch process repeatability was not attained. One of the 14 arrays had feature etch-depths close enough to design specifications for optical testing, but 5- micron IR illumination of the 1-4 and 1-2 beamfanners yielded no convincing results of beam splitting in the detector plane 340 microns from the surface of the beamfanner array.

Synthesis and Visible-Light Photocatalytic Activity of CeO₂ Nanoboxes Based on Pearson’s Principle.

PubMed

Ge, Shengsong; Bao, Liwei; Shao, Qian; Zhang, Qiaoxia; Liu, Zingyun

2017-01-01

The CeO₂ nanoboxes with well-defined hollow structure were fabricated by template-engaged coordinating etching of Cu₂O cubes based on Pearson’s hard and soft acid-base principle. The morphologically uniform CeO₂ nanoboxes have an average edge length of 400 nm and shell thickness of around 60 nm. The strong chemical affinity between Cu+ and S₂O(2− 3) was the driving force for the etching of Cu₂O templates and the formation of shells. A possible formation mechanism of CeO₂ nanoboxes was proposed. The synthesized CeO₂ nanoboxes exhibit good photocatalytic activity for photodegradation of acid orange 7 (AO 7) under visible light irradiation.

In-cell overlay metrology by using optical metrology tool

NASA Astrophysics Data System (ADS)

Lee, Honggoo; Han, Sangjun; Hong, Minhyung; Kim, Seungyoung; Lee, Jieun; Lee, DongYoung; Oh, Eungryong; Choi, Ahlin; Park, Hyowon; Liang, Waley; Choi, DongSub; Kim, Nakyoon; Lee, Jeongpyo; Pandev, Stilian; Jeon, Sanghuck; Robinson, John C.

2018-03-01

Overlay is one of the most critical process control steps of semiconductor manufacturing technology. A typical advanced scheme includes an overlay feedback loop based on after litho optical imaging overlay metrology on scribeline targets. The after litho control loop typically involves high frequency sampling: every lot or nearly every lot. An after etch overlay metrology step is often included, at a lower sampling frequency, in order to characterize and compensate for bias. The after etch metrology step often involves CD-SEM metrology, in this case in-cell and ondevice. This work explores an alternative approach using spectroscopic ellipsometry (SE) metrology and a machine learning analysis technique. Advanced 1x nm DRAM wafers were prepared, including both nominal (POR) wafers with mean overlay offsets, as well as DOE wafers with intentional across wafer overlay modulation. After litho metrology was measured using optical imaging metrology, as well as after etch metrology using both SE and CD-SEM for comparison. We investigate 2 types of machine learning techniques with SE data: model-less and model-based, showing excellent performance for after etch in-cell on-device overlay metrology.

Etching radical controlled gas chopped deep reactive ion etching

DOEpatents

Olynick, Deidre; Rangelow, Ivo; Chao, Weilun

2013-10-01

A method for silicon micromachining techniques based on high aspect ratio reactive ion etching with gas chopping has been developed capable of producing essentially scallop-free, smooth, sidewall surfaces. The method uses precisely controlled, alternated (or chopped) gas flow of the etching and deposition gas precursors to produce a controllable sidewall passivation capable of high anisotropy. The dynamic control of sidewall passivation is achieved by carefully controlling fluorine radical presence with moderator gasses, such as CH.sub.4 and controlling the passivation rate and stoichiometry using a CF.sub.2 source. In this manner, sidewall polymer deposition thicknesses are very well controlled, reducing sidewall ripples to very small levels. By combining inductively coupled plasmas with controlled fluorocarbon chemistry, good control of vertical structures with very low sidewall roughness may be produced. Results show silicon features with an aspect ratio of 20:1 for 10 nm features with applicability to nano-applications in the sub-50 nm regime. By comparison, previous traditional gas chopping techniques have produced rippled or scalloped sidewalls in a range of 50 to 100 nm roughness.

Response of murine bone marrow-derived mesenchymal stromal cells to dry-etched porous silicon scaffolds.

PubMed

Hajj-Hassan, Mohamad; Khayyat-Kholghi, Maedeh; Wang, Huifen; Chodavarapu, Vamsy; Henderson, Janet E

2011-11-01

Porous silicon shows great promise as a bio-interface material due to its large surface to volume ratio, its stability in aqueous solutions and to the ability to precisely regulate its pore characteristics. In the current study, porous silicon scaffolds were fabricated from single crystalline silicon wafers by a novel xenon difluoride dry etching technique. This simplified dry etch fabrication process allows selective formation of porous silicon using a standard photoresist as mask material and eliminates the post-formation drying step typically required for the wet etching techniques, thereby reducing the risk of damaging the newly formed porous silicon. The porous silicon scaffolds supported the growth of primary cultures of bone marrow derived mesenchymal stromal cells (MSC) plated at high density for up to 21 days in culture with no significant loss of viability, assessed using Alamar Blue. Scanning electron micrographs confirmed a dense lawn of cells at 9 days of culture and the presence of MSC within the pores of the porous silicon scaffolds. Copyright © 2011 Wiley Periodicals, Inc.

Determination by Small-angle X-ray Scattering of Pore Size Distribution in Nanoporous Track-etched Polycarbonate Membranes

NASA Astrophysics Data System (ADS)

Jonas, A. M.; Legras, R.; Ferain, E.

1998-03-01

Nanoporous track-etched membranes with narrow pore size distributions and average pore size diameters tunable from 100 to 1000 Åare produced by the chemical etching of latent tracks in polymer films after irradiation by a beam of accelerated heavy ions. Nanoporous membranes are used for highly demanding filtration purposes, or as templates to obtain metallic or polymeric nanowires (L. Piraux et al., Nucl. Instr. Meth. Phys. Res. 1997, B131, 357). Such applications call for developments in nanopore size characterization techniques. In this respect, we report on the characterization by small-angle X-ray scattering (SAXS) of nanopore size distribution (nPSD) in polycarbonate track-etched membranes. The obtention of nPSD requires inverting an ill-conditioned inhomogeneous equation. We present different numerical routes to overcome the amplification of experimental errors in the resulting solutions, including a regularization technique allowing to obtain the nPSD without a priori knowledge of its shape. The effect of deviations from cylindrical pore shape on the resulting distributions are analyzed. Finally, SAXS results are compared to results obtained by electron microscopy and conductometry.

Comparison of separation performance of laser-ablated and wet-etched microfluidic devices

PubMed Central

Baker, Christopher A.; Bulloch, Rayford; Roper, Michael G.

2010-01-01

Laser ablation of glass allows for production of microfluidic devices without the need of hydrofluoric acid and photolithography. The goal of this study was to compare the separation performance of microfluidic devices produced using a low-cost laser ablation system and conventional wet etching. During laser ablation, cracking of the glass substrate was prevented by heating the glass to 300°C. A range of laser energy densities was found to produce channel depths ranging from 4 – 35 μm and channel widths from 118 – 162 μm. The electroosmotic flow velocity was lower in laser-ablated devices, 0.110 ± 0.005 cm s−1, as compared to wet-etched microfluidic chips, 0.126 ± 0.003 cm s−1. Separations of both small and large molecules performed on both wet- and laser-ablated devices were compared by examining limits of detection, theoretical plate count, and peak asymmetry. Laser-induced fluorescence detection limits were 10 pM fluorescein for both types of devices. Laser-ablated and wet-etched microfluidic chips had reproducible migration times with ≤ 2.8% RSD and peak asymmetries ranging from 1.0 – 1.8. Numbers of theoretical plates were between 2.8- and 6.2-fold higher on the wet-etched devices compared to laser-ablated devices. Nevertheless, resolution between small and large analytes was accomplished, which indicates that laser ablation may find an application in pedagogical studies of electrophoresis or microfluidic devices, or in settings where hydrofluoric acid cannot be used. PMID:20827468

Compact Submillimeter-Wave Receivers Made with Semiconductor Nano-Fabrication Technologies

NASA Technical Reports Server (NTRS)

Jung, C.; Thomas, B.; Lee, C.; Peralta, A.; Chattopadhyay, G.; Gill, J.; Cooper, K.; Mehdi, I.

2011-01-01

Advanced semiconductor nanofabrication techniques are utilized to design, fabricate and demonstrate a super-compact, low-mass (<10 grams) submillimeter-wave heterodyne front-end. RF elements such as waveguides and channels are fabricated in a silicon wafer substrate using deep-reactive ion etching (DRIE). Etched patterns with sidewalls angles controlled with 1 deg precision are reported, while maintaining a surface roughness of better than 20 nm rms for the etched structures. This approach is being developed to build compact 2-D imaging arrays in the THz frequency range.

Etching twin core fiber for the temperature-independent refractive index sensing

NASA Astrophysics Data System (ADS)

Zhang, Chuanbiao; Ning, Tigang; Li, Jing; Zheng, Jingjing; Gao, Xuekai; Lin, Heng; Pei, Li

2018-04-01

We proposed an ultra-compact chemically etched twin core fiber (TCF) based optic refractive index (RI) sensor, in which the etched fiber was fabricated by immersing in an aqueous solution of hydrofluoric acid (HF) to etch the cladding. Due to the multipath evolutions of light during the TCF, the mode induced interference pattern can be used for measurement. Numerical simulations were performed, demonstrating that only the cladding mode strongly interacts with the surrounding media, and the higher cladding modes will be more sensitive to external medium. In the experiment demonstration, the RI response characteristics of the sensor were investigated, which shows a relatively high RI sensitivity and a much low temperature cross-sensitivity with about 1.06 × 10-6 RIU °C-1. Due to low cost and easy fabrication, the sensor can be a suitable candidate in the biochemical field.

Advanced Mitigation Process (AMP) for Improving Laser Damage Threshold of Fused Silica Optics

NASA Astrophysics Data System (ADS)

Ye, Xin; Huang, Jin; Liu, Hongjie; Geng, Feng; Sun, Laixi; Jiang, Xiaodong; Wu, Weidong; Qiao, Liang; Zu, Xiaotao; Zheng, Wanguo

2016-08-01

The laser damage precursors in subsurface of fused silica (e.g. photosensitive impurities, scratches and redeposited silica compounds) were mitigated by mineral acid leaching and HF etching with multi-frequency ultrasonic agitation, respectively. The comparison of scratches morphology after static etching and high-frequency ultrasonic agitation etching was devoted in our case. And comparison of laser induce damage resistance of scratched and non-scratched fused silica surfaces after HF etching with high-frequency ultrasonic agitation were also investigated in this study. The global laser induce damage resistance was increased significantly after the laser damage precursors were mitigated in this case. The redeposition of reaction produce was avoided by involving multi-frequency ultrasonic and chemical leaching process. These methods made the increase of laser damage threshold more stable. In addition, there is no scratch related damage initiations found on the samples which were treated by Advanced Mitigation Process.

Study on the formation of dodecagonal pyramid on nitrogen polar GaN surface etched by hot H3PO4

NASA Astrophysics Data System (ADS)

Qi, S. L.; Chen, Z. Z.; Fang, H.; Sun, Y. J.; Sang, L. W.; Yang, X. L.; Zhao, L. B.; Tian, P. F.; Deng, J. J.; Tao, Y. B.; Yu, T. J.; Qin, Z. X.; Zhang, G. Y.

2009-08-01

Hot phosphor acid (H3PO4) etching is presented to form a roughened surface with dodecagonal pyramids on laser lift-off N face GaN grown by metalorganic chemical vapor deposition. A detailed analysis of time evolution of surface morphology is described as a function of etching temperature. The activation energy of the H3PO4 etching process is 1.25 eV, indicating the process is reaction-limited scheme. And it is found that the oblique angle between the facets and the base plane increases as the temperature increases. Thermodynamics and kinetics related factors of the formation mechanism of the dodecagonal pyramid are also discussed. The light output power of a vertical injection light-emitting-diode (LED) with proper roughened surface shows about 2.5 fold increase compared with that of LED without roughened surface.

Advanced Mitigation Process (AMP) for Improving Laser Damage Threshold of Fused Silica Optics

PubMed Central

Ye, Xin; Huang, Jin; Liu, Hongjie; Geng, Feng; Sun, Laixi; Jiang, Xiaodong; Wu, Weidong; Qiao, Liang; Zu, Xiaotao; Zheng, Wanguo

2016-01-01

The laser damage precursors in subsurface of fused silica (e.g. photosensitive impurities, scratches and redeposited silica compounds) were mitigated by mineral acid leaching and HF etching with multi-frequency ultrasonic agitation, respectively. The comparison of scratches morphology after static etching and high-frequency ultrasonic agitation etching was devoted in our case. And comparison of laser induce damage resistance of scratched and non-scratched fused silica surfaces after HF etching with high-frequency ultrasonic agitation were also investigated in this study. The global laser induce damage resistance was increased significantly after the laser damage precursors were mitigated in this case. The redeposition of reaction produce was avoided by involving multi-frequency ultrasonic and chemical leaching process. These methods made the increase of laser damage threshold more stable. In addition, there is no scratch related damage initiations found on the samples which were treated by Advanced Mitigation Process. PMID:27484188

Integration of Electrodeposited Ni-Fe in MEMS with Low-Temperature Deposition and Etch Processes

PubMed Central

Schiavone, Giuseppe; Murray, Jeremy; Perry, Richard; Mount, Andrew R.; Desmulliez, Marc P. Y.; Walton, Anthony J.

2017-01-01

This article presents a set of low-temperature deposition and etching processes for the integration of electrochemically deposited Ni-Fe alloys in complex magnetic microelectromechanical systems, as Ni-Fe is known to suffer from detrimental stress development when subjected to excessive thermal loads. A selective etch process is reported which enables the copper seed layer used for electrodeposition to be removed while preserving the integrity of Ni-Fe. In addition, a low temperature deposition and surface micromachining process is presented in which silicon dioxide and silicon nitride are used, respectively, as sacrificial material and structural dielectric. The sacrificial layer can be patterned and removed by wet buffered oxide etch or vapour HF etching. The reported methods limit the thermal budget and minimise the stress development in Ni-Fe. This combination of techniques represents an advance towards the reliable integration of Ni-Fe components in complex surface micromachined magnetic MEMS. PMID:28772683

On particle track detectors

NASA Technical Reports Server (NTRS)

Benton, E. V.; Gruhn, T. A.; Andrus, C. H.

1973-01-01

Aqueous sodium hydroxide is widely used to develop charged particle tracks in polycarbonate film, particularly Lexan. The chemical nature of the etching process for this system has been determined. A method employing ultra-violet absorbance was developed for monitoring the concentration of the etch products in solution. Using this method it was possible to study the formation of the etching solution saturated in etch products. It was found that the system super-saturates to a significant extent before precipitation occurs. It was also learned that the system approaches its equilibrium state rather slowly. It is felt that both these phenomena may be due to the presence of surfactant in the solution. In light of these findings, suggestions are given regarding the preparation and maintenance of the saturated etch solution. Two additional research projects, involving automated techniques for particle track analysis and particle identification using AgCl crystals, are briefly summarized.

Metal catalyst technique for texturing silicon solar cells

DOEpatents

Ruby, Douglas S.; Zaidi, Saleem H.

2001-01-01

Textured silicon solar cells and techniques for their manufacture utilizing metal sources to catalyze formation of randomly distributed surface features such as nanoscale pyramidal and columnar structures. These structures include dimensions smaller than the wavelength of incident light, thereby resulting in a highly effective anti-reflective surface. According to the invention, metal sources present in a reactive ion etching chamber permit impurities (e.g. metal particles) to be introduced into a reactive ion etch plasma resulting in deposition of micro-masks on the surface of a substrate to be etched. Separate embodiments are disclosed including one in which the metal source includes one or more metal-coated substrates strategically positioned relative to the surface to be textured, and another in which the walls of the reaction chamber are pre-conditioned with a thin coating of metal catalyst material.

Decalin-assisted light emitting porous Si formation and its optical, surface and morphological properties

NASA Astrophysics Data System (ADS)

Karatutlu, Ali; Istengir, Sumeyra; Cosgun, Sedat; Seker, Isa; Unal, Bayram

2017-11-01

In this research paper, light emitting porous silicon (Lep-Si) samples were fabricated by a surfactant-mediated chemical stain etching solution in order to form homogenous luminescent nanostructures at room temperature. As an industrially important solvent, decalin (decahydronaphtalene) was used as a surfactant in the HF/HNO3 solutions in order to control the etching process. Morphological, surface and optical properties of the Lep-Si samples were examined using atomic force microscopy, X-ray photoelectron spectroscopy, photoluminescence (PL) spectroscopy, and laser scanning confocal microscopy (LSCM) techniques. These characterization techniques were correlated with the various etching times including depth dependent luminescence profiles for the first time. We report the optimum conditions for production of the most efficient Lep-Si using decalin (decahydronaphtalene) and possible structural origins of light emission using the depth dependent luminescence measurements.

Instrument performance of a radon measuring system with the alpha-track detection technique.

PubMed

Tokonami, S; Zhuo, W; Ryuo, H; Yonehara, H; Yamada, Y; Shimo, M

2003-01-01

An instrument performance test has been carried out for a radon measuring system made in Hungary. The system measures radon using the alpha-track detection technique. It consists of three parts: the passive detector, the etching unit and the evaluation unit. A CR-39 detector is used as the radiation detector. Alpha-track reading and data analysis are carried out after chemical etching. The following subjects were examined in the present study: (1) radon sensitivity, (2) performance of etching and evaluation processes and (3) thoron sensitivity. The radon sensitivity of 6.9 x 10(-4) mm(-2) (Bq m(-3) d)(-1) was acceptable for practical application. The thoron sensitivity was estimated to be as low as 3.3 x 10(-5) mm(-2) (Bq m(-3) d)(-1) from the experimental study.

Dual-hole Photonic Crystal Fiber Intermodal Interference based Refractometer

NASA Astrophysics Data System (ADS)

Liu, Feng; Guo, Xuan; Zhang, Qing; Fu, Xinghu

2017-12-01

A refractive-index (RI) sensor and its sensing characteristics based on intermodal interference of dual-hole Polarization Maintaining Photonic Crystal Fiber (PM-PCF) are demonstrated in this letter. The sensor works from the interference between LP01 and LP11 modes of hydrofluoric acid etched PM-PCF. The influence of corrosion zone radius on the RI sensing sensitivity is also discussed. Via choosing a 2.5 cm etched PM-PCF(the etched area radius is 27.5 μm) and 650 nm laser, the sensor exhibits the RI sensitivity of 7.48 V/RIU. The simple sensor structure and inexpensive demodulation method can make this technology for online refractive index measurement in widespread areas.

Improved bonding of adhesive resin to sintered porcelain with the combination of acid etching and a two-liquid silane conditioner.

PubMed

Kato, H; Matsumura, H; Ide, T; Atsuta, M

2001-01-01

This study determined the bond strengths of adhesive resins joined to a feldspathic porcelain (VMK 68) for the purpose of developing the most durable surface preparation for the porcelain. Three porcelain surfaces-ground, air-abraded with alumina, and etched with hydrofluoric acid-were prepared. A two-liquid porcelain conditioner that contained both 4-methacryloyloxyethyl trimellitate anhydride (4-META) and a silane coupler (Porcelain Liner M) was used as the priming agent. Each of the two liquid components of the conditioner was also used individually in order to examine the effects of the respective chemical ingredients on adhesive bonding. Two methyl methacrylate (MMA)-based resins initiated with tri-n-butylborane (TBB) either with or without 4-META (MMA-TBB and 4-META/MMA-TBB resins) were used as the luting agents. Shear bond strengths were determined both before and after thermocycling. Shear testing results indicated that thermocycling was effective for disclosing poor bonding systems, and that both mechanical and chemical retention were indispensable for bonding the porcelain. Of the combinations assessed, etching with hydrofluoric acid followed by two-liquid priming with the Porcelain Liner M material generated the most durable bond strength (33.3 MPa) for the porcelain bonded with the 4-META/MMA-TBB resin (Super-Bond C&B).

Nanometer Scale Titanium Surface Texturing Are Detected by Signaling Pathways Involving Transient FAK and Src Activations

PubMed Central

Zambuzzi, Willian F.; Bonfante, Estevam A.; Jimbo, Ryo; Hayashi, Mariko; Andersson, Martin; Alves, Gutemberg; Takamori, Esther R.; Beltrão, Paulo J.; Coelho, Paulo G.; Granjeiro, José M.

2014-01-01

Background It is known that physico/chemical alterations on biomaterial surfaces have the capability to modulate cellular behavior, affecting early tissue repair. Such surface modifications are aimed to improve early healing response and, clinically, offer the possibility to shorten the time from implant placement to functional loading. Since FAK and Src are intracellular proteins able to predict the quality of osteoblast adhesion, this study evaluated the osteoblast behavior in response to nanometer scale titanium surface texturing by monitoring FAK and Src phosphorylations. Methodology Four engineered titanium surfaces were used for the study: machined (M), dual acid-etched (DAA), resorbable media microblasted and acid-etched (MBAA), and acid-etch microblasted (AAMB). Surfaces were characterized by scanning electron microscopy, interferometry, atomic force microscopy, x-ray photoelectron spectroscopy and energy dispersive X-ray spectroscopy. Thereafter, those 4 samples were used to evaluate their cytotoxicity and interference on FAK and Src phosphorylations. Both Src and FAK were investigated by using specific antibody against specific phosphorylation sites. Principal Findings The results showed that both FAK and Src activations were differently modulated as a function of titanium surfaces physico/chemical configuration and protein adsorption. Conclusions It can be suggested that signaling pathways involving both FAK and Src could provide biomarkers to predict osteoblast adhesion onto different surfaces. PMID:24999733

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

Self-formation of a nanonet of fluorinated carbon nanowires on the Si surface by combined etching in fluorine-containing plasma

NASA Astrophysics Data System (ADS)

Amirov, I. I.; Gorlachev, E. S.; Mazaletskiy, L. A.; Izyumov, M. O.; Alov, N. V.

2018-03-01

In this work, we report a technique of the self-formation of a nanonet of fluorinated carbon nanowires on the Si surface using a combined etching in fluorine-containing C4F8/Ar and SF6 plasmas. Using scanning electron microscopy, atomic force microscopy and x-ray photoelectron spectroscopy, we show that after the etching of Si in the C4F8/Ar plasma, a fluorinated carbon film of nanometer-scale thickness is formed on its surface and its formation accelerates at elevated temperatures. After a subsequent short-term etching in the SF6 plasma, the film is modified into a nanonet of self-formed fluorinated carbon nanowires.

Behavior of GaSb (100) and InSb (100) surfaces in the presence of H2O2 in acidic and basic cleaning solutions

NASA Astrophysics Data System (ADS)

Seo, Dongwan; Na, Jihoon; Lee, Seunghyo; Lim, Sangwoo

2017-03-01

Gallium antimonide (GaSb) and indium antimonide (InSb) have attracted strong attention as new channel materials for transistors due to their excellent electrical properties and lattice matches with various group III-V compound semiconductors. In this study, the surface behavior of GaSb (100) and InSb (100) was investigated and compared in hydrochloric acid/hydrogen peroxide mixture (HPM) and ammonium hydroxide/hydrogen peroxide mixture (APM) solutions. In the acidic HPM solution, surface oxidation was greater and the etching rates of the GaSb and InSb surfaces increased when the solution is concentrated, which indicates that H2O2 plays a key role in the surface oxidation of GaSb and InSb in acidic HPM solution. However, the GaSb and InSb surfaces were hardly oxidized in basic APM solution in the presence of H2O2 because gallium and indium are in the thermodynamically stable forms of H2GaO3- and InO2-, respectively. When the APM solution was diluted, however, the Ga on the GaSb surface was oxidized by H2O, increasing the etching rate. However, the effect of dilution of the APM solution on the oxidation of the InSb surface was minimal; thus, the InSb surface was less oxidized than the GaSb surface and the change in the etching rate of InSb with dilution of the APM solution was not significant. Additionally, the oxidation behavior of gallium and indium was more sensitive to the composition of the HPM and APM solutions than that of antimony. Therefore, the surface properties and etching characteristics of GaSb and InSb in HPM and APM solutions are mainly dependent on the behavior of the group III elements rather than the group V elements.

Bio-inspired silicon nanospikes fabricated by metal-assisted chemical etching for antibacterial surfaces

NASA Astrophysics Data System (ADS)

Hu, Huan; Siu, Vince S.; Gifford, Stacey M.; Kim, Sungcheol; Lu, Minhua; Meyer, Pablo; Stolovitzky, Gustavo A.

2017-12-01

The recently discovered bactericidal properties of nanostructures on wings of insects such as cicadas and dragonflies have inspired the development of similar nanostructured surfaces for antibacterial applications. Since most antibacterial applications require nanostructures covering a considerable amount of area, a practical fabrication method needs to be cost-effective and scalable. However, most reported nanofabrication methods require either expensive equipment or a high temperature process, limiting cost efficiency and scalability. Here, we report a simple, fast, low-cost, and scalable antibacterial surface nanofabrication methodology. Our method is based on metal-assisted chemical etching that only requires etching a single crystal silicon substrate in a mixture of silver nitrate and hydrofluoric acid for several minutes. We experimentally studied the effects of etching time on the morphology of the silicon nanospikes and the bactericidal properties of the resulting surface. We discovered that 6 minutes of etching results in a surface containing silicon nanospikes with optimal geometry. The bactericidal properties of the silicon nanospikes were supported by bacterial plating results, fluorescence images, and scanning electron microscopy images.

Principles and applications of laser-induced liquid-phase jet-chemical etching

NASA Astrophysics Data System (ADS)

Stephen, Andreas; Metev, Simeon; Vollertsen, Frank

2003-11-01

In this treatment method laser radiation, which is guided from a coaxially expanding liquid jet-stream, locally initiates a thermochemical etching reaction on a metal surface, which leads to selective material removal at high resolution and quality of the treated surface as well as low thermal influence on the workpiece. Electrochemical investigations were performed under focused laser irradiation using a cw-Nd:YAG laser with a maximum power of 15 W and a simultaneous impact of the liquid jet-stream consisting of phosphoric acid with a maximum flow rate of 20 m/s. The time resolved measurements of the electrical potential difference against an electrochemical reference electrode were correlated with the specific processing parameters and corresponding etch rates to identify processing conditions for temporally stable and enhanced chemical etching reactions. Applications of laser-induced liquid-phase jet-chemical etching in the field of sensor technology, micromechanics and micrmoulding technology are presented. This includes the microstructuring of thin film systems, cutting of foils of shape memory alloys or the generation of structures with defined shape in bulk material.

New Deep Reactive Ion Etching Process Developed for the Microfabrication of Silicon Carbide

NASA Technical Reports Server (NTRS)

Evans, Laura J.; Beheim, Glenn M.

2005-01-01

Silicon carbide (SiC) is a promising material for harsh environment sensors and electronics because it can enable such devices to withstand high temperatures and corrosive environments. Microfabrication techniques have been studied extensively in an effort to obtain the same flexibility of machining SiC that is possible for the fabrication of silicon devices. Bulk micromachining using deep reactive ion etching (DRIE) is attractive because it allows the fabrication of microstructures with high aspect ratios (etch depth divided by lateral feature size) in single-crystal or polycrystalline wafers. Previously, the Sensors and Electronics Branch of the NASA Glenn Research Center developed a DRIE process for SiC using the etchant gases sulfur hexafluoride (SF6) and argon (Ar). This process provides an adequate etch rate of 0.2 m/min and yields a smooth surface at the etch bottom. However, the etch sidewalls are rougher than desired, as shown in the preceding photomicrograph. Furthermore, the resulting structures have sides that slope inwards, rather than being precisely vertical. A new DRIE process for SiC was developed at Glenn that produces smooth, vertical sidewalls, while maintaining an adequately high etch rate.

Reduced Noise UV Enhancement of Etch Rates for Nuclear Tracks in CR-39

NASA Astrophysics Data System (ADS)

Sheets, Rebecca; Clarkson, David; Ume, Rubab; Regan, Sean; Sangster, Craig; Padalino, Stephen; McLean, James

2016-10-01

The use of CR-39 plastic as a Solid State Nuclear Track Detector is an effective technique for obtaining data in high-energy particle experiments including inertial confinement fusion. To reveal particle tracks after irradiation, CR-39 is chemically etched in NaOH at 80°C for 6 hours, producing micron-scale signal pits at the nuclear track sites. Using CR-39 irradiated with 5.4 MeV alpha particles and 1.0 MeV protons, we show that exposing the CR-39 to high intensity UV light before etching, with wavelengths between 240 nm and 350 nm, speeds the etch process. Elevated temperatures during UV exposure amplifies this effect, with etch rates up to 50% greater than unprocessed conditions. CR-39 pieces exposed to UV light and heat can also exhibit heightened levels of etch-induced noise (surface features not caused by nuclear particles). By illuminating the CR-39 from the side opposite to the tracks, a similar level of etch enhancement was obtained with little to no noise. The effective wavelength range is reduced, due to strong attenuation of shorter wavelengths. Funded in part by a LLE contract through the DOE.

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.

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 Nd:YAG laser on the solvent evaporation of adhesive systems.

PubMed

Batista, Graziela Ribeiro; Barcellos, Daphne Câmara; Rocha Gomes Torres, Carlos; Damião, Álvaro José; de Oliveira, Hueder Paulo Moisés; de Paiva Gonçalves, Sérgio Eduardo

2015-01-01

This study evaluated the influence of Nd:YAG laser on the evaporation degree (ED) of the solvent components in total-etch and self-etch adhesives. The ED of Gluma Comfort Bond (Heraeus-Kulzer) one-step self-etch adhesive, and Adper Single Bond 2 (3M ESPE), and XP Bond (Dentsply) total-etch adhesives was determined by weight alterations using two techniques: Control--spontaneous evaporation of the solvent for 5 min; Experimental--Nd:YAG laser irradiation for 1 min, followed by spontaneous evaporation for 4 min. The weight loss due to evaporation of the volatile components was measured at baseline and after 10 s, 20 s, 30 s, 40 s, 50 s, 60 s, 70 s, 80 s, 90 s, 100 s, 110 s, 2 min, 3 min, 4 min, and 5 min. Evaporation of solvent components significantly increased with Nd:YAG laser irradiation for all adhesives investigated. Gluma Comfort Bond showed significantly higher evaporation of solvent components than Adper Single Bond 2 and XP Bond. All the adhesives lost weight quickly during the first min of Nd:YAG laser irradiation. The application of Nd:YAG laser on adhesives before light curing had a significant effect on the evaporation of the solvent components, and the ED of Gluma Comfort Bond one-step self-etch adhesive was significantly higher than with Adper Single Bond 2 and XP Bond total-etch adhesives. The use of the Nd:YAG laser on the uncured adhesive technique can promote a greater ED of solvents, optimizing the longevity of the adhesive restorations.

Preparing Al-Mg Substrate for Thermal Spraying: Evaluation of Surface State After Different Pretreatments

NASA Astrophysics Data System (ADS)

Lukauskaitė, R.; Valiulis, A. V.; Černašėjus, O.; Škamat, J.; Rębiś, J. A.

2016-08-01

The article deals with the pretreatment technique for preparing the surface of aluminum alloy EN AW 5754 before thermal spray. The surface after different pretreatments, including degreasing with acetone, chemical etching with acidic and alkali solutions, grit-blasting, cathodic cleaning, and some combinations of these techniques, has been studied. The investigation of pre-treated surfaces covered the topographical study (using scanning electron microscopy, atomic force microscopy, and 3D profilometry), the chemical analysis by x-ray photoelectron spectroscopy, the evaluation of surface wettability (sessile drop method), and the assessment of surface free energy. Compared with all the techniques used in present work, the cathodic cleaning and its combination with grit-blasting provide the most preferable chemistry of the surface. Due to the absence of hydroxides at the surface and, possible, due to the diffusion of magnesium to the surface of substrate, the surface wettability and the surface free energy have been significantly improved. No direct correlation between the surface topography and the surface wettability has been established.

Influence of ultrasound and diamond burs treatments on microtensile bond strength.

PubMed

Conde, Alexandre; Mainieri, Vivian; Mota, Eduardo Goncalves; Oshima, Hugo Mitsuo

2012-01-01

To compare surface treatments with CVDentUS ultrasound tips (UT) and KGSorensen diamond burs (DB) on etched (e) and non-etched (n/e) dentin. The microtensile bond strength (μTBS) was measured and fractography was assessed by scanning electron microscope (SEM). Sixteen molars were divided into four groups of four teeth each according to treatment (DB-n/e; DB-e; UT-n/e; UT-e). The teeth were restored, sectioned into samples for μTBS (n=40) and tested on a EMIC DL-2000 universal machine (0.5 mm/min) and analyzed by SEM for fracture classification. For analysis of the data on μTBS, the two-way ANOVA, using treatment and acid etching as fixed factor, and the Tukey test were used (α=0.05). To failures classification in cohesive in dentin (CD); cohesive in composite resin (CC); cohesive interfacial on base or top of hybrid layer (CBT); cohesive in adhesive (CA); mixed (M); interfacial on smear layer (S) the Fisher's exact test (α=0.05) was performed. The mean values of μTBS (in MPa) in the different groups were as follows: UT-e: 45.31 ± 8.16; DB-e: 34.04 ± 9.29; UT-n/e: 15.17 ± 3.71; and DB-n/e: 9.86 ± 3.80. On analysis of the SEM micrographs, the DB-n/e group showed total obstruction of dentinal tubules; the UT-n/e group showed partial desobstruction of dentinal tubules and irregular surface; the DB-e group showed complete desobstruction of dentinal tubules; and the UT-e group showed complete desobstruction of dentinal tubules and irregular surface. The combination of ultrasound treatment and acid etching provides high values of μTBS. An association exists between CA/CC failures and the UT method, CBT failure and the DB method, CBT/CC failures and etching, S failure and non-etching.

Colorimetric and fluorometric determination of uric acid based on the use of nitrogen-doped carbon quantum dots and silver triangular nanoprisms.

PubMed

Wang, Yanying; Yang, Yan; Liu, Wei; Ding, Fang; Zhao, Qingbiao; Zou, Ping; Wang, Xianxiang; Rao, Hanbing

2018-05-04

A dual-read detection system is described for non-enzymatic and non-aggregation based analysis of uric acid (UA). Silver triangular nanoprisms (AgTNPs) were used as colorimetric probes, while the reduction in the fluorescence of nitrogen-doped carbon quantum dots (N-CQDs) served as the fluorometric readout. The absorption band of the AgTNPs overlaps the emission band of N-CQDs (with a peak at 440 nm). Therefore, fluorescence is reduced owing to an inner filter effect. The AgTNPs are etched if exposed to H 2 O 2 , and round nanodiscs are formed. In the presence of UA, etching of the AgTNPs is suppressed because the facets of the AgTNPs are coated with UA. The absorbance, best measured at 683 nm, increases with the concentration of the pre-added UA. The colorimetric assay works in the 0.1-45 μM UA concentration range, and the fluorometric assay between 1 and 42 μM of UA. The respective detection limits are 50 and 200 nM, respectively. The probe can be used for direct visualization of UA. The method was successfully applied to the determination of UA in urine samples. Graphical abstract The fluorescence of nitrogen-doped carbon quantum dots (N-CQDs) is quenched by AgTNPs (silver triangular nanoprisms). As the AgTNPs are etched by H 2 O 2 , fluorescence recovers in the system after H 2 O 2 is added, and also undergoes a color change. Uric acid (UA) protects the AgTNPs from etching because the facets of the AgTNPs are coated with UA. The fluorescence of N-CQDs decreases. Thus, a dual-read probe is developed for determination of UA.

Method for surface treatment of a cadmium zinc telluride crystal

DOEpatents

James, Ralph; Burger, Arnold; Chen, Kuo-Tong; Chang, Henry

1999-01-01

A method for treatment of the surface of a CdZnTe (CZT) crystal that reduces surface roughness (increases surface planarity) and provides an oxide coating to reduce surface leakage currents and thereby, improve resolution. A two step process is disclosed, etching the surface of a CZT crystal with a solution of lactic acid and bromine in ethylene glycol, following the conventional bromine/methanol etch treatment, and after attachment of electrical contacts, oxidizing the CZT crystal surface.

Comparison of fabrication methods for microstructured deep UV multimode waveguides based on fused silica

NASA Astrophysics Data System (ADS)

Elmlinger, Philipp; Schreivogel, Martin; Schmid, Marc; Kaiser, Myriam; Priester, Roman; Sonström, Patrick; Kneissl, Michael

2016-04-01

The suitability of materials for deep ultraviolet (DUV) waveguides concerning transmittance, fabrication, and coupling properties is investigated and a fused silica core/ambient air cladding waveguide system is presented. This high refractive index contrast system has far better coupling efficiency especially for divergent light sources like LEDs and also a significantly smaller critical bending radius compared to conventional waveguide systems, as simulated by ray-tracing simulations. For the fabrication of 300-ffm-thick multimode waveguides a hydrouoric (HF) acid based wet etch process is compared to selective laser etching (SLE). In order to fabricate thick waveguides out of 300-ffm-thick silica wafers by HF etching, two masking materials, LPCVD silicon nitride and LPCVD poly silicon, are investigated. Due to thermal stress, the silicon nitride deposited wafers show cracks and even break. Using poly silicon as a masking material, no cracks are observed and deep etching in 50 wt% HF acid up to 180 min is performed. While the masked and unmasked silica surface is almost unchanged in terms of roughness, notching defects occur at the remaining polysilicon edge leading to jagged sidewalls. Using SLE, waveguides with high contour accuracy are fabricated and the DUV guiding properties are successfully demonstrated with propagation losses between 0.6 and 0:8 dB=mm. These values are currently limited by sidewall scattering losses.

Cryo-Etched Black Silicon for Use as Optical Black

NASA Technical Reports Server (NTRS)

Yee, Karl Y.; White, Victor E.; Mouroulis, Pantazis; Eastwood, Michael L.

2011-01-01

Stray light reflected from the surface of imaging spectrometer components in particular, the spectrometer slit degrade the image quality. A technique has been developed for rapid, uniform, and cost-effective black silicon formation based on inductively coupled plasma (ICP) etching at cryogenic temperatures. Recent measurements show less than 1-percent total reflectance from 350 2,500 nm of doped black silicon formed in this way, making it an excellent option for texturing of component surfaces for reduction of stray light. Oxygen combines with SF6 + Si etch byproducts to form a passivation layer atop the Si when the etch is performed at cryogenic temperatures. Excess flow of oxygen results in micromasking and the formation of black silicon. The process is repeatable and reliable, and provides control over etch depth and sidewall profile. Density of the needles can be controlled to some extent. Regions to be textured can be patterned lithographically. Adhesion is not an issue as the nanotips are part of the underlying substrate. This is in contrast to surface growth/deposition techniques such as carbon nanotubes (CNTs). The black Si surface is compatible with wet processing, including processing with solvents, the textured surface is completely inorganic, and it does not outgas. In radiometry applications, optical absorbers are often constructed using gold black or CNTs. This black silicon technology is an improvement for these types of applications.

Tuning the thickness of exfoliated quasi-two-dimensional β-Ga2O3 flakes by plasma etching

NASA Astrophysics Data System (ADS)

Kwon, Yongbeom; Lee, Geonyeop; Oh, Sooyeoun; Kim, Jihyun; Pearton, Stephen J.; Ren, Fan

2017-03-01

We demonstrated the thinning of exfoliated quasi-two-dimensional β-Ga2O3 flakes by using a reactive ion etching technique. Mechanical exfoliation of the bulk β-Ga2O3 by using an adhesive tape was followed by plasma etching to tune its thickness. Since β-Ga2O3 is not a van der Waals material, it is challenging to obtain ultra-thin flakes below a thickness of 100 nm. In this study, an etch rate of approximately 16 nm/min was achieved at a power of 200 W with a flow of 50 sccm of SF6, and under these conditions, thinning of β-Ga2O3 flakes from 300 nm down to ˜60 nm was achieved with smooth morphology. We believe that the reaction between SF6 and Ga2O3 results in oxygen and volatile oxygen fluoride compounds, and non-volatile compounds such as GaFX that can be removed by ion bombardment. The opto-electrical properties were also characterized by fabricating solar-blind photodetectors using the plasma-thinned β-Ga2O3 flakes; these detectors showed fast response and decay with excellent responsivity and selectivity. Our results pave the way for tuning the thickness of two-dimensional materials by using this scalable, industry-compatible dry etching technique.

Iodine-Mediated Etching of Gold Nanorods for Plasmonic ELISA Based on Colorimetric Detection of Alkaline Phosphatase.

PubMed

Zhang, Zhiyang; Chen, Zhaopeng; Wang, Shasha; Cheng, Fangbin; Chen, Lingxin

2015-12-23

Here, we propose a plasmonic enzyme-linked immunosorbent assay (ELISA) based on highly sensitive colorimetric detection of alkaline phosphatase (ALP), which is achieved by iodine-mediated etching of gold nanorods (AuNRs). Once the sandwich-type immunocomplex is formed, the ALP bound on the polystyrene microwells will hydrolyze ascorbic acid 2-phosphate into ascorbic acid. Subsequently, iodate is reduced to iodine, a moderate oxidant, which etches AuNRs from rod to sphere in shape. The shape change of AuNRs leads to a blue-shift of longitudinal localized surface plasmon resonance. As a result, the solution of AuNRs changes from blue to red. Benefiting from the highly sensitive detection of ALP, the proposed plasmonic ELISA has achieved an ultralow detection limit (100 pg/mL) for human immunoglobulin G (IgG). Importantly, the visual detection limit (3.0 ng/mL) allows the rapid differential diagnosis with the naked eye. The further detection of human IgG in fetal bovine serum indicates its applicability to the determination of low abundance protein in complex biological samples.

Influence of subsurface defects on damage performance of fused silica in ultraviolet laser

NASA Astrophysics Data System (ADS)

Huang, Jin; Zhou, Xinda; Liu, Hongjie; Wang, Fengrui; Jiang, Xiaodong; Wu, Weidong; Tang, Yongjian; Zheng, Wanguo

2013-02-01

In ultraviolet pulse laser, damage performance of fused silica optics is directly dependent on the absorptive impurities and scratches in subsurface, which are induced by mechanical polishing. In the research about influence of subsurface defects on damage performance, a series of fused silica surfaces with various impurity concentrations and scratch structures were created by hydrofluoric (HF) acid solution etching. Time of Flight secondary ion mass spectrometry and scanning probe microprobe revealed that with increasing etching depth, impurity concentrations in subsurface layers are decreased, the scratch structures become smoother and the diameter:depth ratio is increased. Damage performance test with 355-nm pulse laser showed that when 600 nm subsurface thickness is removed by HF acid etching, laser-induced damage threshold of fused silica is raised by 40 percent and damage density is decreased by over one order of magnitude. Laser weak absorption was tested to explain the cause of impurity elements impacting damage performance, field enhancement caused by change of scratch structures was calculated by finite difference time domain simulation, and the calculated results are in accord with the damage test results.

Method for integrating microelectromechanical devices with electronic circuitry

DOEpatents

Barron, Carole C.; Fleming, James G.; Montague, Stephen

1999-01-01

A method is disclosed for integrating one or more microelectromechanical (MEM) devices with electronic circuitry on a common substrate. The MEM device can be fabricated within a substrate cavity and encapsulated with a sacrificial material. This allows the MEM device to be annealed and the substrate planarized prior to forming electronic circuitry on the substrate using a series of standard processing steps. After fabrication of the electronic circuitry, the electronic circuitry can be protected by a two-ply protection layer of titanium nitride (TiN) and tungsten (W) during an etch release process whereby the MEM device is released for operation by etching away a portion of a sacrificial material (e.g. silicon dioxide or a silicate glass) that encapsulates the MEM device. The etch release process is preferably performed using a mixture of hydrofluoric acid (HF) and hydrochloric acid (HCI) which reduces the time for releasing the MEM device compared to use of a buffered oxide etchant. After release of the MEM device, the TiN:W protection layer can be removed with a peroxide-based etchant without damaging the electronic circuitry.

Anisotropic etching of amorphous perfluoropolymer films in oxygen-based inductively coupled plasmas

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

Ono, Takao; Akagi, Takanori; Center for NanoBio Integration, University of Tokyo, 7-3-1 Hongo, Bunkyo-ku, Tokyo 113-8656

2009-01-01

An amorphous perfluoropolymer, 'Cytop' (Asahi Glass Co., Ltd.), is a preferable material for the fabrication of micro total analysis system devices because of its superior optical transparency over a wide wavelength range and low refractive index of 1.34, which is almost the same as that of water, as well as excellent chemical stability. To establish the precise microfabrication technology for this unique resin, the dry etching of the amorphous perfluoropolymer in Ar/O{sub 2} low-pressure inductively coupled plasma has been studied. A relatively high etch rate of approximately 6.3 {mu}m/min at maximum and highly anisotropic etched features was attained. Plasma measurementsmore » by a single Langmuir probe technique and actinometry revealed that etching is dominated by ion-assisted surface desorption above a 10%O{sub 2} mixing ratio, whereas the supply of active oxygen species is the rate-limiting process below 10%. Moreover, angled x-ray photoelectron spectroscopy measurements of an etched trench pattern revealed that a high anisotropy is attributed to the formation of a carbon-rich sidewall protection layer.« less

Grafted Polystyrene Monolayer Brush as Both Negative and Positive Tone Electron Beam Resist.

PubMed

Aydinoglu, Ferhat; Yamada, Hirotaka; Dey, Ripon K; Cui, Bo

2017-05-23

Although spin coating is the most widely used electron-beam resist coating technique in nanolithography, it cannot typically be applied for nonflat or irregular surfaces. Here, we demonstrate that monolayer polystyrene brush can be grafted on substrates and used as both positive and negative electron-beam resist, which can be applied for such unconventional surfaces. Polystyrene is a popular negative resist when using solvent developer but solvent cannot be used for grafted polystyrene brush that is firmly bonded to the substrate. Instead, we employed two unconventional development methods to lead polystyrene brush to positive or negative tone behavior. Negative tone was achieved by thermal development at 300 °C because exposed thus cross-linked polystyrene brush is more thermally stable against vaporization than unexposed linear one. Surprisingly, positive tone behavior occurred when the brush was grafted onto an aluminum (Al) layer and the film stack was developed using diluted hydrofluoric acid (HF) that etched the underlying Al layer. By transferring the patterns into the silicon (Si) substrates using the thin Al layer as a sacrificial hard mask for dry etch, well-defined structures in Si were obtained in two different electron-beam resist tones as well as in nonflat surfaces.

An Optimization of Electrochemical Etching Conditions for Gold Nanotips Fabrication

NASA Astrophysics Data System (ADS)

Oh, Min Woo; Chong, Haeeun; Park, Doo Jae; Jang, Moonkyu; Bahn, Sebin; Choi, Soo Bong

2018-05-01

We demonstrate a series of experiments to find optimized electrochemical etching condition for fabricating gold nanotip, using square-wave voltage as a bias and using hydrochloric acid diluted by acetone as an etchant. We confirmed that the dilution ratio of 3: 1 between hydrochloric acid and acetone give the smallest tip apex diameter which reproduces our previous result. More importantly, by varying applied bias condition and immersion depth of the platinum ring used as a cathode inside the etchant, we found that the smaller tip apex diameter is achieved when both the amplitude and duty cycle get higher. The success rate, which we define the number of tips having meaningfully less diameter out of total number of tried tips, is also discussed.

Method of fabricating reflection-mode EUV diffraction elements

DOEpatents

Naulleau, Patrick P.

2002-01-01

Techniques for fabricating a well-controlled, quantized-level, engineered surface that serves as substrates for EUV reflection multilayer overcomes problems associated with the fabrication of reflective EUV diffraction elements. The technique when employed to fabricate an EUV diffraction element that includes the steps of: (a) forming an etch stack comprising alternating layers of first and second materials on a substrate surface where the two material can provide relative etch selectivity; (b) creating a relief profile in the etch stack wherein the relief profile has a defined contour; and (c) depositing a multilayer reflection film over the relief profile wherein the film has an outer contour that substantially matches that of the relief profile. For a typical EUV multilayer, if the features on the substrate are larger than 50 nm, the multilayer will be conformal to the substrate. Thus, the phase imparted to the reflected wavefront will closely match that geometrically set by the surface height profile.

Fabrication of Cantilever-Bump Type Si Probe Card

NASA Astrophysics Data System (ADS)

Park, Jeong-Yong; Lee, Dong-Seok; Kim, Dong-Kwon; Lee, Jong-Hyun

2000-12-01

Probe card is most important part in the test system which selects the good or bad chip of integrated circuit (IC) chips. Silicon vertical probe card is able to test multiple semiconductor chips simultaneously. We presented cantilever-bump type vertical probe card. It was fabricated by dry etching using RIE(reactive ion etching) technique and porous silicon micromachining using silicon direct bonded (SDB) wafer. Cantilevers and bumps were fabricated by isotropic etching using RIE@. 3-dimensional structures were formed by porous silicon micromachining technique using SDB wafer. Contact resistance of fabricated probe card was less than 2 Ω and its life time was more than 200,000 turns. The process used in this work is very simple and reproducible, which has good controllability in the tip dimension and spacing. It is expected that the fabricated probe card can reduce testing time, can promote productivity and enables burn-in test.

Evanescent wave assisted nanomaterial coating.

PubMed

Mondal, Samir K; Pal, Sudipta Sarkar; Kumbhakar, Dharmadas; Tiwari, Umesh; Bhatnagar, Randhir

2013-08-01

In this work we present a novel nanomaterial coating technique using evanescent wave (EW). The gradient force in the EW is used as an optical tweezer for tweezing and self-assembling nanoparticles on the source of EW. As a proof of the concept, we have used a laser coupled etched multimode optical fiber, which generates EW for the EW assisted coating. The section-wise etched multimode optical fiber is horizontally and superficially dipped into a silver/gold nanoparticles solution while the laser is switched on. The fiber is left until the solution recedes due to evaporation leaving the fiber in air. The coating time usually takes 40-50 min at room temperature. The scanning electron microscope image shows uniform and thin coating of self-assembled nanoparticles due to EW around the etched section. A coating thickness <200 nm is achieved. The technique could be useful for making surface-plasmon-resonance-based optical fiber probes and other plasmonic circuits.

Effects of self-etching primer on shear bond strength of orthodontic brackets at different debond times.

PubMed

Turk, Tamer; Elekdag-Turk, Selma; Isci, Devrim

2007-01-01

To evaluate the effect of a self-etching primer on shear bond strengths (SBS) at the different debond times of 5, 15, 30, and 60 minutes and 24 hours. Brackets were bonded to human premolars with different etching protocols. In the control group (conventional method [CM]) teeth were etched with 37% phosphoric acid. In the study group, a self-etching primer (SEP; Transbond Plus Self Etching Primer; 3M Unitek, Monrovia, Calif) was applied as recommended by the manufacturer. Brackets were bonded with light-cure adhesive paste (Transbond XT; 3M Unitek) and light-cured for 20 seconds in both groups. The shear bond test was performed at the different debond times of 5, 15, 30 and 60 minutes and 24 hours. Lowest SBS was attained with a debond time of 5 minutes for the CM group (9.51 MPa) and the SEP group (8.97 MPa). Highest SBS was obtained with a debond time of 24 hours for the CM group (16.82 MPa) and the SEP group (19.11 MPa). Statistically significant differences between the two groups were not observed for debond times of 5, 15, 30, or 60 minutes. However, the SBS values obtained at 24 hours were significantly different (P < .001). Adequate SBS was obtained with self-etching primer during the first 60 minutes (5, 15, 30 and 60 minutes) when compared with the conventional method. It is reliable to load the bracket 5 minutes after bonding using self-etching primer (Transbond Plus) with the light-cure adhesive (Transbond XT).

Method of making an ion beam sputter-etched ventricular catheter for hydrocephalus shunt

NASA Technical Reports Server (NTRS)

Banks, B. A. (Inventor)

1984-01-01

The centricular catheter comprises a multiplicity of inlet microtubules. Each microtubule has both a large opening at its inlet end and a multiplicity of microscopic openings along its lateral surfaces. The microtubules are perforated by an ion beam sputter etch technique. The holes are etched in each microtubule by directing an ion beam through an electro formed mesh mask producing perforations having diameters ranging from about 14 microns to about 150 microns. This structure assures a reliable means for shunting cerebrospinal fluid from the cerebral ventricles to selected areas of the body.

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.

Surface pre-treatment of aluminium by cleaning, chemical ething and conversion coating

NASA Astrophysics Data System (ADS)

Zaki, Mohammad Hafizudden Mohd; Mohd, Yusairie; Isa, Nik Norziehana Che

2017-12-01

Surface pre-treatment is one of the critical treatments for surface modification of aluminium (Al). In this study, pre-treatment of Al surface involved three stages; (1) cleaning (polishing and degreasing), (2) chemical etching (alkaline and acid) and (3) conversion coating (ie: zincate treatment). Cleaning process of Al was conducted by polishing and degreasing with acetone while etching process was done by immersion in 1.25 M NaOH solution (i.e: alkaline etching) followed with acid etching using 8 M HNO3 solution. The zincate treatment was conducted via electroless coating method by immersion of Al into a bath solution containing 0.5 M Zn(NO3)2, 0.1 M HNO3 and 0.2 M NaBH4 (reducing agent) for one hour. Different temperatures (ie: 25 °C, 50 °C, 75 °C, 90 °C) of bath solutions at pH 4 were used to investigate the effect of temperature on zincate treatment. Surface morphology and chemical composition of the pre-treated Al were characterized using Field Emission Scanning Electron Microscopy (FESEM) and Energy Dispersion X-ray analysis (EDX), respectively. The results showed that oxide layer on Al surface decreased after chemical etching process. Temperature of zincate solution has significantly affected the conversion coating process of aluminium. It was found that zinc oxide (ZnO) and zinc borate (ZnO.B2O3) were dominantly formed after zincate treatment at high temperature (ie:90 °C) with curved blade-like structure and composition of Zn, B and O with 13.70 wt.%, 3.52 wt.% and 54.39 wt.%, respectively. However, zincate treatment at low temperature (ie:<50 °C) has produced low metallic Zn.

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.

Peri-implant bone formation and surface characteristics of rough surface zirconia implants manufactured by powder injection molding technique in rabbit tibiae.

PubMed

Park, Young-Seok; Chung, Shin-Hye; Shon, Won-Jun

2013-05-01

To evaluate osseointegration in rabbit tibiae and to investigate surface characteristics of novel zirconia implants made by powder injection molding (PIM) technique, using molds with and without roughened inner surfaces. A total of 20 rabbits received three types of external hex implants with identical geometry on the tibiae: machined titanium implants, PIM zirconia implants without mold etching, and PIM zirconia implants with mold etching. Surface characteristics of the three types of implant were evaluated. Removal torque tests and histomorphometric analyses were performed. The roughness of PIM zirconia implants was higher than that of machined titanium implants. The PIM zirconia implants exhibited significantly higher bone-implant contact and removal torque values than the machined titanium implants (P < 0.001). The PIM zirconia implants using roughened mold showed significantly higher removal torque values than PIM zirconia implants without using roughened mold (P < 0.001). It is concluded that the osseointegration of PIM zirconia implant is promising and PIM using roughened mold etching technique can produce substantially rough surfaces on zirconia implants. © 2012 John Wiley & Sons A/S.

Nanoporous Silicon Carbide for Nanoelectromechanical Systems Applications

NASA Technical Reports Server (NTRS)

Hossain, T.; Khan, F.; Adesida, I.; Bohn, P.; Rittenhouse, T.; Lienhard, Michael (Technical Monitor)

2003-01-01

A major goal of this project is to produce porous silicon carbide (PSiC) via an electroless process for eventual utilization in nanoscale sensing platforms. Results in the literature have shown a variety of porous morphologies in SiC produced in anodic cells. Therefore, predictability and reproducibility of porous structures are initial concerns. This work has concentrated on producing morphologies of known porosity, with particular attention paid toward producing the extremely high surface areas required for a porous flow sensor. We have conducted a parametric study of electroless etching conditions and characteristics of the resulting physical nanostructure and also investigated the relationship between morphology and materials properties. Further, we have investigated bulk etching of SiC using both photo-electrochemical etching and inductively-coupled-plasma reactive ion etching techniques.

Plasma etching of superconducting Niobium tips for scanning tunneling microscopy

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

Roychowdhury, A.; Center for Nanophysics and Advanced Materials, Department of Physics, University of Maryland, College Park, Maryland 20742; Dana, R.

We have developed a reproducible technique for the fabrication of sharp superconducting Nb tips for scanning tunneling microscopy (STM) and scanning tunneling spectroscopy. Sections of Nb wire with 250 μm diameter are dry etched in an SF₆ plasma in a Reactive Ion Etcher. The gas pressure, etching time, and applied power are chosen to control the ratio of isotropic to anisotropic etch rates and produce the desired tip shape. The resulting tips are atomically sharp, with radii of less than 100 nm, mechanically stable, and superconducting. They generate good STM images and spectroscopy on single crystal samples of Au(111), Au(100),more » and Nb(100), as well as a doped topological insulator Bi₂Se₃ at temperatures ranging from 30 mK to 9 K.« less

Method for applying photographic resists to otherwise incompatible substrates

NASA Technical Reports Server (NTRS)

Fuhr, W. (Inventor)

1981-01-01

A method for applying photographic resists to otherwise incompatible substrates, such as a baking enamel paint surface, is described wherein the uncured enamel paint surface is coated with a non-curing lacquer which is, in turn, coated with a partially cured lacquer. The non-curing lacquer adheres to the enamel and a photo resist material satisfactorily adheres to the partially cured lacquer. Once normal photo etching techniques are employed the lacquer coats can be easily removed from the enamel leaving the photo etched image. In the case of edge lighted instrument panels, a coat of uncured enamel is placed over the cured enamel followed by the lacquer coats and the photo resists which is exposed and developed. Once the etched uncured enamel is cured, the lacquer coats are removed leaving an etched panel.

Effects of Etching Time and NaOH Concentration on the Production of Alumina Nanowires Using Porous Anodic Alumina Template

NASA Astrophysics Data System (ADS)

Sadeghpour-Motlagh, M.; Mokhtari-Zonouzi, K.; Aghajani, H.; Kakroudi, M. Ghassemi

2014-06-01

In this work, two-step anodizing of commercial aluminum foil in acid oxalic solution was applied for producing alumina film. Then the anodic alumina film was etched in sodium hydroxide (NaOH) solution resulting dense and aligned alumina nanowires. This procedure leads to splitting of alumina nanotubes. Subsequently nanowires are produced. The effects of NaOH solution concentration (0.2-1 mol/L) and etching time (60-300 s) at constant temperature on characteristic of nanotubes and produced nanowires were investigated using scanning electron microscopy. The results show that an increase in NaOH solution concentration increases the rate of nanowires production and in turn the manipulation process will be more specific.

Freestanding silicon quantum dots: origin of red and blue luminescence.

PubMed

Gupta, Anoop; Wiggers, Hartmut

2011-02-04

In this paper, we studied the behavior of silicon quantum dots (Si-QDs) after etching and surface oxidation by means of photoluminescence (PL) measurements, Fourier transform infrared spectroscopy (FTIR) and electron paramagnetic resonance spectroscopy (EPR). We observed that etching of red luminescing Si-QDs with HF acid drastically reduces the concentration of defects and significantly enhances their PL intensity together with a small shift in the emission spectrum. Additionally, we observed the emergence of blue luminescence from Si-QDs during the re-oxidation of freshly etched particles. Our results indicate that the red emission is related to the quantum confinement effect, while the blue emission from Si-QDs is related to defect states at the newly formed silicon oxide surface.

Enlargement of halloysite clay nanotube lumen by selective etching of aluminum oxide.

PubMed

Abdullayev, Elshad; Joshi, Anupam; Wei, Wenbo; Zhao, Yafei; Lvov, Yuri

2012-08-28

Halloysite clay tubes have 50 nm diameter and chemically different inner and outer walls (inner surface of aluminum oxide and outer surface of silica). Due to this different chemistry, the selective etching of alumina from inside the tube was realized, while preserving their external diameter (lumen diameter changed from 15 to 25 nm). This increases 2-3 times the tube lumen capacity for loading and further sustained release of active chemical agents such as metals, corrosion inhibitors, and drugs. In particular, halloysite loading efficiency for the benzotriazole increased 4 times by selective etching of 60% alumina within the tubes' lumens. Specific surface area of the tubes increased over 6 times, from 40 to 250 m(2)/g, upon acid treatment.

WSi2/Si multilayer sectioning by reactive ion etching for multilayer Laue lens fabrication

NASA Astrophysics Data System (ADS)

Bouet, N.; Conley, R.; Biancarosa, J.; Divan, R.; Macrander, A. T.

2010-09-01

Reactive ion etching (RIE) has been employed in a wide range of fields such as semiconductor fabrication, MEMS (microelectromechanical systems), and refractive x-ray optics with a large investment put towards the development of deep RIE. Due to the intrinsic differing chemistries related to reactivity, ion bombardment, and passivation of materials, the development of recipes for new materials or material systems can require intense effort and resources. For silicon in particular, methods have been developed to provide reliable anisotropic profiles with good dimensional control and high aspect ratios1,2,3, high etch rates, and excellent material to mask etch selectivity. A multilayer Laue lens4 is an x-ray focusing optic, which is produced by depositing many layers of two materials with differing electron density in a particular stacking sequence where the each layer in the stack satisfies the Fresnel zone plate law. When this stack is sectioned to allow side-illumination with radiation, the diffracted exiting radiation will constructively interfere at the focal point. Since the first MLLs were developed at Argonne in the USA in 20064, there have been published reports of MLL development efforts in Japan5, and, very recently, also in Germany6. The traditional technique for sectioning multilayer Laue lens (MLL) involves mechanical sectioning and polishing7, which is labor intensive and can induce delamination or structure damage and thereby reduce yield. If a non-mechanical technique can be used to section MLL, it may be possible to greatly shorten the fabrication cycle, create more usable optics from the same amount of deposition substrate, and perhaps develop more advanced structures to provide greater stability or flexibility. Plasma etching of high aspect-ratio multilayer structures will also expand the scope for other types of optics fabrication (such as gratings, zone plates, and so-on). However, well-performing reactive ion etching recipes have been developed for only a small number of materials, and even less recipes exist for concurrent etching of more than one element so a fully material specific process needs to be developed. In this paper, sectioning of WSi2/Si multilayers for MLL fabrication using fluorinated gases is investigated. The main goals were to demonstrate the feasibility of this technique, achievement of high anisotropy, adequate sidewall roughness control and high etching rates. We note that this development for MLL sidewalls should be distinguished from work on improving aspect ratios in traditional Fresnel zone plates. Aspect ratios for MLL sidewalls are not similarly constrained.

Macroscale Transformation Optics Enabled by Photoelectrochemical Etching.

PubMed

Barth, David S; Gladden, Christopher; Salandrino, Alessandro; O'Brien, Kevin; Ye, Ziliang; Mrejen, Michael; Wang, Yuan; Zhang, Xiang

2015-10-28

Photoelectrochemical etching of silicon can be used to form lateral refractive index gradients for transformation optical devices. This technique allows the fabrication of macroscale devices with large refractive index gradients. Patterned porous layers can also be lifted from the substrate and transferred to other materials, creating more possibilities for novel devices. © 2015 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim.

InGaN directional coupler made with a one-step etching technique

NASA Astrophysics Data System (ADS)

Gao, Xumin; Yuan, Jialei; Yang, Yongchao; Zhang, Shuai; Shi, Zheng; Li, Xin; Wang, Yongjin

2017-06-01

We propose, fabricate and characterize an on-chip integration of light source, InGaN waveguide, directional coupler and photodiode, in which AlGaN layers are used as top and bottom optical claddings to form an InGaN waveguide for guiding the in-plane emitted light from the InGaN/GaN multiple-quantum-well light-emitting diode (MQW-LED). The difference in etch rate caused by different exposure windows leads to an etching depth discrepancy using the one-step etching technique, which forms the InGaN directional coupler with the overlapped underlying slab. Light propagation results directly confirm effective light coupling in the InGaN directional coupler, which is achieved through high-order guided modes. The InGaN waveguide couples the modulated light from the InGaN/GaN MQW-LED and transfers part of light to the coupled waveguide via the InGaN directional coupler. The in-plane InGaN/GaN MQW-photodiode absorbs the guided light by the coupled InGaN waveguide and induces the photocurrent. The on-chip InGaN photonic integration experimentally demonstrates an in-plane light communication with a data transmission of 50 Mbps.

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.

Method for surface treatment of a cadmium zinc telluride crystal

DOEpatents

James, R.; Burger, A.; Chen, K.T.; Chang, H.

1999-08-03

A method for treatment of the surface of a CdZnTe (CZT) crystal is disclosed that reduces surface roughness (increases surface planarity) and provides an oxide coating to reduce surface leakage currents and thereby, improve resolution. A two step process is disclosed, etching the surface of a CZT crystal with a solution of lactic acid and bromine in ethylene glycol, following the conventional bromine/methanol etch treatment, and after attachment of electrical contacts, oxidizing the CZT crystal surface. 3 figs.

Decontamination of metals using chemical etching

DOEpatents

Lerch, Ronald E.; Partridge, Jerry A.

1980-01-01

The invention relates to chemical etching process for reclaiming contaminated equipment wherein a reduction-oxidation system is included in a solution of nitric acid to contact the metal to be decontaminated and effect reduction of the reduction-oxidation system, and includes disposing a pair of electrodes in the reduced solution to permit passage of an electrical current between said electrodes and effect oxidation of the reduction-oxidation system to thereby regenerate the solution and provide decontaminated equipment that is essentially radioactive contamination-free.

A Fundamental Approach to Adhesion: Synthesis, Surface Analysis, Thermodynamics and Mechanics.

DTIC Science & Technology

1978-02-01

Polyphenylquinoxaline LSS - Lap Shear Strength Pasa-Jell - Commercial acid etch (See p. 15 ) Turco - Commercial base etch (See p. 17 ) CTBN - Carboxyl-Terminated...solvent- cast films or powders. SEM/EDAX results were obtained from the fracture surfaces of lap-shear tested specimens. Epoxy and two epoxy/ CTBN bulk...A - - 24 CTBN 1300X8 (Goodrich carboxyl- 5 5 terminated butadiene-acrylonitrile) Piperidine 5 5 5 L9 III. RESULTS AND DISCUSS10N A. Titanium 6-4 (SEM