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Sample records for acid etched surface

  1. [Recovery of fluoride orally on the acid-etched tooth surface].

    PubMed

    Tanaka, M; Kobayashi, K; Okumura, F; Ono, H; Kadoma, Y; Imai, Y

    1989-01-01

    There are many reports concerning the recovery phenomenon of acid-etched enamel surfaces of teeth. Many studies of surface hardness, acid resistant properties, radiolucency, and surface morphology suggest that orally the acid-etched enamel reverts to a state nearly similar to that of the intact enamel before the acid etching. This study was conducted in order to verify the existence of the recovery phenomenon of fluoride on acid-etched enamel, because the surface layer of a high fluoride concentration is removed from the surface enamel by the acid etching. The deciduous upper central incisors of both sides were etched with phosphoric acid. The fluoride content of one incisor was measured immediately after the etching and that of the opposite incisor was also measured in vivo after 4 weeks, during which period no special fluoride was used. The fluoride content of the tooth surface in the mouth after 4 weeks significantly increased by about 50 ppm, when compared to that immediately after the acid etching. No significant relationship was found between the fluoride increase and the fluoride concentration of the patients' saliva and drinking water which were the probable supply sources of fluoride for the teeth. No relationship was found between the fluoride increase and the number of second deciduous molars with defects or fillings, which was counted as a measure of the patient's susceptibility to caries.

  2. Effect of acid etching of glass ionomer cement surface on the microleakage of sandwich restorations.

    PubMed

    Bona, Alvaro Della; Pinzetta, Caroline; Rosa, Vinícius

    2007-06-01

    The purposes of this study were to evaluate the sealing ability of different glass ionomer cements (GICs) used for sandwich restorations and to assess the effect of acid etching of GIC on microleakage at GIC-resin composite interface. Forty cavities were prepared on the proximal surfaces of 20 permanent human premolars (2 cavities per tooth), assigned to 4 groups (n=10) and restored as follows: Group CIE - conventional GIC (CI) was applied onto the axial and cervical cavity walls, allowed setting for 5 min and acid etched (E) along the cavity margins with 35% phosphoric acid for 15 s, washed for 30 s and water was blotted; the adhesive system was applied and light cured for 10 s, completing the restoration with composite resin light cured for 40 s; Group CIN - same as Group CIE, except for acid etching of the CI surface; Group RME - same as CIE, but using a resin modified GIC (RMGIC); Group RMN - same as Group RME, except for acid etching of the RMGIC surface. Specimens were soaked in 1% methylene blue dye solution at 24 degrees C for 24 h, rinsed under running water for 1 h, bisected longitudinally and dye penetration was measured following the ISO/TS 11405-2003 standard. Results were statistically analyzed by Kruskal-Wallis and chi-square tests (a=0.05). Dye penetration scores were as follow: CIE - 2.5; CIN - 2.5; RME - 0.9; and RMN - 0.6. The results suggest that phosphoric acid etching of GIC prior to the placement of composite resin does not improve the sealing ability of sandwich restorations. The RMGIC was more effective in preventing dye penetration at the GIC-resin composite-dentin interfaces than CI.

  3. Facile transition from hydrophilicity to superhydrophilicity and superhydrophobicity on aluminum alloy surface by simple acid etching and polymer coating

    NASA Astrophysics Data System (ADS)

    Liu, Wenyong; Sun, Linyu; Luo, Yuting; Wu, Ruomei; Jiang, Haiyun; Chen, Yi; Zeng, Guangsheng; Liu, Yuejun

    2013-09-01

    The transition from the hydrophilic surface to the superhydrophilic and superhydrophobic surface on aluminum alloy via hydrochloric acid etching and polymer coating was investigated by contact angle (CA) measurements and scanning electron microscope (SEM). The effects of etching and polymer coating on the surface were discussed. The results showed that a superhydrophilic surface was facilely obtained after acid etching for 20 min and a superhydrophobic surface was readily fabricated by polypropylene (PP) coating after acid etching. When the etching time was 30 min, the CA was up to 157̊. By contrast, two other polymers of polystyrene (PS) and polypropylene grafting maleic anhydride (PP-g-MAH) were used to coat the aluminum alloy surface after acid etching. The results showed that the CA was up to 159̊ by coating PP-g-MAH, while the CA was only 141̊ by coating PS. By modifying the surface with the silane coupling agent before PP coating, the durability and solvent resistance performance of the superhydrophobic surface was further improved. The micro-nano concave-convex structures of the superhydrophilic surface and the superhydrophobic surface were further confirmed by scanning electron microscope (SEM). Combined with the natural hydrophilicity of aluminum alloy, the rough micro-nano structures of the surface led to the superhydrophilicity of the aluminum alloy surface, while the rough surface structures led to the superhydrophobicity of the aluminum alloy surface by combination with the material of PP with the low surface free energy.

  4. 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

  5. Investigation of Acid-Etched CO2 Laser Ablated Enamel Surfaces Using Polarization Sensitive Optical Coherence Tomography

    PubMed Central

    Nahm, Byung J.; Kang, Hobin; Chan, Kenneth; Fried, Daniel

    2012-01-01

    A carbon dioxide laser operating at the highly absorbed wavelength of 9.3μm with a pulse duration of 10–15μs is ideally suited for caries removal and caries prevention. The enamel thermally modified by the laser has enhanced resistance to acid dissolution. This is an obvious advantage for caries prevention; however, it is often necessary to etch the enamel surface to increase adhesion to composite restorative materials and such surfaces may be more resistant to etching. The purpose of the study was to non-destructively measure the susceptibility of laser-ablated enamel surfaces to acid dissolution before and after acid-etching using Polarization Sensitive Optical Coherence Tomography (PS-OCT). PS-OCT was used to acquire images of bovine enamel surfaces after exposure to laser irradiation at ablative fluence, acid-etching, and a surface softened dissolution model. The integrated reflectivity from lesion and the lesion depth were measured using PS-OCT. Samples were also sectioned for examination by Polarized Light Microscopy (PLM). PS-OCT images showed that acid-etching greatly accelerated the formation of subsurface lesions on both laser-irradiated and non-irradiated surfaces (P<0.05). A 37.5% phosphoric acid etch removed the laser modified enamel layer after 5–10 seconds. PMID:23539418

  6. Investigation of acid-etched CO2 laser ablated enamel surfaces using polarization sensitive optical coherence tomography

    NASA Astrophysics Data System (ADS)

    Nahm, Byung J.; Kang, Hobin; Chan, Kenneth; Fried, Daniel

    2012-01-01

    A carbon dioxide laser operating at the highly absorbed wavelength of 9.3μm with a pulse duration of 10-15μs is ideally suited for caries removal and caries prevention. The enamel thermally modified by the laser has enhanced resistance to acid dissolution. This is an obvious advantage for caries prevention; however, it is often necessary to etch the enamel surface to increase adhesion to composite restorative materials and such surfaces may be more resistant to etching. The purpose of the study was to non-destructively measure the susceptibility of laser-ablated enamel surfaces to acid dissolution before and after acid-etching using Polarization Sensitive Optical Coherence Tomography (PS-OCT). PS-OCT was used to acquire images of bovine enamel surfaces after exposure to laser irradiation at ablative fluence, acid-etching, and a surface softened dissolution model. The integrated reflectivity from lesion and the lesion depth were measured using PS-OCT. Samples were also sectioned for examination by Polarized Light Microscopy (PLM). PS-OCT images showed that acid-etching greatly accelerated the formation of subsurface lesions on both laser-irradiated and non-irradiated surfaces (P<0.05). A 37.5% phosphoric acid etch removed the laser modified enamel layer after 5-10 seconds.

  7. Nitric-phosphoric acid etching effects on the surface chemical composition of CdTe thin film.

    NASA Astrophysics Data System (ADS)

    Irfan, Irfan; Ding, Huanjun; Xia, Wei; Lin, Hao; Tang, Ching W.; Gao, Yongli

    2009-03-01

    Nitric-phosphoric (NP) acid etching has been regarded as one of the most successful methods for the formation of low resistance back contact with the metal electrode in CdTe based solar cells. We report back surface chemical composition for eight different durations of NP etching of CdTe polycrystalline thin film. We studied the surfaces with x-ray photoemission spectroscopy (XPS), ultraviolet photoemission spectroscopy (UPS), inverse photoemission spectroscopy (IEPS) and atomic force microscopy (AFM). Etching dependence on the back surface composition and electronic structure was observed. Valence and conduction band shifts relative to the Fermi level of the system with different etching duration were analyzed. The sample was left in open ambient condition for three weeks and XPS data were obtained again in order to study the difference in surface chemical composition with the pristine CdTe film. Unetched and highly etched part of the sample were sputtered and the depth profile analyzed.

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

    PubMed

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

    2016-05-27

    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.

  9. 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

  10. Comparative Study of the Effect of Acid Etching on Enamel Surface Roughness between Pumiced and Non-pumiced Teeth

    PubMed Central

    Abreu, Lucas Guimarães; Paiva, Saul Martins; Pretti, Henrique; Lages, Elizabeth Maria Bastos; Júnior, João Batista Novães; Ferreira, Ricardo Alberto Neto

    2015-01-01

    Background: The objective was to perform a comparative analysis of the effect of acid etching on enamel roughness between pumiced and non-pumiced teeth. Materials and Methods: The sample was composed of 32 dental surfaces divided into two groups: Group 1-16 surfaces having received pumice prophylaxis; and Group 2-16 surfaces not having received pumice prophylaxis. The teeth were kept in saline until the first record of surface roughness prior to etching. For each surface, a roughness graph was obtained through trials using a surface roughness tester. This procedure was repeated two more times at different locations for a total of three readings which, later, were converted in a mean value. The teeth were then acid etched with a 37% phosphoric acid for 60 s, rinsed with water, air dried, and tested with the roughness tester again using the same protocol described for baseline. The Quantikov image analysis program was used to measure the length of the graphs. The average value of the lengths was recorded for each surface before and after etching. The increase in roughness caused by acid etching was calculated and compared between groups. Results: The mean increase in roughness caused by the etching was 301 µm (11.37%) in Group 1 and 214 µm (8.33%) in Group 2. No statistically significant difference was found between samples with and without pumice prophylaxis (P = 0.283). Conclusion: The present study showed that the effect of acid etching on enamel roughness was not significantly affected by prior pumice prophylaxis. PMID:26435607

  11. Comparison of shear bond strength of composite resin to enamel surface with laser etching versus acid etching: An in vitro evaluation

    PubMed Central

    Hoshing, Upendra A; Patil, Suvarna; Medha, Ashish; Bandekar, Siddhesh Dattatray

    2014-01-01

    Introduction: The aim of the study is in vitro evaluation of the shear bond strength of composite resin bonded to enamel which is pretreated using acid etchant and Er,Cr:Ysgg. Materials and Methods: 40 extracted human teeth were divided in two groups of 20 each (Groups A and B). In Group A, prepared surface of enamel was etched using 37% phosphoric acid (Scotchbond, 3M). In Group B, enamel was surface treated by a an Er, Cr: YSGG laser system (Waterlase MD, Biolase Technology Inc., San Clemente, CA, USA) operating at a wavelength of 2,780 nm and having a pulse duration of 140-200 microsecond with a repetition rate of 20 Hz and 40 Hz. Bonding agent ((Scotchbond Multipurpose, 3M) was applied over the test areas on 20 samples of Groups A and B each, and light cured. Composite resin (Ceram X duo Nanoceramic restorative, Densply) was applied onto the test areas as a 3 × 3 mm diameter bid, and light cured. The samples were tested for shear bond strength. Results: Mean shear bond strength for acid-etched enamel (26.41 ± 0.66MPa, range 25.155 to 27.150 MPa) was significantly higher (P < 0.01) than for laser-etched enamel (16.23 ± 0.71MPa, range 15.233 to 17.334 MPa). Conclusions: For enamel surface, mean shear bond strength of bonded composite obtained after laser etching were significantly lower than those obtained after acid etching. PMID:25125842

  12. Shear bond strength of resin cement to an acid etched and a laser irradiated ceramic surface

    PubMed Central

    Motro, Pelin Fatma Karagoz; Yurdaguven, Haktan

    2013-01-01

    PURPOSE To evaluate the effects of hydrofluoric acid etching and Er,Cr:YSGG laser irradiation on the shear bond strength of resin cement to lithium disilicate ceramic. MATERIALS AND METHODS Fifty-five ceramic blocks (5 mm × 5 mm × 2 mm) were fabricated and embedded in acrylic resin. Their surfaces were finished with 1000-grit silicon carbide paper. The blocks were assigned to five groups: 1) 9.5% hydrofluoric-acid etching for 60 s; 2-4), 1.5-, 2.5-, and 6-W Er,Cr:YSGG laser applications for 60 seconds, respectively; and 5) no treatment (control). One specimen from each group was examined using scanning electron microscopy. Ceramic primer (Rely X ceramic primer) and adhesive (Adper Single Bond) were applied to the ceramic surfaces, followed by resin cement to bond the composite cylinders, and light curing. Bonded specimens were stored in distilled water at 37℃ for 24 hours. Shear bond strengths were determined by a universal testing machine at 1 mm/min crosshead speed. Data were analyzed using Kruskal-Wallis and Mann-Whitney U-tests (α=0.05). RESULTS Adhesion was significantly stronger in Group 2 (3.88 ± 1.94 MPa) and Group 3 (3.65 ± 1.87 MPa) than in Control group (1.95 ± 1.06 MPa), in which bonding values were lowest (P<.01). No significant difference was observed between Group 4 (3.59 ± 1.19 MPa) and Control group. Shear bond strength was highest in Group 1 (8.42 ± 1.86 MPa; P<.01). CONCLUSION Er,Cr:YSGG laser irradiation at 1.5 and 2.5 W increased shear bond strengths between ceramic and resin cement compared with untreated ceramic surfaces. Irradiation at 6 W may not be an efficient ceramic surface treatment technique. PMID:23755333

  13. Characterization and biocompatibility of a titanium dental implant with a laser irradiated and dual-acid etched surface.

    PubMed

    Hsu, Shan-Hui; Liu, Bai-Shuan; Lin, Wen-Hung; Chiang, Heng-Chieh; Huang, Shih-Ching; Cheng, Shih-Shyong

    2007-01-01

    The biological properties of commercial pure titanium (cp-Ti) dental implants can be improved by surface treatment. In this study, the cp-Ti surfaces were prepared to enable machined surfaces (TM) to be compared to the machined, sandblasted, laser irradiated and dual-acid etched surfaces (TA). The surface elements and roughness were characterized. The biocompatibility was evaluated by cell and organ culture in vitro. The removal torque was measured in rabbit implantation. Surface characterization revealed that TA surface was more oxidized than TM surface. The TA surface had micrometric, beehive-like coarse concaves. The average roughness (2.28 mum) was larger than that typical of acid-etched surfaces. Extracts of both materials were not cytotoxic to bone cells. The morphology of cells attached on the TA surface was superior to that on the TM surface. TA promoted cell migration and repaired damaged bones more effectively in organ culture. The formation of bone-like nodules on TA disk exceeded that on TM disk. Rabbit tibia implantation also proved that TA implant had greater removal torque value. These results suggested that TA had good osteoconductivity and was a potential material for dental implantation. PMID:17264387

  14. 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.

  15. Copper-assisted, anti-reflection etching of silicon surfaces

    SciTech Connect

    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.

  16. 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. PMID:27315775

  17. 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.

  18. Changes in the surface of bone and acid-etched and sandblasted implants following implantation and removal

    PubMed Central

    Eroglu, Cennet Neslihan; Ertugrul, Abdullah Seckin; Eskitascioglu, Murat; Eskitascioglu, Gurcan

    2016-01-01

    Objective: The aim of this study was to determine whether there are any changes in the surface of bone or implant structures following the removal of a screwed dental implant. Materials and Methods: For this, six individual samples of acid-etched and sandblasted implants from three different manufacturers’ implant systems were used. They were screwed in a D1 bovine bone, and they were removed after primary stabilization. The bone and implant surfaces are evaluated with scanning electron microscope. Results: Through examination of the surfaces of the bone prior to implantation and of the used and unused implant surfaces, it was found that inhomogeneity in the implant surface can cause microcracking in the bone. Conclusions: This is attributed to the stress induced during the implantation of self-tapping implants and suggests that a tap drill may be required in some instances to protect the implant surface. PMID:27011744

  19. Nanoparticle-based etching of silicon surfaces

    DOEpatents

    Branz, Howard; Duda, Anna; Ginley, David S.; Yost, Vernon; Meier, Daniel; Ward, James S.

    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.

  20. Surface Topographical Changes of a Failing Acid-Etched Long-Term in Function Retrieved Dental Implant.

    PubMed

    Monje, Alberto; González-García, Raúl; Fernández-Calderón, María Coronada; Hierro-Oliva, Margarita; González-Martín, María Luisa; Del Amo, Fernando Suarez-Lopez; Galindo-Moreno, Pablo; Wang, Hom-Lay; Monje, Florencio

    2016-02-01

    The aim of the present study was to report the main topographical and chemical changes of a failing 18-year in function retrieved acid-etching implant in the micro- and nanoscales. A partially edentulous 45 year old rehabilitated with a dental implant at 18 years of age exhibited mobility. After careful examination, a 3.25 × 13-mm press-fit dental implant was retrieved. Scanning electron microscope (SEM) analysis was carried out to study topographical changes of the retrieved implant compared with an unused implant with similar topographical characteristics. Moreover, X-ray photoelectron spectroscopy (XPS) analysis was used to study the surface composition of the retrieved failing implant. Clear changes related to the dual dioxide layer are present as visible in ≥×500 magnification. In addition, it was found that, for the retrieved implant, the surface composition consisted mainly of Ti2p, O1s, C1s, and Al2p. Also, a meaningful decrease of N and C was noticed, whereas the peaks of Ti2p, Al2p, and O1s increased when analyzing deeper (up to ×2000s) in the sample. It was shown that the superficial surface of a retrieved press-fit dual acid-etched implant 18 years after placement is impaired. However, the causes and consequences for these changes cannot be determined. PMID:25642739

  1. Surface Topographical Changes of a Failing Acid-Etched Long-Term in Function Retrieved Dental Implant.

    PubMed

    Monje, Alberto; González-García, Raúl; Fernández-Calderón, María Coronada; Hierro-Oliva, Margarita; González-Martín, María Luisa; Del Amo, Fernando Suarez-Lopez; Galindo-Moreno, Pablo; Wang, Hom-Lay; Monje, Florencio

    2016-02-01

    The aim of the present study was to report the main topographical and chemical changes of a failing 18-year in function retrieved acid-etching implant in the micro- and nanoscales. A partially edentulous 45 year old rehabilitated with a dental implant at 18 years of age exhibited mobility. After careful examination, a 3.25 × 13-mm press-fit dental implant was retrieved. Scanning electron microscope (SEM) analysis was carried out to study topographical changes of the retrieved implant compared with an unused implant with similar topographical characteristics. Moreover, X-ray photoelectron spectroscopy (XPS) analysis was used to study the surface composition of the retrieved failing implant. Clear changes related to the dual dioxide layer are present as visible in ≥×500 magnification. In addition, it was found that, for the retrieved implant, the surface composition consisted mainly of Ti2p, O1s, C1s, and Al2p. Also, a meaningful decrease of N and C was noticed, whereas the peaks of Ti2p, Al2p, and O1s increased when analyzing deeper (up to ×2000s) in the sample. It was shown that the superficial surface of a retrieved press-fit dual acid-etched implant 18 years after placement is impaired. However, the causes and consequences for these changes cannot be determined.

  2. Bone contact around osseointegrated implants: histologic analysis of a dual-acid-etched surface implant in a diabetic patient.

    PubMed

    Bugea, Calogero; Luongo, Roberto; Di Iorio, Donato; Cocchetto, Roberto; Celletti, Renato

    2008-04-01

    The clinical applicability and predictability of osseointegrated implants in healthy patients have been studied extensively. Although successful treatment of patients with medical conditions including diabetes, arthritis, and cardiovascular disease has been described, insufficient information is available to determine the effects of diabetes on the process of osseointegration. An implant placed and intended to support an overdenture in a 65-year-old diabetic woman was prosthetically unfavorable and was retrieved after 2 months. It was then analyzed histologically. No symptoms of implant failure were detected, and histomorphometric evaluation showed the bone-to-implant contact percentage to be 80%. Osseointegration can be obtained when implants with a dual-acid-etched surface are placed in properly selected diabetic patients. PMID:18546810

  3. Fabrication, characterization, and biological assessment of multilayer DNA coatings on sandblasted-dual acid etched titanium surface.

    PubMed

    Liu, Li; Song, Li-Na; Yang, Guo-Li; Zhao, Shi-Fang; He, Fu-Ming

    2011-06-01

    As local gene therapy has received attention, immobilizing functional gene onto irregular oral implant surface has become an advanced challenge. Electrostatic layer-by-layer (LBL) assembly technique could achieve this goal and allow local and efficient administration of genes to the target cells. In this study, multilayers of cationic lipid/plasmid DNA (pEGFP-C1) complex (LDc) and anionic hyaluronic acid were assembled onto sandblasted-dual acid etched titanium disks by the LBL technique. Surface characteristics of the coatings were performed by x-ray photospectroscopy (XPS), contact angle measurements, and scanning electron microscopy (SEM). The cell biological characteristics of the coatings were evaluated by in vitro experiments. SEM results demonstrated that the porous titanium surface was gradually flattened with the increase of the multilayer. The XPS survey indicated that the N element was found from the coating. The coating degradation and pEGFP-C1 releasing kinetics showed that the more assembled layer numbers were, the larger the amount of DNA released in the first 30 h. MC3T3-E1 cells were cultured directly on the DNA-loaded surface. Higher enhanced green fluorescent protein (EGFP) expression efficiency was achieved by increasing the number of layers when cells were cultured after 24 or 72 h. The MC3T3-E1 cell viability on the surface of multilayer DNA coatings was significantly higher than that on control porous titanium surface. It was concluded that the approach established by the LBL technique had great potential in immobilizing gene coatings onto the porous titanium surface and subsequently influenced the function of the cultured cell. PMID:21448994

  4. Effect of modifications of dual acid-etched implant surfaces on periimplant bone formation. Part II: calcium phosphate coatings.

    PubMed

    Schliephake, H; Aref, A; Scharnweber, D; Rösler, S; Sewing, A

    2009-01-01

    The aim of the present study was to test the hypothesis that calcium phosphate coatings of dual acid-etched surfaces (DAEs) can improve periimplant bone regeneration. Ten adult female foxhounds received experimental titanium screw implants in the mandible 3 months after removal of all premolar teeth. Five types of surface states were evaluated in each animal: (i) implants with a machined surface (MS) (Control 1); (ii) implants with a DAE (Control 2); (iii) implants with a DAE coated with collagen I (Control 3); (iv) implants with a DAE with mineralized collagen I; and (v) implants with a DAE with a hydroxylapatite (HA) coating. Periimplant bone regeneration was assessed by histomorphometry after 1 and 3 months in five dogs each by measuring bone implant contact (BIC) and the volume density of the newly formed periimplant bone (BVD). After 1 month, mean BIC of experimental implants did not differ significantly from implants with DAE and collagen-coated surfaces, but was significantly higher than the MS implants. BVD was enhanced significantly only in implants with mineralized collagen coating compared with DAE and collagen-coated controls. After 3 months, the mean values of BIC had increased significantly in the group of implants with HA and mineralized collagen coating but were not significantly different from implants with DAE and collagen-coated surfaces. The same held true for the mean BVD values. In conclusion, the present study could not verify the hypothesis that calcium phosphate coatings of DAEs in the present form enhanced periimplant bone formation compared with the DAE surface alone. PMID:19126106

  5. Surface Properties and Osteoblastic Cytocompatibility of Two Blasted and Acid-Etched Titanium Implant Systems with Distinct Microtopography

    PubMed Central

    Mesquita, Pedro; Gomes, Pedro de Sousa; Sampaio, Paula; Juodzbalys, Gintaras; Afonso, Américo

    2012-01-01

    ABSTRACT Objectives The aim of this study is to compare two commercially available screw-type sandblasted and acid-etched (SLA) Ti implant systems from Eckermann Laboratorium S.L., with similar geometry and distinct microtopography, regarding surface properties and osteoblastic cytocompatibility. Material and Methods Implant I (referred as a conventional SLA system) and Implant II (a system patented as Eckcyte®) were characterized for macro and microtopograpphy, surface roughness and chemical composition. For the cytocompatibility studies, human bone marrow osteoblastic cells were seeded over the implants' surface, and the cell response was assessed for cell adhesion and proliferation, alkaline phosphatase (ALP) activity and matrix mineralization. Results Implant I presented a rough surface with irregularly shaped and sized cavities among flatter-appearing areas, whereas Implant II exhibited a homogeneous rough microporous surface. Compared to Implant I, Implant II presented higher Ra values (0.8 [SD 0.008] μm and 1.21 [SD 0.15] μm, respectively, P < 0.05) and also increased values of Rz, Rt and Rsm, a more negative value of Rsk, and similar RKu values. XPS showed the expected presence of Ti, O, C and N; Al, Si, F, P and Ca were detected in low concentrations. Implant II exhibited significantly lower Al levels. Both implants supported the adhesion, proliferation and differentiation of osteoblastic cells. Implant II showed a thicker fibrilar cell layer and an earlier onset and more abundant matrix mineralization. Conclusions The homogeneous rough and microporous surface of Implant II is most probably a main contributor for its improved cell response. PMID:24422006

  6. Micro-shear bond strength and surface micromorphology of a feldspathic ceramic treated with different cleaning methods after hydrofluoric acid etching

    PubMed Central

    STEINHAUSER, Henrique Caballero; TURSSI, Cecília Pedroso; FRANÇA, Fabiana Mantovani Gomes; do AMARAL, Flávia Lucisano Botelho; BASTING, Roberta Tarkany

    2014-01-01

    Objective The aim of this study was to evaluate the effect of feldspathic ceramic surface cleaning on micro-shear bond strength and ceramic surface morphology. Material and Methods Forty discs of feldspathic ceramic were prepared and etched with 10% hydrofluoric acid for 2 minutes. The discs were randomly distributed into five groups (n=8): C: no treatment, S: water spray + air drying for 1 minute, US: immersion in ultrasonic bath for 5 minutes, F: etching with 37% phosphoric acid for 1 minute, followed by 1-minute rinse, F+US: etching with 37% phosphoric acid for 1 minute, 1-minute rinse and ultrasonic bath for 5 minutes. Composite cylinders were bonded to the discs following application of silane and hydrophobic adhesive for micro-shear bond strength testing in a universal testing machine at 0.5 mm/min crosshead speed until failure. Stereomicroscopy was used to classify failure type. Surface micromorphology of each treatment type was evaluated by scanning electron microscopy at 500 and 2,500 times magnification. Results One-way ANOVA test showed no significant difference between treatments (p=0.3197) and the most common failure types were cohesive resin cohesion followed by adhesive failure. Micro-shear bond strength of the feldspathic ceramic substrate to the adhesive system was not influenced by the different surface cleaning techniques. Absence of or less residue was observed after etching with hydrofluoric acid for the groups US and F+US. Conclusions Combining ceramic cleaning techniques with hydrofluoric acid etching did not affect ceramic bond strength, whereas, when cleaning was associated with ultrasound, less residue was observed. PMID:24676577

  7. ZERODUR: bending strength data for etched surfaces

    NASA Astrophysics Data System (ADS)

    Hartmann, Peter; Leys, Antoine; Carré, Antoine; Kerz, Franca; Westerhoff, Thomas

    2014-07-01

    In a continuous effort since 2007 a considerable amount of new data and information has been gathered on the bending strength of the extremely low thermal expansion glass ceramic ZERODUR®. By fitting a three parameter Weibull distribution to the data it could be shown that for homogenously ground surfaces minimum breakage stresses exist lying much higher than the previously applied design limits. In order to achieve even higher allowable stress values diamond grain ground surfaces have been acid etched, a procedure widely accepted as strength increasing measure. If surfaces are etched taking off layers with thickness which are comparable to the maximum micro crack depth of the preceding grinding process they also show statistical distributions compatible with a three parameter Weibull distribution. SCHOTT has performed additional measurement series with etch solutions with variable composition testing the applicability of this distribution and the possibility to achieve further increase of the minimum breakage stress. For long term loading applications strength change with time and environmental media are important. The parameter needed for prediction calculations which is combining these influences is the stress corrosion constant. Results from the past differ significantly from each other. On the basis of new investigations better information will be provided for choosing the best value for the given application conditions.

  8. Orthodontic bonding to acid- or laser-etched prebleached enamel

    PubMed Central

    Ozdemir, Fulya; Cakan, Umut; Gonul, Nese

    2013-01-01

    Objective Bonding forces of brackets to enamel surfaces may be affected by the procedures used for bleaching and enamel etching. The aim of this study was to investigate the bonding strength of orthodontic brackets to laser-etched surfaces of bleached teeth. Methods In a nonbleached control group, acid etching (group A) or Er:YAG laser application (group B) was performed prior to bracket bonding (n = 13 in each group). Similar surface treatments were performed at 1 day (groups C and D; n = 13 in each subgroup) or at 3 weeks (groups E and F; n = 13 in each subgroup) after 38% hydrogen peroxide bleaching in another set of teeth. The specimens were debonded after thermocycling. Results Laser etching of bleached teeth resulted in clinically unacceptable low bonding strength. In the case of acid-etched teeth, waiting for 3 weeks before attachment of brackets to the bleached surfaces resulted in similar, but not identical, bond strength values as those obtained with nonbleached surfaces. However, in the laser-etched groups, the bonding strength after 3 weeks was the same as that for the nonbleached group. Conclusions When teeth bleached with 38% hydrogen peroxide are meant to be bonded immediately, acid etching is preferable. PMID:23814709

  9. Method of sputter etching a surface

    DOEpatents

    Henager, Jr., Charles H.

    1984-01-01

    The surface of a target is textured by co-sputter etching the target surface with a seed material adjacent thereto, while the target surface is maintained at a pre-selected temperature. By pre-selecting the temperature of the surface while sputter etching, it is possible to predetermine the reflectance properties of the etched surface. The surface may be textured to absorb sunlight efficiently and have minimal emittance in the infrared region so as to be well-suited for use as a solar absorber for photothermal energy conversion.

  10. Method of sputter etching a surface

    DOEpatents

    Henager, C.H. Jr.

    1984-02-14

    The surface of a target is textured by co-sputter etching the target surface with a seed material adjacent thereto, while the target surface is maintained at a pre-selected temperature. By pre-selecting the temperature of the surface while sputter etching, it is possible to predetermine the reflectance properties of the etched surface. The surface may be textured to absorb sunlight efficiently and have minimal emittance in the infrared region so as to be well-suited for use as a solar absorber for photothermal energy conversion. 4 figs.

  11. 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

  12. 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

  13. 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

  14. Comparison of alkaline phosphatase activity of MC3T3-E1 cells cultured on different Ti surfaces: modified sandblasted with large grit and acid-etched (MSLA), laser-treated, and laser and acid-treated Ti surfaces

    PubMed Central

    Li, Lin-Jie; Kim, So-Nam

    2016-01-01

    PURPOSE In this study, the aim of this study was to evaluate the effect of implant surface treatment on cell differentiation of osteoblast cells. For this purpose, three surfaces were compared: (1) a modified SLA (MSLA: sand-blasted with large grit, acid-etched, and immersed in 0.9% NaCl), (2) a laser treatment (LT: laser treatment) titanium surface and (3) a laser and acid-treated (LAT: laser treatment, acid-etched) titanium surface. MATERIALS AND METHODS The MSLA surfaces were considered as the control group, and LT and LAT surfaces as test groups. Alkaline phosphatase expression (ALP) was used to quantify osteoblastic differentiation of MC3T3-E1 cell. Surface roughness was evaluated by a contact profilometer (URFPAK-SV; Mitutoyo, Kawasaki, Japan) and characterized by two parameters: mean roughness (Ra) and maximum peak-to-valley height (Rt). RESULTS Scanning electron microscope revealed that MSLA (control group) surface was not as rough as LT, LAT surface (test groups). Alkaline phosphatase expression, the measure of osteoblastic differentiation, and total ALP expression by surface-adherent cells were found to be highest at 21 days for all three surfaces tested (P<.05). Furthermore, ALP expression levels of MSLA and LAT surfaces were significantly higher than expression levels of LT surface-adherent cells at 7, 14, and 21 days, respectively (P<.05). However, ALP expression levels between MSLA and LAT surface were equal at 7, 14, and 21 days (P>.05). CONCLUSION This study suggested that MSLA and LAT surfaces exhibited more favorable environment for osteoblast differentiation when compared with LT surface, the results that are important for implant surface modification studies. PMID:27350860

  15. Etching of Crystalline ZnO Surfaces upon Phosphonic Acid Adsorption: Guidelines for the Realization of Well-Engineered Functional Self-Assembled Monolayers.

    PubMed

    Ostapenko, Alexandra; Klöffel, Tobias; Eußner, Jens; Harms, Klaus; Dehnen, Stefanie; Meyer, Bernd; Witte, Gregor

    2016-06-01

    Functionalization of metal oxides by means of covalently bound self-assembled monolayers (SAMs) offers a tailoring of surface electronic properties such as their work function and, in combination with its large charge carrier mobility, renders ZnO a promising conductive oxide for use as transparent electrode material in optoelectronic devices. In this study, we show that the formation of phosphonic acid-anchored SAMs on ZnO competes with an unwanted chemical side reaction, leading to the formation of surface precipitates and severe surface damage at prolonged immersion times of several days. Combining atomic force microscopy (AFM), X-ray diffraction (XRD), and thermal desorption spectroscopy (TDS), the stability and structure of the aggregates formed upon immersion of ZnO single crystal surfaces of different orientations [(0001̅), (0001), and (101̅0)] in phenylphosphonic acid (PPA) solution were studied. By intentionally increasing the immersion time to more than 1 week, large crystalline precipitates are formed, which are identified as zinc phosphonate. Moreover, the energetics and the reaction pathway of this transformation have been evaluated using density functional theory (DFT), showing that zinc phosphonate is thermodynamically more favorable than phosphonic acid SAMs on ZnO. Precipitation is also found for phosphonic acids with fluorinated aromatic backbones, while less precipitation occurs upon formation of SAMs with phenylphosphinic anchoring units. By contrast, no precipitates are formed when PPA monolayer films are prepared by sublimation under vacuum conditions, yielding smooth surfaces without noticeable etching. PMID:27159837

  16. Evaluation of an endosseous titanium implant with a sandblasted and acid-etched surface in the canine mandible: radiographic results.

    PubMed

    Cochran, D L; Nummikoski, P V; Higginbottom, F L; Hermann, J S; Makins, S R; Buser, D

    1996-09-01

    Previous studies have demonstrated in short-term experiments that sandblasted and acid-etched (SLA) titanium implant had a greater bone-to-implant contact than a titanium plasma-sprayed (TPS) implant in non-oral bone. In the present study, an SLA implant was compared radiographically to a TPS implant under unloaded and loaded conditions in the canine mandible for up to 15 months. 69 implants were placed in 6 foxhounds. Standardized radiographs were taken at baseline, preload, 3, 6, 9, and 12 months of loading. Loaded implants were restored with gold crowns similar to the natural dentition. Radiographic assessment of the bone response to the implants was carried out by measuring the distance between the implant shoulder and the most coronal bone-to-implant contact (DIB) and by evaluated of bone density changes using computer-assisted densitometric image analysis (CADIA). 5 different areas-of-interest (AOI) were defined coronally and apically along the implant. DIB measurements revealed that SLA implants had significantly less bone height loss (0.52 mm) than TPS implants (0.69 mm) at the preload evaluation (p = 0.0142) as well as at 3 months of loading (0.73 mm/1.06 mm; p = 0.0337). This difference was maintained between the implant types during the 1-year follow-up period. The same trend was also evident for CADIA measurements with SLA implants showing higher crestal bone density values when comparing preload to baseline data (p = 0.0890) and 3 months to baseline data (p = 0.0912). No measurable bone density changes were apparent in the apical areas of either implant. These results suggest that SLA implants are superior to TPS implants as measured radiographically in oral bone under unloaded and loaded conditions.

  17. In Vitro Evaluation of Microleakage Around Orthodontic Brackets Using Laser Etching and Acid Etching Methods

    PubMed Central

    Toodehzaeim, Mohammad Hossein; Yassaei, Sogra; Karandish, Maryam; Farzaneh, Sedigeh

    2014-01-01

    Objective: path of microleakage between the enamel and adhesive potentially allows microbial ingress that may consequently cause enamel decalcification. The aim of this study was to compare microleakage of brackets bonded either by laser or acid etching techniques. Materials and Method: The specimens were 33 extracted premolars that were divided into three groups as the acid etching group (group 1), laser etching with Er:YAG at 100 mJ and 15 Hz for 15s (group 2), and laser etching with Er:YAG at 140 mJ and 15 Hz for 15s (group 3). After photo polymerization, the teeth were subjected to 500 thermal cycles. Then the specimens were sealed with nail varnish, stained with 2% methylen blue for 24hs, sectioned, and examined under a stereomicroscope. They were scored for marginal microleakage that occurred between the adhesive-enamel and bracket-adhesive interfaces from the occlusal and gingival margins. Data were analyzed with the Kruskal- Wallis test. Results: For the adhesive-enamel and bracket-adhesive surfaces, significant differences were not observed between the three groups. Conclusion: According to this study, the Er:YAG laser with 1.5 and 2.1 watt settings may be used as an adjunctive for preparing the surface for orthodontic bracket bonding. PMID:25628661

  18. Dental zirconia can be etched by hydrofluoric acid.

    PubMed

    Sriamporn, Tool; Thamrongananskul, Niyom; Busabok, Chumphol; Poolthong, Sushit; Uo, Motohiro; Tagami, Junji

    2014-01-01

    The surface morphology and crystal structure change of dental zirconia after hydrofluoric acid (HF) etching were evaluated. Four groups of sintered zirconia specimens were 1) control group, 2) immersion in 9.5%HF at 25°C for 1, 2, 3, or 24 h, 3) immersion in 9.5%HF at 80°C for 1, 3, 5, or 30 min and 4) immersion in 48%HF at 25°C for 30 or 60 min. The specimens were evaluated under SEM and XRD. The SEM analysis revealed changes in surface topography for all the HF-etched zirconia specimens. The irregularities surface increased with increasingly longer immersion times and higher etching solution temperatures. The XRD analysis of the HFetched zirconia specimens revealed the presence of a crystalline monoclinic phase along with a tetragonal form. It was concluded HF can etch dental zirconia ceramic, creating micro-morphological changes. Tetragonal-to-monoclinic phase transformation was induced on the etched zirconia surface.

  19. Effect of erbium-doped: yttrium, aluminium and garnet laser irradiation on the surface microstructure and roughness of sand-blasted, large grit, acid-etched implants

    PubMed Central

    Lee, Ji-Hun; Kwon, Young-Hyuk; Herr, Yeek; Shin, Seung-Il

    2011-01-01

    Purpose The present study was performed to evaluate the effect of erbium-doped: yttrium, aluminium and garnet (Er:YAG) laser irradiation on sand-blasted, large grit, acid-etched (SLA) implant surface microstructure according to varying energy levels and application times of the laser. Methods The implant surface was irradiated by the Er:YAG laser under combined conditions of 100, 140, or 180 mJ/pulse and an application time of 1 minute, 1.5 minutes, or 2 minutes. Scanning electron microscopy (SEM) was used to examine the surface roughness of the specimens. Results All experimental conditions of Er:YAG laser irradiation, except the power setting of 100 mJ/pulse for 1 minute and 1.5 minutes, led to an alteration in the implant surface. SEM evaluation showed a decrease in the surface roughness of the implants. However, the difference was not statistically significant. Alterations of implant surfaces included meltdown and flattening. More extensive alterations were present with increasing laser energy and application time. Conclusions To ensure no damage to their surfaces, it is recommended that SLA implants be irradiated with an Er:YAG laser below 100 mJ/pulse and 1.5 minutes for detoxifying the implant surfaces. PMID:21811689

  20. 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.

  1. Comparative Study of the Early Loading of Resorbable Blasting Media and Sandblasting with Large-grit and Acid-etching Surface Implants: A Retrospective Cohort Study

    PubMed Central

    Kim, Sung-Beom; Kim, Young-Kyun; Kim, Su-Gwan; Oh, Ji-Su; Kim, Byung-Hoon

    2014-01-01

    Purpose: This study compares the prognosis (the survival rate and marginal bone loss) of resorbable blasting media (RBM) surface implants and sandblasting with large-grit and acid-etching (SLA) surface implants in the early loading. Methods: This study targeted 123 patients treated by implants installation from January 2008 to March 2010. The loading was initiated in the maxilla within three to four months and in the mandible within one to two months. The types of restoration were single crown and fixed partial prosthesis. Those functioned over one year. The implants were classified by the surface of implants as Group 1: RBM surface (GS III; OSSTEM, Busan, Korea) and, Group 2: SLA surface (Superline; Dentium, Seoul, Korea). The groups were categorized by maxilla and mandible and compared by survival rate, marginal bone loss through clinical records evaluation, and radiographic measurements. Results: The marginal bone loss in the maxilla was 0.14±0.34 mm (Group 1) and 0.30±0.37 mm (Group 2), a statistically significant difference (P <0.05). In the mandible those were 0.28±0.54 mm (Group 1) and 0.20±0.33 mm (Group 2), not significant (P >0.05). There was no significant difference of marginal bone loss between maxilla and mandible by groups. During observation there was no implant failure, a survival rate of 100%. Conclusion: Both surfaces showed an excellent survival rate, and the marginal bone loss was not substantial. PMID:27489842

  2. 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. PMID:16683674

  3. Early bone response to machined, sandblasting acid etching (SLA) and novel surface-functionalization (SLAffinity) titanium implants: characterization, biomechanical analysis and histological evaluation in pigs.

    PubMed

    Chiang, Hsi-Jen; Hsu, Heng-Jui; Peng, Pei-Wen; Wu, Ching-Zong; Ou, Keng-Liang; Cheng, Han-Yi; Walinski, Christopher J; Sugiatno, Erwan

    2016-02-01

    The purpose of the present study was to examine early tissue response and osseointegration in the animal model. The surface morphologies of SLAffinity were characterized using scanning electron microscopy and atomic force microscopy. The microstructures were examined by X-ray diffraction, and hardness was measured by nanoindentation. Moreover, the safety and toxicity properties were evaluated using computer-aided programs and cell cytotoxicity assays. In the animal model, implants were installed in the mandibular canine-premolar area of 12 miniature pigs. Each pig received three implants: machine, sandblasted, large grit, acid-etched, and SLAffinity-treated implants. The results showed that surface treatment did affect bone-to-implant contact (BIC) significantly. At 3 weeks, the SLAffinity-treated implants were found to present significantly higher BIC values than the untreated implants. The SLAffinity treatments enhanced osseointegration significantly, especially at early stages of bone tissue healing. As described above, the results of the present study demonstrate that the SLAffinity treatment is a reliable surface modification method.

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

    SciTech Connect

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

    2009-09-15

    The influence of surface chemistry in plasma etching of multicomponent oxides was investigated through measurements of the ion energy dependence of the etch yield. Using pulsed-laser-deposited Ca{sub x}Ba{sub (1-x)}Nb{sub 2}O{sub 6} (CBN) and SrTiO{sub 3} thin films as examples, it was found that the etching energy threshold shifts toward values larger or smaller than the sputtering threshold depending on whether or not ion-assisted chemical etching is the dominant etching pathway and whether surface chemistry is enhancing or inhibiting desorption of the film atoms. In the case of CBN films etched in an inductively coupled Cl{sub 2} plasma, it is found that the chlorine uptake is inhibiting the etching reaction, with the desorption of nonvolatile NbCl{sub 2} and BaCl{sub 2} compounds being the rate-limiting step.

  5. Modeling Wet Chemical Etching of Surface Flaws on Fused Silica

    SciTech Connect

    Feit, M D; Suratwala, T I; Wong, L L; Steele, W A; Miller, P E; Bude, J D

    2009-10-28

    Fluoride-based wet chemical etching of fused silica optical components is useful to open up surface fractures for diagnostic purposes, to create surface topology, and as a possible mitigation technique to remove damaged material. To optimize the usefulness of etching , it is important to understand how the morphology of etched features changes as a function of the amount of material removed. In this study, we present two geometric etch models that describe the surface topology evolution as a function of the amount etched. The first model, referred to as the finite-difference etch model, represents the surface as an array of points in space where at each time-step the points move normal to the local surface. The second model, referred to as the surface area-volume model, more globally describes the surface evolution relating the volume of material removed to the exposed surface area. These etch models predict growth and coalescence of surface fractures such as those observed on scratches and ground surfaces. For typical surface fractures, simulations show that the transverse growth of the cracks at long etch times scales with the square root of etch time or the net material removed in agreement with experiment. The finite-difference etch model has also been applied to more complex structures such as the etching of a CO{sub 2} laser-mitigated laser damage site. The results indicate that etching has little effect on the initial morphology of this site implying little change in downstream scatter and modulation characteristics upon exposure to subsequent high fluence laser light. In the second part of the study, the geometric etch model is expanded to include fluid dynamics and mass transport. This later model serves as a foundation for understanding related processes such as the possibility of redeposition of etch reaction products during the etching, rinsing or drying processes.

  6. Adult stem cells properties in terms of commitment, aging and biological safety of grit-blasted and Acid-etched ti dental implants surfaces.

    PubMed

    Gardin, Chiara; Ferroni, Letizia; Bressan, Eriberto; Calvo-Guirado, José L; Degidi, Marco; Piattelli, Adriano; Zavan, Barbara

    2014-01-01

    Titanium (Ti) is one of the most widely used biomaterials for manufacturing dental implants. The implant surface properties strongly influence osseointegration. The aim of the present study was to in vitro investigate the characteristics of Ti dental implants in terms of mutagenicity, hemocompatibility, biocompatibility, osteoinductivity and biological safety. The Ames test was used to test the mutagenicity of the Ti dental implants, and the hemolysis assay for evaluating their hemocompatibility. Human adipose - derived stem cells (ADSCs) were then seeded onto these implants in order to evaluate their cytotoxicity. Gene expression analyzing with real-time PCR was carried out to investigate the osteoinductivity of the biomaterials. Finally, the genetic stability of the cells cultured onto dental implants was determined by karyotyping. Our results demonstrated that Ti dental implants are not mutagenic, do not cause hemolysis, and are biocompatible. The MTT assay revealed that ADSCs, seeded on Ti dental implants, proliferate up to 30 days in culture. Moreover, ADSCs loaded on Ti dental implants show a substantial expression of some osteoblast specific markers, such as COL1A1, OPN, ALPL, and RUNX2, as well as chromosomal stability after 30 days of culture in a medium without osteogenic factors. In conclusion, the grit-blasted and acid-etched treatment seems to favor the adhesion and proliferation of ADSCs and improve the osteoinductivity of Ti dental implant surfaces.

  7. Adult Stem Cells Properties in Terms of Commitment, Aging and Biological Safety of Grit-Blasted and Acid-Etched Ti Dental Implants Surfaces

    PubMed Central

    Gardin, Chiara; Ferroni, Letizia; Bressan, Eriberto; Calvo - Guirado, José L.; Degidi, Marco; Piattelli, Adriano; Zavan, Barbara

    2014-01-01

    Titanium (Ti) is one of the most widely used biomaterials for manufacturing dental implants. The implant surface properties strongly influence osseointegration. The aim of the present study was to in vitro investigate the characteristics of Ti dental implants in terms of mutagenicity, hemocompatibility, biocompatibility, osteoinductivity and biological safety. The Ames test was used to test the mutagenicity of the Ti dental implants, and the hemolysis assay for evaluating their hemocompatibility. Human adipose - derived stem cells (ADSCs) were then seeded onto these implants in order to evaluate their cytotoxicity. Gene expression analyzing with real-time PCR was carried out to investigate the osteoinductivity of the biomaterials. Finally, the genetic stability of the cells cultured onto dental implants was determined by karyotyping. Our results demonstrated that Ti dental implants are not mutagenic, do not cause hemolysis, and are biocompatible. The MTT assay revealed that ADSCs, seeded on Ti dental implants, proliferate up to 30 days in culture. Moreover, ADSCs loaded on Ti dental implants show a substantial expression of some osteoblast specific markers, such as COL1A1, OPN, ALPL, and RUNX2, as well as chromosomal stability after 30 days of culture in a medium without osteogenic factors. In conclusion, the grit-blasted and acid-etched treatment seems to favor the adhesion and proliferation of ADSCs and improve the osteoinductivity of Ti dental implant surfaces. PMID:25635249

  8. In vivo assessment of bone ingrowth potential of three-dimensional e-beam produced implant surfaces and the effect of additional treatment by acid etching and hydroxyapatite coating.

    PubMed

    Biemond, J Elizabeth; Hannink, Gerjon; Jurrius, Annemarijn M G; Verdonschot, Nico; Buma, Pieter

    2012-03-01

    The bone ingrowth potential of three-dimensional E-beam-produced implant surfaces was examined by histology and compared to a porous plasma-sprayed control. The effects of acid etching and a hydroxyapatite (HA) coating were also evaluated by histology. Specimens were implanted in the distal femur of 10 goats. Histological analysis of bone ingrowth was performed 6 weeks after implantation. The E-beam-produced surfaces showed significantly better bone ingrowth compared to the plasma-sprayed control. Additional treatment of the E-beam surface structures with a HA coating, further improved bone ingrowth potential of these structures significantly. Acid etching of the E-beam structures did not influence bone ingrowth significantly. In conclusion, the HA-coated, E-beam-produced structures are promising potential implant surfaces.

  9. Photoinduced laser etching of a diamond surface

    SciTech Connect

    Kononenko, V V; Komlenok, M S; Pimenov, S M; Konov, V I

    2007-11-30

    Nongraphitising ablation of the surface of a natural diamond single crystal irradiated by nanosecond UV laser pulses is studied experimentally. For laser fluences below the diamond graphitisation threshold, extremely low diamond etching rates (less than 1nm/1000 pulses) are obtained and the term nanoablation is used just for this process. The dependence of the nanoablation rate on the laser fluence is studied for samples irradiated both in air and in oxygen-free atmosphere. The effect of external heating on the nanoablation rate is analysed and a photochemical mechanism is proposed for describing it. (interaction of laser radiation with matter. laser plasma)

  10. Shear bond strength of orthodontic brackets after acid-etched and erbium-doped yttrium aluminum garnet laser-etched

    PubMed Central

    Alavi, Shiva; Birang, Reza; Hajizadeh, Fatemeh

    2014-01-01

    Background: Laser ablation has been suggested as an alternative method to acid etching; however, previous studies have obtained contrasting results. The purpose of this study was to compare the shear bond strength (SBS) and fracture mode of orthodontic brackets that are bonded to enamel etched with acid and erbium-doped yttrium aluminum garnet (Er:YAG) laser. Materials and Methods: In this experimental in vitro study, buccal surfaces of 15 non-carious human premolars were divided into mesial and distal regions. Randomly, one of the regions was etched with 37% phosphoric acid for 15 s and another region irradiated with Er:YAG laser at 100 mJ energy and 20 Hz frequency for 20 s. Stainless steel brackets were then bonded using Transbond XT, following which all the samples were stored in distilled water for 24 h and then subjected to 500 thermal cycles. SBS was tested by a chisel edge, mounted on the crosshead of universal testing machine. After debonding, the teeth were examined under ×10 magnification and adhesive remnant index (ARI) score determined. SBS and ARI scores of the two groups were then compared using t-test and Mann-Whitney U test. Significant level was set at P < 0.05. Results: The mean SBS of the laser group (16.61 ± 7.7 MPa) was not significantly different from that of the acid-etched group (18.86 ± 6.09 MPa) (P = 0.41). There was no significant difference in the ARI scores between two groups (P = 0.08). However, in the laser group, more adhesive remained on the brackets, which is not suitable for orthodontic purposes. Conclusion: Laser etching at 100 mJ energy produced bond strength similar to acid etching. Therefore, Er:YAG laser may be an alternative method for conventional acid-etching. PMID:25097641

  11. Effects of rhBMP-2 on Sandblasted and Acid Etched Titanium Implant Surfaces on Bone Regeneration and Osseointegration: Spilt-Mouth Designed Pilot Study.

    PubMed

    Kim, Nam-Ho; Lee, So-Hyoun; Ryu, Jae-Jun; Choi, Kyung-Hee; Huh, Jung-Bo

    2015-01-01

    This study was conducted to evaluate effects of rhBMP-2 applied at different concentrations to sandblasted and acid etched (SLA) implants on osseointegration and bone regeneration in a bone defect of beagle dogs as pilot study using split-mouth design. Methods. For experimental groups, SLA implants were coated with different concentrations of rhBMP-2 (0.1, 0.5, and 1 mg/mL). After assessment of surface characteristics and rhBMP-2 releasing profile, the experimental groups and untreated control groups (n = 6 in each group, two animals in each group) were placed in split-mouth designed animal models with buccal open defect. At 8 weeks after implant placement, implant stability quotients (ISQ) values were recorded and vertical bone height (VBH, mm), bone-to-implant contact ratio (BIC, %), and bone volume (BV, %) in the upper 3 mm defect areas were measured. Results. The ISQ values were highest in the 1.0 group. Mean values of VBH (mm), BIC (%), and BV (%) were greater in the 0.5 mg/mL and 1.0 mg/mL groups than those in 0.1 and control groups in buccal defect areas. Conclusion. In the open defect area surrounding the SLA implant, coating with 0.5 and 1.0 mg/mL concentrations of rhBMP-2 was more effective, compared with untreated group, in promoting bone regeneration and osseointegration. PMID:26504807

  12. Effects of rhBMP-2 on Sandblasted and Acid Etched Titanium Implant Surfaces on Bone Regeneration and Osseointegration: Spilt-Mouth Designed Pilot Study

    PubMed Central

    Kim, Nam-Ho; Lee, So-Hyoun; Ryu, Jae-Jun; Choi, Kyung-Hee; Huh, Jung-Bo

    2015-01-01

    This study was conducted to evaluate effects of rhBMP-2 applied at different concentrations to sandblasted and acid etched (SLA) implants on osseointegration and bone regeneration in a bone defect of beagle dogs as pilot study using split-mouth design. Methods. For experimental groups, SLA implants were coated with different concentrations of rhBMP-2 (0.1, 0.5, and 1 mg/mL). After assessment of surface characteristics and rhBMP-2 releasing profile, the experimental groups and untreated control groups (n = 6 in each group, two animals in each group) were placed in split-mouth designed animal models with buccal open defect. At 8 weeks after implant placement, implant stability quotients (ISQ) values were recorded and vertical bone height (VBH, mm), bone-to-implant contact ratio (BIC, %), and bone volume (BV, %) in the upper 3 mm defect areas were measured. Results. The ISQ values were highest in the 1.0 group. Mean values of VBH (mm), BIC (%), and BV (%) were greater in the 0.5 mg/mL and 1.0 mg/mL groups than those in 0.1 and control groups in buccal defect areas. Conclusion. In the open defect area surrounding the SLA implant, coating with 0.5 and 1.0 mg/mL concentrations of rhBMP-2 was more effective, compared with untreated group, in promoting bone regeneration and osseointegration. PMID:26504807

  13. Improvement of photocatalytic activity of brookite titanium dioxide nanorods by surface modification using chemical etching

    NASA Astrophysics Data System (ADS)

    Zhang, Linjie; Menendez-Flores, Victor M.; Murakami, Naoya; Ohno, Teruhisa

    2012-05-01

    Surface morphology of brookite titanium dioxide (TiO2) nanorods was modified by chemical etching with aqueous hydrogen (H2O2)-ammonia (NH3) or sulfuric acid (H2SO4) solution. The brookite nanorods after chemical etching were characterized by TEM, SAED, FE-SEM, XRD and specific surface area measurements. Brookite nanorods after chemical etching with H2O2-NH3 solution exposed new crystal faces in the tips, and nanorods with sharper tips were observed. On the other hand, etching with H2SO4 at 200 °C induced morphological changes in the tip faces and broadened the angle between tip faces as a result of dissolution along the [0 0 1] direction, though brookite nanorods were only slightly etched after etching with H2SO4 at room temperature. Photocatalytic activity of brookite nanorods was tested by toluene decomposition in gas phase under ultraviolet irradiation. Brookite nanorods etched with H2O2-NH3 solution showed higher photocatalytic activity than that of brookite nanorods before etching. In the case of H2SO4 etching at 200 °C, brookite nanorods after etching exhibited lower photocatalytic activity. One reason for this may be that the formation of newly exposed crystal faces by H2O2-NH3 etching improved separation of redox sites due to their strong oxidation ability.

  14. Two modes of surface roughening during plasma etching of silicon: Role of ionized etch products

    SciTech Connect

    Nakazaki, Nobuya Tsuda, Hirotaka; Takao, Yoshinori; Eriguchi, Koji; Ono, Kouichi

    2014-12-14

    Atomic- or nanometer-scale surface roughening has been investigated during Si etching in inductively coupled Cl{sub 2} plasmas, as a function of rf bias power or ion incident energy E{sub i}, by varying feed gas flow rate, wafer stage temperature, and etching time. The experiments revealed two modes of surface roughening which occur depending on E{sub i}: one is the roughening mode at low E{sub i} < 200–300 eV, where the root-mean-square (rms) roughness of etched surfaces increases with increasing E{sub i}, exhibiting an almost linear increase with time during etching (t < 20 min). The other is the smoothing mode at higher E{sub i}, where the rms surface roughness decreases substantially with E{sub i} down to a low level < 0.4 nm, exhibiting a quasi-steady state after some increase at the initial stage (t < 1 min). Correspondingly, two different behaviors depending on E{sub i} were also observed in the etch rate versus √(E{sub i}) curve, and in the evolution of the power spectral density distribution of surfaces. Such changes from the roughening to smoothing modes with increasing E{sub i} were found to correspond to changes in the predominant ion flux from feed gas ions Cl{sub x}{sup +} to ionized etch products SiCl{sub x}{sup +} caused by the increased etch rates at increased E{sub i}, in view of the results of several plasma diagnostics. Possible mechanisms for the formation and evolution of surface roughness during plasma etching are discussed with the help of Monte Carlo simulations of the surface feature evolution and classical molecular dynamics simulations of etch fundamentals, including stochastic roughening and effects of ion reflection and etch inhibitors.

  15. 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.

  16. Five-year retrospective radiographic follow-up study of dental implants with sandblasting with large grit, and acid etching-treated surfaces

    PubMed Central

    2015-01-01

    Objectives The purpose of this study is to evaluate five-year radiographic follow-up results of the Korean sandblasting with large grit, and acid etching (SLA)-treated implant system. Materials and Methods The subjects of the study are 54 patients who have been followed-up to date, of the patients who underwent implant surgery from May 1, 2009 to April 30, 2011. In all, 176 implant placements were performed. Radiographs were taken before the first surgery, immediately after the first and second surgeries, immediately and six months after the final prosthesis installation, and every year after that. Bone loss was evaluated by the method suggested by Romanos and Nentwig. Results A total of 176 implant placements were performed-122 in men and 54 in women. These patients have been followed-up for an average of 4.9 years. In terms of prosthetic appliances, there were 156 bridges and 20 single prostheses. Nine implants installed in the maxillary molar area, three in the mandibular molar area and two in the maxillary premolar area were included in group M, with bone loss less than 2 mm at the crestal aspect of the implant. Of these, eight implants were single prostheses. In all, six implants failed-four in the mandible and two in the maxilla. All of these failures occurred in single-implant cases. The implant survival rate was 98.1% on the maxilla and 94.3% on the mandible, with an overall survival of 96.6%. Conclusion Within the limitations of this study, implants with the SLA surface have a very superior survival rate in relatively poor bone environments such as the maxilla. PMID:26734558

  17. Effect of acid etching time and technique on bond strength of an etch-and-rinse adhesive.

    PubMed

    Faria-e-Silva, André L; Silva, João L; Almeida, Thauanna G; Veloso, Francielle B; Ribeiro, Sandra M; Andrade, Tiago D; Vilas-Boas, Bruna V; Martins, Marisa C; Menezes, Murilo S

    2011-01-01

    The aim of this study was to evaluate the effect of acid etching time and technique on bond strength of a two-step etch-and-rinse adhesive system to dentin and enamel. Thirty human third molars were mesio-distally sectioned, parallel to the long axis of each tooth, in two halves. Buccal/lingual surfaces were abraded to obtain both flat exposed enamel and dentine. The etchant was applied with and without the use of dispensing tips provided by manufacturer. When the tip was not used, the etchant was agitated (active) over the substrate or left undisturbed (passive). The etchings were done for 15 or 30s. After rinsing the acid, the adhesive XP Bond (Dentsply Caulk, Milford, DE, USA) was applied and light-cured. Resin composite cylinders were built up on dentin and enamel substrates. A shear load was applied to the samples at a crosshead speed of 0.5 mm/min until failure. Data were statistically analyzed by three-way ANOVA and Tukey test (alpha = 0.05). There was no difference between the etching techniques in bonding to enamel. Application with the tip or active without the tip promoted higher bond strength to dentin than passive application. Extending the etching time reduced the bond strength to dentin and did not alter the values for enamel. The passive application without tips produced the lowest bond strength when the etchant was applied for 15s. All techniques demonstrated similar values for application during 30s. The acid etching time and technique significantly influence the bond strength of etch-and-rinse adhesive to dentin. PMID:22010410

  18. Strongly reduced Si surface recombination by charge injection during etching in diluted HF/HNO3.

    PubMed

    Greil, Stefanie M; Schöpke, Andreas; Rappich, Jörg

    2012-08-27

    Herein, we investigate the behaviour of the surface recombination of light-induced charge carriers during the etching of Si in alkaline (KOH) and acidic etching solutions of HF/HNO(3)/CH(3)COOH (HNA) or HF/HNO(3)/H(3)PO(4) (HNP) at different concentration ratios of HF and HNO(3) by means of photoluminescence (PL) measurements. The surface recombination velocity is strongly reduced during the first stages of etching in HF/HNO(3)-containing solutions pointing to a interface well passivated by the etching process, where a positive surface charge is induced by hole injection from NO-related surface species into the Si near-surface region (back surface field effect). This injected charge leads to a change in band bending by about 150 mV that repulses the light-induced charge carriers from the surface and therefore enhances the photoluminescence intensity, since non-radiative surface recombination is reduced.

  19. Bond strengths of all-ceramics: acid vs laser etching.

    PubMed

    Gökçe, B; Ozpinar, B; Dündar, M; Cömlekoglu, E; Sen, B H; Güngör, M A

    2007-01-01

    Various applications of dental lasers on dental materials have been proposed for surface modifications. This study evaluated whether laser etching could be an alternative to hydrofluoric acid (HF) etching. One hundred and ten lithia-based all-ceramic specimens (Empress 2) (R: 4 mm, h: 4 mm) were prepared and divided into five groups (n = 22/group). The untreated specimens served as the control, while one of the experimental groups was treated with 9.5% HF for 30 seconds. Three remaining test groups were treated with different laser (Er:YAG laser wavelength:2940 nm, OpusDent) power settings: 300 mJ, 600 mJ and 900 mJ. Ten specimens in each group were luted to the other 10 specimens by a dual-curing cement (Variolink II), and shear-bond strength (SBS) tests were performed (Autograph, crosshead speed: 0.5 mm/minute). The results were statistically analyzed (Kruskal Wallis and Mann Whitney-U, alpha = .05). Mean SBS (MPa) were 31.9 +/- 4.0, 41.4 +/- 4.3, 42.8 +/- 6.2, 29.2 +/- 4.5 and 27.4 +/- 3.8 for the control and HF, 300, 600 and 900 mJ groups, respectively. SEM evaluations revealed different surface morphologies depending on the laser parameters. The differences between HF acid and 300 mJ, when compared with the control, 600 and 900 mJ groups, were significant (p < .05). The 300 mJ laser group exhibited the highest shear-bond strength values, indicating that laser etching could also be used for surface treatments.

  20. Surface modification via wet chemical etching of single-crystalline silicon for photovoltaic application.

    PubMed

    Reshak, A H; Shahimin, M M; Shaari, S; Johan, N

    2013-11-01

    The potential of solar cells have not been fully tapped due to the lack of energy conversion efficiency. There are three important mechanisms in producing high efficiency cells to harvest solar energy; reduction of light reflectance, enhancement of light trapping in the cell and increment of light absorption. The current work represent studies conducted in surface modification of single-crystalline silicon solar cells using wet chemical etching techniques. Two etching types are applied; alkaline etching (KOH:IPA:DI) and acidic etching (HF:HNO3:DI). The alkaline solution resulted in anisotropic profile that leads to the formation of inverted pyramids. While acidic solution formed circular craters along the front surface of silicon wafer. This surface modification will leads to the reduction of light reflectance via texturizing the surface and thereby increases the short circuit current and conversion rate of the solar cells. PMID:24139943

  1. Surface modification via wet chemical etching of single-crystalline silicon for photovoltaic application.

    PubMed

    Reshak, A H; Shahimin, M M; Shaari, S; Johan, N

    2013-11-01

    The potential of solar cells have not been fully tapped due to the lack of energy conversion efficiency. There are three important mechanisms in producing high efficiency cells to harvest solar energy; reduction of light reflectance, enhancement of light trapping in the cell and increment of light absorption. The current work represent studies conducted in surface modification of single-crystalline silicon solar cells using wet chemical etching techniques. Two etching types are applied; alkaline etching (KOH:IPA:DI) and acidic etching (HF:HNO3:DI). The alkaline solution resulted in anisotropic profile that leads to the formation of inverted pyramids. While acidic solution formed circular craters along the front surface of silicon wafer. This surface modification will leads to the reduction of light reflectance via texturizing the surface and thereby increases the short circuit current and conversion rate of the solar cells.

  2. Effects of plasma etching solar cell front surfaces

    SciTech Connect

    Taylor, W.E.; Bunyan, S.M.; Olson, C.E.

    1980-01-01

    A front surface plasma etch with Freon 14+8% O/sub 2/ or sulfur hexafluoride (SF/sub 6/) was found to improve terrestrial solar cell output. SEM studies of these samples revealed surface pitting on Freon 14 etched samples. About 50% of the improvement from Freon etched samples can be attributed to the light capturing effects of surface pits. Output increases from SF/sub 6/ plasma etched cells were found to be comparable with Freon etched cells after subtraction of the light trapping effects. The excess output improvement might be attributed to reduced junction depth or removal of near surface lattice damage. Investigations attempting to identify the cause are described. 1 ref.

  3. Bone growth enhancement in vivo on press-fit titanium alloy implants with acid etched microtexture.

    PubMed

    Daugaard, Henrik; Elmengaard, Brian; Bechtold, Joan E; Soballe, Kjeld

    2008-11-01

    Early bone ongrowth secures long-term fixation of primary implants inserted without cement. Implant surfaces roughened with a texture on the micrometer scale are known to be osseoconductive. The aim of this study was to evaluate the bone formation at the surface of acid etched implants modified on the micro-scale. We compared implants with a nonparticulate texture made by chemical milling (hydrofluoric acid, nitric acid) (control) with implants that had a dual acid etched (hydrofluoric acid, hydrochloric acid) microtexture surface superimposed on the primary chemically milled texture. We used an experimental joint replacement model with cylindrical titanium implants (Ti-6Al-4V) inserted paired and press-fit in cancellous tibia metaphyseal bone of eight canines for 4 weeks and evaluated by histomorphometric quantification. A significant twofold median increase was seen for bone ongrowth on the acid etched surface [median, 36.1% (interquartile range, 24.3-44.6%)] compared to the control [18.4% (15.6-20.4%)]. The percentage of fibrous tissue at the implant surface and adjacent bone was significantly less for dual acid textured implants compared with control implants. These results show that secondary roughening of titanium alloy implant surface by dual acid etching increases bone formation at the implant bone interface. PMID:18186059

  4. Bone growth enhancement in vivo on press-fit titanium alloy implants with acid etched microtexture

    PubMed Central

    Daugaard, Henrik; Elmengaard, Brian; Bechtold, Joan E.; Soballe, Kjeld

    2013-01-01

    Early bone ongrowth secures long-term fixation of primary implants inserted without cement. Implant surfaces roughened with a texture on the micrometer scale are known to be osseoconductive. The aim of this study was to evaluate the bone formation at the surface of acid etched implants modified on the micro-scale. We compared implants with a nonparticulate texture made by chemical milling (hydrofluoric acid, nitric acid) (control) with implants that had a dual acid etched (hydrofluoric acid, hydrochloric acid) microtexture surface superimposed on the primary chemically milled texture. We used an experimental joint replacement model with cylindrical titanium implants (Ti-6Al-4V) inserted paired and press-fit in cancellous tibia metaphyseal bone of eight canines for 4 weeks and evaluated by histomorphometric quantification. A significant twofold median increase was seen for bone ongrowth on the acid etched surface [median, 36.1% (interquartile range, 24.3–44.6%)] compared to the control [18.4% (15.6–20.4%)]. The percentage of fibrous tissue at the implant surface and adjacent bone was significantly less for dual acid textured implants compared with control implants. These results show that secondary roughening of titanium alloy implant surface by dual acid etching increases bone formation at the implant bone interface. PMID:18186059

  5. The removal torque of titanium screw inserted in rabbit tibia treated by dual acid etching.

    PubMed

    Cho, Sung-Am; Park, Kyung-Tae

    2003-09-01

    Chemical acid etching alone of the titanium implant surface have the potential to greatly enhance osseointegration without adding particulate matter (e.g. TPS or hydroxyapatite) or embedding surface contaminants (e.g. grit particles). The aims of the present study were to evaluate any differences between the machined and dual acid etching implants with the removal torque as well as topographic analysis. A total of 40 custom-made, screw-shaped, commercially pure titanium implants with length of 5 mm and an outer diameter of 3.75 mm were divided into 4 groups, 10 screws in each, and chemical modification of the titanium implant surfaces were achieved using HF and HCl/H(2)SO(4) dual acid etching. The first exposure was to hydrofluoric acid and the second was to a combination of hydrochloric acid and sulfuric acid. The tibia metaphysics was exposed by incisions through the skin, fascia, and periosteum. One implant of each group was inserted in every rabbit, 2 in each proximal tibia metaphysics. Every rabbit received 3 implants with acid etched surfaces and 1 implant with a machined surface. Twelve weeks post-surgically, 7 rabbits were sacrificed, Subsequently, the leg was stabilized and the implant was removed under reverse torque rotation with a digital torque gauge (Mark-10 Corporation, USA) (Fig. 1). Twelve weeks after implant placement, the removal torque mean values were the dual acid etched implants (24%HF+HCl/H(2)SO(4), group C) required a higher average force (34.7 Ncm), than the machined surface implants (group A) (p=0.045) (Mann-Whiteney test). Scanning electron micrographs of acid etching of the titanium surface created an even distribution of very small (1-2 microm) peaks and valleys, while machining of the titanium surface created typical microscopically grooved surface characteristics. Nonetheless, there was no difference in surface topography between each acid etched implant groups. Therefore, chemically acid etching implant surfaces have higher

  6. 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

  7. Optimal conditions for the preparation of superhydrophobic surfaces on al substrates using a simple etching approach

    NASA Astrophysics Data System (ADS)

    Ruan, Min; Li, Wen; Wang, Baoshan; Luo, Qiang; Ma, Fumin; Yu, Zhanlong

    2012-07-01

    Many methods have been proposed to develop the fabrication techniques for superhydrophobic surfaces. However, such techniques are still at their infant stage and suffer many shortcomings. In this paper, the superhydrophobic surfaces on an Al substrate were prepared by a simple etching method. Effects of etching time, modifiers, and modification concentration and time were investigated, and optimal conditions for the best superhydrophobicity were studied. It was demonstrated that for etching the aluminum plate in Beck's dislocation, if the etching time was 15 s, modifier was Lauric acid-ethanol solution, and modification concentration and time was 5% and 1.5 h, respectively, the surface exhibited a water contact angle as high as 167.5° and a contact angle hysteresis as low as 2.3°.

  8. 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

  9. Etching of silicon surfaces using atmospheric plasma jets

    NASA Astrophysics Data System (ADS)

    Paetzelt, H.; Böhm, G.; Arnold, Th

    2015-04-01

    Local plasma-assisted etching of crystalline silicon by fine focused plasma jets provides a method for high accuracy computer controlled surface waviness and figure error correction as well as free form processing and manufacturing. We investigate a radio-frequency powered atmospheric pressure He/N2/CF4 plasma jet for the local chemical etching of silicon using fluorine as reactive plasma gas component. This plasma jet tool has a typical tool function width of about 0.5 to 1.8 mm and a material removal rate up to 0.068 mm3 min-1. The relationship between etching rate and plasma jet parameters is discussed in detail regarding gas composition, working distance, scan velocity and RF power. Surface roughness after etching was characterized using atomic force microscopy and white light interferometry. A strong smoothing effect was observed for etching rough silicon surfaces like wet chemically-etched silicon wafer backsides. Using the dwell-time algorithm for a deterministic surface machining by superposition of the local removal function of the plasma tool we show a fast and efficient way for manufacturing complex silicon structures. In this article we present two examples of surface processing using small local plasma jets.

  10. Surface engineering on CeO₂ nanorods by chemical redox etching and their enhanced catalytic activity for CO oxidation.

    PubMed

    Gao, Wei; Zhang, Zhiyun; Li, Jing; Ma, Yuanyuan; Qu, Yongquan

    2015-07-21

    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 Ce(3+) 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.

  11. Morphological categorization of acid-base resistant zones with self-etching primer adhesive systems.

    PubMed

    Inoue, Go; Nikaido, Toru; Sadr, Alireza; Tagami, Junji

    2012-01-01

    This study investigated the influence of the composition of self-etching primer adhesive systems on the morphology of acid-base resistant zones (ABRZs). One-step self-etching primer systems (Clearfil Tri-S Bond, G-Bond, and One-Up Bond F Plus) and two-step self-etching primer systems (Clearfil SE Bond, Clearfil Protect Bond, UniFil Bond, and Mac Bond II) were used in this study. Each adhesive was applied on prepared dentin disk surfaces, and a resin composite was placed between two dentin disks. All resin-bonded specimens were subjected to acid-base challenge. Observation under a scanning electron microscope (SEM) revealed the creation of an ABRZ adjacent to the hybrid layer for all the self-etch primer adhesive systems, even when non-fluoride releasing adhesives were used. The presence of fluoride in two-step self-etching adhesive significantly increased the thickness of ABRZ created. Results suggested that an ABRZ was created with the use of self-etching primer adhesive systems, but its morphology differed between one-and two-step self-etching primer adhesive systems and was influenced by fluoride release activity.

  12. Surface Modification of Nitinol by Chemical and Electrochemical Etching

    NASA Astrophysics Data System (ADS)

    Yang, Zhendi; Wei, Xiaojin; Cao, Peng; Gao, Wei

    2013-07-01

    In this paper, Nitinol, an equiatomic binary alloy of nickel and titanium, was surface modified for its potential biomedical applications by chemical and electrochemical etching. The main objective of the surface modification is to reduce the nickel content on the surface of Nitinol and simultaneously to a rough surface microstructure. As a result, better biocompatibility and better cell attachment would be achieved. The effect of the etching parameters was investigated, using scanning electron microscopy (SEM) equipped with energy dispersive X-ray spectrometry (EDX) and X-ray photoelectron spectrometry (XPS). The corrosion property of modified Nitinol surfaces was investigated by electrochemical work station. After etching, the Ni content in the surface layer has been reduced and the oxidation of Ti has been enhanced.

  13. Physico/chemical characterization and in vivo evaluation of nanothickness bioceramic depositions on alumina-blasted/acid-etched Ti-6Al-4V implant surfaces.

    PubMed

    Coelho, Paulo G; Lemons, Jack E

    2009-08-01

    The objective of this study was to physico/chemically characterize and evaluate the in vivo performance of two nanothickness ion beam assisted depositions (IBAD) of bioceramic coatings on implants in a beagle model. Alumina-blasted/acid-etched (AB/AE) Ti-6Al-4V implants were subjected to two different IBAD depositions (IBAD I and IBAD II), which were physico/chemically characterized by SEM, EDS, XPS, XPS + ion-beam milling (depth profiling), XRD, AFM, and ToF-SIMS. A beagle dog tibia model was utilized for histomorphometric and biomechanical (torque) comparison between AB/AE, IBAD I, IBAD II, and plasma-sprayed hydroxyapatite (PSHA) coated implants that remained in vivo for 3 and 5 weeks. The coatings were characterized as amorphous Ca-P with high Ca/P stoichiometries with thicknesses of an order of magnitude difference (IBAD I = 30-50 nm and IBAD II = 300-500 nm). The histomorphometric and biomechanical testing results showed that the 300-500 nm thickness deposition (IBAD II) and PSHA positively modulated bone healing at early implantation times. PMID:18508352

  14. Shear Bond Strength of an Etch-and-rinse Adhesive to Er:YAG Laser- and/or Phosphoric Acid-treated Dentin

    PubMed Central

    Davari, Abdolrahim; Sadeghi, Mostafa; Bakhshi, Hamid

    2013-01-01

    Background and aims. Er:YAG laser irradiation has been claimed to improve the adhesive properties of dentin; therefore, it has been proposed as an alternative to acid etching. The aim of this in vitro study was to investigate the shear bond strength of an etch-and-rinse adhesive system to dentin surfaces following Er:YAG laser and/or phosphoric acid etching. Materials and methods. The roots of 75 sound maxillary premolars were sectioned below the CEJ and the crowns were embedded in auto-polymerizing acrylic resin with the buccal surfaces facing up. The buccal surfaces were ground using a diamond bur and polished until the dentin was exposed; the samples were randomly divided into five groups (n=15) according to the surface treatment: (1) acid etching; (2) laser etching; (3) laser etching followed by acid etching; (4) acid etching followed by laser etching and (5) no acid etching and no laser etching (control group). Composite resin rods (Point 4, Kerr Co) were bonded to treated dentin surfaces with an etch-and-rise adhesive system (Optibond FL, Kerr Co) and light-cured.After storage for two weeks at 37°C and 100% humidity and then thermocycling, bond strength was measured with a Zwick Universal Testing Machine at a crosshead speed of 1 mm/min. Data was analyzed using parametric and non-parametric tests (P<0.05). Results. Mean shear bond strength for acid etching (20.1±1.8 MPa) and acid+laser (15.6±3.5 MPa) groups were significantly higher than those for laser+acid (15.6±3.5 MPa), laser etching (14.1±3.4 MPa) and control (8.1±2.1 MPa) groups. However, there were no significant differences between acid etching and acid+laser groups, and between laser+acid and laser groups. Conclusion. When the cavity is prepared by bur, it is not necessary to etch the dentin surface by Er:YAG laser following acid etching and acid etching after laser etching. PMID:23875083

  15. An in vitro comparison of acid etched vs. nonacid etched dentin bonding agents/composite interfaces over primary dentin.

    PubMed

    Donly, K J; Keprta, M; Stratmann, R G

    1991-01-01

    The purpose of this study was to evaluate acid etchant penetration on dentin bonding agents and its effect on the composite resin bond strength. Forty primary molars were mounted, then the buccal and lingual surfaces were prepared into dentin. The teeth were divided into four groups of 10, and four dentin bonding agents were placed on the buccal and lingual surfaces of exposed dentin, as recommended by the manufacturers. One surface of each tooth was etched randomly for 60 sec with 35% phosphoric acid. A standardized tube of composite resin was placed on each dentin surface and polymerized for 60 sec. The tubes were sheared off with an Instron Testing Machine. The specimens then were sectioned to be examined by a scanning electron microscope (SEM). Results demonstrated shear strengths (kg/cm2) of etched (e) and unetched (u) bonding agents to be: Scotchbond (3M Dental Products, St. Paul, MN) (e) 116.7 +/- 37.7, (u) 116.7 +/- 63.0; Scotchbond 2 (3M Dental Products, St. Paul, MN) (e) 112.0 +/- 40.6, (u) 127.0 +/- 38.7; Gluma (Bayer Dental, Leverkusen, Federal Republic of Germany) (e) 80.1 +/- 21.7, (u) 107.0 +/- 16.6; Bondlite (Kerr Manufacturing Co., Romulus, MI) (e) 53.4 +/- 34.7, (u) 79.1 +/- 26.3. The analysis of variance (ANOVA) demonstrated a statistical significance in variance at the P less than 0.001 level. Scheffe's Test indicated no statistically significant differences between the bond strengths of etched vs. nonetched dentin bonding agents and composite resin. SEM evaluation indicated that the acid etchant penetrated none of the dentin bonding agents. PMID:1886824

  16. 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

  17. Immunohistochemical and ultrastructural evaluation of the effects of phosphoric acid etching on dentin proteoglycans.

    PubMed

    Oyarzún, A; Rathkamp, H; Dreyer, E

    2000-12-01

    It has been reported that phosphoric acid (PA) produces structural and molecular alterations in dentin collagen fibrils; however, no relevant information exists on the influence of etching with PA on dentin non-collagenous macromolecules. The present study investigated, by immunohistochemistry and ultrastructural histochemistry, the behavior of dentin proteoglycans (PG) after etching human dentin samples with 35% PA gel (thickened with colloidal silica) or with a 35% PA liquid for 15, 30 and 120 s. Immunolabeling with a mouse monoclonal anti-chondroitin sulfate antibody demonstrated that glycosaminoglycans (GAG) were preserved within dentinal tubules opened to the surface after etching with PA gel. In addition, the cationic tracer polyethyleneimine, used for the ultramicroscopic localization of PG anionic sites, revealed that treatment of dentin samples with PA gel preserved the polyanionic peritubular PG in the etched area. On the other hand, etching with the PA liquid produced loss of peritubular GAG and PG anionic sites in the etched dentin surface. The results obtained indicated that similar concentrations of PA in gel or liquid formulations differently affect the organization of dentin PG. The clinical significance of these in vitro findings and the structural and molecular interactions of dentin PG with adhesive systems are still unknown.

  18. Halogens on Semiconductor Surfaces: Adsorption, Oxidation, and Etching.

    NASA Astrophysics Data System (ADS)

    Stepniak, Frank

    This dissertation presents studies of Si, GaAs, and InP surfaces following exposure to the halogens Cl _2 and Br_2. Synchrotron radiation photoemission is used to investigate the oxidation states of Si near the Si/SiO_2 interface as a function of Cl_2 exposure. Oxidation of highly ordered surfaces shows no dependence of the oxidation state concentration on Cl_2 inclusion in the gas mixture. For less-than-ideal Si surfaces, oxidation with O_2 -only results in a broader transition region, and presumably, inferior electrical properties. The addition of Cl_2 in the oxidizing gas reduced the concentration of intermediate oxides by a factor of two for these disordered starting Si surfaces. A new feature is also measured from Cl-Si bonds that we associate with passivation of Si defects at the oxide interface. The adsorption and reactivity of Br_2 and Cl_2 on GaAs(110) and InP(110) was studied in the temperature range of 25 K < T < 625 K with photoemission spectroscopy and scanning tunneling microscopy. Initial halogen adsorption was dissociative at all temperatures and we find that a simple model where the halogen atoms bond to a single Ga or As surface site can not account for the complex surface chemistry and morphology. Thermally-activated etching was observed after warming a surface with chemisorbed Br or Cl. Etching resulted from the formation and eventual temperature dependent desorption of the trihalides of Ga and As. For halogen exposures where T < 650 K, monohalide-like surface bonding persist during the etching process and the etched surface is rough. For T > 700 K, the surface is essentially free of halogen and etching occurs in a nearly layer-by-layer fashion.

  19. 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

  20. Surface/interface morphology and bond strength to glass ceramic etched for different periods.

    PubMed

    Naves, Lucas Z; Soares, Carlos J; Moraes, Rafael R; Gonçalves, Luciano S; Sinhoreti, Mário Alexandre C; Correr-Sobrinho, Lourenço

    2010-01-01

    This study evaluated the influence of etching periods on the surface/interface morphology and bond strength to glass ceramic with or without application of an unfilled resin after silane. Ceramic discs were divided into 12 groups, defined by etching time with 10% hydrofluoric acid: G1/G7--etching for 10 seconds, G2/G8--20 seconds; G3/G9--40 seconds; G4/G10--60 seconds; G5/G11--120 seconds and G6/G12--60 + 60 seconds. All the groups were silanated after etching and G7 - G12 received a layer of unfilled resin after silane. Microshear testing using resin cement was performed, with 12 resin cylinders tested per group. The data was submitted to two-way ANOVA and the Student-Newman-Keuls' test (p<0.05). Evaluation of the etching pattern and bonding interfaces was conducted by SEM. The bond strength means (MPa) were: 19.4 +/- 3.5, 22.3 +/- 5.1, 22.2 +/- 3.2, 17.8 +/- 2.1, 15.3 +/- 3.0 and 14.3 +/- 1.8 for G1-G6 and 17.4 +/- 4.8, 21.3 +/- 2.1, 21.1 +/- 2.3, 24.7 +/- 5.8, 20.4 +/- 2.2 and 18.5 +/- 4.6 for G7-G12. Poor etching was detected after 10 seconds of conditioning; whereas deep channels were extensively observed on surfaces etched for 120 and 60 + 60 seconds. Unfilled voids underlying the ceramic-cement interface were detected when only silane was applied. Full completion of the irregularities on G11 was detected using unfilled resin. When only silane was applied, the 60-second group and those etched for longer periods showed lower bond strengths. When both silane and unfilled resin were applied, all etching periods generally showed similar values. In conclusion, the etching period influenced the surface/interface topography and bond strength to ceramic. The application of unfilled resin was able to infiltrate all unfilled voids beneath the ceramic-cement interface, except on re-etched surfaces.

  1. Preliminary surface analysis of etched, bleached, and normal bovine enamel

    SciTech Connect

    Ruse, N.D.; Smith, D.C.; Torneck, C.D.; Titley, K.C. )

    1990-09-01

    X-ray photoelectron spectroscopic (XPS) and secondary ion-mass spectroscopic (SIMS) analyses were performed on unground un-pumiced, unground pumiced, and ground labial enamel surfaces of young bovine incisors exposed to four different treatments: (1) immersion in 35% H2O2 for 60 min; (2) immersion in 37% H3PO4 for 60 s; (3) immersion in 35% H2O2 for 60 min, in distilled water for two min, and in 37% H3PO4 for 60 s; (4) immersion in 37% H3PO4 for 60 s, in distilled water for two min, and in 35% H2O2 for 60 min. Untreated unground un-pumiced, unground pumiced, and ground enamel surfaces, as well as synthetic hydroxyapatite surfaces, served as controls for intra-tooth evaluations of the effects of different treatments. The analyses indicated that exposure to 35% H2O2 alone, besides increasing the nitrogen content, produced no other significant change in the elemental composition of any of the enamel surfaces investigated. Exposure to 37% H3PO4, however, produced a marked decrease in calcium (Ca) and phosphorus (P) concentrations and an increase in carbon (C) and nitrogen (N) concentrations in unground un-pumiced specimens only, and a decrease in C concentration in ground specimens. These results suggest that the reported decrease in the adhesive bond strength of resin to 35% H2O2-treated enamel is not caused by a change in the elemental composition of treated enamel surfaces. They also suggest that an organic-rich layer, unaffected by acid-etching, may be present on the unground un-pumiced surface of young bovine incisors. This layer can be removed by thorough pumicing or by grinding. An awareness of its presence is important when young bovine teeth are used in a model system for evaluation of resin adhesiveness.

  2. Characterization of electric discharge machining, subsequent etching and shot-peening as a surface treatment for orthopedic implants

    NASA Astrophysics Data System (ADS)

    Stráský, Josef; Havlíková, Jana; Bačáková, Lucie; Harcuba, Petr; Mhaede, Mansour; Janeček, Miloš

    2013-09-01

    Presented work aims at multi-method characterization of combined surface treatment of Ti-6Al-4V alloy for biomedical use. Surface treatment consists of consequent use of electric discharge machining (EDM), acid etching and shot peening. Surface layers are analyzed employing scanning electron microscopy and energy dispersive X-ray spectroscopy. Acid etching by strong Kroll's reagent is capable of removing surface layer of transformed material created by EDM. Acid etching also creates partly nanostructured surface and significantly contributes to the enhanced proliferation of the bone cells. The cell growth could be positively affected by the superimposed bone-inspired structure of the surface with the morphological features in macro-, micro- and nano-range. Shot peening significantly improves poor fatigue performance after EDM. Final fatigue performance is comparable to benchmark electropolished material without any adverse surface effect. The proposed three-step surface treatment is a low-cost process capable of producing material that is applicable in orthopedics.

  3. Effect of hydrofluoric acid etching duration on the roughness and flexural strength of a lithium disilicate-based glass ceramic.

    PubMed

    Zogheib, Lucas Villaça; Bona, Alvaro Della; Kimpara, Estevão Tomomitsu; McCabe, John F

    2011-01-01

    The aim of this study was to examine the effect of different acid etching times on the surface roughness and flexural strength of a lithium disilicate-based glass ceramic. Ceramic bar-shaped specimens (16 mm x 2 mm x 2 mm) were produced from ceramic blocks. All specimens were polished and sonically cleaned in distilled water. Specimens were randomly divided into 5 groups (n=15). Group A (control) no treatment. Groups B-E were etched with 4.9% hydrofluoric acid (HF) for 4 different etching periods: 20 s, 60 s, 90 s and 180 s, respectively. Etched surfaces were observed under scanning electron microscopy. Surface profilometry was used to examine the roughness of the etched ceramic surfaces, and the specimens were loaded to failure using a 3-point bending test to determine the flexural strength. Data were analyzed using one-way ANOVA and Tukey's test (?=0.05). All etching periods produced significantly rougher surfaces than the control group (p<0.05). Roughness values increased with the increase of the etching time. The mean flexural strength values were (MPa): A=417 ± 55; B=367 ± 68; C=363 ± 84; D=329 ± 70; and E=314 ± 62. HF etching significantly reduced the mean flexural strength as the etching time increased (p=0.003). In conclusion, the findings of this study showed that the increase of HF etching time affected the surface roughness and the flexural strength of a lithium disilicate-based glass ceramic, confirming the study hypothesis.

  4. Surface Modification of Polymer Photoresists in Fluorocarbon Plasma Etching

    NASA Astrophysics Data System (ADS)

    Wang, Mingmei; Kushner, Mark

    2009-10-01

    In plasma etching of high aspect ratio (AR), nm sized features, erosion of polymer photoresist (PR) can perturb the feature profile (e.g., bowing). Although cross-linking of PR due to ion and VUV fluxes could make it more resistive to etching, typically the PR etch rate is too high to maintain the pattern when the AR is large (> 20). In dielectric plasma etching using fluorocarbon gases, one strategy to prevent PR erosion is to deposit a (CxFy)n polymer on its surface. This process may be enhanced in dc-augmented capacitively coupled plasmas (CCPs) by sputtering of Si and CxFy from the dc biased electrode. Dangling bonds generated on the PR surface by ion, photon or electron bombardment trap Si and CxFy radicals forming Si-C and C-C bonds. Sputtered Si atoms can also react with CxFy radicals to produce more reactive CxFy-1 radicals which are more easily incorporated into the PR. In this talk we discuss scaling laws for radical production derived from a computational investigation of a dc-augmented dual frequency CCP reactor sustained in Ar/C4F8/O2. Fluxes of Si radicals are produced by sputtering of the dc electrode. Rates of polymer deposition on and sputtering of PR, and consequences of PR erosion (and deposition) on feature profiles will be discussed.

  5. Scanning Acoustic Microscopy Investigation of Frequency-Dependent Reflectance of Acid-Etched Human Dentin Using Homotopic Measurements

    PubMed Central

    Marangos, Orestes; Misra, Anil; Spencer, Paulette; Katz, J. Lawrence

    2013-01-01

    Composite restorations in modern restorative dentistry rely on the bond formed in the adhesive-infiltrated acid-etched dentin. The physical characteristics of etched dentin are, therefore, of paramount interest. However, characterization of the acid-etched zone in its natural state is fraught with problems stemming from a variety of sources including its narrow size, the presence of water, heterogeneity, and spatial scale dependency. We have developed a novel homotopic (same location) measurement methodology utilizing scanning acoustic microscopy (SAM). Homotopic measurements with SAM overcome the problems encountered by other characterization/ imaging methods. These measurements provide us with acoustic reflectance at the same location of both the pre- and post-etched dentin in its natural state. We have applied this methodology for in vitro measurements on dentin samples. Fourier spectra from acid-etched dentin showed amplitude reduction and shifts of the central frequency that were location dependent. Through calibration, the acoustic reflectance of acid-etched dentin was found to have complex and non-monotonic frequency dependence. These data suggest that acid-etching of dentin results in a near-surface graded layer of varying thickness and property gradations. The measurement methodology described in this paper can be applied to systematically characterize mechanical properties of heterogeneous soft layers and interfaces in biological materials. PMID:21429849

  6. Optical fiber nanoprobe preparation for near-field optical microscopy by chemical etching under surface tension and capillary action.

    PubMed

    Mondal, Samir K; Mitra, Anupam; Singh, Nahar; Sarkar, S N; Kapur, Pawan

    2009-10-26

    We propose a technique of chemical etching for fabrication of near perfect optical fiber nanoprobe (NNP). It uses photosensitive single mode optical fiber to etch in hydro fluoric (HF) acid solution. The difference in etching rate for cladding and photosensitive core in HF acid solution creates capillary ring along core-cladding boundary under a given condition. The capillary ring is filled with acid solution due to surface tension and capillary action. Finally it creates near perfect symmetric tip at the apex of the fiber as the height of the acid level in capillary ring decreases while width of the ring increases with continuous etching. Typical tip features are short taper length (approximately 4 microm), large cone angle (approximately 38 degrees ), and small probe tip dimension (<100 nm). A finite difference time domain (FDTD) analysis is also presented to compare near field optics of the NNP with conventional nanoprobe (CNP). The probe may be ideal for near field optical imaging and sensor applications.

  7. Temperature Rise Induced by Light Curing Unit Can Shorten Enamel Acid-Etching Time

    PubMed Central

    Najafi Abrandabadi, Ahmad; Sheikh-Al-Eslamian, Seyedeh Mahsa; Panahandeh, Narges

    2015-01-01

    Objectives: The aim of this in-vitro study was to assess the thermal effect of light emitting diode (LED) light curing unit on the enamel etching time. Materials and Methods: Three treatment groups with 15 enamel specimens each were used in this study: G1: Fifteen seconds of etching, G2: Five seconds of etching, G3: Five seconds of etching plus LED light irradiation (simultaneously). The micro shear bond strength (μSBS) of composite resin to enamel was measured. Results: The mean μSBS values ± standard deviation were 51.28±2.35, 40.47±2.75 and 50.00±2.59 MPa in groups 1, 2 and 3, respectively. There was a significant difference between groups 1 and 2 (P=0.013) and between groups 2 and 3 (P=0.032) in this respect, while there was no difference between groups 1 and 3 (P=0.932). Conclusion: Simultaneous application of phosphoric acid gel over enamel surface and light irradiation using a LED light curing unit decreased enamel etching time to five seconds without compromising the μSBS. PMID:27559352

  8. Phosphoric acid-etching promotes bond strength and formation of acid-base resistant zone on enamel.

    PubMed

    Li, N; Nikaido, T; Alireza, S; Takagaki, T; Chen, J-H; Tagami, J

    2013-01-01

    This study examined the effect of phosphoric acid (PA) etching on the bond strength and acid-base resistant zone (ABRZ) formation of a two-step self-etching adhesive (SEA) system to enamel. An etch-and-rinse adhesive (EAR) system Single Bond (SB) and a two-step SEA system Clearfil SE Bond (SE) were used. Human teeth were randomly divided into four groups according to different adhesive treatments: 1) SB; 2) SE; 3) 35% PA etching→SE primer→SE adhesive (PA/SEp+a); (4) 35% PA etching→SE adhesive (PA/SEa). Microshear bond strength to enamel was measured and then statistically analyzed using one-way analysis of variance and the Tukey honestly significant difference test. The failure mode was recorded and analyzed by χ( 2 ) test. The etching pattern of the enamel surface was observed with scanning electron microscope (SEM). The bonded interface was exposed to a demineralizing solution (pH=4.5) for 4.5 hours and then 5% sodium hypochlorite with ultrasonication for 30 minutes. After argon-ion etching, the interfacial ultrastructure was observed using SEM. The microshear bond strength to enamel of the SE group was significantly lower (p<0.05) than that of the three PA-etched groups, although the latter three were not significantly different from one another. The ABRZ was detected in all the groups. In morphological observation, the ABRZ in the three PA-etched groups were obviously thicker compared with the SE group with an irregular wave-shaped edge.

  9. Effect of acid etching time and technique on interfacial characteristics of the adhesive-dentin bond using differential staining.

    PubMed

    Wang, Yong; Spencer, Paulette

    2004-06-01

    Dentin bonding using the total-etch method has been claimed to be technique-sensitive. The aim of this study is to examine the effect of acid-etch variations on the dentin demineralization and interfacial structure of the adhesive-dentin bond using a differential staining technique. Single Bond adhesive with 35% phosphoric acid gel was used. The occlusal one-third of the crown was removed from 60 extracted, unerupted human third molars. Smear layers were created by abrading the dentin with 600 grit SiC under water for 30 s. The prepared teeth were randomly assigned to four groups according to etching time (Group 1, 10 s; Group 2, 15 s; Group 3, 30 s; Group 4, 60 s). In each group, the etching gel was: (i) applied and spread to the dentin surface and left to stand undisturbed; (ii) applied and gently agitated during etching; (iii) applied without using dispensing tips for the syringe and left for the same period as above. After rinsing, the etched dentin was then treated with the adhesive per manufacturers' instructions. 3-5 micro m thin sections of the adhesive/dentin (a/d) interface were cut with a microtome and stained with Goldner's trichrome. Stained, thin sections from each prepared tooth were imaged with light microscopy. The depth and extent of dentin demineralization, and the a/d interdiffusion zone were clearly visible by this differential staining microtechnique. The thickness of the interdiffusion zone increased as a function of etching time. However, the etchant gel application methods have a significant influence on dentin demineralization. Although agitating acid gel facilitates the penetration and etching into dentin, it should not be recommended, especially for longer etching time. These results indicated that the etching technique has a large effect on the profile of both dentin demineralization and interfacial structure.

  10. Metal-oxide-semiconductor characterization of silicon surfaces thermally oxidized after reactive ion etching and magnetically enhanced reactive ion etching

    SciTech Connect

    Settlemyer, K.T. Jr.; Ruzyllo, J.; Hwang, D.K.

    1993-03-01

    In this study the performance of reactive ion etching (RIE) and magnetically enhanced reactive ion etching (MERIE) processes in pregate oxidation etching of the field oxide are compared. The comparison is carried out through metal-oxide-semiconductor (MOS) characterization of oxides and interfaces formed on etched silicon surfaces. The results revealed differences in the outcome of RIE and MERIE processes with the latter displaying overall superior characteristics. MERIE induced surface damage is shallower, and is mostly removed during oxide growth. RIE damage propagates deeper into the Si bulk and still influences the MOS devices even after the top Si layers are converted into the oxide. The results obtained emphasize the importance of adequate cleaning of silicon surfaces following RIE/MERIE processes. 5 refs., 4 figs.

  11. Laser micromachined and acid-etched Fabry-Perot cavities in silica fibres

    NASA Astrophysics Data System (ADS)

    Machavaram, V. R.; Tuck, C. J.; Teagle, M. C.; Badcock, R. A.; Fernando, G. F.

    2006-01-01

    This paper reports on two techniques for creating Fabry-Perot cavities in conventional single- and multi-mode optical fibres. The authors have reported previously on the design and fabrication of extrinsic fibre Fabry-Perot interferometric multi-functional sensors. Here, the authors report on two novel techniques for creating intrinsic fibre optic sensors based on the Fabry-Perot etalon. The first technique involved the use of hydrofluoric acid to preferentially etch the core of the optical fibre. This technique is simple to carry out and provides a cost-effective means for manufacturing intrinsic fibre Fabry-Perot sensors. In the second technique, a 157 nm excimer laser along with a custom-designed beam delivery system was used to ablate (micro-machine) near-paralleled walled cavities through the diameter of the optical fibre (outer diameter of 125 μm). The paper details the experimental methodology and the associated instrumentation for the two techniques. The acid etched and laser ablated cavities were characterised using a 3-D surface profiler, optical and scanning electron microscopy. The feasibility of using these cavities as intrinsic fibre Fabry-Perot strain sensors is demonstrated. This was achieved by surface-mounting the acid etched cavities on to composite tensile test specimens. The output from the optical fibre devices was compared with surface-mounted electrical resistance strain gauges.

  12. Superamphiphobic surface by nanotransfer molding and isotropic etching.

    PubMed

    Lee, Sang Eon; Kim, Han-Jung; Lee, Su-Han; Choi, Dae-Geun

    2013-06-25

    We present a novel method of fabricating superhydrophobic and superoleophobic surfaces with nanoscale reentrant curvature by nanotransfer molding and controlled wet etching of the facile undercut. This method produces completely ordered re-entrant nanostructures and prevents capillary-induced bundling effects. The mushroom-like, re-entrant, overhanging structure demonstrates superhydrophobic and superoleophobic characteristics, as tested by water droplet bouncing and contact angle measurements, and has high transparency on a flexible substrate. Widespread use as self-cleaning surfaces is expected in the near future.

  13. Surface Smoothing and etching by gas cluster ion beam

    NASA Astrophysics Data System (ADS)

    Song, J. H.; Choi, W. K.

    2003-08-01

    Ar and CO2 gas cluster ion beam with a few nm size were generated by an adiabatic expansion through Laval nozzle. The existence and the mean size distribution of the cluster were analyzed by time-of-flight measurement. Crater induced by Ar cluster ion beam and crown-like hillock by CO2 cluster ion impact on Si(100) were observed by an atomic force microcopy. CO2 cluster ion was irradiated on Si at 25 kV with the variations of ion dose from 1010 to 1013 cluster ions(CI)/cm2, at the flux of 109/cm2 s. Through this isolated cluster ion impact, the interaction mechanism between cluster ion with solid surface was suggested to be made of three steps: surface embossment, surface sputtering and smoothing, and surface etching. Another surface smoothing and etching experiment using CO2 cluster ion beam were carried out over ITO/glass and Cr-masked Si3N4 thin film surfaces at 25 kV.

  14. Bonding to enamel/dentin etched with phosphoric and hydrofluoric acids.

    PubMed

    Barghi, Nassar; Covington, Kendra; Fischer, Dan E; Herbold, Edward T

    2004-10-01

    Repairing porcelain intraorally allows clinicians to provide their patients with a conservative means of treating fractured or debonded restorations. This requires, however, the etching of both porcelain and tooth structure with etching solutions. It is thus relevant to understand the effect that different etching procedures have on shear bond strengths of composite resins to both dentin and enamel structures. Based on the results of this investigation, the authors recommend isolation of tooth structures and the etching of porcelain with hydrofluoric acid.

  15. HF-based etching processes for improving laser damage resistance of fused silica optical surfaces

    SciTech Connect

    Suratwala, T I; Miller, P E; Bude, J D; Steele, R A; Shen, N; Monticelli, M V; Feit, M D; Laurence, T A; Norton, M A; Carr, C W; Wong, L L

    2010-02-23

    The effect of various HF-based etching processes on the laser damage resistance of scratched fused silica surfaces has been investigated. Conventionally polished and subsequently scratched fused silica plates were treated by submerging in various HF-based etchants (HF or NH{sub 4}F:HF at various ratios and concentrations) under different process conditions (e.g., agitation frequencies, etch times, rinse conditions, and environmental cleanliness). Subsequently, the laser damage resistance (at 351 or 355 nm) of the treated surface was measured. The laser damage resistance was found to be strongly process dependent and scaled inversely with scratch width. The etching process was optimized to remove or prevent the presence of identified precursors (chemical impurities, fracture surfaces, and silica-based redeposit) known to lead to laser damage initiation. The redeposit precursor was reduced (and hence the damage threshold was increased) by: (1) increasing the SiF{sub 6}{sup 2-} solubility through reduction in the NH4F concentration and impurity cation impurities, and (2) improving the mass transport of reaction product (SiF{sub 6}{sup 2-}) (using high frequency ultrasonic agitation and excessive spray rinsing) away from the etched surface. A 2D finite element crack-etching and rinsing mass transport model (incorporating diffusion and advection) was used to predict reaction product concentration. The predictions are consistent with the experimentally observed process trends. The laser damage thresholds also increased with etched amount (up to {approx}30 {micro}m), which has been attributed to: (1) etching through lateral cracks where there is poor acid penetration, and (2) increasing the crack opening resulting in increased mass transport rates. With the optimized etch process, laser damage resistance increased dramatically; the average threshold fluence for damage initiation for 30 {micro}m wide scratches increased from 7 to 41 J/cm{sup 2}, and the statistical

  16. Surface and thin film studies of the etching of molybdenum by xenon difluoride

    NASA Astrophysics Data System (ADS)

    Celik, Ozgur

    The controlled etching of micro/nano structures is essential for a variety of technological applications, including microelectromechanical systems (MEMS) fabrication. XeF2 is an isotropic and highly selective etching gas used to remove semiconductors and metals in the fabrication of MEMS and other devices. While the kinetics of XeF2 etching Si has been widely documented, XeF2 etching of metals is not widely understood. For better process control and device quality, it is important to understand the etching mechanism at the molecular level. In this work, we explore the surface and gas phase chemistry of XeF2 etching Mo films. Studies on the general characteristics of etching Mo blanket films were carried out on 1000AMo/475ASiO2/100ANi/glass samples at different sample temperatures and etchant pressures in a standalone etching chamber. They were analyzed ex-situ by atomic force microscopy (AFM) and x-ray photoelectron spectroscopy (XPS) for investigating morphology and chemical composition of the surfaces after etchings, respectively. Rutherford back scattering (RBS) was used to measure the thickness of the films and the depth profile of near-surface species after etching. Downstream mass spectrometry was used to identify the volatile products of the etching process. The composition and chemical state of the etched surface (reaction layer) is further investigated by in-vacuo etching and XPS analysis experiments using 3750AMo/quartz samples in an integrated etching/analysis system. The XPS studies have clarified issues on: (i) the thickness and chemical composition of the reaction layer during etching, (ii) the effects of the surface native oxides and adventitious hydrocarbons on the initiation and progress of etching, (iii) the re-deposition of etched products. Post-etching thermal processing and XPS analysis studies were performed to investigate the chemical composition of residues left after etching. Kinetics of etching blanket Mo films was investigated using total

  17. Micro/nanofabrication of poly(L-lactic acid) using focused ion beam direct etching

    NASA Astrophysics Data System (ADS)

    Oyama, Tomoko Gowa; Hinata, Toru; Nagasawa, Naotsugu; Oshima, Akihiro; Washio, Masakazu; Tagawa, Seiichi; Taguchi, Mitsumasa

    2013-10-01

    Micro/nanofabrication of biocompatible and biodegradable poly(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 attachment properties.

  18. Hydrofluoric acid etched stainless steel wire for solid-phase microextraction.

    PubMed

    Xu, Hua-Ling; Li, Yan; Jiang, Dong-Qing; Yan, Xiu-Ping

    2009-06-15

    Stainless steel wire has been widely used as the substrate of solid-phase microextraction (SPME) fibers to overcome the shortcomings of conventional silica fibers such as fragility, by many researchers. However, in previous reports various sorbent coatings are always required in conjunction with the stainless steel wire for SPME. In this work, we report the bare stainless steel wire for SPME without the need for any additional coatings taking advantage of its high mechanical and thermal stability. To evaluate the performance of stainless steel wire for SPME, polycyclic aromatic hydrocarbons (PAHs), benzene, toluene, ethylbenzene, chlorobenzene, n-propylbenzene, aniline, phenol, n-hexane, n-octane, n-decane, n-undecane, n-dodecane, chloroform, trichloroethylene, n-octanol, and butanol were tested as analytes. Although the stainless steel wire had almost no extraction capability toward the tested analytes before etching, it did exhibit high affinity to the tested PAHs after etching with hydrofluoric acid. The etched stainless steel wire gave a much bigger enhancement factor (2541-3981) for the PAHs than the other analytes studied (< or = 515). Etching with hydrofluoric acid produced a porous and flower-like structure with Fe(2)O(3), FeF(3), Cr(2)O(3), and CrF(2) on the surface of the stainless steel wire, giving high affinity to the PAHs due to cation-pi interaction. On the basis of the high selectivity of the etched stainless steel wire for PAHs, a new SPME method was developed for gas chromatography with flame ionization detection to determine PAHs with the detection limits of 0.24-0.63 microg L(-1). The precision for six replicate extractions using one SPME fiber ranged from 2.9% to 5.3%. The fiber-to-fiber reproducibility for three parallel prepared fibers was 4.3-8.8%. One etched stainless steel wire can stand over 250 cycles of SPME without significant loss of extraction efficiency. The developed etched stainless steel wire is very stable, highly selective, and

  19. 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

  20. Formation of plasma induced surface damage in silica glass etching for optical waveguides

    NASA Astrophysics Data System (ADS)

    Choi, D. Y.; Lee, J. H.; Kim, D. S.; Jung, S. T.

    2004-06-01

    Ge, B, P-doped silica glass films are widely used as optical waveguides because of their low losses and inherent compatibility with silica optical fibers. These films were etched by ICP (inductively coupled plasma) with chrome etch masks, which were patterned by reactive ion etching (RIE) using chlorine-based gases. In some cases, the etched surfaces of silica glass were very rough (root-mean square roughness greater than 100 nm) and we call this phenomenon plasma induced surface damage (PISD). Rough surface cannot be used as a platform for hybrid integration because of difficulty in alignment and bonding of active devices. PISD reduces the etch rate of glass and it is very difficult to remove residues on a rough surface. The objective of this study is to elucidate the mechanism of PISD formation. To achieve this goal, PISD formation during different etching conditions of chrome etch mask and silica glass was investigated. In most cases, PISD sources are formed on a glass surface after chrome etching, and metal compounds are identified in theses sources. Water rinse after chrome etching reduces the PISD, due to the water solubility of metal chlorides. PISD is decreased or even disappeared at high power and/or low pressure in glass etching, even if PISD sources were present on the glass surface before etching. In conclusion, PISD sources come from the chrome etching process, and polymer deposition on these sources during the silica etching cause the PISD sources to grow. In the area close to the PISD source there is a higher ion flux, which causes an increase in the etch rate, and results in the formation of a pit.

  1. Bone contact around acid-etched implants: a histological and histomorphometrical evaluation of two human-retrieved implants.

    PubMed

    Degidi, Marco; Petrone, Giovanna; Iezzi, Giovanna; Piattelli, Adriano

    2003-01-01

    The surface characteristics of dental implants play an important role in their clinical success. One of the most important surface characteristics of implants is their surface topography or roughness. Many techniques for preparing dental implant surfaces are in clinical use: turning, plasma spraying, coating, abrasive blasting, acid etching, and electropolishing. The Osseotite surface is prepared by a process of thermal dual etching with hydrochloric and sulfuric acid, which results in a clean, highly detailed surface texture devoid of entrapped foreign material and impurities. This seems to enhance fibrin attachment to the implant surface during the clotting process. The authors retrieved 2 Osseotite implants after 6 months to repair damage to the inferior alveolar nerve. Histologically, both implants appeared to be surrounded by newly formed bone. No gaps or fibrous tissues were present at the interface. The mean bone-implant contact percentage was 61.3% (+/- 3.8%). PMID:12614080

  2. Color Stability of Enamel following Different Acid Etching and Color Exposure Times

    PubMed Central

    Jahanbin, Arezoo; Basafa, Mohammad; Moazzami, Mostafa; Basafa, Behnoush; Eslami, Neda

    2014-01-01

    Background and aims. The aim of this study was to evaluate the effect of different etching times on enamel color stability after immediate versus delayed exposure to colored artificial saliva (CAS). Materials and methods. Human first premolars were divided into five groups of twenty. A colorimeter was used according to the CIE system on the mid-buccal and mid-lingual surfaces to evaluate initial tooth color. Samples in group A remained unetched. In groups B to E, buccal and lingual surfaces were initially etched with phosphoric acid for 15 and 60 seconds, respectively. Then, the samples in groups A and C were immersed in colored artificial saliva (cola+saliva). In group B, the teeth were immersed in simple artificial saliva (AS). Samples in groups D and E were immersed in AS for 24 and 72 hours, respectively before being immersed in colored AS. The teeth were immersed for one month in each solution before color measurement. During the test period, the teeth were retrieved from the staining solution and stored in AS for five minutes. This was repeated 60 times. Color changes of buccal and lingual surfaces were calculated. Kruskal-Wallis and Wilcoxon tests were used for statistical analysis (α ≤0.05). Results. There were no significant differences between the groups in term of ΔE of buccal (P = 0.148) and lingual surfaces (P = 0.73). Conclusion. Extended time of etching did not result in significant enamel color change. Immediate and delayed exposure of etched enamel to staining solutions did not result in clinically detectable tooth color changes. PMID:25093048

  3. Apparatus For Etching Or Depositing A Desired Profile Onto A Surface

    DOEpatents

    Rushford, Michael C.; Britten, Jerald A.

    2004-05-25

    An apparatus and method for modifying the surface of an object by contacting said surface with a liquid processing solution using the liquid applicator geometry and Marangoni effect (surface tension gradient-driven flow) to define and confine the dimensions of the wetted zone on said object surface. In particular, the method and apparatus involve contouring or figuring the surface of an object using an etchant solution as the wetting fluid and using real-time metrology (e.g. interferometry) to control the placement and dwell time of this wetted zone locally on the surface of said object, thereby removing material from the surface of the object in a controlled manner. One demonstrated manifestation is in the deterministic optical figuring of thin glasses by wet chemical etching using a buffered hydrofluoric acid solution and Marangoni effect.

  4. Nanoscale Etching and Indentation of Silicon Surfaces with Carbon Nanotubes

    NASA Technical Reports Server (NTRS)

    Dzegilenko, Fedor N.; Srivastava, Deepak; Saini, Subhash

    1998-01-01

    The possibility of nanolithography of silicon and germanium surfaces with bare carbon nanotube tips of scanning probe microscopy devices is considered with large scale classical molecular dynamics (MD) simulations employing Tersoff's reactive many-body potential for heteroatomic C/Si/Ge system. Lithography plays a key role in semiconductor manufacturing, and it is expected that future molecular and quantum electronic devices will be fabricated with nanolithographic and nanodeposition techniques. Carbon nanotubes, rolled up sheets of graphene made of carbon, are excellent candidates for use in nanolithography because they are extremely strong along axial direction and yet extremely elastic along radial direction. In the simulations, the interaction of a carbon nanotube tip with silicon surfaces is explored in two regimes. In the first scenario, the nanotubes barely touch the surface, while in the second they are pushed into the surface to make "nano holes". The first - gentle scenario mimics the nanotube-surface chemical reaction induced by the vertical mechanical manipulation of the nanotube. The second -digging - scenario intends to study the indentation profiles. The following results are reported in the two cases. In the first regime, depending on the surface impact site, two major outcomes outcomes are the selective removal of either a single surface atom or a surface dimer off the silicon surface. In the second regime, the indentation of a silicon substrate by the nanotube is observed. Upon the nanotube withdrawal, several surface silicon atoms are adsorbed at the tip of the nanotube causing significant rearrangements of atoms comprising the surface layer of the silicon substrate. The results are explained in terms of relative strength of C-C, C-Si, and Si-Si bonds. The proposed method is very robust and does not require applied voltage between the nanotube tips and the surface. The implications of the reported controllable etching and hole-creating for

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

    NASA Technical Reports Server (NTRS)

    Sovey, J. S.

    1978-01-01

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

  6. Surface cleaning and etching of rare-earth-doped phosphate glass

    NASA Astrophysics Data System (ADS)

    Barnes, Amy S.; Pantano, Carlo G.; Conzone, Samuel D.

    2001-11-01

    The surface reactions of phosphate glasses are important for the processing and application of photonic devices, biomedical materials and conventional optical components. Of particular concern are the leaching of optically-active dopant species, surface layer formation and roughening during polishing, cleaning and other fabrication processes. In this study, the effects of various cleaning treatments, and both acid and base etching, were evaluated using surface analytical techniques (XPS, AFM). It is shown that in these phosphate glasses, the aluminum and rare-earth oxides have limited aqueous solubility, whereas the phosphate network is soluble over a wider range of pH. Thus, under those conditions where polishing damage can be removed by etching the surface, a localized precipitation of rare-earth oxides occurs which influences the final roughness and surface composition. Conversely, under conditions where this precipitation can be eliminated, an in-depth leaching of the surface occurs. These aqueous surface reactions were similar for both the optically-active and passive IOG-1 glasses. An optimized surface preparation method is described.

  7. Washable and wear-resistant superhydrophobic surfaces with self-cleaning property by chemical etching of fibers and hydrophobization.

    PubMed

    Xue, Chao-Hua; Li, Ya-Ru; Zhang, Ping; Ma, Jian-Zhong; Jia, Shun-Tian

    2014-07-01

    Superhydrophobic poly(ethylene terephthalate) (PET) textile surfaces with a self-cleaning property were fabricated by treating the microscale fibers with alkali followed by coating with polydimethylsiloxane (PDMS). Scanning electron microscopy analysis showed that alkali treatment etched the PET and resulted in nanoscale pits on the fiber surfaces, making the textiles have hierarchical structures. Coating of PDMS on the etched fibers affected little the roughening structures while lowered the surface energy of the fibers, thus making the textiles show slippery superhydrophobicity with a self-cleaning effect. Wettability tests showed that the superhydrophobic textiles were robust to acid/alkaline etching, UV irradiation, and long-time laundering. Importantly, the textiles maintained superhydrophobicity even when the textiles are ruptured by severe abrasion. Also colorful images could be imparted to the superhydrophobic textiles by a conventional transfer printing without affecting the superhydrophobicity.

  8. Aspects of native oxides etching on n-GaSb(1 0 0) surface

    NASA Astrophysics Data System (ADS)

    Cotirlan, C.; Ghita, R. V.; Negrila, C. C.; Logofatu, C.; Frumosu, F.; Lungu, G. A.

    2016-02-01

    Gallium antimonide (GaSb) is the basis of the most photovoltaic and thermophotovoltaic (TPV) systems and its innovative technological aspects based on modern ultra-high vacuum techniques are in trend for device achievement. The real surface of GaSb is modified by technological processes that can conduce to problems related to the reproducible control of its surface properties. The GaSb surface is reactive in atmosphere due to oxygen presence and exhibits a native oxide layer. The evolution of native oxides during the ion sputtering, chemical etching and thermal annealing processes for preparing the surface is presented in detailed way. Ratios of surface constituents are obtained by Angle Resolved X-ray Photoelectron Spectroscopy (ARXPS). Moreover, Scanning Electron Microscopy (SEM), Energy Dispersive X-ray Spectroscopy (EDS), Atomic Force Microscopy (AFM) and Low-Energy Electron Diffraction (LEED) are used for characterization. The surface stoichiometry is changed using a specific etchant (e.g. citric acid) at different etching time and is analyzed by ARXPS, SEM, EDS and AFM methods. The experimental results provide useful information regarding surface native oxides characteristics on n-GaSb(1 0 0) to be taken into account for development of low resistance contacts for TPV devices based on GaSb alloy.

  9. Radical surface interactions in industrial silicon plasma etch reactors

    NASA Astrophysics Data System (ADS)

    Cunge, G.; Vempaire, D.; Ramos, R.; Touzeau, M.; Joubert, O.; Bodard, P.; Sadeghi, N.

    2010-06-01

    Silicon etching in Cl2-based plasmas is an important step for the fabrication of IC circuits but the plasma surface interactions involved in this process remain poorly understood. Based on the developments in plasma and reactor wall diagnostics, this paper reviews the recent progress in the understanding of radicals' interactions with surfaces during silicon etching processes. X-ray photoelectron spectroscopy analysis of the reactor walls shows that during Si etching in Cl2/O2 plasmas, the initial Al2O3 chamber walls are coated with a thin SiOCl layer. Broadband absorption spectroscopy with UV light emitting diodes is used to measure the densities of SiClX radicals (X = 0-2) and Cl2 molecules in steady state plasmas running with the chamber walls coated with different materials. To estimate the surface sticking/recombination probability of these radicals on different surfaces, we have performed time-resolved absorption measurements in the afterglow of pulsed discharges. Our work, in agreement with previous results, shows that the Cl2/Cl density ratio in the discharge is driven mainly by the chemical nature of the chamber walls explaining why process drifts are often observed in Cl2/O2 plasmas. The recombination coefficient of Cl atoms on SiOCl surfaces is about 0.007, while it is about 0.1 on clean walls (AlF3). Based on these results, we discuss the best strategy leading to reproducible process control, the present strategy being a systematic reactor cleaning/conditioning between wafers. The SiOCl layer deposition mechanism is then discussed in detail. The sticking coefficient of SiCl on this surface is near unity, while SiCl2 appears to be weakly reactive toward it. Therefore, SiCl (and SiCl+ ions) are the main vectors of Si deposition on the reactor walls, where their subsequent oxidization by O atoms leads to the formation of a SiOCl deposit. Furthermore, we show that SiCl reaction in the plasma volume with Cl2, through the exchange reaction SiCl + Cl2 → Si

  10. 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

  11. A Comparison of Shear Bond Strengths of Metal and Ceramic Brackets using Conventional Acid Etching Technique and Er:YAG Laser Etching

    PubMed Central

    Yassaei, Sogra; Fekrazad, Reza; Shahraki, Neda; Goldani Moghadam, Mahdjoube

    2014-01-01

    Background and aims. The aim of this study was to compare shear bond strength (SBS) of metal and ceramic brackets bonded to enamel using acid versus Er:YAG laser etching. Materials and methods. Eighty premolars were divided into 4 groups: AM (acid etching/ metal brackets), AC (acid etching/ ceramic brackets), LM (laser etching/ metal brackets) and LC (laser etching/ ceramic brackets). Enamel condition-ing was done using acid in AC and AM and Er:YAG laser in LC and LM. Brackets were debonded with a Dartec machine and the SBSs were determined. Adhesive remnant index was evaluated under a stereomicroscope. Two additional teeth were conditioned with acid and laser for scanning electron microscopy examination. Comparisons of SBS value were done by ANOVA test. Results. statistical analyses showed that SBSs of acid groups were significantly higher than that of laser groups, but dif-ferences between SBS values of AC/ AM and LC/LM were not significant. SEM examination revealed different etching pattern. Conclusion. Low power Er:YAG laser etching offers clinically acceptable SBS which besides its other superiorities to acid etching can be an appropriate alternative for bonding of ceramic brackets. PMID:25024836

  12. Micro structuration of gaas surface by wet etching: towards a specific surface behavior.

    PubMed

    Bienaime, Alex; Elie-Caille, Celine; Leblois, Therese

    2012-08-01

    Resonant microelectromechanical systems are promising devices for real time and highly sensitive measurements. The sensitivity of such sensors to additional mass loadings which can be increased thanks to the miniaturisation of devices is of prime importance for biological applications. The miniaturisation of structures passes through a photolithographic process and wet chemical etching. So, this paper presents new results on the anisotropic chemical etching of the gallium arsenide (GaAs) crystal used for this application, in several solutions. This paper focuses on the micro/nanostructuration of the sensing surface to increase the sensor sensitivity. Indeed, this active surface will be biofunctionalized to operate in biological liquid media in view of biomolecules detection. Several experimental conditions of etching bath composition, concentration and temperature were examined to obtain a large variety of geometrical surfaces topographies and roughness. According to the orientation dependence of the chemical etching process, the experiments were also performed on various GaAs crystal plates. The bath 1 H3PO4:9 H2O2:1 H2O appeared to be particularly adapted to the fabrication of the GaAs microstructured membrane: indeed, the bath is highly stable, anisotropic, and, as a function of temperature, it allows the production of a large variety of GaAs surface topographies.

  13. 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

    2014-03-01

    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.

  14. 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.

  15. The evolution of the surface morphology of silicon during aqueous etching

    NASA Astrophysics Data System (ADS)

    Newton, Theresa Anne

    The morphology of etched silicon surfaces is of great technological importance because silicon is widely used in the production of microelectronics and microelectromechanical systems (MEMS). In this thesis, I use scanning tunneling microscopy (STM), a kinetic Monte Carlo etching simulator, and micromachined test patterns to investigate the chemical reactions controlling aqueous etching of silicon. The kinetic dependence of the rate of Si(111) etching in NH4F on [HF] and [OH--] is measured. The etch rate is found to have an approximately first order dependence on [OH--] and essentially no dependence on [HF]. This rate dependence lends support to a proposed mechanism in which the rate-limiting step in NH4F etching of silicon is the oxidation of the surface site, followed by quick removal of the oxidized site by HF. The site-specific rates of isopropanol and ethanol reaction on a Si(111) surface are studied through a combination of kinetic competition with an etchant of known anisotropy and concentration-dependent morphological changes. These rates are quantified by comparing STM images with kinetic Monte Carlo simulations of the etched surface. The isopropoxide ion binds to a surface site and slows etching at the bound site. This changes the anisotropy of the etchant. Ethanol induces similar morphological changes. The effect of alcohol pK a is also studied using a micromachined test pattern. Low p Ka halogenated alcohols are also studied. There is a strong correlation between the macroscopic and microscopic etch rate anisotropies of non-halogenated alcohols; however, halogenated alcohols had little effect on the macroscopic etch rate anisotropies. The sensitivity of surface vibrational spectroscopy to surface morphology is also studied. The variation in the lineshape of the Si--H stretch vibration of etched Si(111) surfaces due to atomic-scale etch pits, anisotropic etching, and surface steps is modeled through the use of kinetic Monte Carlo simulations. The in

  16. Deep GaN etching by inductively coupled plasma and induced surface defects

    SciTech Connect

    Ladroue, J.; Meritan, A.; Boufnichel, M.; Lefaucheux, P.; Ranson, P.; Dussart, R.

    2010-09-15

    GaN etching was studied in Cl{sub 2}/Ar plasmas as a function of process parameters. In addition, for a better understanding of the etching mechanisms, Langmuir probe measurements and optical emission spectroscopy were carried out. Etch rate was found to depend strongly on bias power. After optimization, an etch rate greater than 1000 nm/min was achieved. A second part of this work is dedicated to the etched surface defects. An original method to estimate GaN dislocation density and to localize nanopipes in the material is presented. Columnar defects could also appear with impurities in the etching reactor. The authors also present a possible formation mechanism of those columnar defects.

  17. Modifying of etching anisotropy of silicon substrates by surface active agents

    NASA Astrophysics Data System (ADS)

    Rola, Krzysztof; Zubel, Irena

    2011-04-01

    The influence of alcohol additives on etch rate anisotropy of Si(hkl) planes has been studied. The etching processes were carried out in 3 and 5 M KOH aqueous solutions saturated and non-saturated with alcohols. Isopropanol, 1-propanol and tert-butanol were examined. It has been showed that the etching process cannot be controlled only by the surface tension of the solution. Saturation of the etching solution with alcohols modifies etch rate anisotropy, lowering the ratio of the etch rate of (110) and vicinal planes to the etch rate of (100) plane. The morphology of Si(hkl) planes etched in 3 M KOH solution saturated with tert-butyl alcohol has been studied in detail. Smooth (331) and (221) planes have been achieved in this solution. The (100) plane turned out to be densely covered by hillocks, opposite to the (100) plane etched in weak-alkaline solution saturated with isopropanol. To explain this phenomenon, the mechanism of hillocks formation on Si(100) surface has been proposed.

  18. Modifying of etching anisotropy of silicon substrates by surface active agents

    NASA Astrophysics Data System (ADS)

    Rola, Krzysztof P.; Zubel, Irena

    2011-04-01

    The influence of alcohol additives on etch rate anisotropy of Si( hkl) planes has been studied. The etching processes were carried out in 3 and 5 M KOH aqueous solutions saturated and non-saturated with alcohols. Isopropanol, 1-propanol and tert-butanol were examined. It has been showed that the etching process cannot be controlled only by the surface tension of the solution. Saturation of the etching solution with alcohols modifies etch rate anisotropy, lowering the ratio of the etch rate of (110) and vicinal planes to the etch rate of (100) plane. The morphology of Si( hkl) planes etched in 3 M KOH solution saturated with tert-butyl alcohol has been studied in detail. Smooth (331) and (221) planes have been achieved in this solution. The (100) plane turned out to be densely covered by hillocks, opposite to the (100) plane etched in weak-alkaline solution saturated with isopropanol. To explain this phenomenon, the mechanism of hillocks formation on Si(100) surface has been proposed.

  19. Reduction in surface roughness and aperture size effect for XeF2 etching of Si

    NASA Astrophysics Data System (ADS)

    Sugano, Koji; Tabata, Osamu

    2003-01-01

    Low etching pressure and addition of buffer gas successfully decrease the etched surface roughness and the aperture effect which represent challenges toward the application of silicon etching with XeF2 to MEMS fabrication. Etched roughness and aperture effect are extremely high and limit factors for the design rules of MEMS. By lowering the charge pressure of XeF2 from 390 to 65 Pa, the etched roughness decreased from 870.8 and 174.4 Å and the uniformity ((depth for 25 μm mask aperture)(depth for 175 μm mask aperture)× 100 %) improved from 71.3 to 88.7%. By adding N2 or reaction products including Xe and SiF4 as buffer gas, surface roughness was reduced and the surface morphology changed.

  20. Resin–dentin bonds to EDTA-treated vs. acid-etched dentin using ethanol wet-bonding

    PubMed Central

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

    2013-01-01

    Objective To compare resin–dentin bond strengths and the micropermeability of hydrophobic vs. hydrophilic resins bonded to acid-etched or EDTA-treated dentin, using the ethanol wet-bonding technique. Methods Flat dentin surfaces from extracted human third molars were conditioned before bonding with: 37% H3PO4 (15 s) or 0.1 M EDTA (60 s). Five experimental resin blends of different hydrophilicities and one commercial adhesive (SBMP: Scotchbond Multi-Purpose) were applied to ethanol wet-dentin (1 min) and light-cured (20 s). The solvated resins were used as primers (50% ethanol/50% comonomers) and their respective neat resins were used as the adhesive. The resin-bonded teeth were stored in distilled water (24 h) and sectioned in beams for microtensile bond strength testing. Modes of failure were examined by stereoscopic light microscopy and SEM. Confocal tandem scanning microscopy (TSM) interfacial characterization and micropermeability were also performed after filling the pulp chamber with 1 wt% aqueous rhodamine-B. Results The most hydrophobic resin 1 gave the lowest bond strength values to acid-etched dentin and all beams failed prematurely when the resin was applied to EDTA-treated dentin. Resins 2 and 3 gave intermediate bond strengths to both conditioned substrates. Resin 4, an acidic hydrophilic resin, gave the highest bond strengths to both EDTA-treated and acid-etched dentin. Resin 5 was the only hydrophilic resin showing poor resin infiltration when applied on acid-etched dentin. Significance The ethanol wet-bonding technique may improve the infiltration of most of the adhesives used in this study into dentin, especially when applied to EDTA-treated dentin. The chemical composition of the resin blends was a determining factor influencing the ability of adhesives to bond to EDTA-treated or 37% H3PO4 acid-etched dentin, when using the ethanol wet-bonding technique in a clinically relevant time period. PMID:20074787

  1. The effect of HF etching on the surface quality and figure of fused silica optics

    NASA Astrophysics Data System (ADS)

    Xu, Jiafeng; Xu, Xueke; Wei, Chaoyang; Gao, Wenlan; Yang, Minghong; Shao, Jianda; Liu, Shijie

    2015-08-01

    The effect of deep HF etching on the surface quality and figure of fused silica optics has been investigated systematically. Fused silica samples (100 mm in diameter x 10 mm thick) were manufactured using the conventional grinding and polishing process. These processed samples are etched with different removal depth. Initially, the surface quality of fused silica samples is characterized in terms of surface roughness and surface defects. Many digs not more than 1μm deep are emerged which originates from the micron grinding cracks and crack pits. These digs worsened the surface roughness and frosted the sample. While submillimeter subsurface damage exposed through etching appear as sparkling dots under the high power lamp. The average total length of millimeter scratches on single surfaces is over 200 mm. Not all millimeter scratches could be exposed until removal depth of up to 2 μm. Finally, the surface figure behavior during deep etching has also been figured out. Etching on the edge of the upper surface of samples placed horizontally went faster than on the inside parts. The surface of samples placed vertically assumed a more complicated removal distribution, which can be both explained in terms of "fringe tip effect". For the change of surface figure PV, the initial surface figure feature plays an important role as well as the etching removal distribution.

  2. HF-(NH₄)₂S₂O₈-HCl Mixtures for HNO₃- and NOx-free Etching of Diamond Wire- and SiC-Slurry-Sawn Silicon Wafers: Reactivity Studies, Surface Chemistry, and Unexpected Pyramidal Surface Morphologies.

    PubMed

    Stapf, André; Gondek, Christoph; Lippold, Marcus; Kroke, Edwin

    2015-04-29

    The wet-chemical treatment of silicon wafers is an important production step in photovoltaic and semiconductor industries. Solutions containing hydrofluoric acid, ammonium peroxodisulfate, and hydrochloric acid were investigated as novel acidic, NOx-free etching mixtures for texturization and polishing of monocrystalline silicon wafers. Etching rates as well as generated surface morphologies and properties are discussed in terms of the composition of the etching mixture. The solutions were analyzed with Raman and UV/vis spectroscopy as well as ion chromatography (IC). The silicon surfaces were investigated by scanning electron microscopy (SEM), confocal laser scanning microscopy (CLSM), diffuse reflection infrared spectroscopy (DRIFT), and X-ray photoelectron spectroscopy (XPS). Surprisingly, pyramidal surface structures were found after etching SiC-slurry as well as diamond wire-sawn monocrystalline Si(100) wafers with hydrochloric acid-rich HF-(NH4)2S2O8-HCl mixtures. Acidic etching solutions are generally not known for anisotropic etching. Thus, the HNO3-free mixtures might allow to replace KOH/i-propanol and similar alkaline solutions for texturization of monosilicon wafers at room temperature with less surface contamination. Besides, common HNO3-based etching mixtures may be replaced by the nitrate-free system, leading to significant economic and ecological advantages.

  3. HVPE homoepitaxial growth of high quality bulk GaN using acid wet etching method and its mechanism analysis

    NASA Astrophysics Data System (ADS)

    Liu, Nanliu; Cheng, Yutian; Wu, Jiejun; Li, Xingbin; Yu, Tongjun; Xiong, Huan; Li, Wenhui; Chen, Jiao; Zhang, Guoyi

    2016-11-01

    In this paper, crack-free 2-inch bulk GaN wafer with the thickness up to 3 mm was obtained by HVPE homoepitaxy. A new method of acid wet etching was used to pre-treat GaN substrate before re-growth. The formation of the mesh-like subsurface crack and interface layer were found to be suppressed between the re-growth layer and as-grown GaN substrate. EDS and time varied contact angle measurement proved that chemical etching would decrease the oxygen related surface adsorption and increase atoms diffusion length during HVPE homoepitaxial growth. Moreover, Morphology, Low temperature photoluminescence measurements indicated a reduction in stress of wet etching treated as-grown GaN substrate due to etching effect on its N face. High quality bulk GaN with the dislocation density of 1×106 cm-2 was achieved by using wet etching and HVPE multiple re-growth. It would offer a simple method to obtain bulk GaN with thicker layer and high quality.

  4. Surface kinetics modeling of silicon and silicon oxide plasma etching. III. Modeling of silicon oxide etching in fluorocarbon chemistry using translating mixed-layer representation

    SciTech Connect

    Kwon, Ohseung; Bai Bo; Sawin, Herbert H.

    2006-09-15

    Silicon oxide etching was modeled using a translating mixed-layer model, a novel surface kinetic modeling technique, and the model showed good agreement with measured data. Carbon and fluorine were identified as the primary contributors to deposition and etching, respectively. Atomic fluorine flux is a major factor that determines the etching behavior. With a chemistry having a small amount of atomic fluorine (such as the C{sub 4}F{sub 8} chemistry), etching yield shows stronger dependence on the composition change in the gas flux.

  5. Versatile route to gapless microlens arrays using laser-tunable wet-etched curved surfaces.

    PubMed

    Hao, Bian; Liu, Hewei; Chen, Feng; Yang, Qing; Qu, Pubo; Du, Guangqing; Si, Jinhai; Wang, Xianhua; Hou, Xun

    2012-06-01

    This work reveals a cost-efficient and flexible approach to various microlens arrays on polymers, which is essential to micro-optics elements. An 800-nm femtosecond laser is employed to control the hydrofluoric (HF) acid etching process on silica glasses, and concave microstructures with smooth curved surfaces are produced by this method. Then, the micro-structured glass templates can serve as molds for replicating microlenses on polymers. In this paper, a high-ordered microlens array with over 16,000 hexagonal-shaped lenses is fabricated on poly (dimethyl siloxane) [PDMS], and its perfect light-gathering ability and imaging performance are demonstrated. The flexibility of this method is demonstrated by successful preparation of several concave molds with different patterns which are difficult to be obtained by other methods. This technique provides a new route to small-scaled, smooth and curved surfaces which is widely used in micro-optics, biochemical analysis and superhydrophobic interface. PMID:22714321

  6. Experimental analysis of the surface roughness evolution of etched glass for micro/nanofluidic devices

    NASA Astrophysics Data System (ADS)

    Ren, J.; Ganapathysubramanian, B.; Sundararajan, S.

    2011-02-01

    Roughness of channel surfaces, both deterministic and random, is known to affect the fluid flow behavior in micro/nanoscale fluidic devices. This has relevance particularly for applications involving non-Newtonian fluids, such as in biomedical lab-on-chip devices. While several studies have investigated effects of relative large, deterministic surface structures on fluid flow, the effect of random roughness on microfluidic flow remains relatively unexplored. In this study, the effects of processing conditions for wet etching of glass including etching time and etching orientation on centre-line average (Ra) and the autocorrelation length (ACL) were investigated. Statistical distribution of the roughness was also studied. Results indicated that ACL can be tailored in the range of 1-4 µm by changing etching time in horizontal etching while Ra was found to increase weakly with etching time in all three etching orientations. Analysis of the experimental data using the Kolmogorov-Smirnov goodness-of-fit hypothesis test shows that the glass surface roughness does not follow a Gaussian distribution, as is typically assumed in the literature. Instead, the T location-scale distribution fits the roughness data with 1.11% error. These results provide promising insights into tailoring surface roughness for improving microfluidic devices.

  7. Early odontoblastic layer response to cavity preparation and acid etching in rats.

    PubMed

    Nemeth, Lidija; Erman, Andreja; Stiblar-Martincic, Draga

    2006-01-01

    The aim of this study was to establish the early odontoblastic layer response and quantitatively to estimate the number of odontoblasts after cavity preparation with and without acid etching. Half of 56 cavities prepared on rats' first upper molars were acid etched. Qualitative and morphometric analyses were made on histological and ultrathin sections 5 min, 6 h, 24 h and 72 h post-operatively. Under the etched cavity, a greater disarrangement of odontoblasts was found, modifications in nuclear shape and condensed chromatin 5 min. post-operatively. An additional reduction of odontoblast number was detected and an increase of aspirated cell number 5 min, 6 h and 24 h post-operatively, pronounced hyperaemia 6, 24 and 72 hours post-operatively and increased odontoblast number 72 hours post-operatively, compared to unetched cavities. In conclusion, injury to the odontoblastic layer was greater, but numerical renewal of the odontoblastic layer began earlier in etched cavities compared to unetched cavities. PMID:17044256

  8. Changes in boron fiber strength due to surface removal by chemical etching

    NASA Technical Reports Server (NTRS)

    Smith, R. J.

    1976-01-01

    The effects of chemical etching on the tensile strength of commercial boron/tungsten fibers were investigated. Fibers with as-received diameters of 203, 143, and 100 micrometers were etched to diameters as small as 43 micrometers. The etching generally resulted in increasing fiber tensile strength with decreasing fiber diameter. And for the 203 micrometer fibers there was an accompanying significant decrease in the coefficient of variation of the tensile strength for diameters down to 89 micrometers. Heat treating these fibers above 1,173 K in a vacuum caused a marked decrease in the average tensile strength of at least 80 percent. But after the fibers were etched, their strengths exceeded the as-received strengths. The tensile strength behavior is explained in terms of etching effects on surface flaws and the residual stress pattern of the as-received fibers.

  9. Gallium arsenide surface chemistry and surface damage in a chlorine high density plasma etch process

    NASA Astrophysics Data System (ADS)

    Eddy, C. R., Jr.; Glembocki, O. J.; Leonhardt, D.; Shamamian, V. A.; Holm, R. T.; Thoms, B. D.; Butler, J. E.; Pang, S. W.

    1997-11-01

    In an effort to monitor ion-driven surface chemistry in the high density plasma etching of GaAs by Cl2/Ar plasma chemistries, we have applied mass spectrometry and careful substrate temperature control. Etch product chlorides were mass analyzed while the substrate temperature was monitored by optical bandgap thermometry and as pressure (neutral flux), microwave power (ion flux) and rf bias of the substrate (ion energy) were varied. By ensuring that the substrate temperature does not deviate during process variations, the changes in product mass peak intensities are a direct measure of changes in the ionassisted surface chemistry which promotes anisotropic etching. Experimental results show that ion-assisted surface chemistry is optimum when sufficient Cl and Cl+ are present in the incident plasma flux. These conditions are met at low coupled microwave powers (<300 W) and low total process pressures (<1.0 mTorr) for input gas mixtures of 25% Cl2 in Ar. Three mechanistic regions are identified for surface chemistry as a function of incident ion energy: 1) largely thermal chemistry for <50 eV; 2) ion-assisted chemistry for 50 200 eV; and 3) sputtering for >200 eV. Photoreflectance measurements of the surface Fermi level show significant damage for ion energies >75 eV. However, in situ and ex situ surface passivations can recover the surface Fermi level for up to 200 eV ion energies, in good correlation to the onset of sputtering and subsurface damage. Thus, anisotropic, low damage pattern transfer is possible for ion energies between 50 and 200 eV.

  10. Dry etching of copper phthalocyanine thin films: effects on morphology and surface stoichiometry.

    PubMed

    Van Dijken, Jaron G; Brett, Michael J

    2012-08-24

    We investigate the evolution of copper phthalocyanine thin films as they are etched with argon plasma. Significant morphological changes occur as a result of the ion bombardment; a planar surface quickly becomes an array of nanopillars which are less than 20 nm in diameter. The changes in morphology are independent of plasma power, which controls the etch rate only. Analysis by X-ray photoelectron spectroscopy shows that surface concentrations of copper and oxygen increase with etch time, while carbon and nitrogen are depleted. Despite these changes in surface stoichiometry, we observe no effect on the work function. The absorbance and X-ray diffraction spectra show no changes other than the peaks diminishing with etch time. These findings have important implications for organic photovoltaic devices which seek nanopillar thin films of metal phthalocyanine materials as an optimal structure.

  11. 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.

  12. Nanohole formation on AlGaAs surfaces by local droplet etching with gallium

    NASA Astrophysics Data System (ADS)

    Heyn, Ch.; Stemmann, A.; Hansen, W.

    2009-03-01

    We demonstrate the self-assembled generation of nanoholes on AlGaAs surfaces by local droplet etching (LDE). For the etching process, Ga is deposited on the surface, where liquid droplets are formed in a Volmer-Weber-like growth mode. The etching takes place locally at the interface between droplets and substrate and removes a significant amount of substrate material. The structural properties of the LDE nanoholes are studied with atomic force microscopy as function of etching temperature and Ga coverage. A bimodal depth distribution with flat and deep holes is observed. The formation of flat holes can be almost suppressed by optimized etching parameters. The depth of deep holes was adjusted by the process parameters up to a maximum depth of 15 nm. The density of deep holes is in the range 5×10 -7-1×10 -8 cm -2 and depends only slightly on the etching parameters. However, the density can be significantly increased by repeated etching.

  13. Effect of the application time of phosphoric acid and self-etch adhesive systems to sclerotic dentin

    PubMed Central

    MENA-SERRANO, Alexandra Patricia; GARCIA, Eugenio Jose; PEREZ, Miguel Muñoz; MARTINS, Gislaine Cristine; GRANDE, Rosa Helena Miranda; LOGUERCIO, Alessandro Dourado; REIS, Alessandra

    2013-01-01

    Objectives: To evaluate the effect of application time on the resin-dentin bond strength (µTBS) and etching pattern of adhesive systems applied on sclerotic dentine. Material and Methods: A total of forty-two bovine incisors had their roots removed. The 1-step self-etch GO (SDI), the 2-step self-etch Adper SE Bond (3MESPE) and the 35% phosphoric acid (3MESPE) from the 2-step etch-and-rinse Adper Single Bond 2 (3MESPE) were applied on the bovine incisal surfaces according to the manufacturer's instructions or duplicating the recommended conditioning time. After adhesive application, thirty teeth were restored with composite resin, stored for 24 h in distilled water at 37º C, and sectioned into resin-dentin bonded sticks (0.8 mm2) and tested according to the µTBS at 0.5 mm/min. The etching pattern of the remaining twelve teeth (n=4 for each material) was examined under scanning electron microscopy. Each tooth was divided into a buccal-to-lingual direction into three thirds, and each third randomly assigned to the groups: control (no treatment), according to the manufacturers' instructions and duplicating the recommended application time. The µTBS and the relative percentage of the tubule area opening were evaluated by two-way repeated measures ANOVA and Tukey's tests (α=0.05). Results: The duplication of the conditioning time favored only the GO adhesive (p<0.05). Both application methods significantly increased the tubule area opening (p<0.05) compared to the controls. Conclusions: The efficacy of duplicating the conditioning time was only effective for the 1-step self-etch adhesive system tested. PMID:23739856

  14. Sensing structure based on surface plasmonic resonance in single mode optical fibers chemically etched

    NASA Astrophysics Data System (ADS)

    Coelho, L.; Almeida, J. M.; Santos, J. L.; Ferreira, R. A. S.; André, P. S.; Viegas, D.

    2013-05-01

    Many optical systems based on Surface Plasmon Resonance (SPR) have been developed for work as refractometers, chemical sensors or even for measure the thickness of metal and dielectric thin films. These kinds of systems are usually large, expensive and cannot be used for remote sensing. Optical fiber sensors based on SPR has been widely studied for the last 20 years with several configurations mostly using multimode optical fibers with large cores and plastic claddings. Sensors based on SPR present very high sensitivity to refractive index variations when compared to the traditional refractive index sensors. Here we propose a SPR sensor based in a single mode fiber. The fiber end is chemically etched by emersion in a 48% hydrofluoric acid solution, resulting a single mode fiber with the cladding removed in a small section. A resonance dip around 1580 nm was attained in good agreement with the simulation scenario that takes into account the real characteristics of the fiber.

  15. X-ray photoelectron spectroscopy study of chemically-etched Nd-Ce-Cu-O surfaces

    NASA Technical Reports Server (NTRS)

    Vasquez, R. P.; Gupta, A.; Kussmaul, A.

    1991-01-01

    Acetic acid, Br2, and HCl solutions are investigated for removing insulating species from Nd(1.85)Ce(0.15)CuO(4-delta) (NCCO) thin film surfaces. X-ray photoelectron spectroscopy (XPS) shows that the HCl etch is most effective, yielding O 1s spectra comparable to those obtained from samples cleaned in vacuum and a clear Fermi edge in the valence band region. Reduction and oxidation reversibly induces and eliminates, respectively, Fermi level states for undoped samples, but has no clearly observable effect on the XPS spectra for doped samples. Reactivity to air is much less for NCCO compared to hole superconductors, which is attributed to the lack of reactive alkaline earth elements in NCCO.

  16. Controlling optical properties and surface morphology of dry etched porous silicon

    NASA Astrophysics Data System (ADS)

    Cheung, Maurice C.-K.; Roche, Philip J. R.; Hajj-Hassan, Mohamad; Kirk, Andrew G.; Mi, Zetian; Chodavarapu, Vamsy P.

    2011-01-01

    Porous silicon is a potentially useful substrate for fluorescence and scattering enhancement, with a large surface to volume ratio and thermal stability providing a potentially regenerable host matrix for sensor development. A simple process using XeF2 gas phase etching for creating porous silicon is explained. Moreover, how pores diameter can be controlled reproducibly with commensurate effects upon the silicon reflection and pore distribution is discussed. In previous work with this new system, it was clear that control on pore size and morphology was required and a systematic optimization of process conditions was performed to produce greater consistency of the result. The influence of the duration of the pre-etching processing in HF, concentration of the HF in the pre-etching process, and the XeF2 exposure time during the dry etching on surface morphology, pore size, and optical reflectance is explored.

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

    SciTech Connect

    Oyama, Tomoko Gowa; Nagasawa, Naotsugu; Taguchi, Mitsumasa; Hinata, Toru; Washio, Masakazu; Oshima, Akihiro; Tagawa, Seiichi

    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 attachment properties.

  18. 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.

  19. Facet dependent binding and etching: ultra-sensitive colorimetric visualization of blood uric acid by unmodified silver nanoprisms.

    PubMed

    Tan, Kanghui; Yang, Guang; Chen, Huide; Shen, Pengfei; Huang, Yucheng; Xia, Yunsheng

    2014-09-15

    By combination of experiments and density functional theory calculations, we present a simple but effective "facet dependent binding and etching" strategy for non-enzymatic and non-aggregated colorimetric sensing of blood uric acid (UA), using unmodified Ag nanoprisms as the signal readout. In the absence of UA, the triangular Ag nanoprisms are etched alongside (110) facets by H2O2 and form round nanodiscs, and a more than 160 nm surface plasmon resonance (SPR) blue shift is observed. Because of special affinity between UA and side facets of the Ag nanoprisms, pre-added UA can well protect the Ag nanoprisms from etching. Such protection effect can be used for well quantifying UA in the range of 10-3000 nM, based on the inverse proportion of the SPR blue shift with the added analyte. Due to very thin plate morphology (5 nm) and facet dependent binding/etching effects of the Ag nanoprisms, the sensing system has ultrahigh sensitivity. The detection limit is only 10nM, which is about 2 to 4 orders of magnitude lower than that of previous colorimetric sensing systems. In addition to accurate quantitation, the proposed strategy can conveniently discriminate the patient of hyperuricemia from normal person by naked eyes. So, the present simple, low-cost and visualized UA chemosensor has great potential in the applications for point-of-care diagnostics.

  20. Reaction ion etching process for improving laser damage resistance of fused silica optical surface.

    PubMed

    Sun, Laixi; Liu, Hongjie; Huang, Jin; Ye, Xin; Xia, Handing; Li, Qingzhi; Jiang, Xiaodong; Wu, Weidong; Yang, Liming; Zheng, Wanguo

    2016-01-11

    Laser induced damage of fused silica optics occurs primarily on optical surface or subsurface resulting from various defects produced during polishing/grinding process. Many new kinds of surface treatment processes are explored to remove or control the defects on fused silica surface. In this study, we report a new application of reaction ion etching (RIE)-based surface treatment process for manufacture of high quality fused silica optics. The influence of RIE processes on laser damage resistance as a function of etching depth and the evolution of typical defects which are associated with laser damage performance were investigated. The results show that the impurity element defects and subsurface damage on the samples surface were efficiently removed and prevented. Pure silica surface with relatively single-stable stoichiometry and low carbon atomic concentration was created during the etching. The laser damage resistance of the etched samples increased dramatically. The increase of roughness and ODC point defect with deeper etching are believed to be the main factors to limit further increase of the damage resistance of fused silica. The study is expected to contribute to the development of fused silica optics with high resistance to laser induced degradation in the future. PMID:26832251

  1. Strong suppression of near-surface thermal transport by metal-assisted chemical etching of Si

    NASA Astrophysics Data System (ADS)

    Feser, Joseph; Cahill, David

    2013-03-01

    Recently, we reported that the thermal conductivity of Si nanowire arrays roughened by metal-assisted chemical etching (MAC-etch) is strongly correlated to both the magnitude of the roughness and a broadening of the one-phonon Raman linewidth. We hypothesized that microstructural disorder induced by the etching chemistry leads to changes in the Raman linewidth and reduced thermal conductivity. Here, we simplify the study of such effects by chemically roughening Si wafers instead of nanowires. We have studied the effects of various roughening procedures on the near-surface thermal transport properties using time-domain thermoreflectance. We find that the thermal conductance of the near-surface region is systematically reduced by the MAC-etch process, despite the expectation that pristine roughened surfaces should have increased conductance due to enhanced surface area. In addition, highly roughened surfaces show strong picosecond acoustic echoes with reflection coefficient indicative of a soft interface. These features are consistent with the presence of strong disorder or nanoporosity in the near-surface region created by the MAC-etch process.

  2. Etching properties and electrical characterization of surfaces of silicon-on-insulator substrates in presence of halogens

    SciTech Connect

    Abbadie, A.; Hamaide, G.; Chaupin, M.; Brunier, F.; Mariolle, D.; Martinez, E.; Maehliss, J.

    2012-03-15

    We have studied the etching properties of silicon-on-insulator (SOI) substrates in recently developed chromium-free solutions containing halogens. We have shown that the presence of halogen compounds X (I{sup -}, Br{sup -}...) in HF/HNO{sub 3}/CH{sub 3}COOH solutions is required for a selective and preferential etching on SOI. The etching rate of such solutions increases with the dissolved halogen concentrations. The chemical reactivity of Si-X (X = Br{sup -}, I{sup -}..) bonds has been analyzed by X-ray Photoelectron Spectroscopy (XPS), Pseudo-MOS (flatband potential) and Kelvin Force Microscopy (KFM) measurements. A negative shift of flatband potential values is explained by an increasing concentration of halogen compounds in the solution and a substitution of Si-H (F) bonds by Si-X bonds during the reaction. Though Si-X bonds, and more particularly Si-I bonds, have been confirmed only at trace levels using XPS, we believe that the formation of Si-X bonds is supported by a mechanism of surface dipoles. Unexpectedly, no significant change in work function could be detected using KFM measurements. Some suggestions, based on KFM technique improvements, are made to explain such results. Finally, though the interaction mechanism between silicon, fluoride, iodide, and nitric acid is not clearly elucidated by our experimental results, the formation of Si-halogen bonds is crucial for etching and defect decoration capability.

  3. Etching properties and electrical characterization of surfaces of silicon-on-insulator substrates in presence of halogens

    NASA Astrophysics Data System (ADS)

    Abbadie, A.; Hamaide, G.; Mariolle, D.; Chaupin, M.; Brunier, F.; Martinez, E.; Mähliß, J.

    2012-03-01

    We have studied the etching properties of silicon-on-insulator (SOI) substrates in recently developed chromium-free solutions containing halogens. We have shown that the presence of halogen compounds X (I-, Br-…) in HF/HNO3/CH3COOH solutions is required for a selective and preferential etching on SOI. The etching rate of such solutions increases with the dissolved halogen concentrations. The chemical reactivity of Si-X (X = Br-, I-..) bonds has been analyzed by X-ray Photoelectron Spectroscopy (XPS), Pseudo-MOS (flatband potential) and Kelvin Force Microscopy (KFM) measurements. A negative shift of flatband potential values is explained by an increasing concentration of halogen compounds in the solution and a substitution of Si-H (F) bonds by Si-X bonds during the reaction. Though Si-X bonds, and more particularly Si-I bonds, have been confirmed only at trace levels using XPS, we believe that the formation of Si-X bonds is supported by a mechanism of surface dipoles. Unexpectedly, no significant change in work function could be detected using KFM measurements. Some suggestions, based on KFM technique improvements, are made to explain such results. Finally, though the interaction mechanism between silicon, fluoride, iodide, and nitric acid is not clearly elucidated by our experimental results, the formation of Si-halogen bonds is crucial for etching and defect decoration capability.

  4. A high efficiency industrial polysilicon solar cell with a honeycomb-like surface fabricated by wet etching using a photoresist mask

    NASA Astrophysics Data System (ADS)

    Zhang, Hong; Ding, Bin; Chen, Tianhang

    2016-11-01

    In this paper, an effective and low cost method of texturization was introduced into the fabrication process for industrial multicrystalline silicon solar cell production. The purpose of the method was to reduce reflectance by creating a honeycomb-like textured surface using a masked wet etching process. A negative photoresist film was selected as an etching mask. Although large surface roughness of wafer was considered to affect the adhesion and acid resistance of etching mask, a honeycomb-like textured surface with a pitch of 18 μm was fabricated successfully. The etched pits had a nearly smooth spherical segment surface, an average aperture of 15.1 μm, and a depth of 6.5 μm. This regular textured surface had a low light reflectivity of approximately 20.5% and greatly increased the carrier lifetime. Compared with multicrystalline silicon solar cells textured by conventional acid etching, the average short circuit current increased by 2.2% and the average efficiency increased from 17.41% to 17.75%, a net gain of 0.34%. And a high throughput above 2400 pieces per hour was obtained. This texturing technique is expected to promote the application of diamond-wire cut multicrystalline silicon wafers with the low saw-damage in the future.

  5. Early endosseous integration enhanced by dual acid etching of titanium: a torque removal study in the rabbit.

    PubMed

    Klokkevold, P R; Johnson, P; Dadgostari, S; Caputo, A; Davies, J E; Nishimura, R D

    2001-08-01

    Textured implant surfaces are thought to enhance endosseous integration. Torque removal forces have been used as a biomechanical measure of anchorage, or endosseous integration, in which the greater forces required to remove implants may be interpreted as an increase in the strength of bony integration. The purpose of this study was to compare the torque resistance to removal of screw-shaped titanium implants having a dual acid-etched surface (Osseotite) with implants having either a machined surface, or a titanium plasma spray surface that exhibited a significantly more complex surface topography. Three custom screw-shaped implant types - machined, dual acid-etched (DAE), and titanium plasma sprayed (TPS) - were used in this study. Each implant surface was characterized by scanning electron microscopy and optical profilometry. One DAE implant was placed into each distal femur of eighteen adult New Zealand White rabbits along with one of the other implant types. Thus, each rabbit received two DAE implants and one each of the machined, or TPS, implants. All implants measured 3.25 mm in diameter x 4.00 mm in length without holes, grooves or slots to resist rotation. Eighteen rabbits were used for reverse torque measurements. Groups of six rabbits were sacrificed following one, two and three month healing periods. Implants were removed by reverse torque rotation with a digital torque-measuring device. Three implants with the machined surface preparation failed to achieve endosseous integration. All other implants were anchored by bone. Mean torque values for machined, DAE and TPS implants at one, two and three months were 6.00+/-0.64 N-cm, 9.07+/-0.67 N-cm and 6.73+/-0.95 N-cm; 21.86+/-1.37 N-cm, 27.63+/-3.41 N-cm and 27.40+/-3.89 N-cm; and 27.48+/-1.61 N-cm, 44.28+/-4.53 N-cm and 59.23+/-3.88 N-cm, respectively. Clearly, at the earliest time point the stability of DAE implants was comparable to that of TPS implants, while that of the machined implants was an order of

  6. Antireflective grassy surface on glass substrates with self-masked dry etching

    PubMed Central

    2013-01-01

    Although recently developed bio-inspired nanostructures exhibit superior optic performance, their practical applications are limited due to cost issues. We present highly transparent glasses with grassy surface fabricated with self-masked dry etch process. Simultaneously generated nanoclusters during reactive ion etch process with simple gas mixture (i.e., CF4/O2) enables lithography-free, one-step nanostructure fabrication. The resulting grassy surfaces, composed of tapered subwavelength structures, exhibit antireflective (AR) properties in 300 to 1,800-nm wavelength ranges as well as improved hydrophilicity for antifogging. Rigorous coupled-wave analysis calculation provides design guidelines for AR surface on glass substrates. PMID:24289255

  7. Nanoscale Etching and Indentation of Silicon(001) Surface with Carbon Nanotube Tips

    NASA Technical Reports Server (NTRS)

    Dzegilenko, Fendor N.; Srivastava, Deepak; Saini, Subhash

    1998-01-01

    The possibility of nanoscale etching and indentation of Si(001)(2x1) surface by (8,0) and (10,10) carbon nanotube tips is demonstrated, for the first time, by classical molecular dynamics simulations employing Tersoff's many-body potential for a mixed C/Si/Ge system. In the nanotube tip barely touching the surface scenario atomistic etching is observed, where as in the nanoindentation scenario nanotube tip penetrates the surface without much hindrance. The results are explained in terms of the relative strength of C-C, C-Si, and Si-Si bonds.

  8. Enhancement on photocatalytic activity of an amorphous titanium oxide film with nano-textured surface by selective-fluorination etching process

    SciTech Connect

    Shih, Pin-Chun; Huang, Cheng-Hao; Chen, Tai-Hong; Lai, Li-Wen; Lu, Yi-Shan; Liu, Day-Shan

    2014-04-01

    Highlights: • The amorphous TiO{sub x} film surface was modified via selective fluorination etching process. • The resulting nano-textured surface markedly enriched the specific surface area and surface acidity. • The photocatalytic activity was comparable to an annealed TiO{sub x} film with anatase structure. - Abstract: A selective-fluorination etching process achieved by an UV light pre-irradiation and the subsequently fluorination etching was developed to enhance the photocatalytic activity of a low-temperature deposited amorphous titanium oxide (a-TiO{sub x}) film. Textured surface on the a-TiO{sub x} films formed by this process were investigated using atomic force microscope and field emission scanning electron microscope. Evidence of the fluorine ions introduced into the a-TiO{sub x} films was examined using Fourier transform infrared spectrometry and X-ray photoelectron spectroscopy. The etching thickness of the a-TiO{sub x} film was found to be deeply relevant to the film pre-irradiated by the UV light. An a-TiO{sub x} film with nano-textured surface, which was favorable to enlarge the specific surface area, thus was obtainable from the notable etching selectivity of the film pre-irradiated by UV light through a nano-sized mask. In addition, the surface acidity of the a-TiO{sub x} film was enhanced by the formation of the Ti-F chemical bonds originating from the fluorination etching process, which also was functional to facilitate the production of surface OH free radicals. Accordingly, the resulting fluorinated a-TiO{sub x} film with nano-textured surface performed a quality photocatalytic activity comparable to that of the high-temperature achieved TiO{sub x} film with anatase structures.

  9. The Effect of HF/NH4F Etching on the Morphology of Surface Fractures on Fused Silica

    SciTech Connect

    Wong, L; Suratwala, T; Feit, M D; Miller, P E; Steele, R A

    2008-04-03

    The effects of HF/NH{sub 4}F, wet chemical etching on the morphology of individual surface fractures (indentations, scratches) and of an ensemble of surface fractures (ground surfaces) on fused silica glass has been characterized. For the individual surface fractures, a series of static or dynamic (sliding) Vickers and Brinnell indenters were used to create radial, lateral, Hertzian cone and trailing indentation fractures on a set of polished fused silica substrates which were subsequently etched. After short etch times, the visibility of both surface and subsurface cracks is significantly enhanced when observed by optical microscopy. This is attributed to the removal of the polishing-induced Bielby layer and the increased width of the cracks following etching allowing for greater optical scatter at the fracture interface. The removal of material during etching was found to be isotropic except in areas where the etchant has difficulty penetrating or in areas that exhibit significant plastic deformation/densification. Isolated fractures continue to etch, but will never be completely removed since the bottom and top of the crack both etch at the same rate. The etching behavior of ensembles of closely spaced cracks, such as those produced during grinding, has also been characterized. This was done using a second set of fused silica samples that were ground using either fixed or loose abrasives. The resulting samples were etched and both the etch rate and the morphology of the surfaces were monitored as a function of time. Etching results in the formation of a series of open cracks or cusps, each corresponding to the individual fractures originally on the surface of the substrate. During extended etching, the individual cusps coalesce with one another, providing a means of reducing the depth of subsurface damage and the peak-to-valley roughness. In addition, the material removal rate of the ground surfaces was found to scale with the surface area of the cracks as a

  10. Effects of wet etch processing on laser-induced damage of fused silica surfaces

    SciTech Connect

    Battersby, C.L.; Kozlowski, M.R.; Sheehan, L.M.

    1998-12-22

    Laser-induced damage of transparent fused silica optical components by 355 nm illumination occurs primarily at surface defects produced during the grinding and polishing processes. These defects can either be surface defects or sub-surface damage.Wet etch processing in a buffered hydrogen fluoride (HF) solution has been examined as a tool for characterizing such defects. A study was conducted to understand the effects of etch depth on the damage threshold of fused silica substrates. The study used a 355 nm, 7.5 ns, 10 Hz Nd:YAG laser to damage test fused silica optics through various wet etch processing steps. Inspection of the surface quality was performed with Nomarski microscopy and Total Internal Reflection Microscopy. The damage test data and inspection results were correlated with polishing process specifics. The results show that a wet etch exposes subsurface damage while maintaining or improving the laser damage performance. The benefits of a wet etch must be evaluated for each polishing process.

  11. 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. PMID:24372961

  12. 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.

  13. In vivo Acid Etching Effect on Bacteria within Caries-Affected Dentin

    PubMed Central

    Gu, F.; Bresciani, E.; Barata, T.J.; Fagundes, T.C.; Navarro, M.F.; Dickens, S.H.; Fenno, J.C.; Peters, M.C.

    2010-01-01

    Acid etching procedures may disrupt residual bacteria and contribute to the success of incomplete caries removal followed by adhesive restoration. This study evaluated the in vivo effect of acid etching on cariogenic bacterial activity within affected dentin after minimally invasive treatment of caries lesions. Twenty-eight carious permanent teeth received standardized selective caries removal and random acid etch treatment (E) or not (NE) prior to adhesive restoration. Baseline and 3-month dentin biopsies were collected. The number of bacteria and activity of total bacterial cells and Streptococcus mutans were determined by quantitative PCR and RT-PCR. No statistically significant differences were observed in total bacterial number and activity between E and NE treatments (p > 0.3008). For NE, however, the residual S. mutans bacterial cells were reduced (p = 0.0027), while the activity per cell was significantly increased (p = 0.0010) after reentry at 3 months after restoration. This effect was not observed in group E. Although no significant differences were found between groups, this study suggests that acid etching of affected dentin prior to adhesive restoration may directly or indirectly have an inhibitive effect on the activity of residual cariogenic bacteria. Further research is required to investigate this potential effect. PMID:20861631

  14. A Silicon-Based, Sequential Coat-and-Etch Process to Fabricate Nearly Perfect Substrate Surfaces

    SciTech Connect

    Mirkarimi, P B; Spiller, E; Baker, S L; Stearns, D G; Robinson, J C; Olynick, D L; Salmassi, F; Liddle, J A; Liang, T; Stivers, A R

    2005-07-05

    For many thin-film applications substrate imperfections such as particles, pits, scratches, and general roughness, can nucleate film defects which can severely detract from the coating's performance. Previously we developed a coat-and-etch process, termed the ion beam thin film planarization process, to planarize substrate particles up to {approx} 70 nm in diameter. The process relied on normal incidence etching; however, such a process induces defects nucleated by substrate pits to grow much larger. We have since developed a coat-and-etch process to planarize {approx}70 nm deep by 70 nm wide substrate pits; it relies on etching at an off-normal incidence angle, i.e., an angle of {approx} 70{sup o} from the substrate normal. However, a disadvantage of this pit smoothing process is that it induces defects nucleated by substrate particles to grow larger. Combining elements from both processes we have been able to develop a silicon-based, coat-and-etch process to successfully planarize {approx}70 nm substrate particles and pits simultaneously to at or below 1 nm in height; this value is important for applications such as extreme ultraviolet lithography (EUVL) masks. The coat-and-etch process has an added ability to significantly reduce high-spatial frequency roughness, rendering a nearly perfect substrate surface.

  15. Etching characteristics of chromium thin films by an electron beam induced surface reaction

    NASA Astrophysics Data System (ADS)

    Wang, Jianhua; Griffis, D. P.; Garcia, R.; Russell, P. E.

    2003-04-01

    In this paper, we demonstrate the etching of chromium (Cr) film on quartz through a surface reaction induced by an electron beam and enhanced with XeF2 gas. We have studied the influences of the electron beam energy, the gas flow rate and the specimen composition on the etch rate. The electron beam energy has significant influence on the etch rate. The etch rate made by an electron beam of 20 keV is five times higher compared to that made by a beam of 10 keV. The XeF2 gas flow rate shows little effect on the etch rate when the gas pressure is higher than 2 × 10-6 Torr. The structure and grain size of the Cr film did not show any apparent change under exposure to XeF2 or when irradiated by an electron beam, while the composition of Cr has a significant effect on the etch process. The material removal of Cr induced by an electron beam means that it can be applied to the direct fabrication of microstructures on Cr films and that it solves the contamination problem in Cr mask repair.

  16. Bond strength of composite to dentin: effect of acid etching and laser irradiation through an uncured self-etch adhesive system

    NASA Astrophysics Data System (ADS)

    Castro, F. L. A.; Carvalho, J. G.; Andrade, M. F.; Saad, J. R. C.; Hebling, J.; Lizarelli, R. F. Z.

    2014-08-01

    This study evaluated the effect on micro-tensile bond strength (µ-TBS) of laser irradiation of etched/unetched dentin through an uncured self-etching adhesive. Dentinal surfaces were treated with Clearfil SE Bond Adhesive (CSE) either according to the manufacturer’s instructions (CSE) or without applying the primer (CSE/NP). The dentin was irradiated through the uncured adhesive, using an Nd:YAG laser at 0.75 or 1 W power settings. The adhesive was cured, composite crowns were built up, and the teeth were sectioned into beams (0.49 mm2) to be stressed under tension. Data were analyzed using one-way ANOVA and Tukey statistics (α = 5%). Dentin of the fractured specimens and the interfaces of untested beams were observed under scanning electron microscopy (SEM). The results showed that non-etched irradiated surfaces presented higher µ-TBS than etched and irradiated surfaces (p < 0.05). Laser irradiation alone did not lead to differences in µ-TBS (p > 0.05). SEM showed solidification globules on the surfaces of the specimens. The interfaces were similar on irradiated and non-irradiated surfaces. Laser irradiation of dentin through the uncured adhesive did not lead to higher µ-TBS when compared to the suggested manufacturer’s technique. However, this treatment brought benefits when performed on unetched dentin, since bond strengths were higher when compared to etched dentin.

  17. NCMS PWB program report surface finishes team task WBS No. 3.1.1: Phase 1, Etching Studies: Chemical etching of copper for improved solderability

    SciTech Connect

    Stevenson, J.O.; Guilinger, T.R.; Hosking, F.M.; Yost, F.G.; Sorensen, N.R.

    1995-06-01

    Sandia National Laboratories has established a Cooperative Research and Development Agreement with consortium members of the National Center for Manufacturing Sciences (NCMS) to develop fundamental generic technology in the area of printed wiring board materials and surface finishes. Improved solderability of copper substrates is an important component of the Sandia-NCMS program. We are investigating the effects of surface roughness on the wettability and solderability behavior of several different types of copper board finishes. In this paper, we present roughness and solderability characterizations for a variety of chemically-etched copper substrates. Initial testing on six chemical etches demonstrate that surface roughness can be greatly enhanced through chemical etching. Noticeable improvements in solder wettability were observed to accompany increases in roughness. A number of different algorithms and measures of roughness were used to gain insight into surface morphologies that lead to improved solderability.

  18. Laser surface pretreatment of 100Cr6 bearing steel - Hardening effects and white etching zones

    NASA Astrophysics Data System (ADS)

    Buling, Anna; Sändker, Hendrik; Stollenwerk, Jochen; Krupp, Ulrich; Hamann-Steinmeier, Angela

    2016-08-01

    In order to achieve a surface pretreatment of the bearing steel 100Cr6 (1-1.5 wt.% Cr) a laser-based process was used. The obtained modification may result in an optimization of the adhesive properties of the surface with respect to an anticorrosion polymer coating on the basis of PEEK (poly-ether-ether-ketone), which is applied on the steel surface by a laser melting technique. This work deals with the influence of the laser-based pretreatment regarding the surface microstructure and the micro-hardness of the steel, which has been examined by scanning electron microscopy (SEM), light microscopy and automated micro-hardness testing. The most suitable parameter set for the laser-based pretreatment leads to the formation of very hard white etching zones (WEZ) with a thickness of 23 μm, whereas this pretreatment also induces topographical changes. The occurrence of the white etching zones is attributed to near-surface re-austenitization and rapid quenching. Moreover, dark etching zones (DEZ) with a thickness of 32 μm are found at the laser path edges as well as underneath the white etching zones (WEZ). In these areas, the hardness is decreased due to the formation of oxides as a consequence of re-tempering.

  19. Energy dispersive X-ray spectroscopy analysis of Si sidewall surface etched by deep-reactive ion etching

    NASA Astrophysics Data System (ADS)

    Matsutani, Akihiro; Nishioka, Kunio; Sato, Mina

    2016-06-01

    We investigated the composition of a passivation film on a sidewall etched by deep-reactive ion etching (RIE) using SF6/O2 and C4F8 plasma, by energy-dispersive X-ray (EDX) spectroscopy. It was found that the compositions of carbon and fluorine in the passivation film on the etched sidewall depend on the width and depth of the etched trench. It is important to understand both the plasma behavior and the passivation film composition to carry out fabrication by deep-RIE. We consider that these results of the EDX analysis of an etched sidewall will be useful for understanding plasma behavior in order to optimize the process conditions of deep-RIE.

  20. Evaluation of Bone Healing on Sandblasted and Acid Etched Implants Coated with Nanocrystalline Hydroxyapatite: An In Vivo Study in Rabbit Femur

    PubMed Central

    Melin Svanborg, Lory; Meirelles, Luiz; Franke Stenport, Victoria; Currie, Fredrik; Andersson, Martin

    2014-01-01

    This study aimed at investigating if a coating of hydroxyapatite nanocrystals would enhance bone healing over time in trabecular bone. Sandblasted and acid etched titanium implants with and without a submicron thick coat of hydroxyapatite nanocrystals (nano-HA) were implanted in rabbit femur with healing times of 2, 4, and 9 weeks. Removal torque analyses and histological evaluations were performed. The torque analysis did not show any significant differences between the implants at any healing time. The control implant showed a tendency of more newly formed bone after 4 weeks of healing and significantly higher bone area values after 9 weeks of healing. According to the results from this present study, both control and nano-HA surfaces were biocompatible and osteoconductive. A submicron thick coating of hydroxyapatite nanocrystals deposited onto blasted and acid etched screw shaped titanium implants did not enhance bone healing, as compared to blasted and etched control implants when placed in trabecular bone. PMID:24723952

  1. Water adsorption on etched hydrophobic surfaces of L-, D- and DL-valine crystals

    NASA Astrophysics Data System (ADS)

    Segura, J. J.; Verdaguer, A.; Fraxedas, J.

    2014-03-01

    The adsorption of water on etched (001) surfaces of L-, D- and DL-valine crystals has been characterized by atomic force microscopy (AFM) using different operational modes (contact, non-contact and electrostatic) above and below the dew point, the temperature at which water vapor from humid air condenses into liquid water at constant atmospheric pressure. The analysis of the images suggests the formation of aggregates of solvated valine molecules that easily diffuse on the hydrophobic terraces only constrained by step barriers of the well-defined chiral parallelepipedic patterns induced by the etching process.

  2. Etching study of poled lithium tantalate crystal using wet etching technique with ultrasonic assistance

    NASA Astrophysics Data System (ADS)

    Gao, Z. D.; Wang, Q. J.; Zhang, Y.; Zhu, S. N.

    2008-02-01

    Utilizing the difference in etching rates of the positive and negative domains in an acid solution, domain pattern can be fabricated on the polarity surface of a congruent lithium tantalate crystal. Our results show that the ultrasonic agitation can improve the etching rate. An enhanced factor up to six was realized under a 50 W of ultrasonic power in a mixture with volumetric ratio of HF to H 2SO 4 at 1:2. The dependences of etching morphology on etching time and etching etchant for congruent lithium tantalate crystal were studied. The technique is applicable to fabricating three-dimensional microstructures on the surface of ferroelectric crystals.

  3. Silicon Wafer Surface-Temperature Monitoring System for Plasma Etching Process

    NASA Astrophysics Data System (ADS)

    Yamada, Y.; Ishii, J.; Nakaoka, A.; Mizojiri, Y.

    2011-08-01

    A thermoreflectance temperature measuring system was developed with the aim to realize monitoring of the silicon wafer surface temperature during plasma etching. The thermoreflectance detects variations in temperature through changes in optical reflectance. To overcome such difficulties as low sensitivity and limitation in installation space and position for in situ measurements, the differential thermoreflectance utilizing two orthogonal polarizations was introduced. Noise such as fluctuations in the incident beam intensity or changes of loss in the optical path would affect both polarizations equally and would not affect the measurement. The large angle of incidence of the beam allows measurement to be performed from outside the viewing ports of existing plasma etching process chambers through the gap between the plasma electrode and the silicon wafer. In this article, an off-line measurement result is presented, with results for bare wafers as well as for wafers with metal depositions. A prototype system developed for tests in plasma etching facilities in a production line is described.

  4. Fabrication of superhydrophobic surfaces on engineering material surfaces with stearic acid

    NASA Astrophysics Data System (ADS)

    Wang, Qi; Zhang, Bingwu; Qu, Mengnan; Zhang, Junyan; He, Deyan

    2008-01-01

    Via a simple wet chemical etching followed by stearic acid modification, the presence of synergistic binary structures at micro- and nanometer scales and stearic acid bestows superhydrophobic property on steel and aluminum alloy surfaces. The as-prepared surfaces show superhydrophobic not only for pure water but also for corrosive liquids such as acid, basic and salt solutions. The stable superhydrophobicity of steel and aluminum alloy surfaces will extend their applications as engineering materials.

  5. Etching of Niobium Sample Placed on Superconducting Radio Frequency Cavity Surface in Ar/CL2 Plasma

    SciTech Connect

    Janardan Upadhyay, Larry Phillips, Anne-Marie Valente

    2011-09-01

    Plasma based surface modification is a promising alternative to wet etching of superconducting radio frequency (SRF) cavities. It has been proven with flat samples that the bulk Niobium (Nb) removal rate and the surface roughness after the plasma etchings are equal to or better than wet etching processes. To optimize the plasma parameters, we are using a single cell cavity with 20 sample holders symmetrically distributed over the cell. These holders serve the purpose of diagnostic ports for the measurement of the plasma parameters and for the holding of the Nb sample to be etched. The plasma properties at RF (100 MHz) and MW (2.45 GHz) frequencies are being measured with the help of electrical and optical probes at different pressures and RF power levels inside of this cavity. The niobium coupons placed on several holders around the cell are being etched simultaneously. The etching results will be presented at this conference.

  6. 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

  7. Characterization and adsorption properties of diatomaceous earth modified by hydrofluoric acid etching.

    PubMed

    Tsai, Wen-Tien; Lai, Chi-Wei; Hsien, Kuo-Jong

    2006-05-15

    This work was a study of the chemical modification of diatomaceous earth (DE) using hydrofluoric acid (HF) solution. Under the experimental conditions investigated, it was found that HF under controlled conditions significantly etched inward into the interior of the existing pore structure in the clay mineral due to its high content of silica, leaving a framework possessing a larger BET surface area (ca. 10 m2 g(-1)) in comparison with that (ca. 4 m2 g(-1)) of its precursor (i.e., DE). Further, the results indicated that the HF concentration is a more determining factor in creating more open pores than other process parameters (temperature, holding time, and solid/liquid ratio). This observation was also in close agreement with the examinations by the silicon analysis, scanning electron microscopy, X-ray diffraction, and Fourier transform infrared spectroscopy. The adsorption kinetics and the adsorption isotherm of methylene blue onto the resulting clay adsorbent can be well described by a pseudo-second-order reaction model and the Freundlich model, respectively.

  8. Surface morphological instability of silicon (100) crystals under microwave ion physical etching

    NASA Astrophysics Data System (ADS)

    Yafarov, R. K.; Shanygin, V. Ya.

    2016-02-01

    This paper presents the results of studies of the dynamics of relaxation modification of the morphological characteristics of atomically clean surfaces of silicon (100) crystals with different types of conductivity after microwave ion physical etching in an argon atmosphere. For the first time, the effect of the electronic properties on the morphological characteristics and the surface free energy of silicon crystals is experimentally shown and proven by physicochemical methods.

  9. Low Temperature Plasma Surface Interactions: Atomic Layer Etching And Atmospheric Pressure Plasma Jet Modification Of Biomaterials

    NASA Astrophysics Data System (ADS)

    Oehrlein, Gottlieb

    2013-09-01

    Control of plasma-surface interactions is essential for successful application of low temperature plasma to materials processing. We review work performed in our laboratory in two areas: First, low pressure plasma surface interaction mechanisms aimed at achieving atomic precision in etching materials in the semiconductor industry. We discuss sequential reactions of surface passivation followed by directional low energy ion attack for ``volatile product'' removal to establish for what conditions self-limiting behavior required for Atomic Layer Etching (ALE) can be established using prototypical SiO2 -Si/fluorocarbon-Ar materials/etching systems. Second, studies of plasma-surface interactions related to application of a non-equilibrium atmospheric pressure plasma jet (APPJ) for modification of biomaterials are discussed. Changes in surface chemistry/biological activity of lipopolysaccharide (LPS) exposed to the APPJ plume/effluent in a controlled environment are reviewed. The results clarify how jet chemistry and interactions of plasma with the environment impact the consequences of APPJ-biomaterial-surface interactions. Based on collaborations with D. Metzler, S. Engelmann, R. Bruce, E. Joseph, E. Bartis, C. Hart, Q.-Y. Yang, J. Seog, T.-Y. Chung, H.-W. Chang, and D.B. Graves. We gratefully acknowledge funding from US Department of Energy (DE-SC0005105; DE-SC0001939) and National Science Foundation (CBET-1134273; PHY-1004256).

  10. Beam Simulation Studies of Plasma-Surface Interactions in Fluorocarbon Etching of Silicon and Silicon Dioxide

    NASA Astrophysics Data System (ADS)

    Gray, David C.

    1992-01-01

    A molecular beam apparatus has been constructed which allows the synthesis of dominant species fluxes to a wafer surface during fluorocarbon plasma etching. These species include atomic F as the primary etchant, CF _2 as a potential polymer forming precursor, and Ar^{+} or CF _{rm x}^{+} type ions. Ionic and neutral fluxes employed are within an order of magnitude of those typical of fluorocarbon plasmas and are well characterized through the use of in -situ probes. Etching yields and product distributions have been measured through the use of in-situ laser interferometry and line-of-sight mass spectrometry. XPS studies of etched surfaces were performed to assess surface chemical bonding states and average surface stoichiometry. A useful design guide was developed which allows optimal design of straight -tube molecular beam dosers in the collisionally-opaque regime. Ion-enhanced surface reaction kinetics have been studied as a function of the independently variable fluxes of free radicals and ions, as well as ion energy and substrate temperature. We have investigated the role of Ar ^{+} ions in enhancing the chemistries of F and CF_2 separately, and in combination on undoped silicon and silicon dioxide surfaces. We have employed both reactive and inert ions in the energy range most relevant to plasma etching processes, 20-500 eV, through the use of Kaufman and ECR type ion sources. The effect of increasing ion energy on the etching of fluorine saturated silicon and silicon dioxide surfaces was quantified through extensions of available low energy physical sputtering theory. Simple "site"-occupation models were developed for the quantification of the ion-enhanced fluorine etching kinetics in these systems. These models are suitable for use in topography evolution simulators (e.g. SAMPLE) for the predictive modeling of profile evolution in non-depositing fluorine-based plasmas such as NF_3 and SF_6. (Copies available exclusively from MIT Libraries, Rm. 14

  11. Improvement of polycrystalline silicon wafer solar cell efficiency by forming nanoscale pyramids on wafer surface using a self-mask etching technique.

    PubMed

    Lin, Hsin-Han; Chen, Wen-Hwa; Hong, Franklin C-N

    2013-05-01

    The creation of nanostructures on polycrystalline silicon wafer surface to reduce the solar reflection can enhance the solar absorption and thus increase the solar-electricity conversion efficiency of solar cells. The self-masking reactive ion etching (RIE) was studied to directly fabricate nanostructures on silicon surface without using a masking process for antireflection purpose. Reactive gases comprising chlorine (Cl2), sulfur hexafluoride (SF6), and oxygen (O2) were activated by radio-frequency plasma in an RIE system at a typical pressure of 120-130 mTorr to fabricate the nanoscale pyramids. Poly-Si wafers were etched directly without masking for 6-10 min to create surface nanostructures by varying the compositions of SF6, Cl2, and O2 gas mixtures in the etching process. The wafers were then treated with acid (KOH:H2O = 1:1) for 1 min to remove the damage layer (100 nm) induced by dry etching. The damage layer significantly reduced the solar cell efficiencies by affecting the electrical properties of the surface layer. The light reflectivity from the surface after acid treatment could be significantly reduced to <10% for the wavelengths between 500 and 900 nm. The effects of RIE and surface treatment conditions on the surface nanostructures and the optical performance as well as the efficiencies of solar cells will be presented and discussed. The authors have successfully fabricated large-area (156 × 156 mm(2)) subwavelength antireflection structure on poly-Si substrates, which could improve the solar cell efficiency reproducibly up to 16.27%, higher than 15.56% using wet etching.

  12. Improvement of polycrystalline silicon wafer solar cell efficiency by forming nanoscale pyramids on wafer surface using a self-mask etching technique.

    PubMed

    Lin, Hsin-Han; Chen, Wen-Hwa; Hong, Franklin C-N

    2013-05-01

    The creation of nanostructures on polycrystalline silicon wafer surface to reduce the solar reflection can enhance the solar absorption and thus increase the solar-electricity conversion efficiency of solar cells. The self-masking reactive ion etching (RIE) was studied to directly fabricate nanostructures on silicon surface without using a masking process for antireflection purpose. Reactive gases comprising chlorine (Cl2), sulfur hexafluoride (SF6), and oxygen (O2) were activated by radio-frequency plasma in an RIE system at a typical pressure of 120-130 mTorr to fabricate the nanoscale pyramids. Poly-Si wafers were etched directly without masking for 6-10 min to create surface nanostructures by varying the compositions of SF6, Cl2, and O2 gas mixtures in the etching process. The wafers were then treated with acid (KOH:H2O = 1:1) for 1 min to remove the damage layer (100 nm) induced by dry etching. The damage layer significantly reduced the solar cell efficiencies by affecting the electrical properties of the surface layer. The light reflectivity from the surface after acid treatment could be significantly reduced to <10% for the wavelengths between 500 and 900 nm. The effects of RIE and surface treatment conditions on the surface nanostructures and the optical performance as well as the efficiencies of solar cells will be presented and discussed. The authors have successfully fabricated large-area (156 × 156 mm(2)) subwavelength antireflection structure on poly-Si substrates, which could improve the solar cell efficiency reproducibly up to 16.27%, higher than 15.56% using wet etching. PMID:23847751

  13. Improvement of polycrystalline silicon wafer solar cell efficiency by forming nanoscale pyramids on wafer surface using a self-mask etching technique

    PubMed Central

    Lin, Hsin-Han; Chen, Wen-Hwa; Hong, Franklin C.-N.

    2013-01-01

    The creation of nanostructures on polycrystalline silicon wafer surface to reduce the solar reflection can enhance the solar absorption and thus increase the solar-electricity conversion efficiency of solar cells. The self-masking reactive ion etching (RIE) was studied to directly fabricate nanostructures on silicon surface without using a masking process for antireflection purpose. Reactive gases comprising chlorine (Cl2), sulfur hexafluoride (SF6), and oxygen (O2) were activated by radio-frequency plasma in an RIE system at a typical pressure of 120–130 mTorr to fabricate the nanoscale pyramids. Poly-Si wafers were etched directly without masking for 6–10 min to create surface nanostructures by varying the compositions of SF6, Cl2, and O2 gas mixtures in the etching process. The wafers were then treated with acid (KOH:H2O = 1:1) for 1 min to remove the damage layer (100 nm) induced by dry etching. The damage layer significantly reduced the solar cell efficiencies by affecting the electrical properties of the surface layer. The light reflectivity from the surface after acid treatment could be significantly reduced to <10% for the wavelengths between 500 and 900 nm. The effects of RIE and surface treatment conditions on the surface nanostructures and the optical performance as well as the efficiencies of solar cells will be presented and discussed. The authors have successfully fabricated large-area (156 × 156 mm2) subwavelength antireflection structure on poly-Si substrates, which could improve the solar cell efficiency reproducibly up to 16.27%, higher than 15.56% using wet etching. PMID:23847751

  14. Quantitative coverage and stability of hydrogen-passivation layers on HF-etched Si(1-x)Gex surfaces

    NASA Astrophysics Data System (ADS)

    Wilde, Markus; Fukutani, Katsuyuki; Koh, Shinji; Sawano, Kentarou; Shiraki, Yasuhiro

    2005-07-01

    This study investigates the stability of surface hydride layers passivating silicon-germanium alloys against contamination in ambient conditions after treatment in dilute hydrofluoric acid (HF), which is of central importance to the fabrication of SiGe-based semiconductor devices. We report quantitative hydrogen coverages on HF-etched Si(1-x)Gex surfaces (x=0,0.30,0.60,0.82), determined after air-to-vacuum transfer by H-specific H1(N15,αγ)C12 nuclear reaction analysis. Combination of this coverage information with analysis of the zero-point vibrational properties and N15-ion-induced desorption kinetics of the surface H atoms enables the distinction of well-passivated SiGe surfaces terminated exclusively by hydrides of Si and Ge from those partially covered by contaminating adsorbates. It is found that the resistance of HF-etched Si(1-x)Gex alloys against recontamination is drastically reduced at increasing Ge contents. Pure Si(100)-H is stably passivated at least up to 1week in air by a layer of 1.3±0.1 monolayer total H coverage. Si0.70Ge0.30 initially resembles H-passivated Si(100) but shows indications of moderate contamination after 1week in air. The HF treatment does not produce stable passivation layers on Ge-rich alloys (x⩾0.60), which suffer heavy recontamination within minutes after removal from the HF solution.

  15. Surface Passivation of CdZnTe Detector by Hydrogen Peroxide Solution Etching

    NASA Technical Reports Server (NTRS)

    Hayes, M.; Chen, H.; Chattopadhyay, K.; Burger, A.; James, R. B.

    1998-01-01

    The spectral resolution of room temperature nuclear radiation detectors such as CdZnTe is usually limited by the presence of conducting surface species that increase the surface leakage current. Studies have shown that the leakage current can be reduced by proper surface preparation. In this study, we try to optimize the performance of CdZnTe detector by etching the detector with hydrogen peroxide solution as function of concentration and etching time. The passivation effect that hydrogen peroxide introduces have been investigated by current-voltage (I-V) measurement on both parallel strips and metal-semiconductor-metal configurations. The improvements on the spectral response of Fe-55 and 241Am due to hydrogen peroxide treatment are presented and discussed.

  16. Wet-Etch Figuring: Optical Surfacing by Controlled Application of Etchant Solution Using the marangoni Effect

    SciTech Connect

    Rushford, M C; Britten, J A; Hoaglan, C R; Thomas, I M; Summers, L J; Dixit, S D

    2001-05-17

    Wet-etch figuring (WEF), a computer-controlled method for generating arbitrarily shaped optical surfaces using wet chemical etching, has been developed. This method uses applicator geometry and surface tension gradients (the Marangoni Effect) to define and confine the footprint of a wetted etchant zone on the surface. Capillary forces attach the flowing etchant solution to the underside of the optic being figured. No mechanical or thermal stresses or residues are applied to the optic by this process. This enables interferometric measurement of the glass thickness while surfacing, which then controls the placement and dwell time of the wetted zone. The result is a truly deterministic, closed-loop figuring process with a high degree of optical precision. This process can figure sub-millimeter thickness, large-aperture plates or sheets that are very difficult to finish by conventional methods. Automated linear and circular spot etching tools were used to demonstrate surfacing on 380 micron-thick glass sheets, to Strehl better than 0.8, as specified by data array or Zernike polynomials.

  17. Hybrid silicon honeycomb/organic solar cells with enhanced efficiency using surface etching

    NASA Astrophysics Data System (ADS)

    Liu, Ruiyuan; Sun, Teng; Liu, Jiawei; Wu, Shan; Sun, Baoquan

    2016-06-01

    Silicon (Si) nanostructure-based photovoltaic devices are attractive for their excellent optical and electrical performance, but show lower efficiency than their planar counterparts due to the increased surface recombination associated with the high surface area and roughness. Here, we demonstrate an efficiency enhancement for hybrid nanostructured Si/polymer solar cells based on a novel Si honeycomb (SiHC) structure using a simple etching method. SiHC structures are fabricated using a combination of nanosphere lithography and plasma treatment followed by a wet chemical post-etching. SiHC has shown superior light-trapping ability in comparison with the other Si nanostructures, along with a robust structure. Anisotropic tetramethylammonium hydroxide etching not only tunes the final surface morphologies of the nanostructures, but also reduces the surface roughness leading to a lower recombination rate in the hybrid solar cells. The suppressed recombination loss, benefiting from the reduced surface-to-volume ratio and roughness, has resulted in a high open-circuit voltage of 600 mV, a short-circuit current of 31.46 mA cm-2 due to the light-trapping ability of the SiHCs, and yields a power conversion efficiency of 12.79% without any other device structure optimization.

  18. Hybrid silicon honeycomb/organic solar cells with enhanced efficiency using surface etching

    NASA Astrophysics Data System (ADS)

    Liu, Ruiyuan; Sun, Teng; Liu, Jiawei; Wu, Shan; Sun, Baoquan

    2016-06-01

    Silicon (Si) nanostructure-based photovoltaic devices are attractive for their excellent optical and electrical performance, but show lower efficiency than their planar counterparts due to the increased surface recombination associated with the high surface area and roughness. Here, we demonstrate an efficiency enhancement for hybrid nanostructured Si/polymer solar cells based on a novel Si honeycomb (SiHC) structure using a simple etching method. SiHC structures are fabricated using a combination of nanosphere lithography and plasma treatment followed by a wet chemical post-etching. SiHC has shown superior light-trapping ability in comparison with the other Si nanostructures, along with a robust structure. Anisotropic tetramethylammonium hydroxide etching not only tunes the final surface morphologies of the nanostructures, but also reduces the surface roughness leading to a lower recombination rate in the hybrid solar cells. The suppressed recombination loss, benefiting from the reduced surface-to-volume ratio and roughness, has resulted in a high open-circuit voltage of 600 mV, a short-circuit current of 31.46 mA cm‑2 due to the light-trapping ability of the SiHCs, and yields a power conversion efficiency of 12.79% without any other device structure optimization.

  19. Hybrid silicon honeycomb/organic solar cells with enhanced efficiency using surface etching.

    PubMed

    Liu, Ruiyuan; Sun, Teng; Liu, Jiawei; Wu, Shan; Sun, Baoquan

    2016-06-24

    Silicon (Si) nanostructure-based photovoltaic devices are attractive for their excellent optical and electrical performance, but show lower efficiency than their planar counterparts due to the increased surface recombination associated with the high surface area and roughness. Here, we demonstrate an efficiency enhancement for hybrid nanostructured Si/polymer solar cells based on a novel Si honeycomb (SiHC) structure using a simple etching method. SiHC structures are fabricated using a combination of nanosphere lithography and plasma treatment followed by a wet chemical post-etching. SiHC has shown superior light-trapping ability in comparison with the other Si nanostructures, along with a robust structure. Anisotropic tetramethylammonium hydroxide etching not only tunes the final surface morphologies of the nanostructures, but also reduces the surface roughness leading to a lower recombination rate in the hybrid solar cells. The suppressed recombination loss, benefiting from the reduced surface-to-volume ratio and roughness, has resulted in a high open-circuit voltage of 600 mV, a short-circuit current of 31.46 mA cm(-2) due to the light-trapping ability of the SiHCs, and yields a power conversion efficiency of 12.79% without any other device structure optimization.

  20. The effect of inductively-coupled-plasma reactive ion etching power on the etching rate and the surface roughness of a sapphire substrate.

    PubMed

    Chang, Chun-Ming; Shiao, Ming-Hua; Yang, Chin-Tien; Cheng, Chung-Ta; Hsueh, Wen-Jeng

    2014-10-01

    In this study, patterned sapphire substrates are fabricated using nanosphere lithography (NSL) and inductively-coupled-plasma reactive ion etching (ICP-RIE). Polystyrene nanospheres of approximately 600 nm diameter are self-assembled on c-plane sapphire substrates by spin-coating. The diameter of the polystyrene nanospheres is modified to adjust the etching mask pitch cycle using oxygen plasma in the ICP-RIE system. A nickel thin film mask of 100 nm thickness is deposited by electron-beam evaporation on a substrate covered with treated nanospheres. The sapphire substrate is then etched in an inductively coupled plasma system using BCl3/Ar gas, to fabricate a structure with a periodic sub-micron hole array with different sidewall intervals. The DC bias voltage, the sapphire etching rate, the surface roughness, are studied as a function of the ICP and the RF power. Different sub-micron hole arrays with spacing cycles of 89 nm, 139 nm and 167 nm are successfully fabricated on the sapphire substrate, using suitable etching parameters. PMID:25942926

  1. Surface etching for light trapping in encapsulated InP solar cells

    NASA Technical Reports Server (NTRS)

    Jenkins, Phillip; Landis, Geoffrey A.

    1991-01-01

    Reducing the reflection from the surface of InP is important for increasing the efficiency of solar cells and photodetectors. In this paper a new technique for reducing reflectance of glass-encapsulated InP is reported. Low-angle grooves are produced on the surface by a maskless anisotropic etch. Light reflected from the low angle grooves is trapped by total internal reflection at the glass/air interface and directed back to the InP surface. A significant decrease in surface reflection is measured.

  2. UV-induced graft polymerization of acrylic acid in the sub-micronchannels of oxidized PET track-etched membrane

    NASA Astrophysics Data System (ADS)

    Korolkov, Ilya V.; Mashentseva, Anastassiya A.; Güven, Olgun; Taltenov, Abzal A.

    2015-12-01

    In this article, we report on functionalization of track-etched membrane based on poly(ethylene terephthalate) (PET TeMs) oxidized by advanced oxidation systems and by grafting of acrylic acid using photochemical initiation technique for the purpose of increasing functionality thus expanding its practical application. Among advanced oxidation processes (H2O2/UV) system had been chosen to introduce maximum concentration of carboxylic acid groups. Benzophenone (BP) photo-initiator was first immobilized on the surfaces of cylindrical pores which were later filled with aq. acrylic acid solution. UV-irradiation from both sides of PET TeMs has led to the formation of grafted poly(acrylic acid) (PAA) chains inside the membrane sub-micronchannels. Effect of oxygen-rich surface of PET TeMs on BP adsorption and subsequent process of photo-induced graft polymerization of acrylic acid (AA) were studied by ESR. The surface of oxidized and AA grafted PET TeMs was characterized by UV-vis, ATR-FTIR, XPS spectroscopies and by SEM.

  3. Nondestructive nanofabrication on Si(100) surface by tribochemistry-induced selective etching

    PubMed Central

    Guo, Jian; Yu, Bingjun; Chen, Lei; Qian, Linmao

    2015-01-01

    A tribochemistry-induced selective etching approach is proposed for the first time to produce silicon nanostructures without lattice damage. With a ~1 nm thick SiOx film as etching mask grown on Si(100) surface (Si(100)/SiOx) by wet-oxidation technique, nano-trenches can be produced through the removal of local SiOx mask by a SiO2 tip in humid air and the post-etching of the exposed Si in potassium hydroxide (KOH) solution. The material removal of SiOx mask and Si under low load is dominated by the tribochemical reaction at the interface between SiO2 tip and Si/SiOx sample, where the contact pressure is much lower than the critical pressure for initial yield of Si. High resolution transmission electron microscope (HRTEM) observation indicates that neither the material removal induced by tribochemical reaction nor the wet etching in KOH solution leads to lattice damage of the fabricated nanostructures. The proposed approach points out a new route in nondestructive nanofabrication. PMID:26559014

  4. No Positive Effect of Acid Etching or Plasma Cleaning on Osseointegration of Titanium Implants in a Canine Femoral Condyle Press-Fit Model

    PubMed Central

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

    2013-01-01

    Purpose: 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. Methods: 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. Results: 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. Conclusions: 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. PMID:23341850

  5. Adaptive wettability-enhanced surfaces ordered on molded etched substrates using shrink film

    NASA Astrophysics Data System (ADS)

    Jayadev, Shreshta; Pegan, Jonathan; Dyer, David; McLane, Jolie; Lim, Jessica; Khine, Michelle

    2013-01-01

    Superhydrophobic surfaces in nature exhibit desirable properties including self-cleaning, bacterial resistance, and flight efficiency. However, creating such intricate multi-scale features with conventional fabrication approaches is difficult, expensive, and not scalable. By patterning photoresist on pre-stressed shrink-wrap film, which contracts by 95% in surface area when heated, such features over large areas can be obtained easily. Photoresist serves as a dry etch mask to create complex and high-aspect ratio microstructures in the film. Using a double-shrink process, we introduce adaptive wettability-enhanced surfaces ordered on molded etched (AWESOME) substrates. We first create a mask out of the children’s toy ‘Shrinky-Dinks’ by printing dots using a laserjet printer. Heating this thermoplastic sheet causes the printed dots to shrink to a fraction of their original size. We then lithographically transfer the inverse pattern onto photoresist-coated shrink-wrap polyolefin film. The film is then plasma etched. After shrinking, the film serves as a high-aspect ratio mold for polydimethylsiloxane, creating a superhydrophobic surface with water contact angles >150° and sliding angles <10°. We pattern a microarray of ‘sticky’ spots with a dramatically different sliding angle compared to that of the superhydrophobic region, enabling microtiter-plate type assays without the need for a well plate.

  6. Plasma etching of Hf-based high-k thin films. Part II. Ion-enhanced surface reaction mechanisms

    SciTech Connect

    Martin, Ryan M.; Blom, Hans-Olof; Chang, Jane P.

    2009-03-15

    The mechanism for ion-enhanced chemical etching of hafnium aluminate thin films in Cl{sub 2}/BCl{sub 3} plasmas was investigated in this work, specifically how the film composition, ion energy, and plasma chemistry determine their etch rates. Several compositions of Hf{sub 1-x}Al{sub x}O{sub y} thin films ranging from pure HfO{sub 2} to pure Al{sub 2}O{sub 3} were etched in BCl{sub 3}/Cl{sub 2} plasmas and their etch rates were found to scale with {radical}(E{sub ion}) in both Cl{sub 2} and BCl{sub 3} plasmas. In Cl{sub 2} plasmas, a transition point was observed around 50 eV, where the etch rate was significantly enhanced while the linear dependence to {radical}(E{sub ion}) was maintained, corresponding to a change in the removal of fully chlorinated to less chlorinated reaction products. In BCl{sub 3} plasma, deposition dominates at ion energies below 50 eV, while etching occurs above that energy with an etch rate of three to seven times that in Cl{sub 2}. The faster etch rate in BCl{sub 3} was attributed to a change in the dominant ion from Cl{sub 2}{sup +} in Cl{sub 2} plasma to BCl{sub 2}{sup +} in BCl{sub 3}, which facilitated the formation of more volatile etch products and their removal. The surface chlorination (0-3 at. %) was enhanced with increasing ion energy while the amount of boron on the surface increases with decreasing ion energy, highlighting the effect of different plasma chemistries on the etch rates, etch product formation, and surface termination.

  7. 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

  8. Homogeneous alignment of nematic liquid crystals by ion beam etched surfaces

    NASA Technical Reports Server (NTRS)

    Wintucky, E. G.; Mahmood, R.; Johnson, D. L.

    1979-01-01

    A wide range of ion beam etch parameters capable of producing uniform homogeneous alignment of nematic liquid crystals on SiO2 films are discussed. The alignment surfaces were generated by obliquely incident (angles of 5 to 25 deg) argon ions with energies in the range of 0.5 to 2.0 KeV, ion current densities of 0.1 to 0.6 mA sq cm and etch times of 1 to 9 min. A smaller range of ion beam parameters (2.0 KeV, 0.2 mA sq cm, 5 to 10 deg and 1 to 5 min.) were also investigated with ZrO2 films and found suitable for homogeneous alignment. Extinction ratios were very high (1000), twist angles were small ( or = 3 deg) and tilt-bias angles very small ( or = 1 deg). Preliminary scanning electron microscopy results indicate a parallel oriented surface structure on the ion beam etched surfaces which may determine alignment.

  9. Metal-assisted chemical etching of Ge surface and its effect on photovoltaic devices

    NASA Astrophysics Data System (ADS)

    Lee, Seunghyo; Choo, Hyeokseong; Kim, Changheon; Oh, Eunseok; Seo, Dongwan; Lim, Sangwoo

    2016-05-01

    Ge surfaces were etched by means of metal-assisted chemical etching (MaCE). The behavior of the MaCE reaction in diluted H2O2 was compared with that of a conventional etchant of HF/H2O2/H2O mixture (FPM). Herein we first report that a pyramidal structure on Ge (0 0 1) can be prepared by MaCE in dilute H2O2 solution, without the use of HF. Contrastingly, an octagonal trench structure was prepared by 4/5/1 FPM treatment of Ge (0 0 1) surface. This octagonal structure consisted of a square base, four large facets connected to the base, and other four small facets adjacent to the four large facets, which were considered to be (0 0 1), {1 1 0}, and {1 1 1}, respectively. The octagonal trench was formed as a result of the difference in etch rate of Ge depending on the orientation: {1 0 0} > {1 1 0} > {1 1 1}. Ge surfaces treated by MaCE exhibited improved solar cell efficiency due to their improved light absorption, which led to significant increases in the cells' short circuit current and fill factor. The results suggest that optimized MaCE procedures can be an effective method to improve the performance of Ge-based photovoltaic devices.

  10. 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.

  11. Raman mapping analysis for removal of surface secondary phases of CZTS films using chemical etching

    NASA Astrophysics Data System (ADS)

    Wei, Zhengfei; Newman, Michael J.; Tsoi, Wing C.; Watson, Trystan M.

    2016-09-01

    Raman spectroscopy has been widely used as a non-destructive surface characterization method for the Cu2ZnSnS4 (CZTS) thin films. Secondary phases, which often co-exist with CZTS, are detrimental to the device performance. In this work, removal of the secondary phases using sodium sulfide (Na2S) aqueous solution etching in various time durations was investigated. Raman scattering mapping provides a direct visualization of phase distribution in CZTS-based materials on a relatively large scale (1 mm × 10 mm). Both as-grown and etched CZTS absorber layers were examined by Raman spectroscopy with a 532 nm excitation laser light in the range of 50-500 cm-1. A clear reduction of the secondary phases (mainly SnS) at the surface after etching was confirmed by Raman spectroscopy and scanning electron microscopy. Room temperature photoluminescence (PL) reveals a pronounced correlation between the amount of secondary phases and photoluminescence peak position. The PL spectra of the regions with more Sn-rich secondary phases show clearly a shift to high wavelength of the peak position, in comparison with regions with less Sn-rich secondary phases. These observed PL changes could be due to Sn-rich defects which may cause recombination processes.

  12. Effect of storage and acid etching on the tensile bond strength of composite resins to glass ionomer cement.

    PubMed

    Mesquita, M F; Domitti, S S; Consani, S; de Goes, M F

    1999-01-01

    This in vitro study evaluates the effect of storage time and acid etching on the tensile bond strength of glass ionomer cement to composite resins. The bonded assemblies were stored at 100% relative humidity and 37 degrees C for 1 hour, 1 day, 1 week, 1 month and 3 months. The test specimen was loaded at tension to failure on an Otto Wolpert-Werke testing instrument with a crosshead speed of 6 mm/min. The results showed a significant statistical difference for etched Vidrion F when compared to etched Ketac Bond at all storage periods. The unetched samples were statistically similar at 3 months, with the highest values for Vidrion F.

  13. Nanotexturing process on microtextured surfaces of silicon solar cells by SF6/O2 reactive ion etching.

    PubMed

    Ji, Hyungyong; Choi, Jaeho; Lim, Gyoungho; Parida, Bhaskar; Kim, Keunjoo; Jo, Jung Hee; Kim, Hong Seub

    2013-12-01

    We investigated a nanotexturing process on the microtextured surface of single crystalline silicon solar cell by the reactive ion etching process in SF6/O2 mixed gas ambient. P-type Si wafer samples were prepared using a chemical wet etching process to address saw damage removal and achieve microtexturing. The microtextured wafers were further processed for nanotexturing by exposure to reactive ions within a circular tray of wafer carrier containing many small holes for uniform etching. As the dry etching times were increased to 2, 4 and finally to 8 min, surface structures were observed in a transition from nanoholes to nanorods, and a variation in wafer color from dark blue to black. The surface nanostructures showed a lowered photoreflectance and enhanced quantum efficiency within the visible light region with wavelengths of less than 679 nm. The nanohole structure etched for 2 min showed enhanced conversion efficiency when compared to the bare sample; however, the nanorod structure etched for 8 min exhibited the decreased efficiency with a reduced short circuit current, indicating that the surface nanostructural damage with the enlarged nanoperimetric surface area is sensitive to surface passivation from the surface recombination process.

  14. Influence of acid-etching and ceramic primers on the repair of a glass ceramic.

    PubMed

    Queiroz, J R C; Souza, Rodrigo O A; Nogueira Junior, L; Ozcan, M; Bottino, M A

    2012-01-01

    The objective of this study was to evaluate the influence of different primers on the microtensile bond strength (μTBS) between a feldspathic ceramic and two composites. Forty blocks (6.0 x 6.0 x 5.0 mm³) were prepared from Vita Mark II . After polishing, they were randomly divided into 10 groups according to the surface treatment: Group 1, hydrofluoric acid 10% (HF) + silane; Group 2, CoJet + silane; Group 3, HF + Metal/Zirconia Primer; Group 4, HF + Clearfil Primer; Group 5, HF + Alloy Primer; Group 6, HF + V-Primer; Group 7, Metal/Zirconia Primer; Group 8, Clearfil Primer; Group 9, Alloy Primer; Group 10, V-Primer. After each surface treatment, an adhesive was applied and one of two composite resins was incrementally built up. The sticks obtained from each block (bonded area: 1.0 mm² ± 0.2 mm) were stored in distilled water at 37 degrees C for 30 days and submitted to thermocycling (7,000 cycles; 5 degrees C/55 degrees C ± 1 degree C). The μTBS test was carried out using a universal testing machine (1.0 mm/min). Data were analyzed using ANOVA and a Tukey test (a = 0.05). The surface treatments significantly affected the results (P < 0.05); no difference was observed between the composites (P > 0.05). The bond strength means (MPa) were as follows: Group 1a = 29.6; Group 1b = 33.7; Group 2a = 28.9; Group 2b = 27.1; Group 3a = 13.8; Group 3b = 14.9; Group 4a = 18.6; Group 4b = 19.4; Group 5a = 15.3; Group 5b = 16.5; Group 6a = 11; Group 6b = 18; Groups 7a to 10b = 0. While the use of primers alone was not sufficient for adequate bond strengths to feldspathic ceramic, HF etching followed by any silane delivered higher bond strength. PMID:22414522

  15. Influence of acid-etching and ceramic primers on the repair of a glass ceramic.

    PubMed

    Queiroz, J R C; Souza, Rodrigo O A; Nogueira Junior, L; Ozcan, M; Bottino, M A

    2012-01-01

    The objective of this study was to evaluate the influence of different primers on the microtensile bond strength (μTBS) between a feldspathic ceramic and two composites. Forty blocks (6.0 x 6.0 x 5.0 mm³) were prepared from Vita Mark II . After polishing, they were randomly divided into 10 groups according to the surface treatment: Group 1, hydrofluoric acid 10% (HF) + silane; Group 2, CoJet + silane; Group 3, HF + Metal/Zirconia Primer; Group 4, HF + Clearfil Primer; Group 5, HF + Alloy Primer; Group 6, HF + V-Primer; Group 7, Metal/Zirconia Primer; Group 8, Clearfil Primer; Group 9, Alloy Primer; Group 10, V-Primer. After each surface treatment, an adhesive was applied and one of two composite resins was incrementally built up. The sticks obtained from each block (bonded area: 1.0 mm² ± 0.2 mm) were stored in distilled water at 37 degrees C for 30 days and submitted to thermocycling (7,000 cycles; 5 degrees C/55 degrees C ± 1 degree C). The μTBS test was carried out using a universal testing machine (1.0 mm/min). Data were analyzed using ANOVA and a Tukey test (a = 0.05). The surface treatments significantly affected the results (P < 0.05); no difference was observed between the composites (P > 0.05). The bond strength means (MPa) were as follows: Group 1a = 29.6; Group 1b = 33.7; Group 2a = 28.9; Group 2b = 27.1; Group 3a = 13.8; Group 3b = 14.9; Group 4a = 18.6; Group 4b = 19.4; Group 5a = 15.3; Group 5b = 16.5; Group 6a = 11; Group 6b = 18; Groups 7a to 10b = 0. While the use of primers alone was not sufficient for adequate bond strengths to feldspathic ceramic, HF etching followed by any silane delivered higher bond strength.

  16. Surface roughness in XeF2 etching of a-Si/c-Si(100)

    NASA Astrophysics Data System (ADS)

    Stevens, A. A. E.; Beijerinck, H. C. W.

    2005-01-01

    Single wavelength ellipsometry and atomic force microscopy (AFM) have been applied in a well-calibrated beam-etching experiment to characterize the dynamics of surface roughening induced by chemical etching of a ~12 nm amorphous silicon (a-Si) top layer and the underlying crystalline silicon (c-Si) bulk. In both the initial and final phase of etching, where either only a-Si or only c-Si is exposed to the XeF2 flux, we observe a similar evolution of the surface roughness as a function of the XeF2 dose proportional to D(XeF2)β with β~0.2. In the transition region from the pure amorphous to the pure crystalline silicon layer, we observe a strong anomalous increase of the surface roughness proportional to D(XeF2)β with β~1.5. Not only the growth rate of the roughness increases sharply in this phase, also the surface morphology temporarily changes to a structure that suggests a cusplike shape. Both features suggest that the remaining a-Si patches on the surface act effectively as a capping layer which causes the growth of deep trenches in the c-Si. The ellipsometry data on the roughness are corroborated by the AFM results, by equating the thickness of the rough layer to 6 σ, with σ the root-mean-square variation of the AFM's distribution function of height differences. In the AFM data, the anomalous behavior is reflected in a too small value of σ which again suggests narrow and deep surface features that cannot be tracked by the AFM tip. The final phase morphology is characterized by an effective increase in surface area by a factor of two, as derived from a simple bilayer model of the reaction layer, using the experimental etch rate as input. We obtain a local reaction layer thickness of 1.5 monolayer consistent with the 1.7 ML value of Lo et al. [Lo et al., Phys. Rev. B 47, 648 (1993)] that is also independent of surface roughness.

  17. Two-photon polarization-selective etching of emergent nano-structures on diamond surfaces.

    PubMed

    Lehmann, A; Bradac, C; Mildren, R P

    2014-01-01

    Optical techniques have advanced considerably in recent years to enable processing of surfaces with a resolution less than the wavelength of light. Despite the highly selective nature of light-matter interactions, however, efforts to increase resolution to the scale of single atoms are hampered by rapid and efficient dissipation of the absorbed energy to the surrounding matrix. Here we show that two-photon surface excitation using ultraviolet light provides a method for selectively removing carbon from diamond surfaces. Polished surfaces etched by this method develop ultra-deep subwavelength structures with morphologies dependent on the polarization of the incident laser with respect to the crystal axes. As well as revealing a practical and versatile method for nano-patterning of diamond surfaces, we show that the results comprise mesoscopic evidence for bond scission via a highly localized optical interaction that may lead to the development of new optical approaches for ultra-nanoscale (<10 nm) surface structuring. PMID:24594857

  18. Metal etching with reactive gas cluster ion beams using pickup cell

    SciTech Connect

    Toyoda, Noriaki; Yamada, Isao

    2012-11-06

    Mixed gas cluster ion beams were formed using pickup cell for metal etching. O{sub 2} neutral clusters pick up acetic acid and formed mixed cluster beam. By using O{sub 2}-GCIB with acetic acid, enhancement of Cu etching was observed. Because of dense energy deposition by GCIB, etching of Cu proceeds by CuO formation, enhancement of chemical reaction with acetic acid and desorption of etching products. Surface roughening was not observed on poly crystalline Cu because of the small dependence of etching rate on crystal orientation. Halogen free and low-temperature metal etching with GCIB using pickup cell is possible.

  19. Metal etching with reactive gas cluster ion beams using pickup cell

    NASA Astrophysics Data System (ADS)

    Toyoda, Noriaki; Yamada, Isao

    2012-11-01

    Mixed gas cluster ion beams were formed using pickup cell for metal etching. O2 neutral clusters pick up acetic acid and formed mixed cluster beam. By using O2-GCIB with acetic acid, enhancement of Cu etching was observed. Because of dense energy deposition by GCIB, etching of Cu proceeds by CuO formation, enhancement of chemical reaction with acetic acid and desorption of etching products. Surface roughening was not observed on poly crystalline Cu because of the small dependence of etching rate on crystal orientation. Halogen free and low-temperature metal etching with GCIB using pickup cell is possible.

  20. Effect of hydrofluoric acid etching on shear bond strength of an indirect resin composite to an adhesive cement.

    PubMed

    Hori, Sayaka; Minami, Hiroyuki; Minesaki, Yoshito; Matsumura, Hideo; Tanaka, Takuo

    2008-07-01

    This study evaluated the effect of 1% hydrofluoric acid (HF) treatment on the bonding of an adhesive cement (Panavia F 2.0) to an indirect resin composite (Estenia C&B). Pairs of composite disks (10 and 8 mm in diameter by 3 mm thickness) were prepared. Adhesive surfaces were pretreated with either airborne particle abrasion or HF etching before being soaked for 30 seconds, five minutes or 10 minutes, with or without application of silane coupling agent. Adhesive specimens were fabricated by cementing a pair of treated disks. Shear bond strength was determined before and after 50,000 times of thermocycling (4 and 60 degrees C). All data were statistically analyzed using two-way ANOVA and Bonferroni's test (a=0.05). Bond strength achieved with five minutes of HF etching (18.3+/-1.1 MPa) was significantly higher (P=0.0025) than that obtained with airborne particle abrasion followed by application of silane coupling agent (14.3+/-1.8 MPa) after thermocycling.

  1. Fabrication of superhydrophobic and highly oleophobic silicon-based surfaces via electroless etching method

    NASA Astrophysics Data System (ADS)

    Nguyen, Thi Phuong Nhung; Dufour, Renaud; Thomy, Vincent; Senez, Vincent; Boukherroub, Rabah; Coffinier, Yannick

    2014-03-01

    This study reports on a simple method for the preparation of superhydrophobic and highly oleophobic nanostructured silicon surfaces. The technique relies on metal-assisted electroless etching of silicon in sodium tetrafluoroborate (NaBF4) aqueous solution. Then, silver particles were deposited on the obtained surfaces, changing their overall physical morphology. Finally, the surfaces were coated by either C4F8, a fluoropolymer deposited by plasma, or by SiOx overlayers chemically modified with 1H,1H,2H,2H-perfluorodecyltrichlorosilane (PFTS) through silanization reaction. All these surfaces exhibit a superhydrophobic character (large apparent contact angle and low hysteresis with respect to water). In addition, they present high oleophobic properties, i.e. a high repellency to low surface energy liquids with various contact angle hysteresis, both depending on the morphology and type of coating.

  2. 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

  3. Effect of sodium sulfite, carboxylic monomer, and phosphoric acid etching on bonding of tri-n-butylborane initiated resin to human enamel.

    PubMed

    Nogawa, Hiroshi; Koizumi, Hiroyasu; Akazawa, Nobutaka; Hiraba, Haruto; Nakamura, Mitsuo; Matsumura, Hideo

    2015-03-01

    The purpose of the present study is evaluation of bonding durability of tri-n-butylborane (TBB) initiated resin without 4-methacryloyloxyethyl trimellitate anhydride (4-META) joined to human enamel. Ground human enamel was bonded with TBB resin under six surface conditions: 1) as ground, 2) primed with Teeth Primer, 3) sodium sulfite solution, 4) 4-META solution, 5) acetone-water, and 6) phosphoric acid etching. Pre- and post-thermocycling bond strengths and change in strength after thermocycling were compared. Etching enamel with 35-45% phosphoric acid enhanced bonding durability between enamel and TBB-initiated resin. Priming with Teeth Primer or 4-META solution improved bond strength between enamel and TBB-initiated resin. Sodium sulfite had little effect on enamel bonding in the present bonding systems. PMID:25807904

  4. Nonhomogeneous surface properties of parylene-C film etched by an atmospheric pressure He/O2 micro-plasma jet in ambient air

    NASA Astrophysics Data System (ADS)

    Wang, Tao; Yang, Bin; Chen, Xiang; Wang, Xiaolin; Yang, Chunsheng; Liu, Jingquan

    2016-10-01

    Surface properties of parylene-C film etched by an atmospheric pressure He/O2 micro-plasma jet in ambient air were investigated. The morphologies and chemical compositions of the etched surface were analyzed by optical microscopy, SEM, EDS, XPS and ATR-FTIR. The microscopy and SEM images showed the etched surface was nonhomogeneous with six discernable ring patterns from the center to the outside domain, which were composed of (I) a central region; (II) an effective etching region, where almost all of the parylene-C film was removed by the plasma jet with only a little residual parylene-C being functionalized with carboxyl groups (Cdbnd O, Osbnd Cdbnd O-); (III) an inner etching boundary; (IV) a middle etching region, where the film surface was smooth and partially removed; (V) an outer etching boundary, where the surface was decorated with clusters of debris, and (VI) a pristine parylene-C film region. The analysis of the different morphologies and chemical compositions illustrated the different localized etching process in the distinct regions. Besides, the influence of O2 flow rate on the surface properties of the etched parylene-C film was also investigated. Higher volume of O2 tended to weaken the nonhomogeneous characteristics of the etched surface and improve the etched surface quality.

  5. Stretchability of Silver Films on Thin Acid-Etched Rough Polydimethylsiloxane Substrates Fabricated by Electrospray Deposition

    NASA Astrophysics Data System (ADS)

    Mehdi, S. M.; Cho, K. H.; Kang, C. N.; Choi, K. H.

    2015-07-01

    This paper investigates the fabrication of Ag films through the electrospray deposition (ESD) technique on sub-millimeter-thick acid-etched rough polydimethylsiloxane (PDMS) substrates having both low and high modulus of elasticity. The main focus of the study is on the stretchable behavior of ESD-deposited Ag nanoparticles-based thin films on these substrates when subjected to axial strains. Experimental results suggest that the as-fabricated films on thin acid-etched rough low modulus PDMS has an average stretchability of 5.6% with an average increase in the resistance that is 23 times that of the initial resistance at electrical failure (complete rupture of the films). Comparatively, the stretchability of Ag films on the high modulus PDMS was found to be 3 times higher with 4.65 times increase in the resistance at electrical failure. Also, a high positive value of the piezoresistive coefficient for these films suggests that the resistivity changes during stretching, and thus deviation from the simplified models is inevitable. Based on these results, new models are presented that quantify the changes in resistance with strain.

  6. Mechanism for low-etching resistance and surface roughness of ArF photoresist during plasma irradiation

    SciTech Connect

    Jinnai, Butsurin; Koyama, Koji; Kato, Keisuke; Yasuda, Atsushi; Momose, Hikaru; Samukawa, Seiji

    2009-03-01

    ArF excimer laser lithography was introduced to fabricate nanometer-scale devices and uses chemically amplified photoresist polymers including photoacid generators (PAGs). Because plasma-etching processes cause serious problems related to the use of ArF photoresists, such as line-edge roughness and low etching selectivity, we have to understand the interaction between plasma and ArF photoresist polymers. Investigating the effects of surface temperature and the irradiation species from plasma, we have found that ion irradiation by itself did not drastically increase the roughness or etching rate of ArF photoresist films unless it was combined with ultraviolet/vacuum ultraviolet (UV/VUV) photon irradiation. The structures of ArF photoresist polymers were largely unchanged by ion irradiation alone but were destroyed by combinations of ion and UV/VUV-photon irradiation. Our results suggested that PAG-mediated deprotection induced by UV/VUV-photon irradiation was amplified at surface temperatures above 100 deg. C. The etching rate and surface roughness of plasma-etched ArF photoresists are affected by the irradiation species and surface temperature during plasma etching. UV/VUV-photon irradiation plays a particularly important role in the interaction between plasma and ArF photoresist polymers.

  7. Removal and deposition efficiencies of the long-lived 222Rn daughters during etching of germanium surfaces

    NASA Astrophysics Data System (ADS)

    Zuzel, G.; Wójcik, M.; Majorovits, B.; Lampert, M. O.; Wendling, P.

    2012-06-01

    Removal and deposition efficiencies of the long-lived 222Rn daughters during etching from and onto surfaces of standard and high purity germanium were investigated. The standard etching procedure of Canberra-France used during production of high purity n-type germanium diodes was applied to germanium discs, which have been exposed earlier to a strong radon source for deposition of its progenies. An uncontaminated sample was etched in a solution containing 210Pb, 210Bi and 210Po. All isotopes were measured before and after etching with appropriate detectors. In contrast to copper and stainless steel, they were removed from germanium very efficiently. However, the reverse process was also observed. Considerable amounts of radioactive lead, bismuth and polonium isotopes present initially in the artificially polluted etchant were transferred to the clean high purity surface during processing of the sample.

  8. CH4/Ar/H2/SF6 Plasma Etching for Surface Oxide Removal of Indium Bumps

    NASA Astrophysics Data System (ADS)

    Huang, Yue; Lin, Chun; Ye, Zhen-Hua; Liao, Qing-Jun; Ding, Rui-Jun

    2015-07-01

    Plasma etching for surface indium oxide removal by methane/argon/hydrogen/sulfur hexafluoride (CH4/Ar/H2/SF6) mixture has been implemented. The morphology of the indium bumps was not deteriorated after the plasma etching. High-resolution O 1 s x-ray photoelectron spectroscopy (XPS) proved that the In-O component decreased from 44.5% for the nonetched sample to 10.8% for the sample after plasma etching. The surface modification of the indium bumps might be in the form of doped fluorine according to the XPS results. The zero-bias resistance derived from current-voltage ( I- V) measurements for plasma-etched infrared detectors was comparable to that for nonetched ones, indicating that such plasma treatment is suitable for processing sensitive materials such as mercury cadmium telluride.

  9. Ab initio calculations on etching of graphite and diamond surfaces by atomic hydrogen

    SciTech Connect

    Kanai, C.; Watanabe, K.; Takakuwa, Y.

    2001-06-15

    Etching of graphite and hydrogenated diamond C(100) 2{times}1 surfaces by irradiating atomic hydrogen, which is one of the key reactions to promote epitaxial diamond growth by chemical vapor deposition, has been investigated by ab initio pseudopotential calculations. We demonstrate the reaction pathways and determine the activation energies for breaking C-C bonds on the surfaces by irradiating hydrogen atoms. The activation energy for C-C bond breaking on graphite is found to be only one-half of that on the hydrogenated diamond surface. This indicates that graphite, which is a typical nondiamond phase unnecessarily generated on the diamond surface during epitaxial growth, can be selectively eliminated by atomic hydrogen, resulting in methane desorption. Our result supports the growth rate enhancement in diamond epitaxy observed in a recent experiment by gas-source molecular beam epitaxy under hydrogen beam irradiation.

  10. Reducing intrinsic loss in superconducting resonators by surface treatment and deep etching of silicon substrates

    SciTech Connect

    Bruno, A.; Lange, G. de; Asaad, S.; Enden, K. L. van der; Langford, N. K.; DiCarlo, L.

    2015-05-04

    We present microwave-frequency NbTiN resonators on silicon, systematically achieving internal quality factors above 1 M in the quantum regime. We use two techniques to reduce losses associated with two-level systems: an additional substrate surface treatment prior to NbTiN deposition to optimize the metal-substrate interface and deep reactive-ion etching of the substrate to displace the substrate-vacuum interfaces away from high electric fields. The temperature and power dependence of resonator behavior indicate that two-level systems still contribute significantly to energy dissipation, suggesting that more interface optimization could further improve performance.

  11. Visualization of the cytoplasmic surface of Torpedo postsynaptic membranes by freeze-etch and immunoelectron microscopy

    PubMed Central

    1987-01-01

    The synapse-specific Mr 43,000 protein (43K protein) and the acetylcholine receptor were visualized by freeze-etch immunoelectron microscopy in preparations of purified Torpedo postsynaptic membranes. Vesicles were immobilized on glass and then sheared open by sonication to expose the cytoplasmic surface. Membranes were labeled with monoclonal antibodies to the 43K protein or the acetylcholine receptor. The cytoplasmic surface was devoid of filamentous structure, and the 43K protein and the cytoplasmic projection of the acetylcholine receptor were associated with prominent surface particles. Acetylcholine receptor and 43K protein, in membrane surfaces in direct contact with glass coated with polyornithine, segregated into dense particle aggregates separated by smooth membrane patches, whereas those in contact with glass coated with Alcian Blue underwent little or no detectable rearrangement. After treatment of vesicles at alkaline pH to remove the 43K protein, the cytoplasmic surfaces were still covered by a dense array of particles that were more uniform in shape and appeared slightly shorter than those seen on unextracted membranes, but similar in height to the extracellular projection. Monoclonal antibodies to the acetylcholine receptor labeled these particles, while antibodies to 43K protein did not. We conclude that the 43K protein is in direct association with the receptor and that complexes of the receptor and 43K protein can undergo surface-induced lateral redistribution. In addition, the cytoplasmic projection of the acetylcholine receptor is sufficiently large to be readily detected by freeze-etch electron microscopy and is similar in height to the extracellular projection. PMID:3312239

  12. Fabrication of long-range surface plasmon polaritons waveguide by wet chemical etching

    NASA Astrophysics Data System (ADS)

    Xie, Ying; Liu, Tong; Zhao, Xuliang; Zhang, Meiling; Chen, Changming; Wang, Fei; Sun, Xiaoqiang; Zhang, Daming

    2014-06-01

    The fabrication of long-range surface plasmon polaritons (LRSPPs) waveguides based on a thin Au stripe embedded in poly(methyl-methacrylate-glycidly-methacrylate) polymers was investigated. By patterning the photoresist, a wet chemical etching technique was used to avoid sharp pin-like and shark-fin-like structures on the edges of the Au stripe. The surface morphology of the Au film and polymer cladding were studied by atomic force microscopy (AFM), as well as by using the waveguide configuration of the Au stripe. AFM images proved the elimination of parasitic structures. A 2 cm long, 4 μm wide, and 25 nm thick Au stripe waveguide exhibited a propagation loss of approximately 4.3 dB cm-1 measured by the cut-back method and end-fire excitation of LRSPP mode guiding at 1550 nm. The demonstration of optical signal transmission indicates that the LRSPP waveguide fabricated by wet chemical etching is a potential solution to on-chip optical interconnections.

  13. Influence of Organic Acids from the Oral Biofilm on the Bond Strength of Self-Etch Adhesives to Dentin.

    PubMed

    Amaral, Cristiane Mariote; Correa, Danielly de Sá; Miragaya, Luciana Meirelles; Silva, Eduardo Moreira da

    2015-10-01

    The aim of this study was to evaluate the microtensile bond strength of self-etch adhesive systems to dentin after storage in acids from oral biofilm. Three adhesive systems were used in the study: a two-step self-etch adhesive for use with a silorane-based resin composite (Filtek P90 adhesive system - P90), a two-step self-etch adhesive (Clearfil SE Bond - CSE) and a one-step self-etch adhesive (Adper Easy One - AEO). The bond strength of these products was evaluated by bonding resin composite (Filtek Z350 for CSE and AEO; and Filtek P90 for P90) to 90 bovine dentin tooth fragments, according to the manufacturer's instructions. After 24 h of water storage at 37 °C, the specimens were sectioned into beams (1 mm2) divided and stored in distilled water, lactic acid and propionic acid, for 7 and 30 days. After storage, the specimens were tested for microtensile bond strength. Data were analyzed by three-way ANOVA and Tukey´s test (α=0.05). CSE presented the highest microtensile bond strength after storage in distilled water for 7 and 30 days. The microtensile bond strength of all adhesive systems was lower after storage in lactic acid and propionic acid than after water storage. Significant difference was not found between storage times. PMID:26647935

  14. Transparent, superhydrophobic, and wear-resistant surfaces using deep reactive ion etching on PDMS substrates.

    PubMed

    Ebert, Daniel; Bhushan, Bharat

    2016-11-01

    Surfaces that simultaneously exhibit superhydrophobicity, low contact angle hysteresis, and high transmission of visible light are of interest for many applications, such as optical devices, solar panels, and self-cleaning windows. Superhydrophobicity could also find use in medical devices where antifouling characteristics are desirable. These applications also typically require mechanical wear resistance. The fabrication of such surfaces is challenging due to the competing goals of superhydrophobicity and transmittance in terms of the required degree of surface roughness. In this study, deep reactive ion etching (DRIE) was used to create rough surfaces on PDMS substrates using a O2/CF4 plasma. Surfaces then underwent an additional treatment with either octafluorocyclobutane (C4F8) plasma or vapor deposition of perfluorooctyltrichlorosilane (PFOTCS) following surface activation with O2 plasma. The effects of surface roughness and the additional surface modifications were examined with respect to the contact angle, contact angle hysteresis, and optical transmittance. To examine wear resistance, a sliding wear experiment was performed using an atomic force microscope (AFM).

  15. Transparent, superhydrophobic, and wear-resistant surfaces using deep reactive ion etching on PDMS substrates.

    PubMed

    Ebert, Daniel; Bhushan, Bharat

    2016-11-01

    Surfaces that simultaneously exhibit superhydrophobicity, low contact angle hysteresis, and high transmission of visible light are of interest for many applications, such as optical devices, solar panels, and self-cleaning windows. Superhydrophobicity could also find use in medical devices where antifouling characteristics are desirable. These applications also typically require mechanical wear resistance. The fabrication of such surfaces is challenging due to the competing goals of superhydrophobicity and transmittance in terms of the required degree of surface roughness. In this study, deep reactive ion etching (DRIE) was used to create rough surfaces on PDMS substrates using a O2/CF4 plasma. Surfaces then underwent an additional treatment with either octafluorocyclobutane (C4F8) plasma or vapor deposition of perfluorooctyltrichlorosilane (PFOTCS) following surface activation with O2 plasma. The effects of surface roughness and the additional surface modifications were examined with respect to the contact angle, contact angle hysteresis, and optical transmittance. To examine wear resistance, a sliding wear experiment was performed using an atomic force microscope (AFM). PMID:27454031

  16. Investigation of Si(h k l) surfaces etched in KOH solutions saturated with tertiary-butyl alcohol

    NASA Astrophysics Data System (ADS)

    Rola, K. P.; Zubel, I.

    2011-11-01

    Anisotropic etching of silicon in KOH solutions saturated with tertiary-butyl alcohol (tert-butanol) was studied in this paper. The influence of KOH concentration of the solution with tert-butanol on Si(1 0 0) surface roughness and convex corners undercut were examined. It was shown that the largest reduction of convex corner undercut is achievable at low (3 M) concentration of KOH, at which, though, the (1 0 0) surface is densely covered with hillocks. The study on etch rate anisotropy and surface morphology of silicon substrates with different crystallographic orientations etched in 3 M KOH solutions with tert-butanol was conducted. The advantage of tert-butanol over isopropanol in terms of shaping three-dimensional structures in the (2 2 1) substrate was presented. The impact of agitation of the etching solution on roughness of (1 1 0) and (h h 1) surfaces and the distribution of hillocks on (1 0 0) and (h 1 1) surfaces were shown. Based on surface tension measurements and theoretical considerations, an adsorption explanation of the visible difference in (1 0 0) surface morphologies in the case of solutions saturated with tert-butanol and isopropanol was proposed. The KOH solution with tert-butanol could be particularly useful for texturing Si(1 0 0) surfaces, due to the possibility of achieving a dense surface coverage with hillocks in the solution saturated with the alcohol.

  17. Tailoring the surface of ZnO nanorods into corrugated nanorods via a selective chemical etch method

    NASA Astrophysics Data System (ADS)

    Duan, Xiangyang; Chen, Guangde; Li, Chu; Yin, Yuan; Jin, Wentao; Guo, Lu'an; Ye, Honggang; Zhu, Youzhang; Wu, Yelong

    2016-07-01

    Using the chemical vapour deposition method, we successfully converted smooth ZnO nanorods (NRs) into corrugated NRs by simply increasing the reaction time. The surface morphology and crystallographic structure of the corrugated NRs were investigated. The corrugated NRs were decorated by alternant (11\\bar{2}1) and (11\\bar{2}\\bar{1}) planes at the exposed side surfaces while the conventional \\{10\\bar{1}0\\} planes disappeared. No twinning boundaries were found in the periodically corrugated structures, indicating that they were type II corrugated NRs. Further investigation told us that they were selectively etched. We introduced a hydrothermal method to synthesize the smooth ZnO NRs and then etched them in a tube furnace at 950 °C with a flow of carbon monoxide. By separating the growth stage and the selective etching stage, we explicitly demonstrated a successfully selective etching effect on ZnO NRs with a carbon monoxide reducing atmosphere for the first time. An etching mechanism based on the selective reaction between carbon monoxide and the different exposed surfaces was proposed. Our results will improve the understanding of the growth mechanism on coarse or corrugated NRs and provide a new strategy for the application of surface controlled nanostructured materials.

  18. Tailoring the surface of ZnO nanorods into corrugated nanorods via a selective chemical etch method.

    PubMed

    Duan, Xiangyang; Chen, Guangde; Li, Chu; Yin, Yuan; Jin, Wentao; Guo, Lu'an; Ye, Honggang; Zhu, Youzhang; Wu, Yelong

    2016-07-22

    Using the chemical vapour deposition method, we successfully converted smooth ZnO nanorods (NRs) into corrugated NRs by simply increasing the reaction time. The surface morphology and crystallographic structure of the corrugated NRs were investigated. The corrugated NRs were decorated by alternant [Formula: see text] and [Formula: see text] planes at the exposed side surfaces while the conventional [Formula: see text] planes disappeared. No twinning boundaries were found in the periodically corrugated structures, indicating that they were type II corrugated NRs. Further investigation told us that they were selectively etched. We introduced a hydrothermal method to synthesize the smooth ZnO NRs and then etched them in a tube furnace at 950 °C with a flow of carbon monoxide. By separating the growth stage and the selective etching stage, we explicitly demonstrated a successfully selective etching effect on ZnO NRs with a carbon monoxide reducing atmosphere for the first time. An etching mechanism based on the selective reaction between carbon monoxide and the different exposed surfaces was proposed. Our results will improve the understanding of the growth mechanism on coarse or corrugated NRs and provide a new strategy for the application of surface controlled nanostructured materials. PMID:27276661

  19. Modifying the surface charge of single track-etched conical nanopores in polyimide

    NASA Astrophysics Data System (ADS)

    Ali, M.; Schiedt, B.; Healy, K.; Neumann, R.; Ensinger, W.

    2008-02-01

    Chemical modification of nanopore surfaces is of great interest as it means that the surface composition is no longer fixed by the choice of substrate material, even to the point where large biomolecules can be attached to the pore walls. Controlling nanopore transport characteristics is one important application of surface modification which is very relevant given the significant interest in sensors based on the transport of ions and molecules through nanopores. Reported here is a method to change the surface charge polarity of single track-etched conical nanopores in polyimide, which also has the potential to attach more complex molecules to the carboxyl groups on the nanopore walls. These carboxyl groups were converted into terminal amino groups, first by activation with N-(3-dimethylaminopropyl)-N-ethylcarbodiimide (EDC) and N-hydroxysuccinimide (NHS) followed by the covalent coupling of ethylenediamine. This results in a changed surface charge polarity. Regeneration of a carboxyl-terminated surface was also possible, by reaction of the amino groups with succinic anhydride. The success of these reactions was confirmed by measurements of the pore's pH sensitive current-voltage (I-V) characteristics before and after the chemical modification, which depend on surface charge. The permselectivity of the pores also changed accordingly with the modification.

  20. Synthesis and characterization of hybrid micro/nano-structured NiTi surfaces by a combination of etching and anodizing.

    PubMed

    Huan, Z; Fratila-Apachitei, L E; Apachitei, I; Duszczyk, J

    2014-02-01

    The purpose of this study was to generate hybrid micro/nano-structures on biomedical nickel-titanium alloy (NiTi). To achieve this, NiTi surfaces were firstly electrochemically etched and then anodized in fluoride-containing electrolyte. With the etching process, the NiTi surface was micro-roughened through the formation of micropits uniformly distributed over the entire surface. Following the subsequent anodizing process, self-organized nanotube structures enriched in TiO2 could be superimposed on the etched surface under specific conditions. Furthermore, the anodizing treatment significantly reduced water contact angles and increased the surface free energy compared to the surfaces prior to anodizing. The results of this study show for the first time that it is possible to create hybrid micro/nano-structures on biomedical NiTi alloys by combining electrochemical etching and anodizing under controlled conditions. These novel structures are expected to significantly enhance the surface biofunctionality of the material when compared to conventional implant devices with either micro- or nano-structured surfaces.

  1. Synthesis and characterization of hybrid micro/nano-structured NiTi surfaces by a combination of etching and anodizing

    NASA Astrophysics Data System (ADS)

    Huan, Z.; Fratila-Apachitei, L. E.; Apachitei, I.; Duszczyk, J.

    2014-02-01

    The purpose of this study was to generate hybrid micro/nano-structures on biomedical nickel-titanium alloy (NiTi). To achieve this, NiTi surfaces were firstly electrochemically etched and then anodized in fluoride-containing electrolyte. With the etching process, the NiTi surface was micro-roughened through the formation of micropits uniformly distributed over the entire surface. Following the subsequent anodizing process, self-organized nanotube structures enriched in TiO2 could be superimposed on the etched surface under specific conditions. Furthermore, the anodizing treatment significantly reduced water contact angles and increased the surface free energy compared to the surfaces prior to anodizing. The results of this study show for the first time that it is possible to create hybrid micro/nano-structures on biomedical NiTi alloys by combining electrochemical etching and anodizing under controlled conditions. These novel structures are expected to significantly enhance the surface biofunctionality of the material when compared to conventional implant devices with either micro- or nano-structured surfaces.

  2. Morphology and chemical termination of HF-etched Si{sub 3}N{sub 4} surfaces

    SciTech Connect

    Liu, Li-Hong; Debenedetti, William J. I.; Peixoto, Tatiana; Gokalp, Sumeyra; Shafiq, Natis; Veyan, Jean-François; Chabal, Yves J.; Michalak, David J.; Hourani, Rami

    2014-12-29

    Several reports on the chemical termination of silicon nitride films after HF etching, an important process in the microelectronics industry, are inconsistent claiming N-H{sub x}, Si-H, or fluorine termination. An investigation combining infrared and x-ray photoelectron spectroscopies with atomic force and scanning electron microscopy imaging reveals that under some processing conditions, salt microcrystals are formed and stabilized on the surface, resulting from products of Si{sub 3}N{sub 4} etching. Rinsing in deionized water immediately after HF etching for at least 30 s avoids such deposition and yields a smooth surface without evidence of Si-H termination. Instead, fluorine and oxygen are found to terminate a sizeable fraction of the surface in the form of Si-F and possibly Si-OH bonds. The relatively unique fluorine termination is remarkably stable in both air and water and could lead to further chemical functionalization pathways.

  3. Bubble-Regulated Silicon Nanowire Synthesis on Micro-Structured Surfaces by Metal-Assisted Chemical Etching.

    PubMed

    Li, Yinxiao; Duan, Chuanhua

    2015-11-10

    In this work, we study silicon nanowire synthesis via one-step metal-assisted chemical etching (MACE) on microstructured silicon surfaces with periodic pillar/cavity array. It is found that hydrogen gas produced from the initial anodic reaction can be trapped inside cavities and between pillars, which serves as a mask to prevent local etching, and leads to the formation of patterned vertically aligned nanowire array. A simple model is presented to demonstrate that such bubble entrapment is due to the significant adhesion energy barrier, which is a function of pillar/cavity geometry, contact angle, and nanowire length to be etched. The bubble entrapment can be efficiently removed when extra energy is introduced by sonication to overcome this energy barrier, resulting in nanowire growth in all exposed surfaces. This bubble-regulated MACE process on microstructured surfaces can be used to fabricate nanowire arrays with desired morphologies. PMID:26411775

  4. Reactions of etched, single crystal (111)B-oriented InP to produce functionalized surfaces with low electrical defect densities

    SciTech Connect

    Sturzenegger, M.; Prokopuk, N.; Kenyon, C.N.; Royea, W.J.; Lewis, N.S.

    1999-12-09

    Synthetic routes have been developed that allow attachment of a variety of functional groups to etched, single-crystal InP surfaces. Benzyl halides, alkyl halides, silyl halides, and esters reacted readily with InP to yield covalently attached overlayers on the semiconductor surface. High-resolution X-ray photoelectron spectroscopy (XPS) revealed that the functionalization chemistry was consistent with the reactivity of surficial hydroxyl groups. Analysis of the XP spectra of the (111)B-oriented (P-rich) face in ultrahigh vacuum revealed signals ascribable to a monolayer of oxidized P atoms on the etched (111)B InP surface. The lack of reactivity of the (111)A-oriented (In-rich) face with these same functionalization reagents is therefore attributed to the difference in the nucleophilicity and acidity of the In and P oxides that are present on the (111)A and (111)B faces, respectively. The coverage of benzylic groups obtained through functionalization of (111)B-oriented InP with benzyl halides was estimated to be 4 x 10{sup 14} cm{sup 2}. This coverage implies that the functionalization can only proceed at alternate surface P atom sites in this system, which is expected from molecular packing considerations of these particular functional groups. Photoluminescence decay measurements were performed to investigate the electrical properties of the etched and modified InP surfaces, and these data indicated that the surface recombination velocity of the functionalized InP surface was {approx}10{sup 2} cm s{sup {minus}1}. This low surface recombination velocity implies that <1 electrically active defect is present for every 10{sup 5} atoms on the modified InP surface, indicating that high electrical quality can be maintained while introducing a variety of chemical functionalities onto the (111)B surface of InP.

  5. Chemical etching of deformation sub-structures in quartz

    NASA Astrophysics Data System (ADS)

    Wegner, M. W.; Christie, J. M.

    1983-02-01

    Chemical etching of dislocations has been studied in natural and synthetic quartz single crystals, in deformed synthetic quartz and in naturally and experimentally deformed quartzites. The ability of different etchants to produce polished or preferentially etched surfaces on quartz is described. Dislocation etching was achieved on all crystal planes examined by using a saturated solution of ammonium bifluoride as the etchant. Appropriate etching times were determined for etching quartzites for grain size, subgrain boundaries, deformation lamellae, dislocations and twins. Growth and polished surfaces of synthetic single crystal quartz were similarly etched and dislocation etch pits, characteristic of various orientations were found. The use of ammonium bifluoride proved to be expecially advantageous for the basal plane, producing a polished surface with etch pits, suitable for dislocation etch pit counting. “Double” etch pits have been found on Dauphiné twin boundaries on the basal plane and the first order prism, using this etchant. Slip lines and deformation bands were suitably etched on deformed synthetic crystal surfaces for identification of the slip planes. Other acidic etchants have been explored and their application to the study of deformation structures in quartz crystals is discussed.

  6. Surface Characterization and Osteoconductivity Evaluation of Micro/Nano Surface Formed on Titanium Using Anodic Oxidation Combined with H2O2 Etching and Hydrothermal Treatment.

    PubMed

    Park, Eun-Jin; Song, Yo-Han; Hwang, Moon-Jin; Song, Ho-Jun; Park, Yeong-Joon

    2015-08-01

    In this study, surface characteristics and osteoconductivity were investigated for the micro/nanostructured oxide layers fabricated on titanium using anodic oxidation (ANO), chemical etching (Et), and hydrothermal treatment (HT). Commercially pure titanium (CP-Ti) disks were anodic-oxidized using DC-type power supply in 1 M phosphoric acid electrolyte (P-ANO group). These specimens were further chemically etched using 30% H2O2 solution at 60 °C for 10 min (P-ANO-Et group). The P-ANO-Et-HT group was fabricated by hydrothermally treating the P-ANO-Et specimens in phosphorus-containing alkaline solution at 190 °C for 8 hrs. The P-ANO group showed a porous surface that was evenly covered with micro- and sub-micro pores. The size of these pores was decreased in the P-ANO-Et group. The P-ANO-Et-HT group showed a porous surface that was covered with nano-sized crystallites. Anatase TiO2 structure was observed in P-ANO-Et-HT group. The results of XPS demonstrated that the P-ANO-Et-HT group had a well-crystallized TiC2 structure, while the P-ANO and P-ANO-Et groups had an amorphous and phosphate-containing structure. Hydrophilicity of the P-ANO-Et-HT group was the highest. After MG63 osteoblast-like cells were cultured on the specimens for 3 hrs, SEM images of the cells cultured on P-ANO-Et-HT group specimens showed low initial adhesion. However, the osteoconductivity of these specimens increased more rapidly compared to that of the micro-structured surfaces. These results could be applied to fabricate titanium implants with an optimum micro/nano-surface for enhancing their osteoconductivity.

  7. Comparative Evaluation of Tensile – Bond Strength of An Orthodontic Adhesive with and without Fluoride Application, After Acid Etching -An Invitro Study

    PubMed Central

    Yugandhar, G; Ramana, I Venkata; Srinivas, K; Yadav, S. Sarjeev Singh

    2015-01-01

    Background Fixed appliances hinder the effective control of plaque accumulation and white spot lesions may develop under the ill fitting bands or adjacent to the stainless steel brackets during orthodontic treatment particularly the etching process. Aims and Objectives Comparative study of tensile bond strength of an orthodontic adhesive with and without fluoride application after acid etching to know the effect of fluoride on bond strength. Materials and Methods This study is carried out on 90 non carious human premolar teeth, and divided in 6 groups with each group of 15 specimens. In those Groups I and IV were control group acid etch treatment, Group II and V is 1.23% APF gel (acid etch plus APF gel treatment,) and group III and VI is 8% SnF2 (acid etch plus SnF2 treatment). Samples of Group I, II and III bond strength were tested after 24 h and groups IV, V and VI after one month on microtechtensometer machine. The scanning electron microscope (SEM) investigation was carried out for the 2 specimens for the control group after acid etch and 4 specimens after acid etch with fluoride application for fluoride groups. Results Control and SnF2 treated groups was found to be nearly similar to the control group whereas APF treated group showed less focal holes than the other 2 groups. Conclusion Fluoride application after acid etching without having an adverse effect on bond strength but we can prevent the white spot lesions and caries. PMID:26023648

  8. Surface chemistry of InP ridge structures etched in Cl{sub 2}-based plasma analyzed with angular XPS

    SciTech Connect

    Bouchoule, Sophie Cambril, Edmond; Guilet, Stephane; Chanson, Romain; Pageau, Arnaud; Rhallabi, Ahmed; Cardinaud, Christophe

    2015-09-15

    Two x-ray photoelectron spectroscopy configurations are proposed to analyze the surface chemistry of micron-scale InP ridge structures etched in chlorine-based inductively coupled plasma (ICP). Either a classical or a grazing configuration allows to retrieve information about the surface chemistry of the bottom surface and sidewalls of the etched features. The procedure is used to study the stoichiometry of the etched surface as a function of ridge aspect ratio for Cl{sub 2}/Ar and Cl{sub 2}/H{sub 2} plasma chemistries. The results show that the bottom surface and the etched sidewalls are P-rich, and indicate that the P-enrichment mechanism is rather chemically driven. Results also evidence that adding H{sub 2} to Cl{sub 2} does not necessarily leads to a more balanced surface stoichiometry. This is in contrast with recent experimental results obtained with the HBr ICP chemistry for which fairly stoichiometric surfaces have been obtained.

  9. Plasma treatment of dentin surfaces for improving self-etching adhesive/dentin interface bonding

    PubMed Central

    Dong, Xiaoqing; Li, Hao; Chen, Meng; Wang, Yong; Yu, Qingsong

    2015-01-01

    This study is to evaluate plasma treatment effects on dentin surfaces for improving self-etching adhesive and dentin interface bonding. Extracted unerupted human third molars were used after crown removal to expose dentin. One half of each dentin surface was treated with atmospheric non-thermal argon plasmas, while another half was untreated and used as the same tooth control. Self-etching adhesive and universal resin composite was applied to the dentin surfaces as directed. After restoration, the adhesive-dentin bonding strength was evaluated by micro-tensile bonding strength (μTBS) test. Bonding strength data was analyzed using histograms and Welch’s t-test based on unequal variances. μTBS test results showed that, with plasma treatment, the average μTBS value increased to 69.7±11.5 MPa as compared with the 57.1±17.5 MPa obtained from the untreated controls. After 2 months immersion of the restored teeth in 37 °C phosphate buffered saline (PBS), the adhesive-dentin bonding strengths of the plasma-treated specimens slightly decreased from 69.7±11.5 MPa to 63.9±14.4 MPa, while the strengths of the untreated specimens reduced from 57.1±17.5 MPa to 48.9±14.6 MPa. Water contact angle measurement and scanning electron microscopy (SEM) examination verified that plasma treatment followed by water rewetting could partially open dentin tubules, which could enhance adhesive penetration to form thicker hybrid layer and longer resin tags and consequently improve the adhesive/dentin interface quality. PMID:26273561

  10. The stress relaxation characteristics of composite matrices etched to produce nanoscale surface features.

    PubMed

    Mirani, Rahul D; Pratt, Jonathan; Iyer, Pooja; Madihally, Sundararajan V

    2009-02-01

    Many synthetic and xenogenic natural matrices have been explored in tissue regeneration, however, they lack either mechanical strength or cell colonization characteristics found in natural tissue. Moreover natural matrices such as small intestinal submucosa (SIS) lack sample to sample homogeneity, leading to unpredictable clinical outcomes. This work explored a novel fabrication technique by blending together the useful characteristics of synthetic and natural polymers to form a composite structure by using a NaOH etching process that produces nanoscale surface features. The composite scaffold was formed by sandwiching a thin layer of PLGA between porous layers of gelatin-chitosan. The etching process increased the surface roughness of PLGA membrane, allowing easy spreading of the hydrophilic gelatin-chitosan solution on its hydrophobic surface and reducing the scaffold thickness by nearly 50% than otherwise. The viscoelastic properties of the scaffold, an area of mechanical analysis which remains largely unexplored in tissue regeneration was assessed. Stress relaxation experiments of the "ramp and hold" type performed at variable ranges of temperature (25 degrees C and 37 degrees C), loading rates (3.125% s(-1) and 12.5% s(-1)) and relaxation times (60 s, 100 s and 200 s) found stress relaxation to be sensitive to temperature and the loading rate but less dependent on the relaxation time. Stress relaxation behavior of the composite matrix was compared with SIS structures at 25 degrees C (hydrated), 3.125% s(-1) loading rate and 100 s relaxation time which showed that the synthetic matrix was found to be strain softening as compared to the strain hardening behavior exhibited by SIS. Popularly used quasi-linear viscoelastic (QLV) model to describe biomechanics of soft tissues was utilized. The QLV model predicted the loading behavior with an average error of 3%. The parameters of the QLV model predicted using nonlinear regression analysis appear to be in concurrence

  11. Reactive ion etching-assisted surface-enhanced Raman scattering measurements on the single nanoparticle level

    SciTech Connect

    Wang, Si-Yi; Jiang, Xiang-Xu; Wei, Xin-Pan; Lee, Shuit-Tong E-mail: yaohe@suda.edu.cn; He, Yao E-mail: yaohe@suda.edu.cn; Xu, Ting-Ting

    2014-06-16

    Single-nanoparticle surface-enhanced Raman scattering (SERS) measurement is of essential importance for both fundamental research and practical applications. In this work, we develop a class of single-particle SERS approaches, i.e., reactive ion etching (RIE)-assisted SERS measurements correlated with scanning electron microscopy (SEM) strategy (RIE/SERS/SEM), enabling precise and high-resolution identification of single gold nanoparticle (AuNP) in facile and reliable manners. By using AuNP-coated silicon wafer and quartz glass slide as models, we further employ the developed RIE/SERS/SEM method for interrogating the relationship between SERS substrates and enhancement factor (EF) on the single particle level. Together with theoretical calculation using an established finite-difference-time-domain (FDTD) method, we demonstrate silicon wafer as superior SERS substrates, facilitating improvement of EF values.

  12. A study on the fabrication of superhydrophobic iron surfaces by chemical etching and galvanic replacement methods and their anti-icing properties

    NASA Astrophysics Data System (ADS)

    Li, Kunquan; Zeng, Xingrong; Li, Hongqiang; Lai, Xuejun

    2015-08-01

    Hierarchical structures on iron surfaces were constructed by means of chemical etching by hydrochloric acid (HCl) solution or the galvanic replacement by silver nitrate (AgNO3) solution. The superhydrophobic iron surfaces were successfully prepared by subsequent hydrophobic modification with stearic acid. The superhydrophobic iron surfaces were characterized by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM), energy dispersive X-ray spectroscopy (EDS) and water contact angle (WCA). The effects of reactive concentration and time on the microstructure and the wetting behavior were investigated. In addition, the anti-icing properties of the superhydrophobic iron surfaces were also studied. The FTIR study showed that the stearic acid was chemically bonded onto the iron surface. With the HCl concentration increase from 4 mol/L to 8 mol/L, the iron surface became rougher with a WCA ranging from 127° to 152°. The AgNO3 concentration had little effect on the wetting behavior, but a high AgNO3 concentration caused Ag particle aggregates to transform from flower-like formations into dendritic crystals, owing to the preferential growth direction of the Ag particles. Compared with the etching method, the galvanic replacement method on the iron surface more favorably created roughness required for achieving superhydrophobicity. The superhydrophobic iron surface showed excellent anti-icing properties in comparison with the untreated iron. The icing time of water droplets on the superhydrophobic surface was delayed to 500 s, which was longer than that of 295 s for untreated iron. Meanwhile, the superhydrophobic iron surface maintained superhydrophobicity after 10 icing and de-icing cycles in cold conditions.

  13. Er:YAG laser radiation etching of enamel

    NASA Astrophysics Data System (ADS)

    Dostalova, Tatjana; Jelinkova, Helena; Krejsa, Otakar; Hamal, Karel; Kubelka, Jiri; Prochazka, Stanislav

    1996-12-01

    This study compares the effects of acid treatment and Er:YAG laser radiation on the enamel. The permanent human molars were used. Oval cavities in the buccal surface were prepared and the edges of cavities were irradiated by Er:YAG radiation. The energy of laser was 105 mJ and repetition rate 1 Hz. The radiation was focused by CaF2 lens and the sample was placed in the focus. Ten samples were etched by 35 percent phosphoric acid during 60 s. Than cavities were filled with composite resin following manufacturers directions. By laser etching the structure enamel in section was rougher. The optimal connection between the enamel and composite resin was achieved in 75 percent by acid etching and in 79.2 percent by Er:YAG laser etching. Er:YAG laser etching could be alternative method for etching of enamel.

  14. Chemical and structural changes of quartz surfaces due to structuring by laser-induced backside wet etching.

    PubMed

    Kopitkovas, G; Deckert, V; Lippert, T; Raimondi, F; Schneider, C W; Wokaun, A

    2008-06-14

    Various physical and chemical processes which are involved in laser-induced backside wet etching are investigated. The surface of quartz etched by the laser-induced backside wet etching using a XeCl excimer laser at various fluences is analyzed by Raman microscopy, X-ray photoelectron spectroscopy and fiber-tip attenuated total-reflection Fourier-transform infrared spectroscopy. The investigations reveal the formation of a high amount of amorphous carbon deposits at low laser fluences, which strongly adhere to the quartz surface. Combining X-ray photoelectron spectroscopy and Fourier-transform infrared spectroscopy reveals that the quartz is also chemically and structurally modified due to a loss of oxygen and by a change of the quartz polymorph at intermediate and high laser fluences. These modification and their differences for different fluences are explained by the etching mechanisms itself, i.e. different magnitudes of temperature and pressure jumps. The results show clearly which conditions for etching must be applied to machine high-quality structures, e.g. micro-optical elements in quartz.

  15. Early bone response to sandblasted, dual acid-etched and H2O2/HCl treated titanium implants: an experimental study in the rabbit.

    PubMed

    He, F M; Yang, G L; Li, Y N; Wang, X X; Zhao, S F

    2009-06-01

    The aim of this study was to evaluate the influence of a roughened H(2)O(2)/HCl heat-treated titanium surface on peri-implant bone formation at an early stage in vivo. 24 Ti(6)Al(4)V alloy implants were used; half were treated by sandblasted and dual acid-etched treatments (control group), while the others were treated by sandblasted, dual acid-etched and H(2)O(2)/HCl heat treatments (test group). The morphology and roughness were analyzed by field emission SEM and atomic force microscopy. The implants were inserted into the femora of 12 adult white rabbits. After 2 and 4 weeks, femora block specimens were prepared for histological and histomorphometric analysis. SEM micrographs showed that multilevel and different sized pits were formed on both surfaces. New bone formation was observed on both implant surfaces. Test implants demonstrated a greater mean percentage of bone-implant contact as compared with controls at 2 (46.84 vs. 41.81, p=0.000) and 4 weeks (49.43 vs. 44.87, p=0.006) of healing. It is concluded that the H(2)O(2)/HCl heat-treated rough titanium surface promoted enhanced bone apposition during the early stages of new bone formation around the implant. PMID:19406618

  16. A new reactive atom plasma technology (RAPT) for precision machining: the etching of ULE optical surfaces

    NASA Astrophysics Data System (ADS)

    Fanara, Carlo; Shore, Paul; Nicholls, John R.; Lyford, Nicholas; Sommer, Phil; Fiske, Peter

    2006-06-01

    The next generation of 30-100 metre diameter extremely large telescopes (ELTs) requires large numbers of hexagonal primary mirror segments. As part of the Basic Technology programme run jointly by UCL and Cranfield University, a reactive atomic plasma technology (RAP(tm)) emerged from the US Lawrence Livermore National Laboratory (LLNL), is employed for the finishing of these surfaces. Results are presented on this novel etching technology. The Inductively Coupled Plasma (ICP) operated at atmospheric pressure using argon, activates the chemical species injected through its centre and promotes the fluorine-based chemical reactions at the surface. Process assessment trials on Ultra Low Expansion (ULE(tm)) plates, previously ground at high material removal rates, have been conducted. The quality of the surfaces produced on these samples using the RAP process are discussed. Substantial volumetric material removal rates of up to 0.446(21) mm 3/s at the highest process speed (1,200 mm/min) were found to be possible without pre-heating the substrate. The influences of power transfer, process speed and gas concentration on the removal rates have been determined. The suitability of the RAP process for revealing and removing sub-surface damage induced by high removal rate grinding is discussed. The results on SiC samples are reported elsewhere in this conference.

  17. Vascular stents with submicrometer-scale surface patterning realized via titanium deep reactive ion etching

    NASA Astrophysics Data System (ADS)

    Gott, Shannon C.; Jabola, Benjamin A.; Rao, Masaru P.

    2015-08-01

    Herein, we report progress towards realization of vascular stents that will eventually provide opportunity for evaluating cellular response to rationally-designed, submicrometer-scale surface patterning in physiologically-relevant contexts, i.e. those that provide exposure to the complex multicellular milieu, flow-induced shear, and tissue-device interactions present in vivo. Specifically, using our novel titanium deep reactive ion etching technique (Ti DRIE), we discuss recent advances that have enabled: (a) fabrication of precisely-defined, grating-based surface patterns on planar Ti foils with minimum feature sizes as small as 0.15 μm (b) creation of cylindrical stents from micromachined planar Ti foils; and (c) integration of these processes to produce the first submicrometer-scale surface-patterned Ti stents that are compatible with conventional balloon catheter deployment techniques. We also discuss results from elastoplastic finite element simulations and preliminary mechanical testing of these devices to assess their mechanical performance. These efforts represent key steps towards our long-term goal of developing a new paradigm in stenting, where rationally-designed surface patterning provides a physical means for facilitating healing, and thus, improving outcomes in vascular intervention applications.

  18. Inactivation of Matrix-bound MMPs by Cross-linking Agents in Acid Etched Dentin

    PubMed Central

    Scheffel, Débora Lopes Salles; Hebling, Josimeri; Scheffel, Régis Henke; Agee, Kelly A.; Turco, Gianluca; de Souza Costa, Carlos Alberto; Pashley, David H.

    2014-01-01

    Objectives Published TEM analysis of in vivo resin-dentin bonds shows that in 44 months almost 70% of collagen fibrils from the hybrid layer disappear. Matrix metalloproteinases (MMPs) play an important role in that process and are thought to be the main factor responsible for the solubitization of dentin collagen. Therefore, this study aimed to evaluate the inactivation of matrix-bound MMPs by carbodiimide (EDC) or proanthocyanidin (PA) both cross-linking agents, or the MMP-inhibitor, chlorhexidine (CHX), on acid-etched dentin using a simplified MMP assay method. Methods Dentin beams (1×1×6mm) were obtained from mid-coronal dentin of sound third molars and randomly divided into 6 groups (G) according to the dentin treatment: G1: Deionized water (control), G2: 0.1M EDC, G3: 0.5M EDC, G4: 0.5M EDC+35% HEMA, G5: 5% Proanthocyanidin (PA) and G6: 2% CHX. The beams were etched for 15s with 37% phosphoric acid, rinsed and then immersed for 60s in one of the treatment solutions. The total MMP activity of dentin was analyzed for 1 h by colorimetric assay (Sensolyte). Data were submitted to Wilcoxon non-parametric test and Mann-Whitney tests (p>0.05). Results All experimental cross-linking solutions significantly reduced MMP activity compared to control, except 0.1M EDC (53.6% ±16.1). No difference was observed between cross-linking agents and 2% CHX 0.5M EDC + 35% HEMA (92.3% ±8.0) was similar to 0.5M EDC (89.1% ±6.4), 5% PA (100.8% ±10.9) and 2% CHX (83.4% ±10.9). Conclusion Dentin treatment with cross-linking agents is effective to significantly reduce MMP activity. Mixing 0.5M EDC and 35% HEMA did not influence EDC inhibitor potential. PMID:23786610

  19. Relationship between gas-phase chemistries and surface processes in fluorocarbon etch plasmas: A process rate model

    SciTech Connect

    Sant, S. P.; Nelson, C. T.; Overzet, L. J.; Goeckner, M. J.

    2009-07-15

    In a typical plasma tool, both etch and deposition occur simultaneously. Extensive experimental measurements are used to help develop a general model of etch and deposition processes. This model employs reaction probabilities, or surface averaged cross sections, to link the measurable surface processes, etch and deposition, to the flux of various species to the surfaces. Because the cross sections are quantum mechanical in nature, this surface rate model should be applicable to many low temperature plasma processing systems. Further, the parameters that might be important in reaction cross sections are known from quantum mechanics, e.g., species, energy, temperature, and impact angle. Such parameters might vary from system to system, causing the wide processing variability observed in plasma tools. Finally the model is used to compare measurements of ion flux, ion energy, and fluorocarbon radical flux to the measured process rates. It is found that the model appears to be consistent with calculations of gain/loss rates for the various radicals present in the discharge as well as measured etch and deposition rates.

  20. Ultrastructure of cel organelles by scanning electron microscopy of thick sections surface-etched by an oxygen plasma.

    PubMed

    Humphreys, W J; Henk, W G

    1979-07-01

    Kidney tissue double fixed in glutaraldehyde and osmium tetroxide and embedded in epoxy resin by standard techniques used for transmission electron microscopy was cut into section 1 micron or more thick and surface-etched by an oxygen plasma. Etching caused ash residues (possibly composed partly or organo-metallic complexes) of membranes and other etch resistant cell components to emerge as recognizable structures projecting upward from the surrounding embedment which was combusted and removed as volatile products. using the secondary electron mode for image formation, structural features of cells which could be imaged with clarity with the scanning electron microscopy included: profiles of peripheral and in-folded plasma membranes, the nuclear envelope and profiles of cut mitochondrial matrix granules, cristae and the outer limiting membranes. Resolution was better than that obtainable from most other methods of specimen preparation currently being used in scanning electron microscopy for viewing the internal structures of cells or organelles in bulk samples of tissue.

  1. Optical investigation of the intergrowth structure and accessibility of Brønsted acid sites in etched SSZ-13 zeolite crystals by confocal fluorescence microscopy.

    PubMed

    Sommer, Linn; Svelle, Stian; Lillerud, Karl Petter; Stöcker, Michael; Weckhuysen, Bert M; Olsbye, Unni

    2010-11-01

    Template decomposition followed by confocal fluorescence microscopy reveals a tetragonal-pyramidal intergrowth of subunits in micrometer-sized nearly cubic SSZ-13 zeolite crystals. In order to accentuate intergrowth boundaries and defect-rich areas within the individual large zeolite crystals, a treatment with an etching NaOH solution is applied. The defective areas are visualized by monitoring the spatial distribution of fluorescent tracer molecules within the individual SSZ-13 crystals by confocal fluorescence microscopy. These fluorescent tracer molecules are formed at the inner and outer crystal surfaces by utilizing the catalytic activity of the zeolite in the oligomerization reaction of styrene derivatives. This approach reveals various types of etching patterns that are an indication for the defectiveness of the studied crystals. We can show that specially one type of crystals, denoted as core-shell type, is highly accessible to the styrene molecules after etching. Despite the large crystal dimensions, the whole core-shell type SSZ-13 crystal is utilized for catalytic reaction. Furthermore, the confocal fluorescence microscopy measurements indicate a nonuniform distribution of the catalytically important Brønsted acid sites underlining the importance of space-resolved measurements. PMID:20496927

  2. Evolutionary determination of kinetic Monte Carlo rates for the simulation of evolving surfaces in anisotropic etching of silicon

    NASA Astrophysics Data System (ADS)

    Xing, Y.; Gosálvez, M. A.; Sato, K.; Tian, M.; Yi, H.

    2012-08-01

    This study explores for the first time the possibility of using an evolutionary algorithm (EA) for the determination of atomistic rates for use in kinetic Monte Carlo (KMC) simulations of anisotropic etching of silicon for the manufacture of microelectromechanical systems (MEMS). Traditionally, KMC rates are determined based on (i) computationally expensive density functional theory (DFT) calculations or, when possible, (ii) a combination of physical insight and a labor-intensive, manual procedure where, e.g., experimental and simulated surface morphologies are visually matched for a collection of surface orientations. Compared to these approaches, the evolutionary KMC method proposed in this study provides a more flexible, autonomous procedure to describe correctly a wide variety of etching conditions. We focus on the use of a functional representation of the atomistic rates, referred to as the removal probability function (RPF). This simplifies the EA search space to just a few parameters and reduces the number of required experimental data points to just a few etch rates. By proposing two alternative RPFs with four and six parameters, respectively, we show that the ability to explain the orientation dependence of the etch rate for a wide variety of etchants increases with the number of parameters and conclude that the six-parameter RPF provides sufficiently good simulations for a wide range of etching conditions, including KOH, KOH+IPA, TMAH and TMAH+Triton at different concentrations and temperatures. By uncovering the relationships between the parameters and the concentration of the etchant, it is possible to extend the simulations to nonmeasured etching conditions. Although the use of an RPF effectively restricts the search to a subspace of the atomistic rates, the present results suggest that physically meaningful KMC rates can probably be determined in the near future by direct comparison of macroscopic experiments and simulations through the use of

  3. AFM probes fabricated with masked maskless combined anisotropic etching and p+ surface doping

    NASA Astrophysics Data System (ADS)

    Han, Jianqiang; Li, Xinxin; Bao, Haifei; Zuo, Guomin; Wang, Yuelin; Feng, Fei; Yu, Zhenyin; Ge, Xiaohong

    2006-02-01

    The paper presents a newly developed high-yield micro-fabrication technology for single-crystalline silicon atomic force microscope (AFM) probes. Both the tips and the cantilevers are simultaneously formed by a masked-maskless combined anisotropic etching process. Compared to a conventional tip-to-cantilever sequential fabrication scheme, this tip-and-cantilever simultaneous formation can effectively increase fabrication yield by avoiding the tips damaged during the following processed photolithographic steps for defining the cantilevers. By heavy boron doping at the surface, the conductive AFM probe provides an electrical path to the electric ground of the AFM that helps to eliminate the electrostatic accumulation of charges and, therefore, eliminate undesirable electrostatic forces between the probes and the samples. A fabrication yield as high as 90% has been obtained for the AFM probes for 4 inch wafers. The tips after oxidation-sharpening treatment generally have a radius of 10-30 nm. The cantilever spring constant can be well controlled in the range of 0.025-40 N m-1. High-quality sample scanning results with the formed AFM probes are obtained with a slightly better resolution than that from commercial probes without surface conductive treatment.

  4. Femtosecond laser structuring of silver-containing glass: Silver redistribution, selective etching, and surface topology engineering

    SciTech Connect

    Desmoulin, Jean-Charles; Petit, Yannick; Cardinal, Thierry; Canioni, Lionel; Dussauze, Marc; Lahaye, Michel; Gonzalez, Hernando Magallanes; Brasselet, Etienne

    2015-12-07

    Femtosecond direct laser writing in silver-containing phosphate glasses allows for the three-dimensional (3D) implementation of complex photonic structures. Sample translation along or perpendicular to the direction of the beam propagation has been performed, which led to the permanent formation of fluorescent structures, either corresponding to a tubular shape or to two parallel planes at the vicinity of the interaction voxel, respectively. These optical features are related to significant modifications of the local material chemistry. Indeed, silver depletion areas with a diameter below 200 nm were evidenced at the center of the photo-produced structures while photo-produced luminescence properties are attributed to the formation of silver clusters around the multiphoton interaction voxel. The laser-triggered oxidation-reduction processes and the associated photo-induced silver redistribution are proposed to be at the origin of the observed original 3D luminescent structures. Thanks to such material structuring, surface engineering has been also demonstrated. Selective surface chemical etching of the glass has been obtained subsequently to laser writing at the location of the photo-produced structures, revealing features with nanometric depth profiles and radial dimensions strongly related to the spatial distributions of the silver clusters.

  5. Femtosecond laser structuring of silver-containing glass: Silver redistribution, selective etching, and surface topology engineering

    NASA Astrophysics Data System (ADS)

    Desmoulin, Jean-Charles; Petit, Yannick; Canioni, Lionel; Dussauze, Marc; Lahaye, Michel; Gonzalez, Hernando Magallanes; Brasselet, Etienne; Cardinal, Thierry

    2015-12-01

    Femtosecond direct laser writing in silver-containing phosphate glasses allows for the three-dimensional (3D) implementation of complex photonic structures. Sample translation along or perpendicular to the direction of the beam propagation has been performed, which led to the permanent formation of fluorescent structures, either corresponding to a tubular shape or to two parallel planes at the vicinity of the interaction voxel, respectively. These optical features are related to significant modifications of the local material chemistry. Indeed, silver depletion areas with a diameter below 200 nm were evidenced at the center of the photo-produced structures while photo-produced luminescence properties are attributed to the formation of silver clusters around the multiphoton interaction voxel. The laser-triggered oxidation-reduction processes and the associated photo-induced silver redistribution are proposed to be at the origin of the observed original 3D luminescent structures. Thanks to such material structuring, surface engineering has been also demonstrated. Selective surface chemical etching of the glass has been obtained subsequently to laser writing at the location of the photo-produced structures, revealing features with nanometric depth profiles and radial dimensions strongly related to the spatial distributions of the silver clusters.

  6. Raman-scattering and optical studies of argon-etched GaAs surfaces

    SciTech Connect

    Feng, G.F.; Zallen, R. ); Epp, J.M.; Dillard, J.G. )

    1991-04-15

    We have studied the structual damage in low-energy argon-ion-bombarded (ion-etched) GaAs using Raman scattering and ultraviolet reflectivity. When combined with post-bombardment sequential chemical etching, the Raman results reveal a graded depth profile of the damage layer, with a nearly linear damage dropoff with depth. The total damage-layer thickness is about 600 A for high-fluence bombardment with 3.89-keV Ar{sup +} ions. The spectral effects produced by argon etching are very different from those produced by high-energy ion implantation. The longitudinal-optic Raman line seen for argon-etched GaAs is not shifted and broadened as in ion-implanted GaAs. More striking are the results of the reflectivity measurements. For argon-etched GaAs, the electronic interband peaks are both broadened and strongly red shifted relative to the crystal peaks; for ion-implanted GaAs, only the broadening occurs. Distinct nanocrystals, which account for the effects seen in ion-implanted GaAs, are evidently absent in argon-etched GaAs. Instead, the damage layer caused by argon etching appears to be characterized by a very high density of point defects, which previous work suggests may be arsenic vacancies.

  7. Three dimensional microscopic surface profiles of membranes reconstructed from freeze etching electrol micrographs.

    PubMed

    Krbecek, R; Gebhardt, C; Gruler, H; Sackmann, E

    1979-06-13

    A method of three-dimensional reconstruction of the surface profile of artificial and natural membranes from freeze quenched electron micrographs is presented. The method is based on the analysis of the variation in thickness of platinum layers, deposited under an oblique angle. In essence, it is reminiscent of the method of Eratosthenes to measure the earth's radius. The thickness of etch-like protrusions of membranes could be determined to an accuracy of about 3 A. True distances on curved surfaces rather than projections of distances are obtained. The method has been applied to both model membranes and biological membranes. The essential results are: 1. Detailed information on the symmetry and the molecular structure of the crystalline phases of dimyristoyl phosphatidylcholine was obtained. The microscopic surface profile of the ripple structure observed between the pretransition and the main transition was analysed. In accordance with a previous model we found that the ripple structure is caused by the spontaneous curvature of the monolayers. The surface profiles of the ripple structure and of the low temperature biaxial phase could be clearly distinguished. 2. The sizes and shapes of lipid domains formed by both thermically and charge-induced lateral phase separation were determined. This showed that the visual inspection of electron micrographs may lead to a considerable underestimation of the domain size. Conclusions may be drawn concerning the different phases formed upon lateral phase separation. 3. As a biological example, yeast cell membranes were studied. The method allows one to distinguish between different membrane-bound proteins by measuring the width-to-height ratio of the particles. The deformation of the lipid layer in the environment of the proteins may be determined. This deformation contains information about lipid-mediated long-range interactions between membrane proteins. PMID:378255

  8. Three dimensional microscopic surface profiles of membranes reconstructed from freeze etching electrol micrographs.

    PubMed

    Krbecek, R; Gebhardt, C; Gruler, H; Sackmann, E

    1979-06-13

    A method of three-dimensional reconstruction of the surface profile of artificial and natural membranes from freeze quenched electron micrographs is presented. The method is based on the analysis of the variation in thickness of platinum layers, deposited under an oblique angle. In essence, it is reminiscent of the method of Eratosthenes to measure the earth's radius. The thickness of etch-like protrusions of membranes could be determined to an accuracy of about 3 A. True distances on curved surfaces rather than projections of distances are obtained. The method has been applied to both model membranes and biological membranes. The essential results are: 1. Detailed information on the symmetry and the molecular structure of the crystalline phases of dimyristoyl phosphatidylcholine was obtained. The microscopic surface profile of the ripple structure observed between the pretransition and the main transition was analysed. In accordance with a previous model we found that the ripple structure is caused by the spontaneous curvature of the monolayers. The surface profiles of the ripple structure and of the low temperature biaxial phase could be clearly distinguished. 2. The sizes and shapes of lipid domains formed by both thermically and charge-induced lateral phase separation were determined. This showed that the visual inspection of electron micrographs may lead to a considerable underestimation of the domain size. Conclusions may be drawn concerning the different phases formed upon lateral phase separation. 3. As a biological example, yeast cell membranes were studied. The method allows one to distinguish between different membrane-bound proteins by measuring the width-to-height ratio of the particles. The deformation of the lipid layer in the environment of the proteins may be determined. This deformation contains information about lipid-mediated long-range interactions between membrane proteins.

  9. Roughening of Polyimide Surface for Inkjet Printing by Plasma Etching Using the Polyimide Masked with Polystyrene Nanosphere Array.

    PubMed

    Mun, Mu Kyeom; Park, Jin Woo; Ahn, Jin Ho; Kim, Ki Kang; Yeom, Geun Young

    2015-10-01

    Two key conditions are required for the application of fine-line inkjet printing onto a flexible substrate such as polyimide (PI): linewidth control during the inkjetting process, and a strong adhesion of the polyimide surface to the ink after the ink solidifies. In this study, the properties of a polyimide surface that was roughened through etching in a He/SF6 plasma, using a polystyrene nanosphere array as the etch mask, were investigated. The near-atmospheric-pressure plasma system of the He/SF6 plasma that was used exhibits two notable properties in this context: similar to an atmospheric-pressure plasma system, it can easily handle inline substrate processing; and, similar to a vacuum system, it can control the process gas environment. Through the use of plasma etching, the polyimide surface masked the 120-nm-diameter polystyrene nanospheres, thereby forming a roughened nanoscale polyimide surface. This surface exhibited not only a greater hydrophobicity--with a contact angle of about 150° for water and about 30° for silver ink, indicating better silver linewidth control during the silver inkjetting process--but also a stronger adhesion to the silver ink sprayed onto it when compared with the flat polyimide surface. PMID:26726483

  10. Impact of etching on the surface leakage generation in mesa-type InGaAs/InAlAs avalanche photodetectors.

    PubMed

    Ma, Yingjie; Zhang, Yonggang; Gu, Yi; Chen, Xingyou; Shi, Yanhui; Ji, Wanyan; Xi, Suping; Du, Ben; Li, Xiaoliang; Tang, Hengjing; Li, Yongfu; Fang, Jiaxiong

    2016-04-01

    Effects of mesa etching and geometry on InGaAs/InAlAs avalanche photodiodes (APDs) were investigated by using both wet and inductively coupled plasma (ICP) etching with different mesa shapes as well as etchants. It was found that the mesa geometry had no evident impact on APDs' characteristics regardless of the etching techniques applied. Besides, ICP-etched APDs showed faster punch-through, suppressed premature surface breakdown and lower dark current behaviors compared to the wet-etched devices. Substantially suppressed surface leakage was also observed for ICP-etched devices, showing 1 and 3 orders of magnitude better at room temperature and 77 K respectively, and over 1 order of magnitude higher surface resistivity up to 4×107 Ω cm, in comparison to the wet-etched APDs. Introduction of extra hydrogen and Ar plasma in ICP etching led to detrimental effects to APDs' performance by enhancing the tunneling or recombination at surfaces. Those experimental results were clearly interpreted based on the surface state theories. PMID:27137065

  11. Determination of the Dissolution Slowness Surface by Study of Etched Shapes: II. Comparison of 2D Experimental and Theoretical Etching Shapes

    NASA Astrophysics Data System (ADS)

    Leblois, T.; Tellier, C. R.; Messaoudi, T.

    1997-03-01

    The anisotropic etching behavior of quartz crystal in concentrated ammonium bifluoride solution is studied and analyzed in the framework of a tensorial model. This model allows to simulate bi- or three-dimensional etching shapes from the equation for the representative surface of the dissolution slowness. In this paper, we present experimental results such as surface profile and initially circular cross-sectional profiles of differently singly- or doubly-rotated cuts. The polar diagrams of the dissolution slowness vector in several planes are deduced from experimental data. The comparison between predicted surface and cross-sectional profiles and experimental results is detailed and shows a good agreement. In particular, several examples give evidence that the final etched shapes are correlated to the extrema of the dissolution slowness. However, in several cases, experimental shapes cannot be simply correlated to the presence of extrema. Simulation gives effectively evidence for an important role played by more progressive changes in the curvature of the slowness surface. Consequently, analysis of data merits to be treated carefully. Nous nous proposons d'étudier et d'analyser à l'aide du modèle tensoriel de la dissolution l'attaque chimique anisotrope du cristal de quartz dans une solution concentrée de bifluorure d'ammonium. Ce modèle permet de simuler des formes usinées à deux ou trois dimensions à partir de l'équation de la surface représentative de la lenteur de dissolution du cristal de quartz. Dans cet article, nous présentons des résultats expérimentaux concernant des profils de surface et des sections initialement cylindriques de coupes à simple et double rotation. Les diagrammes polaires du vecteur lenteur de dissolution dans différents plans sont déduits de données expérimentales. La comparaison entre les profils de surface et de section théoriques et les résultats expérimentaux est détaillée et montre un bon accord. En

  12. Combined Effect of Mechanical Grooving and Stain-Etched Surface on Optical and Electrical Properties of Crystalline Silicon Substrates

    NASA Astrophysics Data System (ADS)

    Zarroug, Ahmed; Derbali, Lotfi; Ouertani, Rachid; Dimassi, Wissem; Ezzaouia, Hatem

    2014-05-01

    This paper investigates the combined effect of mechanical grooving and porous silicon (PS) on the front surface reflectance and the electronic properties of crystalline silicon substrates. Mechanical surface texturization leads to reduce the cell reflectance, enhance the light trapping and augment the carrier collection probability. PS was introduced as an efficient antireflective coating (ARC) onto the front surface of crystalline silicon solar cell. Micro-periodic V-shaped grooves were made by means of a micro-groove machining process prior to junction formation. Subsequently, wafers were subjected to an isotropic potassium hydroxide (KOH) etching so that the V-shape would be turned to a U-shape. We found that the successive treatment of silicon surfaces with stain-etching, grooving then alkaline etching enhances the absorption of the textured surface, and decreases the reflectance from 35% to 7% in the 300-1200 nm wavelength range. We obtained a significant increase in the overall light path that generates the building up of the light trapping inside the substrate. We found an improvement in the illuminated I-V characteristics and an increase in the minority carrier lifetime τeff. Such a simple method was adopted to effectively reinforce the overall device performance of crystalline silicon-based solar cells.

  13. Surface characteristics of dentin experimentally exposed to hydrofluoric acid.

    PubMed

    Pioch, Thomas; Jakob, Heiko; García-Godoy, Franklin; Götz, Hermann; Dörfer, Christof E; Staehle, Hans J

    2003-08-01

    The purpose of this study was to test the effect of hydrofluoric acid (HF) on the surface characteristics of dentin in vitro. Dentin was exposed in 50 human molars and divided into five groups according to different etching schedules: (i) no etching, (ii) 15 s HF, (iii) 15 s H3PO4, (iv) 15 s HF and 15 s H3PO4, (v) 15 s H3PO4 and 15 s HF. Teeth were examined under a scanning electron microscope equipped with energy-dispersive X-ray (EDX) or two layers of fluorescence-labeled primer followed by the composite were applied, and the teeth were sectioned and examined using confocal laser scanning microscopy (CLSM). With scanning electron microscopy, no openings of dentinal tubules were found in groups (i), (ii), and (iv). In group (v) only a few tubules were opened and in group (iii) the smear layer was completely removed and tubules appeared open. The EDX analysis revealed that fluoride was incorporated into the dentin surface when HF was used. With CLSM, distinct hybrid layers could be detected only in group (iii). In group (v) the hybrid layer appeared less established compared with group (iii). No dentin hybridization was found in groups (i), (ii), and (iv). It is concluded that HF has the ability to close the openings of dentin tubules which were opened due to etching by phosphoric acid and cannot dissolve the smear layer.

  14. Dependence of selectivity on plasma conditions in selective etching in submicrometer pitch grating on InP surface by CH{sub 4}/H{sub 2} reactive ion etching

    SciTech Connect

    Yamamoto, Norio

    2011-04-01

    We studied selective etching and polymer deposition in submicrometer pitch gratings on the surface of InP using reactive ion etching with methane and hydrogen and investigated the plasma condition dependence of the selectivity. Using a mask structure consisting of regions with and without a thick layer on a grating-patterned thin layer, we achieved selective etching in submicrometer pitch gratings. In experiments conducted on the same surface at the same time, the InP is selectively etched in the window of the grating in the region with the thick layer, but it is not etched, and polymer is deposited, in the window of the grating in the region without the thick layer. We found that the selectivity depends on the plasma conditions, such as the hydrogen flow rate, pressure, and plasma power in reactive ion etching. This dependence might result from the variation in the ionic atoms of hydrogen or hydrocarbon/hydrogen, which are attracted to the charged mask and supplied to the window of the grating.

  15. Effect of Fluoride on the Morphology of Calcium Phosphate Crystals Grown on Acid-Etched Human Enamel

    PubMed Central

    Fan, Y.; Sun, Z.; Moradian-Oldak, J.

    2009-01-01

    The aim of this study was to examine the effect of fluoride ion concentration on the morphology of calcium phosphate crystals grown on acid-etched enamel as a model for tooth enamel erosion. Samples were immersed in calcification solution for 16 h and changes in crystal morphology were monitored by field emission scanning electron microscopy. Without fluoride, plate-like octacalcium phosphate crystals (20 nm thick, 2–10 μm wide) were formed. With 1–10 mg/l fluoride, arrays of denser needle-like nanocrystals (20–30 nm wide, >500 nm in length) were formed. We conclude that there is a minimal fluoride concentration (1 mg/l) that dramatically affects the morphology of calcium phosphate crystals grown on etched enamel in vitro. PMID:19321991

  16. Sensing of human plasma fibrinogen on polished, chemically etched and carbon treated titanium surfaces by diffractive optical element based sensor.

    PubMed

    Silvennoinen, Raimo; Vetterl, Vladimir; Hason, Stanislav; Tuononen, Heikki; Silvennoinen, Martti; Myller, Kari; Cvrcek, Ladislav; Vanek, Jiri; Prachar, Patrik

    2008-07-01

    Adsorption of human plasma fibrinogen (HPF) on 6 differently treated titanium samples (polished, polished and etched, and 4 titanium carbide coatings samples produced by using plasma-enhanced chemical vapour deposition (PECVD) method) is investigated by using diffractive optical element (DOE) sensor. Permittivity (susceptibility) change and fluctuation in optical roughness (R(opt)) of treated titanium surface in the presence of background electrolyte without and with HPF molecules are sensed by using DOE sensor and optical ellipsometry. Correlation between transmitted light and thickness of molecule layer was found. The findings allow to sense temporal organization and severity of adsorption of nano-scale HPF molecules on polished, on polished and etched, and on titanium carbide surface.

  17. Redeposition of etch products on sidewalls during SiO2 etching in a fluorocarbon plasma. I. Effect of particle emission from the bottom surface in a CF4 plasma

    NASA Astrophysics Data System (ADS)

    Min, Jae-Ho; Hwang, Sung-Wook; Lee, Gyeo-Re; Moon, Sang Heup

    2002-09-01

    The effect of etch-product redeposition on sidewall properties during the etching of step-shaped SiO2 patterns in a CF4 plasma was examined using a Faraday cage located in a transformer coupled plasma etcher. Sidewall properties were observed for two cases: with and without particles emitted from the bottom surface in normal contact with the sidewall. Particles sputtered from the bottom surface were redeposited on the sidewall, which contributes to the formation of a passivation layer on the surface of the latter. The passivation layer consisted of silicon oxide, SixOy, and fluorocarbon, CxFy, the latter comprising the major species. Ar plasma experiments confirmed that CxFy or a fluorocarbon polymer must be present on the sidewall in order for the SixOy species to be deposited on the surface. The redeposited particles, which were largely F-deficient fluorocarbon species, as evidenced by x-ray photoelectron spectroscopy analyses, functioned as precursors for fluorocarbon polymerization, resulting in a rough sidewall surface. The chemical etch rates of SiO2 were retarded by the redeposition of particles, which eventually formed a thick layer, eventually covering the bulk SiO2. Auger electron spectroscopy analyses of the sidewall surface affected by the emission from the bottom suggest that the surface consists of three distinct layers: a surface-carbon layer, a redeposition-etch combined layer, and bulk SiO2. copyright 2002 American Vacuum Society.

  18. Investigation of the neutral-solution etch process for refractive SOE antireflective surfaces

    SciTech Connect

    Maish, A.B.

    1991-01-01

    Antireflection of optically clear glass used in photovoltaic concentrator refractive secondary optical elements (SOE's) was investigated using the neutral-solution etch process developed by Schott Glass. Test coupons and SOE's made from barium zinc glass, which does not solarize under ultraviolet exposure, were successfully etched at the center point process variable conditions of 87{degrees}C and 24 hours. Reflectance of the plano-plano dropped from 7.7% to 0.8%, with a corresponding increase in transmission from 91.7% to 98.5%. The etching process uses non-hydrofluoric, relatively non-toxic chemicals in a low-cost process well suited for use by photovoltaic system manufacturers during production. 10 refs., 4 figs., 1 tab.

  19. Etch Effects on Surface loss in High Quality Aluminum on Silicon Superconducting Coplanar Resonators

    NASA Astrophysics Data System (ADS)

    Dunsworth, Andrew; Megrant, Anthony; Barends, Rami; Chen, Yu; Hoi, Iochun; Jeffrey, Evan; Mutus, Josh; Roushan, Pedram; Campbell, Brooks; Chen, Zijun; Chiaro, Ben; Kelly, Julian; Neill, Charles; O'Malley, Peter; Quintana, Chris; Sank, Daniel; Vainsencher, Amit; Wenner, Jim; White, Ted; Cleland, Andrew; Martinis, John; Martinis Group Team

    2014-03-01

    Superconducting coplanar resonators are a powerful tool for studying capacitive loss from two level states (TLS's) in superconducting qubits. We have found evidence that standard processing of aluminum on sapphire superconducting devices leaves behind ~2 nm organic residues which can contribute to loss at the Q >106 level that we are presently working with. Removing these residues is possible on a silicon substrate as it allows various sidewall etchings and profilings via chemical and physical etches. I will present recent Q factor measurements of aluminum on silicon resonators that were defined through a variety of etching conditions. This research was funded by the Office of the Director of National Intelligence (ODNI), Intelligence Advanced Research Projects Activity (IARPA), through the Army Research Office grant JMAR-05.

  20. Investigation of surface damage precursor evolutions and laser-induced damage threshold improvement mechanism during Ion beam etching of fused silica.

    PubMed

    Shi, Feng; Zhong, Yaoyu; Dai, Yifan; Peng, Xiaoqiang; Xu, Mingjin; Sui, Tingting

    2016-09-01

    Surface damage precursor evolution has great influence on laser-induced damage threshold improvement of fused silica surface during Ion beam etching. In this work, a series of ion sputtering experiment are carried out to obtain the evolutions of damage precursors (dot-form microstructures, Polishing-Induced Contamination, Hertz scratches, and roughness). Based on ion sputtering theory, surface damage precursor evolutions are analyzed. The results show that the dot-form microstructures will appear during ion beam etching. But as the ion beam etching depth goes up, the dot-form microstructures can be mitigated. And ion-beam etching can broaden and passivate the Hertz scratches without increasing roughness value. A super-smooth surface (0.238nm RMS) can be obtained finally. The relative content of Fe and Ce impurities both significantly reduce after ion beam etching. The laser-induced damage threshold of fused silica is improved by 34% after ion beam etching for 800nm. Research results can be a reference on using ion beam etching process technology to improve laser-induced damage threshold of fused silica optics. PMID:27607688

  1. The Effect of Laser-Etched Surface Design on Soft Tissue Healing of Two Different Implant Abutment Systems: An Experimental Study in Dogs.

    PubMed

    Neiva, Rodrigo; Tovar, Nick; Jimbo, Ryo; Gil, Luiz F; Goldberg, Paula; Barbosa, Joao Pm; Lilin, Thomas; Coelho, Paulo G

    2016-01-01

    This study describes the early soft tissue morphology around two different implant systems that received either smooth or laser-etched abutments in a beagle dog model. Implants were placed in the healed mandibular molar region of eight beagle dogs and allowed to heal for 7 weeks. When the most apical aspect of the junctional epithelium (JE) was above or within the upper half of the laser-etched region, fibers were oriented perpendicular to the abutment surface. In contrast, JE positioned within the lower half of the laser-etched region or within or below the implant-abutment gap level presented fibers oriented parallel to the abutment surface. PMID:27560671

  2. Effect of Cl{sub 2}- and HBr-based inductively coupled plasma etching on InP surface composition analyzed using in situ x-ray photoelectron spectroscopy

    SciTech Connect

    Bouchoule, S.; Vallier, L.; Patriarche, G.; Chevolleau, T.; Cardinaud, C.

    2012-05-15

    A Cl{sub 2}-HBr-O{sub 2}/Ar inductively coupled plasma (ICP) etching process has been adapted for the processing of InP-based heterostructures in a 300-mm diameter CMOS etching tool. Smooth and anisotropic InP etching is obtained at moderate etch rate ({approx}600 nm/min). Ex situ x-ray energy dispersive analysis of the etched sidewalls shows that the etching anisotropy is obtained through a SiO{sub x} passivation mechanism. The stoichiometry of the etched surface is analyzed in situ using angle-resolved x-ray photoelectron spectroscopy. It is observed that Cl{sub 2}-based ICP etching results in a significantly P-rich surface. The phosphorous layer identified on the top surface is estimated to be {approx}1-1.3-nm thick. On the other hand InP etching in HBr/Ar plasma results in a more stoichiometric surface. In contrast to the etched sidewalls, the etched surface is free from oxides with negligible traces of silicon. Exposure to ambient air of the samples submitted to Cl{sub 2}-based chemistry results in the complete oxidation of the P-rich top layer. It is concluded that a post-etch treatment or a pure HBr plasma step may be necessary after Cl{sub 2}-based ICP etching for the recovery of the InP material.

  3. Amino acid conjugated self assembling molecules for enhancing surface wettability of fiber laser treated titanium surfaces

    NASA Astrophysics Data System (ADS)

    Akkan, Cagri K.; Hür, Deniz; Uzun, Lokman; Garipcan, Bora

    2016-03-01

    Surface wetting properties of implants are one of the most critical parameter, which determine the interaction of proteins and cells with the implant surface. In this regards, acid etching and sand blasting are the mostly used methods at surface modification of Titanium (Ti) for enhanced surface wettability. Besides, these kinds of modifications may cause a conflict whether the surface wettability is influenced by the process related surface contaminations or by the surface roughness. In contrast, lasers might be an option for the alteration of surface wetting properties via supporting micro and/or nano surface topographies while preventing surface chemical contaminations. In this work, we focused on two steps of surface processing approaches of Ti surface: physical and chemical modifications. Herein, we hierarchically structured Ti surfaces by using microsecond modulated pulsed fiber laser. Subsequently, laser structured and non-structured Ti surfaces were further modified with novel histidine and leucine Amino Acid conjugated Self-Assembled Molecules (His1-SAMs2 and Leu3-SAMs) to alter the surface wettability by introducing biologically hydrophilic and hydrophobic groups. Modification of Ti surfaces with His-SAMs and Leu-SAMs ended up with stable wetting properties when compared to non-modified surfaces after 7 days which may enhances the cell-surface interaction.

  4. Electrolytic etch for preventing electrical shorts in solar cells on polymer surfaces

    DOEpatents

    Weber, Michael F.

    1991-10-08

    A method for preventing shorts and shunts in solar cells having in order, an insulating substrate, a conductive metal layer on the substrate, an amorphous silicon layer and a transparent conductive layer. The method includes anodic etching of exposed portions of the metal layer after deposition of the amorphous silicon and prior to depositing the transparent conductive layer.

  5. Plasma chemical modification of track-etched membrane surface layer for improvement of their biomedical properties

    NASA Astrophysics Data System (ADS)

    Kravets, Liubov I.; Ryazantseva, Tatyana V.

    2013-12-01

    The morphological and clinical studies of poly(ethylene terephthalate) track-etched membrane modified by plasma of non-polymerizing gases as drainage materials for antiglaucomatous operations were performed. It was demonstrated their compatibility with eye tissues. Moreover, it was shown that a new drainage has a good lasting hypotensive effect and can be used as operation for refractory glaucoma surgery.

  6. Etching patterns of Co-Cr alloys for bonded cast restorations.

    PubMed

    Ekstrand, K; Ruyter, I E

    1987-09-01

    Resin-bonded bridges may replace missing teeth and act as splints in periodontal treatment. The objective of this study was to investigate the etch pattern after electrolytic etching of selected Co-Cr alloys in hydrochloric acid and to assess the changes in alloy composition after different etching times. The alloys investigated were Vitallium, Wironit, Wironium, Nobilium Hard, and Niranium NN. Alloy specimens were electrolytically etched in a hydrochloric acid solution for 1, 2, 5, and 10 min. The etched specimens were examined in a light microscope and a scanning electron microscope (SEM). Different etching patterns were revealed in the various alloys. Microprobe analyses after the etching of Vitallium showed generally that Co was released and that Cr content increased at the surface. PMID:3305640

  7. Multiple-mask chemical etching

    NASA Technical Reports Server (NTRS)

    Cannon, D. L.

    1969-01-01

    Multiple masking techniques use lateral etching to reduce the total area of the high etch-rate oxide exposed to the chemical etchant. One method uses a short-term etch to remove the top layer from the silicon oxide surface, another acts before the top layer is grown.

  8. Modification of surface energy, dry etching, and organic film removal using atmospheric-pressure pulsed-corona plasma

    SciTech Connect

    Yamamoto, Toshiaki; Newsome, J.R.; Ensor, D.S.

    1995-05-01

    A laboratory-scale atmospheric-pressure plasma reactor, using a nanosecond pulsed corona, was constructed to demonstrate potential applications ranging from modification of surface energy to removal of surface organic films. For surface modification studies, three different substrates were selected to evaluate the surface energies: bare aluminum, polyurethane, and silicon coated with photoresist. The critical surface energy for all materials studied significantly increased after the plasma treatment. The effects of gas composition and plasma treatment time were also investigated. Photoresist, ethylene glycol, and Micro surfactant were used as test organic films. The etching rate of a photoresist coating on silicon was 9 nm/min. Organic film removal using atmospheric pressure plasma technology was shown to be feasible.

  9. Surface layer erosion of natural caries lesions with phosphoric and hydrochloric acid gels in preparation for resin infiltration.

    PubMed

    Meyer-Lueckel, H; Paris, S; Kielbassa, A M

    2007-01-01

    The infiltration of proximal enamel lesions with low-viscosity light curing resins could be a viable approach to stop lesion progression. However, penetration of sealant might be hampered by the comparatively highly mineralized surface layers of natural lesions. Therefore, the aim of this study was to compare the efficacy of three different etching gels in removing the surface layer in various etching times. Extracted human molars and premolars showing proximal white spot lesions were cut across the demineralized areas. Ninety-six lesions expected from visual examination to be confined to the outer enamel (C1) were selected. The cut surface and half of each lesion were varnished, thus serving as control. Subsequently, the lesions were etched with either phosphoric (37%) or hydrochloric (5 or 15%) acid gel for 30-120 s (n = 8/group). Specimens were examined using confocal microscopy and transversal microradiography. Surface layer reduction was significantly increased in lesions etched with 15% HCl gel for 90 and 120 s compared to those etched with H(3)PO(4) gel for 30-120 s (p < 0.05). No significant differences regarding the depths of erosion in the lesions compared to sound enamel could be observed (p > 0.05). An effective reduction in the surface layer of natural enamel caries can be achieved by etching with 15% hydrochloric acid gel for 90-120 s.

  10. Surface rippling by oblique ion incidence during plasma etching of silicon: Experimental demonstration using sheath control plates

    NASA Astrophysics Data System (ADS)

    Nakazaki, Nobuya; Matsumoto, Haruka; Eriguchi, Koji; Ono, Kouichi

    2015-09-01

    In the microfabrication of 3D transistors (e.g. Fin-FET), the sidewall roughness, such as LER and LWR caused by off-normal or oblique ion incidence during plasma etching, is a critical issue to be resolved, which in turn requires a better understanding of the effects of ion incidence angle θi on surface roughening. This paper presents surface roughening and rippling by oblique ion incidence during inductively coupled plasma etching of Si in Cl2, using the experimental setup as in our previous study. The oblique ion incidence was achieved by sheath control plates, which were placed on and electrically connected to the wafer stage. The plates had slits to vary the sheath structure thereon and to extract ions from plasma to samples on the bottom and/or side of the slits. The results indicated that at θi ~ 40° or oblique incidence; ripple structures were formed on surfaces perpendicularly to the direction of ion incidence, on the other hand, at θi ~ 80° or grazing incidence, small ripples or slit like grooves were formed on surfaces parallel to the direction of ion incidence, as predicted in our previous numerical investigations.

  11. Plasma surface interactions in nanoscale processing: Preservation of low-k integrity and high-k gate-stack etching with silicon selectivity

    NASA Astrophysics Data System (ADS)

    Shoeb, Juline

    Plasma-surface interactions are very important in the fabrication of the nm-sized features of integrated circuits. Plasma processes are employed to produce high-resolution patterns in many of the thin layers of silicon integrated circuits and to remove masking layers while maintaining high selectivity. Integrated plasma processes consisting of sequential steps such as etch, clean and surface modification, are used in semiconductor industries. The surface in contact with the process plasma is exposed to the fluxes of neutrals, ions, molecules, electrons and photons. Modeling of surface reaction mechanisms requires the determination of the characterizations of fluxes (e.g. composition, magnitude, energy and angle) and development of the reaction mechanisms of the processes such as adsorption, reflection, bond breaking and etch product evolution, while reproducing the experimental results. When modeling the reaction mechanism for an entirely new material, the experimental data is often fragmentary. Therefore, fundamental principles such as bond energies and volatility of the etch products must be considered to develop the mechanism. In this thesis, results from a computational investigation of porous low-k SiCOH etching in fluorocarbon plasmas, damage during cleaning of CFx polymer etch residue in Ar/O2 and He/H2 plasmas, NH3 plasma pore sealing and low-k degradation due to water uptake, will be discussed. The plasma etching of HfO2 gate-stacks is also computationally investigated with an emphasis on the selectivity between HfO2 and Si.

  12. Enhanced Etching, Surface Damage Recovery, and Submicron Patterning of Hybrid Perovskites using a Chemically Gas-Assisted Focused-Ion Beam for Subwavelength Grating Photonic Applications.

    PubMed

    Alias, Mohd S; Yang, Yang; Ng, Tien K; Dursun, Ibrahim; Shi, Dong; Saidaminov, Makhsud I; Priante, Davide; Bakr, Osman M; Ooi, Boon S

    2016-01-01

    The high optical gain and absorption of organic-inorganic hybrid perovskites have attracted attention for photonic device applications. However, owing to the sensitivity of organic moieties to solvents and temperature, device processing is challenging, particularly for patterning. Here, we report the direct patterning of perovskites using chemically gas-assisted focused-ion beam (GAFIB) etching with XeF2 and I2 precursors. We demonstrate etching enhancement in addition to controllability and marginal surface damage compared to focused-ion beam (FIB) etching without precursors. Utilizing the GAFIB etching, we fabricated a uniform and periodic submicron perovskite subwavelength grating (SWG) absorber with broadband absorption and nanoscale precision. Our results demonstrate the use of FIB as a submicron patterning tool and a means of providing surface treatment (after FIB patterning to minimize optical loss) for perovskite photonic nanostructures. The SWG absorber can be patterned on perovskite solar cells to enhance the device efficiency through increasing light trapping and absorption. PMID:26688008

  13. Enhanced Etching, Surface Damage Recovery, and Submicron Patterning of Hybrid Perovskites using a Chemically Gas-Assisted Focused-Ion Beam for Subwavelength Grating Photonic Applications.

    PubMed

    Alias, Mohd S; Yang, Yang; Ng, Tien K; Dursun, Ibrahim; Shi, Dong; Saidaminov, Makhsud I; Priante, Davide; Bakr, Osman M; Ooi, Boon S

    2016-01-01

    The high optical gain and absorption of organic-inorganic hybrid perovskites have attracted attention for photonic device applications. However, owing to the sensitivity of organic moieties to solvents and temperature, device processing is challenging, particularly for patterning. Here, we report the direct patterning of perovskites using chemically gas-assisted focused-ion beam (GAFIB) etching with XeF2 and I2 precursors. We demonstrate etching enhancement in addition to controllability and marginal surface damage compared to focused-ion beam (FIB) etching without precursors. Utilizing the GAFIB etching, we fabricated a uniform and periodic submicron perovskite subwavelength grating (SWG) absorber with broadband absorption and nanoscale precision. Our results demonstrate the use of FIB as a submicron patterning tool and a means of providing surface treatment (after FIB patterning to minimize optical loss) for perovskite photonic nanostructures. The SWG absorber can be patterned on perovskite solar cells to enhance the device efficiency through increasing light trapping and absorption.

  14. Realization of atomically flat steps and terraces like surface of SrTiO3 (001) single crystal by hot water etching and high temperature annealing

    NASA Astrophysics Data System (ADS)

    Prakash, Bhanu; Chakraverty, S.

    2015-07-01

    We have successfully prepared atomically flat single-terminated SrTiO3(001) surface using a mild and reproducible etching technique combined with high temperature annealing. To achieve single terminated surface, deionised water at 60 °C was used to selectively etch SrO composites from the substrate surface. A clear step-and-terrace like surface morphology is observed by subsequent air annealing at 1000 °C. Atomic Force Microscopy suggests the step height (~0.4 nm) corresponding to the lattice parameter of SrTiO3, which confirms the formation of single-terminated surface. This chemical-free mild etching technique might be useful to prepare single-terminated surface, especially for the perovskites containing reactive elements.

  15. Formation of a pn junction on an anisotropically etched GaAs surface using metalorganic chemical vapor deposition

    NASA Technical Reports Server (NTRS)

    Leon, R. P.; Bailey, S. G.; Mazaris, G. A.; Williams, W. D.

    1986-01-01

    A continuous p-type GaAs epilayer has been deposited on an n-type sawtooth GaAs surface using MOCVD. A wet chemical etching process was used to expose the intersecting (111)Ga and (-1 -1 1)Ga planes with 6-micron periodicity. Charge-collection microscopy was used to verify the presence of the pn junction thus formed and to measure its depth. The ultimate goal of this work is to fabricate a V-groove GaAs cell with improved absorptivity, high short-circuit current, and tolerance to particle radiation.

  16. Etching of enamel for direct bonding with a thulium fiber laser

    NASA Astrophysics Data System (ADS)

    Kabaş Sarp, Ayşe S.; Gülsoy, Murat

    2011-03-01

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

  17. Plasma etched surface scanning inspection recipe creation based on bidirectional reflectance distribution function and polystyrene latex spheres

    NASA Astrophysics Data System (ADS)

    Saldana, Tiffany; McGarvey, Steve; Ayres, Steve

    2014-04-01

    The continual increasing demands upon Plasma Etching systems to self-clean and continue Plasma Etching with minimal downtime allows for the examination of SiCN, SiO2 and SiN defectivity based upon Surface Scanning Inspection Systems (SSIS) wafer scan results. Historically all Surface Scanning Inspection System wafer scanning recipes have been based upon Polystyrene Spheres wafer deposition for each film stack and the subsequent creation of light scattering sizing response curves. This paper explores the feasibility of the elimination of Polystyrene Latex Sphere (PSL) and/or process particle deposition on both filmed and bare Silicon wafers prior to Surface Scanning Inspection System recipe creation. The study will explore the theoretical maximal Surface Scanning Inspection System sensitivity based on PSL recipe creation in conjunction with the maximal sensitivity derived from Bidirectional Reflectance Distribution Function (BRDF) maximal sensitivity modeling recipe creation. The surface roughness (Root Mean Square) of plasma etched wafers varies dependent upon the process film stack. Decrease of the root mean square value of the wafer sample surface equates to higher surface scanning inspection system sensitivity. Maximal sensitivity SSIS scan results from bare and filmed wafers inspected with recipes created based upon Polystyrene/Particle Deposition and recipes created based upon BRDF modeling will be overlaid against each other to determine maximal sensitivity and capture rate for each type of recipe that was created with differing recipe creation modes. A statistically valid sample of defects from each Surface Scanning Inspection system recipe creation mode and each bare wafer/filmed substrate will be reviewed post SSIS System processing on a Defect Review Scanning Electron Microscope (DRSEM). Native defects, Polystyrene Latex Spheres will be collected from each statistically valid defect bin category/size. The data collected from the DRSEM will be utilized to

  18. Topography-based surface tension gradients to facilitate water droplet movement on laser-etched copper substrates.

    PubMed

    Sommers, A D; Brest, T J; Eid, K F

    2013-09-24

    This paper describes a method for creating a topography-based gradient on a metallic surface to help mitigate problems associated with condensate retention. The gradient was designed to promote water droplet migration toward a specified region on the surface which would serve as the primary conduit for drainage using only the roughness of the surface to facilitate the movement of the droplets. In this work, parallel microchannels having a fixed land width but variable spacing were etched into copper substrates to create a surface tension gradient along the surface of the copper. The surfaces were fabricated using a 355 nm Nd:YVO4 laser system and then characterized using spray testing techniques and water droplet (2-10 μL) injection via microsyringe. The distances that individual droplets traveled on the gradient surface were also measured using a goniometer and CCD camera and were found to be between 0.5 and 1.5 mm for surfaces in a horizontal orientation. Droplet movement was spontaneous and did not require the use of chemical coatings. The theoretical design and construction of surface tension gradients were also explored in this work by calculating the minimum gradient needed for droplet movement on a horizontal surface using Wenzel's model of wetting. The results of this study suggest that microstructural patterning could be used to help reduce condensate retention on metallic fins such as those used in heat exchangers in heating, ventilation, air-conditioning, and refrigeration (HVAC&R) applications. PMID:23971937

  19. Topography-based surface tension gradients to facilitate water droplet movement on laser-etched copper substrates.

    PubMed

    Sommers, A D; Brest, T J; Eid, K F

    2013-09-24

    This paper describes a method for creating a topography-based gradient on a metallic surface to help mitigate problems associated with condensate retention. The gradient was designed to promote water droplet migration toward a specified region on the surface which would serve as the primary conduit for drainage using only the roughness of the surface to facilitate the movement of the droplets. In this work, parallel microchannels having a fixed land width but variable spacing were etched into copper substrates to create a surface tension gradient along the surface of the copper. The surfaces were fabricated using a 355 nm Nd:YVO4 laser system and then characterized using spray testing techniques and water droplet (2-10 μL) injection via microsyringe. The distances that individual droplets traveled on the gradient surface were also measured using a goniometer and CCD camera and were found to be between 0.5 and 1.5 mm for surfaces in a horizontal orientation. Droplet movement was spontaneous and did not require the use of chemical coatings. The theoretical design and construction of surface tension gradients were also explored in this work by calculating the minimum gradient needed for droplet movement on a horizontal surface using Wenzel's model of wetting. The results of this study suggest that microstructural patterning could be used to help reduce condensate retention on metallic fins such as those used in heat exchangers in heating, ventilation, air-conditioning, and refrigeration (HVAC&R) applications.

  20. Microtensile bond strength of a resin-based fissure sealant to Er,Cr:YSGG laser-etched primary enamel.

    PubMed

    Sungurtekin-Ekci, Elif; Oztas, Nurhan

    2016-05-01

    The aim of this study was to evaluate the effect of Er,Cr:YSGG laser pre-treatment alone, or associated with acid-etching, on the microtensile bond strength of a resin-based fissure sealant to primary enamel. Twenty-five human primary molars were randomly divided into five groups including (1) 35 % acid etching, (2) 2.5-W laser etching, (3) 3.5-W laser etching, (4) 2.5-W laser etching + acid etching, and (5) 3.5-W laser etching + acid etching. Er,Cr:YSGG laser was used at a wavelength of 2.780 nm and pulse duration of 140-200 μs with a repetition rate of 20 Hz. Following surface pre-treatment, the fissure sealant (ClinPro™, 3M Dental Products) was applied. Each tooth was sectioned and subjected to microtensile testing. Kruskal-Wallis test was used for statistical analysis. The level of significance was set at p < 0.05. The microtensile bond strength values of group 1 were significantly higher than those of group 2, while no statistically significant difference was detected between groups 1, 3, 4, and 5. It was concluded that 3.5-W laser etching produced results comparable to conventional acid etching technique, whereas 2.5-W laser etching was not able to yield adequate bonding performance.

  1. High electron mobility recovery in AlGaN/GaN 2DEG channels regrown on etched surfaces

    NASA Astrophysics Data System (ADS)

    Chan, Silvia H.; Keller, Stacia; Tahhan, Maher; Li, Haoran; Romanczyk, Brian; DenBaars, Steven P.; Mishra, Umesh K.

    2016-06-01

    This paper reports high two-dimensional electron gas mobility attained from the regrowth of the AlGaN gating layer on ex situ GaN surfaces. To repair etch-damaged GaN surfaces, various pretreatments were conducted via metalorganic chemical vapor deposition, followed by a regrown AlGaN/GaN mobility test structure to evaluate the extent of recovery. The developed treatment process that was shown to significantly improve the electron mobility consisted of a N2 + NH3 pre-anneal plus an insertion of a 4 nm or thicker GaN interlayer prior to deposition of the AlGaN gating layer. Using the optimized process, a high electron mobility transistor (HEMT) device was fabricated which exhibited a high mobility of 1450 cm2 V-1 s-1 (R sh = 574 ohm/sq) and low dispersion characteristics. The additional inclusion of an in situ Al2O3 dielectric into the regrowth process for MOS-HEMTs still preserved the transport properties near etch-impacted areas.

  2. Surface- and sidewall-damage of InP-based optoelectronic devices during reactive ion etching using CH{sub 4}/H{sub 2}

    SciTech Connect

    Boettner, T.; Hartnagel, H.L.; Kraeutle, H.; Kuphal, E.; Miethe, K.

    1996-12-31

    Optoelectronic devices demand structurization methods in the sub-{micro}m-range. Systematic investigations are performed on the effect of Reactive Ion Etching (RIE) using CH{sub 4}/H{sub 2} based gases on InP based semiconductors. From Rutherford Backscattering analysis a strong dependence of crystalline damage on process parameters is found leading to a damaged region of less than 3 nm for an optimized process. Capacitance Voltage profiling shows the effect of hydrogen channeling up to 0.5{micro}m deep into the semiconductor creating acceptor passivation which can be completely removed by annealing at low temperature. Using low temperature photoluminescence measurements on Multiquantumwell structures, it is shown that the RIE process does not affect photoluminescence properties of quantumwells remarkably until the covering barrier is etched down to few nm. From these measurements a damage model of the etched semiconductor surface is presented. Sidewall damage of RIE etched InGaAs/InP Mesa-PIN-diodes is characterized by analyzing surface leakage currents. Furthermore, effects of different post-etch treatments on leakage currents are shown. By an optimized CH{sub 4}/H{sub 2}/Ar-RIE process PIN-photodiodes are fabricated with dark current densities as low as 1.8*10{sup {minus}5}Acm{sup {minus}2} (bias voltage is {minus}5V) which are comparable to the best published wet etched Mesa-PIN-photodiodes.

  3. Sputtering yields and surface chemical modification of tin-doped indium oxide in hydrocarbon-based plasma etching

    SciTech Connect

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

    2015-11-15

    Sputtering yields and surface chemical compositions of tin-doped indium oxide (or indium tin oxide, ITO) by CH{sup +}, CH{sub 3}{sup +}, and inert-gas ion (He{sup +}, Ne{sup +}, and Ar{sup +}) incidence have been obtained experimentally with the use of a mass-selected ion beam system and in-situ x-ray photoelectron spectroscopy. It has been found that etching of ITO is chemically enhanced by energetic incidence of hydrocarbon (CH{sub x}{sup +}) ions. At high incident energy incidence, it appears that carbon of incident ions predominantly reduce indium (In) of ITO and the ITO sputtering yields by CH{sup +} and CH{sub 3}{sup +} ions are found to be essentially equal. At lower incident energy (less than 500 eV or so), however, a hydrogen effect on ITO reduction is more pronounced and the ITO surface is more reduced by CH{sub 3}{sup +} ions than CH{sup +} ions. Although the surface is covered more with metallic In by low-energy incident CH{sub 3}{sup +} ions than CH{sup +} ions and metallic In is in general less resistant against physical sputtering than its oxide, the ITO sputtering yield by incident CH{sub 3}{sup +} ions is found to be lower than that by incident CH{sup +} ions in this energy range. A postulation to account for the relation between the observed sputtering yield and reduction of the ITO surface is also presented. The results presented here offer a better understanding of elementary surface reactions observed in reactive ion etching processes of ITO by hydrocarbon plasmas.

  4. Evaluation of dentin bonding performance and acid-base resistance of the interface of two-step self-etching adhesive systems.

    PubMed

    IIda, Yasuhiro; Nikaido, Toru; Kitayama, Shuzo; Takagaki, Tomohiro; Inoue, Go; Ikeda, Masaomi; Foxton, Richard M; Tagami, Junji

    2009-07-01

    The purpose of this study was to evaluate dentin bond strengths and to observe the adhesive-dentin interface after acid-base challenge using fluoride-free and fluoride-releasing self-etching adhesive systems; Clearfil SE Bond (SE), FL-Bond (FL) and FL-Bond II(FL II). Fifteen dentin surfaces from human molars were ground and bonded with one of three adhesive systems. The microtensile bond strength (muTBS) test was performed at a crosshead speed of 1 mm/min. The interface of the bonded specimens after acid-base challenge were also examined by a SEM. The muTBS of SE were significantly higher than those of FL and FL II (p<0.05), however, there were no significant differences between FL and FL II (p>0.05). An acid-base resistant zone (ABRZ) was observed in all the groups, however, formation of the ABRZ was material dependent. Fluoride-release from the adhesive is a key factor to create thick ABRZ.

  5. Optimization of silver-assisted nano-pillar etching process in silicon

    NASA Astrophysics Data System (ADS)

    Azhari, Ayu Wazira; Sopian, Kamaruzzaman; Desa, Mohd Khairunaz Mat; Zaidi, Saleem H.

    2015-12-01

    In this study, a respond surface methodology (RSM) model is developed using three-level Box-Behnken experimental design (BBD) technique. This model is developed to investigate the influence of metal-assisted chemical etching (MACE) process variables on the nanopillars profiles created in single crystalline silicon (Si) substrate. Design-Expert® software (version 7.1) is employed in formulating the RSM model based on five critical process variables: (A) concentration of silver (Ag), (B) concentration of hydrofluoric acid (HF), (C) concentration of hydrogen peroxide (H2O2), (D) deposition time, and (E) etching time. This model is supported by data from 46 experimental configurations. Etched profiles as a function of lateral etching rate, vertical etching rate, height, size and separation between the Si trenches and etching uniformity are characterized using field emission scanning electron microscope (FE-SEM). A quadratic regression model is developed to correlate critical process variables and is validated using the analysis of variance (ANOVA) methodology. The model exhibits near-linear dependence of lateral and vertical etching rates on both the H2O2 concentration and etching time. The predicted model is in good agreement with the experimental data where R2 is equal to 0.80 and 0.67 for the etching rate and lateral etching respectively. The optimized result shows minimum lateral etching with the average pore size of about 69 nm while the maximum etching rate is estimated at around 360 nm/min. The model demonstrates that the etching process uniformity is not influenced by either the etchant concentration or the etching time. This lack of uniformity could be attributed to the surface condition of the wafer. Optimization of the process parameters show adequate accuracy of the model with acceptable percentage errors of 6%, 59%, 1.8%, 38% and 61% for determination of the height, separation, size, the pore size and the etching rate respectively.

  6. Efficient design of experiments for complex response surfaces with application to etching uniformity in a plasma reactor

    NASA Astrophysics Data System (ADS)

    Tatavalli Mittadar, Nirmal

    Plasma etching uniformity across silicon wafers is of paramount importance in the semiconductor industry. The complexity of plasma etching, coupled with lack of instrumentation to provide real-time process information (that could be used for feedback control), necessitate that optimal conditions for uniform etching must be designed into the reactor and process recipe. This is often done empirically using standard design of experiments which, however, are very costly and time consuming. The objective of this study was to develop a general purpose efficient design strategy that requires a minimum number of experiments, and can handle complex constraints in the presence of uncertainties. Traditionally, Response Surface Methodology (RSM) is used in these applications to design experiments to determine the optimal value of decision variables or inputs. We demonstrated that standard RSM, when applied to the problem of plasma etching uniformity, has the following drawbacks (1) inefficient search due to process nonlinearities, (2) lack of converge to the optimum, and, (3) inability to handle complex inequality constraints. We developed a four-phase Efficient Design Strategy (EDS) based on the DACE paradigm (Design and Analysis of Computer Experiments) and Bayesian search algorithms. The four phases of EDS are: (1) exploration of the design space by maximizing information, (2) exploration of the design space for feasible points by maximizing probability of constraint satisfaction, (3) optimization of the objective and (4) constrained local search. We also designed novel algorithms to switch between the different phases. The choice of model parameters for DACE predictors is usually determined by the Maximum Likelihood Estimation (MLE) method. Depending on the dataset, MLE could result in unrealistic predictors that show a peak-and-dip behavior. To solve this problem we developed techniques to detect the presence of peak-and-dip behavior and a new scheme based on Maximum a

  7. Surface etching, chemical modification and characterization of silicon nitride and silicon oxide—selective functionalization of Si3N4 and SiO2

    NASA Astrophysics Data System (ADS)

    Liu, Li-Hong; Michalak, David J.; Chopra, Tatiana P.; Pujari, Sidharam P.; Cabrera, Wilfredo; Dick, Don; Veyan, Jean-François; Hourani, Rami; Halls, Mathew D.; Zuilhof, Han; Chabal, Yves J.

    2016-03-01

    The ability to selectively chemically functionalize silicon nitride (Si3N4) or silicon dioxide (SiO2) surfaces after cleaning would open interesting technological applications. In order to achieve this goal, the chemical composition of surfaces needs to be carefully characterized so that target chemical reactions can proceed on only one surface at a time. While wet-chemically cleaned silicon dioxide surfaces have been shown to be terminated with surficial Si-OH sites, chemical composition of the HF-etched silicon nitride surfaces is more controversial. In this work, we removed the native oxide under various aqueous HF-etching conditions and studied the chemical nature of the resulting Si3N4 surfaces using infrared absorption spectroscopy (IRAS), x-ray photoelectron spectroscopy (XPS), low energy ion scattering (LEIS), and contact angle measurements. We find that HF-etched silicon nitride surfaces are terminated by surficial Si-F and Si-OH bonds, with slightly subsurface Si-OH, Si-O-Si, and Si-NH2 groups. The concentration of surficial Si-F sites is not dependent on HF concentration, but the distribution of oxygen and Si-NH2 displays a weak dependence. The Si-OH groups of the etched nitride surface are shown to react in a similar manner to the Si-OH sites on SiO2, and therefore no selectivity was found. Chemical selectivity was, however, demonstrated by first reacting the -NH2 groups on the etched nitride surface with aldehyde molecules, which do not react with the Si-OH sites on a SiO2 surface, and then using trichloro-organosilanes for selective reaction only on the SiO2 surface (no reactivity on the aldehyde-terminated Si3N4 surface).

  8. Impact of recess etching and surface treatments on ohmic contacts regrown by molecular-beam epitaxy for AlGaN/GaN high electron mobility transistors

    NASA Astrophysics Data System (ADS)

    Joglekar, S.; Azize, M.; Beeler, M.; Monroy, E.; Palacios, T.

    2016-07-01

    Ohmic contacts fabricated by regrowth of n+ GaN are favorable alternatives to metal-stack-based alloyed contacts in GaN-based high electron mobility transistors. In this paper, the influence of reactive ion dry etching prior to regrowth on the contact resistance in AlGaN/GaN devices is discussed. We demonstrate that the dry etch conditions modify the surface band bending, dangling bond density, and the sidewall depletion width, which influences the contact resistance of regrown contacts. The impact of chemical surface treatments performed prior to regrowth is also investigated. The sensitivity of the contact resistance to the surface treatments is found to depend upon the dangling bond density of the sidewall facets exposed after dry etching. A theoretical model has been developed in order to explain the observed trends.

  9. Vacuum Ultraviolet and Ultraviolet Radiation-Induced Effect of Hydrogenated Silicon Nitride Etching: Surface Reaction Enhancement and Damage Generation

    NASA Astrophysics Data System (ADS)

    Fukasawa, Masanaga; Miyawaki, Yudai; Kondo, Yusuke; Takeda, Keigo; Kondo, Hiroki; Ishikawa, Kenji; Sekine, Makoto; Matsugai, Hiroyasu; Honda, Takayoshi; Minami, Masaki; Uesawa, Fumikatsu; Hori, Masaru; Tatsumi, Tetsuya

    2012-02-01

    Photon-enhanced etching of SiNx:H films caused by the interaction between vacuum ultraviolet (VUV)/ultraviolet (UV) radiation and radicals in the fluorocarbon plasma was investigated by a technique with a novel sample setup of the pallet for plasma evaluation. The simultaneous injection of UV radiation and radicals causes a dramatic etch rate enhancement of SiNx:H films. Only UV radiation causes the film shrinkage of SiNx:H films owing to hydrogen desorption from the film. Capacitance-voltage characteristics of SiNx:H/Si substrates were studied before and after UV radiation. The interface trap density increased monotonically upon irradiating the UV photons with a wavelength of 248 nm. The estimated effective interface trap generation probability is 4.74 ×10-7 eV-1·photon-1. Therefore, the monitoring of the VUV/UV spectra during plasma processing and the understanding of its impact on the surface reaction, film damage and electrical performance of underlying devices are indispensable to fabricate advanced devices.

  10. 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.

    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.

  11. Orthodox etching of HVPE-grown GaN

    SciTech Connect

    Weyher, J.L.; Lazar, S.; Macht, L.; Liliental-Weber, Z.; Molnar,R.J.; Muller, S.; Nowak, G.; Grzegory, I.

    2006-08-10

    Orthodox etching of HVPE-grown GaN in molten eutectic of KOH + NaOH (E etch) and in hot sulfuric and phosphoric acids (HH etch) is discussed in detail. Three size grades of pits are formed by the preferential E etching at the outcrops of threading dislocations on the Ga-polar surface of GaN. Using transmission electron microscopy (TEM) as the calibration tool it is shown that the largest pits are formed on screw, intermediate on mixed and the smallest on edge dislocations. This sequence of size does not follow the sequence of the Burgers values (and thus the magnitude of the elastic energy) of corresponding dislocations. This discrepancy is explained taking into account the effect of decoration of dislocations, the degree of which is expected to be different depending on the lattice deformation around the dislocations, i.e. on the edge component of the Burgers vector. It is argued that the large scatter of optimal etching temperatures required for revealing all three types of dislocations in HVPE-grown samples from different sources also depends upon the energetic status of dislocations. The role of kinetics for reliability of etching in both etches is discussed and the way of optimization of the etching parameters is shown.

  12. Effect of cavity preparation method on microtensile bond strength of a self-etching primer vs phosphoric acid etchant to enamel.

    PubMed

    de Souza-Zaroni, Wanessa Christine; Delfino, Carina Sinclér; Ciccone-Nogueira, Juliane Cristina; Palma-Dibb, Regina Guenka; Corona, Silmara Aparecida Milori

    2007-10-01

    This study evaluated the effect of cavity preparation using air abrasion or carbide bur on bond strength to enamel treated with a self-etching primer (Tyrian SPE) or a phosphoric acid etchant. Twenty-four molars were divided into three groups: high-speed; standard handpiece (ST air abrasion) or supersonic handpiece (SP air abrasion) of the same air-abrasive system. The enamel surfaces were treated with one of the two etchants and the same adhesive agent One Step Plus, and then composite buildups were done with Filtek Z250. After 24 h at 37 degrees C, beams (0.8 mm2) were obtained and subjected to tensile stress in a universal testing machine (0.5 mm/min). The data were submitted to analysis of variance and Tukey's test (P < 0.05). For the conditioning agents, it was observed that the specimens conditioned with phosphoric acid presented superior results than the specimens that used Tyrian SPE. For the preparation techniques, it was verified that the SP air abrasion groups showed the highest bond strengths and carbide-bur groups presented the lowest bond strengths when the specimens were conditioned with Tyrian SPE. It can be concluded that the influence of the cavity preparation method was dependent on the conditioning system used, only when using carbide-bur preparation technique.

  13. Bond strengths of a self-etching adhesive to dentin surfaces treated with saliva, blood, and different hemostatic agents.

    PubMed

    Unlu, Nimet; Cebe, Fatma; Cebe, Mehmet Ata; Cetin, Ali Riza; Cobanoglu, Nevin

    2015-01-01

    The aim of this study was to evaluate the microtensile bond strengths of a self-etching adhesive to dentin surfaces after treatment with 4 different hemostatic agents in the presence of saliva and blood. After testing, no significant differences were found between the mean bond strength of Clearfil SE (CSE) Bond resin adhesive to normal dentin and those of CSE to dentin treated with the hemostatic agents ViscoStat Clear, Astringedent, or Astringedent X (P > 0.05). However, the mean bond strength of CSE Bond to dentin treated with Ankaferd Blood Stopper (ABS) was significantly greater than those of the other groups (P < 0.05). Thus, while 3 of the tested hemostatic agents did not have significant effects on the bond strength of composite resin to dentin, ABS increased the bond strength of CSE Bond to dentin. PMID:26147164

  14. In vivo remineralization of acid-etched enamel in non-brushing areas as influenced by fluoridated orthodontic adhesive and toothpaste.

    PubMed

    Praxedes-Neto, Otávio José; Borges, Boniek Castillo Dutra; Florêncio-Filho, Cícero; Farias, Arthur Costa Rodrigues; Drennan, John; De Lima, Kenio Costa

    2012-07-01

    This study aimed to evaluate the in vivo remineralization of acid-etched enamel in non-brushing areas as influenced by fluoridated orthodontic adhesive and toothpaste. One hundred and twenty teeth from 30 volunteers were selected. The teeth were assigned to four treatments: no treatment (negative control); 37% phosphoric acid-etching (PAE) (positive control); PAE + resin-modified glass ionomer cement (RMGIC); and, PAE + composite resin. Patients brushed teeth with fluoridated (n = 15) or non-fluoridated (n = 15) toothpastes, so that etched enamel was protected with screens and it was not in contact with the brush bristles. Remineralization was evaluated by means of laser fluorescence (LF), environmental scanning electronic microscopy, and energy dispersive spectrometry after extraction. The LF means were compared by means of Wilcoxon and Mann Whitney tests. Environmental scanning electron microscopy scores were compared among the groups using a Kruskal Wallis test, whereas the Ca/P ratio was evaluated by means of an Analysis of Variance with subparcels (treatments) and Tukey's post-hoc test. There were no statistically significant differences between the tooth pastes and between the orthodontic adhesives evaluated. Most teeth presented only partial enamel remineralization. Therefore, the fluoride released by the RMGIC was not enough to cause increased crystal regrowth in the acid-etched enamel. The use of fluoridated toothpaste did not provide positive additional effect.

  15. Effect of tooth surface preparation on the bonding of self-etching primer adhesives.

    PubMed

    Adebayo, O A; Burrow, M F; Tyas, M J; Palamara, J

    2012-01-01

    The aim of this study was to determine the bonding effectiveness of four self-etching primer adhesives after various tooth preparation protocols. Enamel/dentin specimens were prepared from 84 permanent molars, divided into three enamel preparation groups (silicon carbide paper [SiC1; erbium, chromium:yttri-um, scandium, gallium, garnet [Er,Cr:YSGG] laser [EL] and diamond bur [DB]) and five dentin preparation groups (SiC, EL, DB, steel[SB], and ceramic burs [CBs]). In each group,specimens were equally divided into four sub-groups and were bonded using Clearfil SEBond (CSE, Kuraray), Xeno IV (XE, Dentsply),Tokuyama Bond Force (TK, Tokuyama) and Filtek Silorane System Adhesive (FS, 3MESPE), as well as a hybrid resin composite(Clearfil Majesty Esthetic, Kuraray) for CSE,XE, and TK, and Filtek Posterior Restorative(3M ESPE) for FS). After 24 hours of water storage at 370C, microshear bond strength(iSBS) testing was carried out. Data were analyzed using analysis of variance (ANOVA)-Tukey test at a=0.05 and bond failure modes assessed. Representative debonded specimens were prepared and examined under the scanning electron microscope (SEM). All adhesives exhibited no significant differences in 1SBS on enamel and dentin under the clinical cavity preparation protocols, except for TK on den-tin. SEM revealed areas of altered subsurface enamel/dentin following EL ablation.

  16. 1/f noise in etched groove surface acoustic wave (SAW) resonators.

    PubMed

    Parker, T E; Andres, D; Greer, J A; Montress, G K

    1994-01-01

    Measurements of 1/f (or flicker) frequency fluctuations in SAW resonators fabricated with etched groove reflectors on single crystal quartz have shown that the observed noise levels vary inversely with device size. These measurements were made on sixteen 450 MHz resonators of four different sizes. The 1/f noise levels were also evaluated on twenty-eight other SAW resonators ranging in frequency from 401 to 915 MHz. This additional data provides valuable information on the dependence of the flicker noise levels on resonator frequency. A model based an localized, independent velocity fluctuations in the quartz is proposed which correctly fits the observed size and frequency dependence of the measured 1/f noise levels. This model suggests that the velocity fluctuations originate in small regions (much less than ~5 mum in diameter) randomly distributed throughout the quartz with an average separation of about 5 mum between independent (incoherent) sources. The magnitude of the localized fractional velocity fluctuations, Deltav/v, averaged over a 5 micron cube is on the order of 1x10 (-9). PMID:18263275

  17. Rate controlled metal assisted chemical etching to fabricate vertical and uniform Si nanowires

    NASA Astrophysics Data System (ADS)

    Song, Ari; Yun, Seokhun; Lokhande, Vaibhav; Ji, Taeksoo

    2016-03-01

    Mac(metal assisted chemical) etching is a simple, low-cost and anisotropic etching method to make Si NWs (silicon nanowires). In this method, smaller surface area is damaged compared to dry etching process, either. Mac etching uses a combination of an oxide removal acid (e.g. HF), an oxidant (e.g. H2O2) with a noble metal (e.g. Au, Ag, Pt, etc.) as the catalyst. Typically, the Si beneath the noble metal is etched faster than the Si without noble metal coverage by electron transfer mechanism at the noble metal /solution and the noble metal/Si interface. While Mac etching to build Si NWs, unwanted etching occurs in the bulk silicon layer resulting from excess hole diffusion caused by the increase in hole concentration at the nearby metal layers. In this study, we explored the ratio of oxidant to oxide removal acid in the Mac etching solution that is most effective in etching the Si underneath the noble metal layer suppressing the unwanted etching. At the optimized ratio, Si NWs were fabricated at a faster rate with good uniformity.

  18. Quantification of proteins using enhanced etching of Ag coated Au nanorods by the Cu2+/bicinchoninic acid pair with improved sensitivity

    NASA Astrophysics Data System (ADS)

    Liu, Wenqi; Hou, Shuai; Yan, Jiao; Zhang, Hui; Ji, Yinglu; Wu, Xiaochun

    2015-12-01

    Plasmonic nanosensors show great potential in ultrasensitive detection, especially with the plasmon peak position as the detection modality. Herein, a new sensitive but simple total protein quantification method termed the SPR-BCA assay is demonstrated by combining plasmonic nanosensors with protein oxidation by Cu2+. The easy tuning of localized surface plasmon resonance (LSPR) features of plasmonic nanostructures makes them ideal sensing platforms. We found that the Cu2+/bicinchoninic acid (BCA) pair exhibits accelerated etching of Au@Ag nanorods and results in the LSPR peak shift. A linear relationship between Cu2+ and the LSPR shift is found in a double logarithmic coordinate. Such double logarithm relationship is transferred to the concentration of proteins. Theoretical simulation shows that Au nanorods with large aspect ratios and small core sizes show high detection sensitivity. Via optimized sensor design, we achieved an increased sensitivity (the limit of detection was 3.4 ng ml-1) and a wide working range (0.5 to 1000 μg ml-1) compared with the traditional BCA assay. The universal applicability of our method to various proteins further proves its potential in practical applications.Plasmonic nanosensors show great potential in ultrasensitive detection, especially with the plasmon peak position as the detection modality. Herein, a new sensitive but simple total protein quantification method termed the SPR-BCA assay is demonstrated by combining plasmonic nanosensors with protein oxidation by Cu2+. The easy tuning of localized surface plasmon resonance (LSPR) features of plasmonic nanostructures makes them ideal sensing platforms. We found that the Cu2+/bicinchoninic acid (BCA) pair exhibits accelerated etching of Au@Ag nanorods and results in the LSPR peak shift. A linear relationship between Cu2+ and the LSPR shift is found in a double logarithmic coordinate. Such double logarithm relationship is transferred to the concentration of proteins. Theoretical

  19. Surface conditions of Nitinol wires, tubing, and as-cast alloys. The effect of chemical etching, aging in boiling water, and heat treatment.

    PubMed

    Shabalovskaya, S A; Anderegg, J; Laab, F; Thiel, P A; Rondelli, G

    2003-04-15

    The surface conditions of Nitinol wires and tubing were evaluated with the use of X-ray photoelectron spectroscopy, high-resolution Auger spectroscopy, electron backscattering, and scanning-electron microscopy. Samples were studied in the as-received state as well as after chemical etching, aging in boiling water, and heat treatment, and compared to a mechanically polished 600-grit-finish Nitinol surface treated similarly. General regularities in surface behavior induced by the examined surface treatments are similar for wires, tubing, and studied as-cast alloy, though certain differences in surface Ni concentration were observed. Nitinol wires and tubing from various suppliers demonstrated great variability in Ni surface concentration (0.5-15 at.%) and Ti/Ni ratio (0.4-35). The wires in the as-received state, with the exception of those with a black oxide originating in the processing procedure, revealed nickel and titanium on the surface in both elemental and oxidized states, indicating a nonpassive surface. Shape-setting heat treatment at 500 degrees C for 15 min resulted in tremendous increase in the surface Ni concentration and complete Ni oxidation. Preliminary chemical etching and boiling in water successfully prevented surface enrichment in Ni, initially resulting from heat treatment. A stoichiometric uniformly amorphous TiO(2) oxide generated during chemical etching and aging in boiling water was reconstructed at 700 degrees C, revealing rutile structure.

  20. Decontamination of U-metal Surface by an Oxidation Etching System

    SciTech Connect

    Stout, R B; Kansa, E J; Shaffer, R J; Weed, H C

    2000-12-18

    A surface oxidation treatment is described to remove surface contamination from uranium (U) metal and/or hydrides of uranium and heavy metals (HM) from U-metal parts. In the case of heavy metal atomic contamination on a surface, and potentially several atomic layers beneath, the surface oxidation treatment combines both chemical and chemically driven mechanical processes. The chemical process is a controlled temperature-time oxidization process that creates a thin film of uranium oxide (UO{sub 2} and higher oxides) on the U-metal surface. The chemically driven mechanical process is strain induced by the volume increase as the U-metal surface transforms to a UO{sub 2} surface film. These volume strains are sufficiently large to cause surface failure spalling/scale formation and thus, removal of a U-oxide film that contains the HM-contaminated surface. The case of a HM-hydride surface contamination layer can be treated similarly by using inert hot gas to decompose the U-hydrides and/or HM-hydrides that are contiguous with the surface. A preliminary analysis to design and to plan for a sequence of tests is developed. The tests will provide necessary and sufficient data to evaluate the effective implementation and operational characteristics of a safe and reliable system. The following description is limited to only a surface oxidation process for HM-decontamination.

  1. Apparatus for edge etching of semiconductor wafers

    NASA Technical Reports Server (NTRS)

    Casajus, A.

    1986-01-01

    A device for use in the production of semiconductors, characterized by etching in a rapidly rotating etching bath is described. The fast rotation causes the surface of the etching bath to assume the form of a paraboloid of revolution, so that the semiconductor wafer adjusted at a given height above the resting bath surface is only attacked by etchant at the edges.

  2. Semiconductor etching by hyperthermal neutral beams

    NASA Technical Reports Server (NTRS)

    Minton, Timothy K. (Inventor); Giapis, Konstantinos P. (Inventor)

    1999-01-01

    An at-least dual chamber apparatus and method in which high flux beams of fast moving neutral reactive species are created, collimated and used to etch semiconductor or metal materials from the surface of a workpiece. Beams including halogen atoms are preferably used to achieve anisotropic etching with good selectivity at satisfactory etch rates. Surface damage and undercutting are minimized.

  3. Simulation of nonlinear superconducting rf losses derived from characteristic topography of etched and electropolished niobium surfaces

    NASA Astrophysics Data System (ADS)

    Xu, Chen; Reece, Charles E.; Kelley, Michael J.

    2016-03-01

    A simplified numerical model has been developed to simulate nonlinear superconducting radiofrequency (SRF) losses on Nb surfaces. This study focuses exclusively on excessive surface resistance (Rs ) losses due to the microscopic topographical magnetic field enhancements. When the enhanced local surface magnetic field exceeds the superconducting critical transition magnetic field Hc , small volumes of surface material may become normal conducting and increase the effective surface resistance without inducing a quench. We seek to build an improved quantitative characterization of this qualitative model. Using topographic data from typical buffered chemical polish (BCP)- and electropolish (EP)-treated fine grain niobium, we have estimated the resulting field-dependent losses and extrapolated this model to the implications for cavity performance. The model predictions correspond well to the characteristic BCP versus EP high field Q0 performance differences for fine grain niobium. We describe the algorithm of the model, its limitations, and the effects of this nonlinear loss contribution on SRF cavity performance.

  4. Correlation of film density and wet etch rate in hydrofluoric acid of plasma enhanced atomic layer deposited silicon nitride

    NASA Astrophysics Data System (ADS)

    Provine, J.; Schindler, Peter; Kim, Yongmin; Walch, Steve P.; Kim, Hyo Jin; Kim, Ki-Hyun; Prinz, Fritz B.

    2016-06-01

    The continued scaling in transistors and memory elements has necessitated the development of atomic layer deposition (ALD) of silicon nitride (SiNx), particularly for use a low k dielectric spacer. One of the key material properties needed for SiNx films is a low wet etch rate (WER) in hydrofluoric (HF) acid. In this work, we report on the evaluation of multiple precursors for plasma enhanced atomic layer deposition (PEALD) of SiNx and evaluate the film's WER in 100:1 dilutions of HF in H2O. The remote plasma capability available in PEALD, enabled controlling the density of the SiNx film. Namely, prolonged plasma exposure made films denser which corresponded to lower WER in a systematic fashion. We determined that there is a strong correlation between WER and the density of the film that extends across multiple precursors, PEALD reactors, and a variety of process conditions. Limiting all steps in the deposition to a maximum temperature of 350 °C, it was shown to be possible to achieve a WER in PEALD SiNx of 6.1 Å/min, which is similar to WER of SiNx from LPCVD reactions at 850 °C.

  5. Influence of warm air-drying on enamel bond strength and surface free-energy of self-etch adhesives.

    PubMed

    Shiratsuchi, Koji; Tsujimoto, Akimasa; Takamizawa, Toshiki; Furuichi, Tetsuya; Tsubota, Keishi; Kurokawa, Hiroyasu; Miyazaki, Masashi

    2013-08-01

    We examined the effect of warm air-drying on the enamel bond strengths and the surface free-energy of three single-step self-etch adhesives. Bovine mandibular incisors were mounted in self-curing resin and then wet ground with #600 silicon carbide (SiC) paper. The adhesives were applied according to the instructions of the respective manufacturers and then dried in a stream of normal (23°C) or warm (37°C) air for 5, 10, and 20 s. After visible-light irradiation of the adhesives, resin composites were condensed into a mold and polymerized. Ten samples per test group were stored in distilled water at 37°C for 24 h and then the bond strengths were measured. The surface free-energies were determined by measuring the contact angles of three test liquids placed on the cured adhesives. The enamel bond strengths varied according to the air-drying time and ranged from 15.8 to 19.1 MPa. The trends for the bond strengths were different among the materials. The value of the γS⁺ component increased slightly when drying was performed with a stream of warm air, whereas that of the γS⁻ component decreased significantly. These data suggest that warm air-drying is essential to obtain adequate enamel bond strengths, although increasing the drying time did not significantly influence the bond strength.

  6. Influence of warm air-drying on enamel bond strength and surface free-energy of self-etch adhesives.

    PubMed

    Shiratsuchi, Koji; Tsujimoto, Akimasa; Takamizawa, Toshiki; Furuichi, Tetsuya; Tsubota, Keishi; Kurokawa, Hiroyasu; Miyazaki, Masashi

    2013-08-01

    We examined the effect of warm air-drying on the enamel bond strengths and the surface free-energy of three single-step self-etch adhesives. Bovine mandibular incisors were mounted in self-curing resin and then wet ground with #600 silicon carbide (SiC) paper. The adhesives were applied according to the instructions of the respective manufacturers and then dried in a stream of normal (23°C) or warm (37°C) air for 5, 10, and 20 s. After visible-light irradiation of the adhesives, resin composites were condensed into a mold and polymerized. Ten samples per test group were stored in distilled water at 37°C for 24 h and then the bond strengths were measured. The surface free-energies were determined by measuring the contact angles of three test liquids placed on the cured adhesives. The enamel bond strengths varied according to the air-drying time and ranged from 15.8 to 19.1 MPa. The trends for the bond strengths were different among the materials. The value of the γS⁺ component increased slightly when drying was performed with a stream of warm air, whereas that of the γS⁻ component decreased significantly. These data suggest that warm air-drying is essential to obtain adequate enamel bond strengths, although increasing the drying time did not significantly influence the bond strength. PMID:23841790

  7. 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.

  8. Study of model superoleophobic surfaces fabricated with a modified Bosch etch method.

    PubMed

    Koch, Brendan M L; Elliott, Janet A W; Amirfazli, A

    2014-11-25

    A set of surfaces featuring pillars with overhanging cap structures, exhibiting superoleophobic behavior, were fabricated using a new method. While such structures have been previously reported, in contrast with previous literature this new method allows for the control of pillar cross-sectional diameter, pillar separation, and Cassie fraction independent from the pillar radius-to-height ratio. Once fabricated the contact angles of the surfaces were examined using water, ethylene glycol, and hexadecane. These surfaces were capable of maintaining a stable Cassie state with hexadecane where surfaces with similar Cassie fraction but vertical sidewalls we had examined previously collapsed into the Wenzel state. The overall behavior of the liquids conforms to prior experience with vertical sidewall structures, with the advancing contact angles tending to remain high and insensitive to changing Cassie fraction while the receding contact angles follow the trends predicted by the Cassie equation much more closely. All experimental evidence taken together, this seems to indicate that the cap structures increase the stability of the Cassie state, but at the expense of increasing drop pinning, over and above what such surface texturing already does. PMID:25347467

  9. Method for cleaning a solar cell surface opening made with a solar etch paste

    DOEpatents

    Rohatgi, Ajeet; Meemongkolkiat, Vichai

    2010-06-22

    A thin silicon solar cell having a back dielectric passivation and rear contact with local back surface field is described. Specifically, the solar cell may be fabricated from a crystalline silicon wafer having a thickness from 50 to 500 micrometers. A barrier layer and a dielectric layer are applied at least to the back surface of the silicon wafer to protect the silicon wafer from deformation when the rear contact is formed. At least one opening is made to the dielectric layer. An aluminum contact that provides a back surface field is formed in the opening and on the dielectric layer. The aluminum contact may be applied by screen printing an aluminum paste having from one to 12 atomic percent silicon and then applying a heat treatment at 750 degrees Celsius.

  10. Surface Modification Energized by Focused Ion Beam: The Influence of Etch Rates & Aspect Ratio on Ripple Wavelengths.

    SciTech Connect

    MoberlyChan, W J

    2006-11-15

    Ion beams have been used to modify surface topography, producing nanometer-scale modulations (and even subnanometer ripples in this work) that have potential uses ranging from designing self-assembly structures, to controlling stiction of micromachined surfaces, to providing imprint templates for patterned media. Modern computer-controlled Focused Ion Beam tools enable alternating submicron patterned zones of such ion-eroded surfaces, as well as dramatically increasing the rate of ion beam processing. The DualBeam FIB/SEM also expedites process development while minimizing the use of materials that may be precious (Diamond) and/or produce hazardous byproducts (Beryllium). A FIB engineer can prototype a 3-by-3-by-3 matrix of variables in tens of minutes and consume as little as zeptoliters of material; whereas traditional ion beam processing would require tens of days and tens of precious wafers. Saturation wavelengths have been reported for ripples on materials such as single crystal silicon or diamond ({approx}200nm); however this work achieves wavelengths >400nm on natural diamond. Conversely, Be can provide a stable and ordered 2-dimensional array of <40nm periodicity; and ripples <0.4nm are also fabricated on carbon surfaces and quantified by HR-TEM and electron diffraction. Rippling is a function of material, ion beam, and angle; but is also controlled by chemical environment, redeposition, and aspect ratio. Ideally a material exhibits a constant yield (atoms sputtered off per incident ion); however, pragmatic FIB processes, coupled with the direct metrological feedback in a DualBeam tool, reveal etch rates do not remain constant for nanometer-scale processing. Control of rippling requires controlled metrology, and robust software tools are developed to enhance metrology. In situ monitoring of the influence of aspect ratio and redeposition at the micron scale correlates to the rippling fundamentals that occur at the nanometer scale and are controlled by the

  11. Petrologic and experimental evidence for the etching of garnets by organic acids in the upper Jurassic Morrision Formation, northwestern New Mexico.

    USGS Publications Warehouse

    Hansley, P.L.

    1987-01-01

    Etching of garnets and partial to complete dissolution of other aluminosilicate minerals were caused by high concentrations of organic acids generated during the maturation of epigenetic organic matter (predominantly type-III kerogen) in the Morrison Formation. The presence of authigenic phases that form near 100oC indicates that temperatures were high enough during diagenesis to cause the thermal degradation of kerogen.-from Author

  12. Bond strength with various etching times on young permanent teeth

    SciTech Connect

    Wang, W.N.; Lu, T.C. )

    1991-07-01

    Tensile bond strengths of an orthodontic resin cement were compared for 15-, 30-, 60-, 90-, or 120-second etching times, with a 37% phosphoric acid solution on the enamel surfaces of young permanent teeth. Fifty extracted premolars from 9- to 16-year-old children were used for testing. An orthodontic composite resin was used to bond the bracket directly onto the buccal surface of the enamel. The tensile bond strengths were tested with an Instron machine. Bond failure interfaces between bracket bases and teeth surfaces were examined with a scanning electron microscope and calculated with mapping of energy-dispersive x-ray spectrometry. The results of tensile bond strength for 15-, 30-, 60-, or 90-second etching times were not statistically different. For the 120-second etching time, the decrease was significant. Of the bond failures, 43%-49% occurred between bracket and resin interface, 12% to 24% within the resin itself, 32%-40% between resin and tooth interface, and 0% to 4% contained enamel fragments. There was no statistical difference in percentage of bond failure interface distribution between bracket base and resin, resin and enamel, or the enamel detachment. Cohesive failure within the resin itself at the 120-second etching time was less than at other etching times, with a statistical significance. To achieve good retention, to decrease enamel loss, and to reduce moisture contamination in the clinic, as well as to save chairside time, a 15-second etching time is suggested for teenage orthodontic patients.

  13. Morphological Changes of Human Dentin after Erbium-Doped Yttrium Aluminum Garnet (Er:YAG) and Carbon Dioxide (CO2) Laser Irradiation and Acid-etch Technique: An Scanning Electron Microscopic (SEM) Evaluation

    PubMed Central

    Shahabi, Sima; Chiniforush, Nasim; Juybanpoor, Nasrin

    2013-01-01

    Introduction: The aim of this study was to investigate the morphological changes of human dentin after Erbium-Doped Yttrium Aluminum Garnet (Er:YAG), Carbon Dioxide(CO2) laser-irradiation and acid-etching by means of scanning electron microscopic (SEM) Methods: 9 extracted human third molars were used in this study. The teeth were divided in three groups: first group, CO2 laser with power of 1.5 w and frequency of 80 Hz; second group, Er:YAG laser with output power of 1.5 W frequency of 10 Hz, very short pulse with water and air spray was applied; and third group, samples were prepared by acid-etching 37% for 15 sec and rinsed with air-water spray for 20 sec. Then, the samples were prepared for SEM examination. Results: Melting and cracks can be observed in CO2 laser but in Er:YAG laser cleanedablated surfaces and exposed dentinal tubules, without smear layer was seen. Conclusion: It can be concluded that Er:YAG laser can be an alternative technique for surface treatment and can be considered as safe as the conventional methods. But CO2 laser has some thermal side effects which make this device unsuitable for this purpose. PMID:25606306

  14. Highly roughened polycaprolactone surfaces using oxygen plasma-etching and in vitro mineralization for bone tissue regeneration: fabrication, characterization, and cellular activities.

    PubMed

    Kim, YongBok; Kim, GeunHyung

    2015-01-01

    Herein, poly(ɛ-caprolactone) (PCL) surfaces were treated to form various roughness values (R(a)=290-445 nm) and polar functional groups on the surfaces using a plasma-etching process, followed by immersion into simulated body fluid (SBF) for apatite formation. The surface morphology, chemical composition, and mean roughness of the plasma-etched PCL surfaces were measured, and various physical and morphological properties (water contact angles, protein absorption ability, and crystallite size of the apatite layer) of the in vitro mineralized PCL surfaces were evaluated. The roughened PCL surface P-3, which was treated with a sufficient plasma exposure time (4 h), achieved homogeneously distributed apatite formation after soaking in SBF for 7 days, as compared with other surfaces that were untreated or plasma-treated for 30 min or 2 h. Furthermore, to demonstrate their feasibility as a biomimetic surface, pre-osteoblast cells (MC3T3-E1) were cultured on the mineralized PCL surfaces, and cell viability, DAPI-phalloidin fluorescence assay, and alizarin red-staining of the P-3 surface were highly improved compared to the P-1 surface treated with a 30-min plasma exposure time; compared to untreated mineralized PCL surface (N-P), P-3 showed even greater improvements in cell viability and DAPI-phalloidin fluorescence assay. Based on these results, we found that the mineralized PCL surface supplemented with the appropriate plasma treatment can be implicitly helpful to achieve rapid hard tissue regeneration. PMID:25486326

  15. 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).

  16. Ion beam sputter etching

    NASA Technical Reports Server (NTRS)

    Banks, Bruce A.; Rutledge, Sharon K.

    1986-01-01

    An ion beam etching process which forms extremely high aspect ratio surface microstructures using thin sputter masks is utilized in the fabrication of integrated circuits. A carbon rich sputter mask together with unmasked portions of a substrate is bombarded with inert gas ions while simultaneous carbon deposition occurs. The arrival of the carbon deposit is adjusted to enable the sputter mask to have a near zero or even slightly positive increase in thickness with time while the unmasked portions have a high net sputter etch rate.

  17. Femtosecond laser etching of dental enamel for bracket bonding.

    PubMed

    Kabas, Ayse Sena; Ersoy, Tansu; Gülsoy, Murat; Akturk, Selcuk

    2013-09-01

    The aim is to investigate femtosecond laser ablation as an alternative method for enamel etching used before bonding orthodontic brackets. A focused laser beam is scanned over enamel within the area of bonding in a saw tooth pattern with a varying number of lines. After patterning, ceramic brackets are bonded and bonding quality of the proposed technique is measured by a universal testing machine. The results are compared to the conventional acid etching method. Results show that bonding strength is a function of laser average power and the density of the ablated lines. Intrapulpal temperature changes are also recorded and observed minimal effects are observed. Enamel surface of the samples is investigated microscopically and no signs of damage or cracking are observed. In conclusion, femtosecond laser exposure on enamel surface yields controllable patterns that provide efficient bonding strength with less removal of dental tissue than conventional acid-etching technique.

  18. Investigation of surface oxide films on InP mesa sidewalls and flat surfaces reactive ion etched using CH{sub 4}/H{sub 2} chemistry

    SciTech Connect

    Lee, B.T.; Kim, D.K.; Ahn, J.H.; Oh, D.G.

    1996-12-31

    Oxide films were observed on InP mesa sidewalls and horizontal surfaces after CH{sub 4}/H{sub 2} reactive ion etch process. Auger electron spectroscopy and X-ray microanalysis in the transmission electron microscopy suggested that the films are In-Si-P or In-P oxides containing more In than P, depending on the RIE instrument utilized. It was suggested that excess In in the film is due to the preferential evaporation of P, and Si is due to the mask erosion during the RIE process. Oxidation of the elements was observed to occur during the subsequent oxygen plasma ashing process. The films presented a serious barrier during the subsequent fabrication processes, such as regrowth and chemical cleaning, while could be effectively removed by cleaning in a diluted HF solution.

  19. Surface-Morphology-Induced Hydrophobicity of Fluorocarbon Films Grown by a Simultaneous Etching and Deposition Process

    NASA Astrophysics Data System (ADS)

    Fang, J. S.; Lin, C. S.; Huang, Y. Y.; Chin, T. S.

    2015-08-01

    Development of facile methods to prepare hydrophobic films is of great important. We report fluorocarbon films deposited by a simple plasma-assisted chemical vapor deposition method using C3F8 and C2H2 with extra Ar and/or O2 gases. The surface characteristics of the films were examined by scanning electron microscopy, atomic force microscopy, and x-ray photoelectron spectroscopy. The hydrophobic and oleophobic properties of the films were evaluated by measurements of static contact angle. The results showed that the film deposited with C3F8, C2H2, Ar, and O2 exhibited a water contact angle of 114°, hexadecane contact angle of 45°, and transmittance of 94.5%. Photoelectron spectra further revealed that the films contained mainly CF and CF2 bonds and thus a high F/C ratio. Introduction of O2 increased the F/C ratio, which combined with the stripe-like surface of the films achieved better hydrophobicity.

  20. Interaction morphology and bond strength of nanofilled simplified-step adhesives to acid etched dentin

    PubMed Central

    Di Hipólito, Vinicius; Reis, André Figueiredo; Mitra, Sumita B.; de Goes, Mario Fernando

    2012-01-01

    Objective: To evaluate the effect of nanofillers incorporated into adhesives on the microtensile bond strength (μ-TBS) and interfacial micromorphology to dentin. Methods: The occlusal enamel of 5 human molars was removed and each tooth sectioned into four quarters. The exposed dentin was treated with one of the following adhesives: Adper Single Bond (SB-unfilled), OptiBond Solo Plus (OS-barium aluminoborosilicate, 400nm Ø), Prime & Bond NT (NT-colloidal silica, 7–40 nm Ø) and Adper Single Bond 2 (SB2-colloidal silica, 5nm Ø). Cylinders of resin-based composite were constructed on the adhesive layers. After 24-hour storage, the restored tooth-quadrants were sectioned to obtain stick-shaped specimens (0.8 mm2, cross-sectional area) and submitted to μ-TBS at a cross-speed of 0.5 mm/min. Data were analyzed using one-way ANOVA and Tukey’s test (alpha = .05). Twenty-eight additional teeth were used for interfacial micro-morphologic analysis by SEM (16-teeth) and TEM (12-teeth). The dentin surfaces of 32 discs were treated with the adhesives (8 discs for adhesive) and laminated to form disc-pairs using a flowable resin composite for SEM/EDS analysis. For TEM, 90nm-thick nondemineralized unstained sections were processed. Results: SB2 showed significant higher bond strength than SB, OS and NT. The SEM/EDS and TEM analysis revealed nanofillers infiltrated within the interfibrillar spaces of the SB2-hybrid layer. Fillers were concentrated around patent tubular orifices and in the adhesive layer for OS and NT. Conclusion: The presence of nanofillers within the interfibrillar spaces of the SB2-hybrid layer suggests its importance in the improvement of the μ-TBS. PMID:23077413

  1. Smoothing single-crystalline SiC surfaces by reactive ion etching using pure NF{sub 3} and NF{sub 3}/Ar mixture gas plasmas

    SciTech Connect

    Tasaka, Akimasa; Kotaka, Yuki; Oda, Atsushi; Saito, Morihiro; Tojo, Tetsuro; Inaba, Minoru

    2014-09-01

    In pure NF{sub 3} plasma, the etching rates of four kinds of single-crystalline SiC wafer etched at NF{sub 3} pressure of 2 Pa were the highest and it decreased with an increase in NF{sub 3} pressure. On the other hand, they increased with an increase in radio frequency (RF) power and were the highest at RF power of 200 W. A smooth surface was obtained on the single-crystalline 4H-SiC after reactive ion etching at NF{sub 3}/Ar gas pressure of 2 Pa and addition of Ar to NF{sub 3} plasma increased the smoothness of SiC surface. Scanning electron microscopy observation revealed that the number of pillars decreased with an increase in the Ar-concentration in the NF{sub 3}/Ar mixture gas. The roughness factor (R{sub a}) values were decreased from 51.5 nm to 25.5 nm for the As-cut SiC, from 0.25 nm to 0.20 nm for the Epi-SiC, from 5.0 nm to 0.7 nm for the Si-face mirror-polished SiC, and from 0.20 nm to 0.16 nm for the C-face mirror-polished SiC by adding 60% Ar to the NF{sub 3} gas. Both the R{sub a} values of the Epi- and the C-face mirror-polished wafer surfaces etched using the NF{sub 3}/Ar (40:60) plasma were similar to that treated with mirror polishing, so-called the Catalyst-Referred Etching (CARE) method, with which the lowest roughness of surface was obtained among the chemical mirror polishing methods. Etching duration for smoothing the single-crystalline SiC surface using its treatment was one third of that with the CARE method.

  2. Modulated regeneration of acid-etched human tooth enamel by a functionalized dendrimer that is an analog of amelogenin.

    PubMed

    Chen, Mei; Yang, Jiaojiao; Li, Jiyao; Liang, Kunneng; He, Libang; Lin, Zaifu; Chen, Xingyu; Ren, Xiaokang; Li, Jianshu

    2014-10-01

    In the bioinspired repair process of tooth enamel, it is important to simultaneously mimic the organic-matrix-induced biomineralization and increase the binding strength at the remineralization interface. In this work, a fourth-generation polyamidoamine dendrimer (PAMAM) is modified by dimethyl phosphate to obtain phosphate-terminated dendrimer (PAMAM-PO3H2) since it has a similar dimensional scale and peripheral functionalities to that of amelogenin, which plays important role in the natural development process of enamel. Its phosphate group has stronger affinity for calcium ion than carboxyl group and can simultaneously provide strong hydroxyapatite (HA)-binding capability. The MTT assay demonstrates the low cytotoxicity of PAMAM-PO3H2. Adsorption tests indicate that PAMAM-PO3H2 can be tightly adsorbed on the human tooth enamel. Scanning electron microscopy and X-ray diffraction are used to analyze the remineralization process. After being incubated in artificial saliva for 3weeks, there is a newly generated HA layer of 11.23μm thickness on the acid-etched tooth enamel treated by PAMAM-PO3H2, while the thickness for the carboxyl-terminated one (PAMAM-COOH) is only 6.02μm. PAMAM-PO3H2 can regulate the remineralization process to form ordered new crystals oriented along the Z-axis and produce an enamel prism-like structure that is similar to that of natural tooth enamel. The animal experiment also demonstrates that PAMAM-PO3H2 can induce significant HA regeneration in the oral cavity of rats. Thus PAMAM-PO3H2 shows great potential as a biomimetic restorative material for human tooth enamel.

  3. Bond strength between resin composite and etched and non-etched glass ionomer.

    PubMed

    Zanata, R L; Navarro, M F; Ishikiriama, A; da Silva e Souza Júnior, M H; Delazari, R C

    1997-01-01

    The authors evaluated, in vitro, the effects of etching glass ionomer cements prior to the application of a bonding agent and a resin composite on the bond strength of the glass ionomer/resin composite interface. Six glass ionomer cements were tested using the same bonding agent/resin composite system (Scotchbond Multipurpose/Z 100). For each material, 16 specimens were prepared and divided into two groups. Eight of the specimens were not etched while eight were etched with 37% phosphoric acid for 15 seconds. All the materials were used according to the manufacturers' instructions. Glass ionomer cylinders were prepared and were mounted in an assembly apparatus and the bonding agent/resin composite transferred to a demarcated area on the cement surface. The specimens were stored for 24 hours in distilled water at 37 degrees C and thermocycled. After thermocycling, the specimens were placed in a testing machine and a shear load applied with a knife-edged rod at the glass ionomer/resin composite interface. The shear bond strength was calculated and expressed in MPa. Data were analyzed by ANOVA and the Tukey-Kramer test. There were no significant differences among the shear bond strengths of the resin composite to etched and non-etched glass ionomer cements.

  4. Effect of chemical etching on the surface roughness of CdZnTe and CdMnTe gamma radiation detectors

    SciTech Connect

    Hossain,A.; Babalola, S.; Bolotnikov, A.E.; Camarda, G.S.; Cui, Y.; Yang, G.; Guo, M.; Kochanowska, D.; Mycielski, A.; Burger, A.; James, R.B.

    2008-08-11

    Generally, mechanical polishing is performed to diminish the cutting damage followed by chemical etching to remove the remaining damage on crystal surfaces. In this paper, we detail the findings from our study of the effects of various chemical treatments on the roughness of crystal surfaces. We prepared several CdZnTe (CZT) and CdMnTe (CMT) crystals by mechanical polishing with 5 {micro}m and/or lower grits of Al{sub 2}O{sub 3} abrasive papers including final polishing with 0.05-{micro}m particle size alumina powder and then etched them for different periods with a 2%, 5% Bromine-Methanol (B-M) solution, and also with an E-solution (HNO{sub 3}:H{sub 2}O:Cr{sub 2}O{sub 7}). The material removal rate (etching rate) from the crystals was found to be 10 {micro}m, 30 {micro}m, and 15 {micro}m per minute, respectively. The roughness of the resulting surfaces was determined by the Atomic Force Microscopy (AFM) to identify the most efficient surface processing method by combining mechanical and chemical polishing.

  5. Uniform nano-ripples on the sidewall of silicon carbide micro-hole fabricated by femtosecond laser irradiation and acid etching

    SciTech Connect

    Khuat, Vanthanh; Chen, Tao; Gao, Bo; Si, Jinhai Ma, Yuncan; Hou, Xun

    2014-06-16

    Uniform nano-ripples were observed on the sidewall of micro-holes in silicon carbide fabricated by 800-nm femtosecond laser and chemical selective etching. The morphology of the ripple was analyzed using scanning electronic microscopy. The formation mechanism of the micro-holes was attributed to the chemical reaction of the laser affected zone with mixed solution of hydrofluoric acid and nitric acid. The formation of nano-ripples on the sidewall of the holes could be attributed to the standing wave generated in z direction due to the interference between the incident wave and the reflected wave.

  6. Industrial ion source technology. [for ion beam etching, surface texturing, and deposition

    NASA Technical Reports Server (NTRS)

    Kaufman, H. R.

    1977-01-01

    Plasma probe surveys were conducted in a 30-cm source to verify that the uniformity in the ion beam is the result of a corresponding uniformity in the discharge-chamber plasma. A 15 cm permanent magnet multipole ion source was designed, fabricated, and demonstrated. Procedures were investigated for texturing a variety of seed and surface materials for controlling secondary electron emission, increasing electron absorption of light, and improved attachment of biological tissue for medical implants using argon and tetrafluoromethane as the working gases. The cross section for argon-argon elastic collisions in the ion-beam energy range was calculated from interaction potentials and permits calculation of beam interaction effects that can determine system pumping requirements. The data also indicate that different optimizations of ion-beam machines will be advantageous for long and short runs, with 1 mA-hr/cm being the rough dividing line for run length. The capacity to simultaneously optimize components in an ion-beam machine for a single application, a capacity that is not evident in competitive approaches such as diode sputtering is emphasized.

  7. Plasma-Enhanced Atomic Layer Deposition of SiN-AlN Composites for Ultra Low Wet Etch Rates in Hydrofluoric Acid.

    PubMed

    Kim, Yongmin; Provine, J; Walch, Stephen P; Park, Joonsuk; Phuthong, Witchukorn; Dadlani, Anup L; Kim, Hyo-Jin; Schindler, Peter; Kim, Kihyun; Prinz, Fritz B

    2016-07-13

    The continued scaling in transistors and memory elements has necessitated the development of atomic layer deposited (ALD) of hydrofluoric acid (HF) etch resistant and electrically insulating films for sidewall spacer processing. Silicon nitride (SiN) has been the prototypical material for this need and extensive work has been conducted into realizing sufficiently lower wet etch rates (WERs) as well as leakage currents to meet industry needs. In this work, we report on the development of plasma-enhanced atomic layer deposition (PEALD) composites of SiN and AlN to minimize WER and leakage current density. In particular, the role of aluminum and the optimum amount of Al contained in the composite structures have been explored. Films with near zero WER in dilute HF and leakage currents density similar to pure PEALD SiN films could be simultaneously realized through composites which incorporate ≥13 at. % Al, with a maximum thermal budget of 350 °C.

  8. Micro-PIXE and micro-RBS characterization of micropores in porous silicon prepared using microwave-assisted hydrofluoric acid etching.

    PubMed

    Ahmad, Muthanna; Grime, Geoffrey W

    2013-04-01

    Porous silicon (PS) has been prepared using a microwave-assisted hydrofluoric acid (HF) etching method from a silicon wafer pre-implanted with 5 MeV Cu ions. The use of microbeam proton-induced X-ray emission (micro-PIXE) and microbeam Rutherford backscattering techniques reveals for the first time the capability of these techniques for studying the formation of micropores. The porous structures observed from micro-PIXE imaging results are compared to scanning electron microscope images. It was observed that the implanted copper accumulates in the same location as the pores and that at high implanted dose the pores form large-scale patterns of lines and concentric circles. This is the first work demonstrating the use of microwave-assisted HF etching in the formation of PS.

  9. Plasma-Enhanced Atomic Layer Deposition of SiN-AlN Composites for Ultra Low Wet Etch Rates in Hydrofluoric Acid.

    PubMed

    Kim, Yongmin; Provine, J; Walch, Stephen P; Park, Joonsuk; Phuthong, Witchukorn; Dadlani, Anup L; Kim, Hyo-Jin; Schindler, Peter; Kim, Kihyun; Prinz, Fritz B

    2016-07-13

    The continued scaling in transistors and memory elements has necessitated the development of atomic layer deposited (ALD) of hydrofluoric acid (HF) etch resistant and electrically insulating films for sidewall spacer processing. Silicon nitride (SiN) has been the prototypical material for this need and extensive work has been conducted into realizing sufficiently lower wet etch rates (WERs) as well as leakage currents to meet industry needs. In this work, we report on the development of plasma-enhanced atomic layer deposition (PEALD) composites of SiN and AlN to minimize WER and leakage current density. In particular, the role of aluminum and the optimum amount of Al contained in the composite structures have been explored. Films with near zero WER in dilute HF and leakage currents density similar to pure PEALD SiN films could be simultaneously realized through composites which incorporate ≥13 at. % Al, with a maximum thermal budget of 350 °C. PMID:27295338

  10. Surface interactions of SO{sub 2} and passivation chemistry during etching of Si and SiO{sub 2} in SF{sub 6}/O{sub 2} plasmas

    SciTech Connect

    Stillahn, Joshua M.; Zhang Jianming; Fisher, Ellen R.

    2011-01-15

    A variety of materials can be etched in SF{sub 6}/O{sub 2} plasmas. Here, the fate of SO{sub 2} at Si and SiO{sub 2} surfaces during etching in SF{sub 6}/O{sub 2} plasmas has been explored using the imaging of radicals interacting with surfaces method. The scattering of SO{sub 2} at Si and SiO{sub 2} surfaces was measured as a function of both the applied rf power and O{sub 2} addition to the plasma. For both surfaces, the surface scattering coefficient (S) of SO{sub 2} during etching is near unity and is largely unaffected by changing plasma parameters such as power and O{sub 2} addition. Notably the etch rate of Si increases monotonically with power, whereas the etch rate of SiO{sub 2} appears insensitive to changes in plasma conditions. As a result, the etch selectivity closely follows the trends of the Si etch rate. Etch rates are compared to other fluorine-containing plasma systems such as NF{sub 3}/O{sub 2} and C{sub 2}F{sub 6}/O{sub 2}. Using mass spectral data and optical emission spectra to characterize the gas phase species combined with compositional analysis from x-ray photoelectron spectroscopy data, the formation and roles of SO{sub 2} in Si and SiO{sub 2} etching are discussed and correlated with etch rate and other gas phase species such as F, O, and S{sub x}O{sub y}F{sub z}.

  11. Scanning electron microscopy and EDX analysis of exocrine and endocrine gland cells of rat pancreas surface-etched in an oxygen plasma.

    PubMed

    Yoshino, M; Miyasaka, S; Sato, H; Seta, S

    1982-01-01

    Pancreas, double-fixed in glutaraldehyde and osmium tetroxide and embedded in epoxy resin was cut into sections 0.5-1 micron thick. The sections were surface-etched in an oxygen plasma produced by exciting oxygen with a radio frequency generator. Structural components of exocrine and endocrine cells were morphologically investigated in the secondary electron image mode of the SEM. Moreover, in order to identify some cell components such as endocrine granules, the morphological image obtained of the etched surface by the SEM were compared with those seen in a TEM, using the serial sections from the same tissue block and at the same cellular level. For a microanalytical investigation, tissues were fixed with glutaraldehyde alone. The structural components of exocrine and endocrine cells were analyzed by SEM/EDX. A better resolution under the SEM was obtained of 0.5-0.8 micron thick sections after surface-etching in an oxygen plasma for 1 minute. Intracellular structures such as nuclear membranes, nucleolus, mitochondria, rough endoplasmic reticulum and zymogen granules were readily identifiable. Moreover, the internal structure of organelles such as cristae of mitochondria was recognized. In the serial sections, the mode of arrangement of intracellular structures in the SEM was well consistent with those in the TEM. The peaks of phosphorus, sulphur and calcium were clearly detected from the intracellular components such as nucleolus, nuclear membranes and secretory granules.

  12. Growth optimization and characterization of GaN epilayers on multifaceted (111) surfaces etched on Si(100) substrates

    SciTech Connect

    Ansah-Antwi, KwaDwo Konadu Chua, Soo Jin; Soh, Chew Beng; Liu, Hongfei

    2015-11-15

    The four nearest Si(111) multifaceted sidewalls were exposed inside an array of 3 μm-wide square holes patterned on an Si(100) substrate, and this patterned Si(100) substrate was used as a substrate for the deposition of a gallium nitride (GaN) epilayer. Subsequently the effect that the growth pressure, the etched-hole profiles, and the etched-hole arrangement had upon the quality of the as-grown GaN was investigated. The coalescence of the as-grown GaN epilayer on the exposed Si(111) facets was observed to be enhanced with reduced growth pressure from 120 to 90 Torr. A larger Si(001) plane area at the bottom of the etched holes resulted in bidirectional GaN domains, which resulted in poor material quality. The bidirectional GaN domains were observed as two sets of six peaks via a high-resolution x-ray diffraction phi scan of the GaN(10-11) reflection. It was also shown that a triangular array of etched holes was more desirable than square arrays of etched holes for the growth high-quality and continuous GaN films.

  13. Investigations of Wafer Scale Etching with Xenon Difluoride

    NASA Astrophysics Data System (ADS)

    Chen, K. N.; Hoivik, N.; Lin, C. Y.; Young, A.; Ieong, M.; Shahidi, G.

    2006-03-01

    A good and uniform bulk silicon wafer etching method can be applied to the wafer thinning process in MEMS and 3D applications. In this study, the use of a Xenon Difluoride (XeF2) gas-phase etching system, operating at room temperature, has been investigated for bulk silicon wafer thinning. We investigated the Si-wafer surface morphology and profile following each XeF2 etching process cycle. Theoretical results are used to compare with the experimental results as well. A clean wafer surface by proper surface treatments is significant to achieve a uniform surface profile and morphology for XeF2 etching. A proper design of etching cycle with nitrogen ambient during etching is necessary to achieve the fastest and uniform silicon etching rate. The silicon etching rate is reported as a function of etching pressure, nitrogen pressure, and etching duration.

  14. 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.

  15. Effect of acid vapor etching on morphological and opto-electric properties of flat silicon and silicon nanowire arrays: A comparative study

    NASA Astrophysics Data System (ADS)

    Amri, Chohdi; Ouertani, Rachid; Hamdi, Abderrahmen; Ezzaouia, Hatem

    2016-03-01

    In this paper, we report a comparative study between porous silicon (pSi) and porous silicon nanowires (pSiNWs). Acid Vapor Etching (AVE) treatment has been used to perform porous structure on flat Si and SiNWs array substrates respectively. SiNW structure is prepared by the widely used Silver catalyzed etching method. SEM and TEM images show that AVE treatment induces porous structure in the whole Si wafer and the SiNW sidewall. Comparatively to pSi, pSiNWs exhibit a low reflectivity in the whole spectral range which decreases with etching duration. However, the reflectivity of pSi changes with porous layer thickness. Both pSi and pSiNWs exhibit a significant PL peak situated at 2 eV. PL peaks are attributed to the quantum confinement effect in the silicon nanocrystallites (SiNCs). We discussed the significant enhancement in the peak intensities and a shift toward lower energy displayed in Raman spectra for both pSi and pSiNWs. We reported a correlative study of the AVE treatment effect on the minority carrier life time of flat silicon and SiNW arrays with the passivation effect of chemical induced silicon oxides highlighted by FTIR spectra.

  16. Organic acids in naturally colored surface waters

    USGS Publications Warehouse

    Lamar, William L.; Goerlitz, D.F.

    1966-01-01

    Most of the organic matter in naturally colored surface waters consists of a mixture of carboxylic acids or salts of these acids. Many of the acids color the water yellow to brown; however, not all of the acids are colored. These acids range from simple to complex, but predominantly they are nonvolatile polymeric carboxylic acids. The organic acids were recovered from the water by two techniques: continuous liquid-liquid extraction with n-butanol and vacuum evaporation at 50?C (centigrade). The isolated acids were studied by techniques of gas, paper, and column chromatography and infrared spectroscopy. About 10 percent of the acids recovered were volatile or could be made volatile for gas chromatographic analysis. Approximately 30 of these carboxylic acids were isolated, and 13 of them were individually identified. The predominant part of the total acids could not be made volatile for gas chromatographic analysis. Infrared examination of many column chromatographic fractions indicated that these nonvolatile substances are primarily polymeric hydroxy carboxylic acids having aromatic and olefinic unsaturation. The evidence suggests that some of these acids result from polymerization in aqueous solution. Elemental analysis of the sodium fusion products disclosed the absence of nitrogen, sulfur, and halogens.

  17. Effect of acid etching on marginal adaptation of mineral trioxide aggregate to apical dentin: microcomputed tomography and scanning electron microscopy analysis.

    PubMed

    Al-Fouzan, Khalid; Al-Garawi, Ziad; Al-Hezaimi, Khalid; Javed, Fawad; Al-Shalan, Thakib; Rotstein, Ilan

    2012-12-01

    The present investigation assessed the effect of acid etching on marginal adaptation of white- and gray-colored mineral trioxide aggregate (MTA) to apical dentin using microcomputed tomography (micro-CT) and scanning electron microscopy (SEM). Sixty-four extracted single-rooted human maxillary teeth were used. Following root-end resection and apical preparation, the teeth were equally divided into four groups according to the following root end filling materials: (i) white-colored MTA (WMTA), (ii) etched WMTA (EWMTA), (iii) gray-colored MTA (GMTA) and (iv) etched GMTA (EGMTA). After 48 h, the interface between root-end filling materials and the dentinal walls was assessed using micro-CT and SEM. Data were statistically analyzed using the Kruskal-Wallis and Dunn tests. Micro-CT analysis revealed gap volumes between the apical cavity dentin walls and EGMTA, GMTA, EWMTA and WMTA of (0.007 1±0.004) mm(3), (0.053±0.002) mm(3), (0.003 6±0.001) mm(3) and (0.005 9±0.002) mm(3) respectively. SEM analysis revealed gap sizes for EGMTA, WMTA, EWMTA and GMTA to be (492.3±13.8) µm, (594.5±17.12) µm, (543.1±15.33) µm and (910.7±26.2) µm respectively. A significant difference in gap size between root end preparations filled with GMTA and EGMTA was found (P<0.05). No significance difference in gap size between WMTA and EWMTA were found in either SEM or micro-CT analysis. In conclusion, pre-etching of apical dentin can provide a better seal for GMTA but not for WMTA. PMID:23306857

  18. 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

  19. 24% Indigenously Prepared Ethylene Diamine Tetra Acetic Acid Compared to Self-Etching Adhesives and their Effect on Shear Bond Strength of Composites in Primary Teeth: An In-vitro Study

    PubMed Central

    Nagar, Priya; Tandil, Yogesh L.; T.P., Chandru; Gupta, Anamika; Kalaria, Devendra; Kumar, Prafful

    2015-01-01

    Background: Over the years, it has been known that 34% phosphoric acid is the benchmark in etchants with the best shear bond strength shown with composites in primary teeth. However, with latest technological advancements and innovations, in order to reduce the number of steps and less damage to the tooth structure, non-rinse conditioner (NRC) & Single-Etch and various other etchants have been tried and tested. These etchants have been found to have shear bond strength comparable to phosphoric acid. In this study, indigenously prepared 24% ethylenediaminetetraacetic acid (EDTA) has been compared with established etchants, as to prove if their shear bond strength was closely related. As it is a well-known fact that EDTA could be less damaging to the enamel during etching and hence can be an alternative for etching of primary teeth. Materials and Methods: For the study 60 caries-free primary molars were used, they were sectioned in the middle, after making area for bonding; the marked area was then etched using different etchants for 30 s. Each of the teeth was then rinsed and bonded with composite resin and thermocycling was done. Shear bond strength testing was done on the composite using Universal Testing Machine. Results: Results of the study showed that phosphoric acid showed the highest bond strength, closely followed by Single Etch (Adper Prompt) and NRC, then by EDTA. Conclusions: About 24% EDTA can be another comparable replacement for phosphoric acid if used with a Single Etch Primer, like Prime and Bond NT on primary teeth. 34% phosphoric acid has the highest bond strength values with composite resin. Single etch followed by NRC has the second and third highest bond strength values, which are comparable to phosphoric acid. PMID:26464540

  20. Surface pH and bond strength of a self-etching primer/adhesive system to intracoronal dentin after application of hydrogen peroxide bleach with sodium perborate.

    PubMed

    Elkhatib, Hanadi; Nakajima, Masatoshi; Hiraishi, Noriko; Kitasako, Yuichi; Tagami, Junji; Nomura, Satoshi

    2003-01-01

    This study compared the dentin bond strength of a self-etching primer/adhesive system with dentin surface pH with or without bleaching and observed the morphological changes in bleached dentin treated with a self-etching primer. Dentin disks were prepared from the coronal-labial region of 32 human anterior teeth. The pulpal surfaces of the dentin disks were polished with 600-grit SiC paper under running water. The dentin surfaces on all specimens were bleached with a mixture of 30% hydrogen peroxide and sodium perborate in 100% humidity at 37 degrees C for one week. The bleaching agent was then rinsed off with water for 5, 15 or 30 seconds. All specimens were stored in water at 37 degrees C. Half of the five-second rinsing specimens were stored in water for an additional week. Dentin surface pH with or without bleaching was examined using a pH-imaging microscope (SCHEM-100). A self-etching primer/adhesive system (Clearfil SE Bond) was applied to bleached or unbleached dentin according to the manufacturer's instructions. After 24-hour water storage, the bonded specimens were prepared for microtensile testing. Microtensile bond strength (microTBS) to dentin was measured using a universal-testing machine (EZ test, Shimadzu, Japan) at a crosshead speed of 1.0 mm/minute. Data were analyzed by one-way ANOVA and Scheffe's test (alpha=0.05). The pH values of the dentin surfaces of the 5 and 15 second rinsing groups were significantly higher than the control group (p<0.05), while the 30-second rinsing and one-week water storage groups had similar surface pH values to the control group (p<0.05). The microTBS of 5, 15 and 30 second rinsing specimens after bleaching were significantly lower than the control specimens (p<0.05). However, after one-week of water storage, the microTBS returned to the control group. The application of a bleaching agent increased the pH value of the dentin surface and decreased the bond strength of the self-etching primer/adhesive system. One

  1. Post-Synthetic Anisotropic Wet-Chemical Etching of Colloidal Sodalite ZIF Crystals.

    PubMed

    Avci, Civan; Ariñez-Soriano, Javier; Carné-Sánchez, Arnau; Guillerm, Vincent; Carbonell, Carlos; Imaz, Inhar; Maspoch, Daniel

    2015-11-23

    Controlling the shape of metal-organic framework (MOF) crystals is important for understanding their crystallization and useful for myriad applications. However, despite the many advances in shaping of inorganic nanoparticles, post-synthetic shape control of MOFs and, in general, molecular crystals remains embryonic. Herein, we report using a simple wet-chemistry process at room temperature to control the anisotropic etching of colloidal ZIF-8 and ZIF-67 crystals. Our work enables uniform reshaping of these porous materials into unprecedented morphologies, including cubic and tetrahedral crystals, and even hollow boxes, by an acid-base reaction and subsequent sequestration of leached metal ions. Etching tests on these ZIFs reveal that etching occurs preferentially in the crystallographic directions richer in metal-ligand bonds; that, along these directions, the etching rate tends to be faster on the crystal surfaces of higher dimensionality; and that the etching can be modulated by adjusting the pH of the etchant solution.

  2. Biomimetic Deposition of Hydroxyapatite by Mixed Acid Treatment of Titanium Surfaces.

    PubMed

    Zhao, J M; Park, W U; Hwang, K H; Lee, J K; Yoon, S Y

    2015-03-01

    A simple chemical method was established for inducing bioactivity of Ti metal. In the present study, two kinds of mixed acid solutions were used to treat Ti specimens to induce Ca-P formation. Following a strong mixed acid activation process, Ca-P coatings successfully formed on the Ti surfaces in the simulated body fluid. Strong mixed acid etching was used to increase the roughness of the metal surface, because the porous and rough surfaces allow better adhesion between Ca-P coatings and substrate. Nano-scale modification of titanium surfaces can alter cellular and tissue responses, which may benefit osseointegration and dental implant therapy. Some specimens were treated with a 5 M NaOH aqueous solution, and then heat treated at 600 °C in order to form an amorphous sodium titanate layer on their surface. This treated titanium metal is believed to form a dense and uniform bone-like apatite layer on its surface in a simulated body fluid (SBF). This study proved that mixed acid treatment is not only important for surface passivation but is also another bioactive treatment for titanium surfaces, an alternative to alkali treatment. In addition, mixed acid treatment uses a lower temperature and shorter time period than alkali treatment.

  3. Biomimetic Deposition of Hydroxyapatite by Mixed Acid Treatment of Titanium Surfaces.

    PubMed

    Zhao, J M; Park, W U; Hwang, K H; Lee, J K; Yoon, S Y

    2015-03-01

    A simple chemical method was established for inducing bioactivity of Ti metal. In the present study, two kinds of mixed acid solutions were used to treat Ti specimens to induce Ca-P formation. Following a strong mixed acid activation process, Ca-P coatings successfully formed on the Ti surfaces in the simulated body fluid. Strong mixed acid etching was used to increase the roughness of the metal surface, because the porous and rough surfaces allow better adhesion between Ca-P coatings and substrate. Nano-scale modification of titanium surfaces can alter cellular and tissue responses, which may benefit osseointegration and dental implant therapy. Some specimens were treated with a 5 M NaOH aqueous solution, and then heat treated at 600 °C in order to form an amorphous sodium titanate layer on their surface. This treated titanium metal is believed to form a dense and uniform bone-like apatite layer on its surface in a simulated body fluid (SBF). This study proved that mixed acid treatment is not only important for surface passivation but is also another bioactive treatment for titanium surfaces, an alternative to alkali treatment. In addition, mixed acid treatment uses a lower temperature and shorter time period than alkali treatment. PMID:26413704

  4. Laser-driven fusion etching process

    DOEpatents

    Ashby, C.I.H.; Brannon, P.J.; Gerardo, J.B.

    1987-08-25

    The surfaces of solids are etched by a radiation-driven chemical reaction. The process involves exposing a substrate coated with a layer of a reactant material on its surface to radiation, e.g., a laser, to induce localized melting of the substrate which results in the occurrence of a fusion reaction between the substrate and coating material. The resultant reaction product and excess reactant salt are then removed from the surface of the substrate with a solvent which is relatively inert towards the substrate. The laser-driven chemical etching process is especially suitable for etching ionic substrates, e.g., LiNbO/sub 3/, such as used in electro-optical/acousto-optic devices. It is also suitable for applications wherein the etching process is required to produce an etched ionic substrate having a smooth surface morphology or when a very rapid etching rate is desired.

  5. Laser-driven fusion etching process

    DOEpatents

    Ashby, Carol I. H.; Brannon, Paul J.; Gerardo, James B.

    1989-01-01

    The surfaces of solid ionic substrates are etched by a radiation-driven chemical reaction. The process involves exposing an ionic substrate coated with a layer of a reactant material on its surface to radiation, e.g. a laser, to induce localized melting of the substrate which results in the occurrance of a fusion reaction between the substrate and coating material. The resultant reaction product and excess reactant salt are then removed from the surface of the substrate with a solvent which is relatively inert towards the substrate. The laser-driven chemical etching process is especially suitable for etching ionic salt substrates, e.g., a solid inorganic salt such as LiNbO.sub.3, such as used in electro-optical/acousto-optic devices. It is also suitable for applications wherein the etching process is required to produce an etched ionic substrate having a smooth surface morphology or when a very rapid etching rate is desired.

  6. Acid drainage response to surface limestone layers

    SciTech Connect

    Geidel, G.; Caruccio, F.T.

    1982-12-01

    A 150 acre drainage basin in an unreclaimed coal strip mine in east-central Ohio was studied and extensively monitored to determine the effect of a surface application of limestone on the ground water quality. Prior to the limestone treatment the ground and surface water of the basin was acidic due to pyrite oxidation in the spoil. In order to assess the effect of the limestone application the basin was divided into seven sub-basins, five of which were treated and two which served as controls. The seeps from the treated sub-basins with low acid concentrations became alkaline due to neutralization but after a long dry period, they returned to their acid condition. The moderately and highly acidic seeps showed a decline in the acid concentrations which could be attributed to a combination of neutralization and a decrease in the rate of pyrite oxidation. The results of this field study and simultaneous laboratory experiments showed that under natural conditions, with no limestone application, the acidity generated by pyrite oxidation in a backfill decreased. A surface application of limestone slightly enhanced the decrease in acidity by both neutralization and decreasing the rate of pyrite oxidation. However, the limestone application did not provide sufficient alkalinity to produce either neutral or alkaline discharges from the abandoned coal strip mine site.

  7. Self-Induced Surface Texturing of AL2O3 by Means of Inductively Coupled Plasma Reactive Ion Etching in CL2 Chemistry

    NASA Astrophysics Data System (ADS)

    Batoni, Paolo; Stokes, Edward B.; Shah, Trushant K.; Hodge, Michael D.; Suleski, Thomas J.

    2007-06-01

    In this work we investigate a pseudo-random surface texturing technique of sapphire by means of inductively coupled plasma reacting ion etching in chlorine chemistry, for which no sophisticated lithographic process is required. Such a surface texturing technique, which we believe offers indicative promise for enhanced light extraction in deep ultraviolet light-emitting diodes has allowed us to texture sapphire samples having a surface larger than 1 cm2 with controlled structures. Fabrication parameters have been characterized, and textured Al2O3 surfaces having submicron features, and nano-scale periodicity have been obtained. Performance, and characterization of our textured Al2O3 surfaces is the hinge of addition work in progress.

  8. Fabrication of IR-transparent microfluidic devices by anisotropic etching of channels in CaF2.

    PubMed

    Lehmkuhl, Brynson; Noblitt, Scott D; Krummel, Amber T; Henry, Charles S

    2015-11-21

    A simple fabrication method for generating infrared (IR) transparent microfluidic devices using etched CaF2 is demonstrated. To etch microfluidic channels, a poly(dimethylsiloxane) (PDMS) microfluidic device was reversibly sealed on a CaF2 plate and acid was pumped through the channel network to perform anisotropic etching of the underlying CaF2 surface. To complete the CaF2 microfluidic device, another CaF2 plate was sealed over the etched channel using a 700 nm thick layer of PDMS adhesive. The impact of different acids and their concentrations on etching was studied, with HNO3 giving the best results in terms of channel roughness and etch rates. Etch rate was determined at etching times ranging from 4-48 hours and showed a linear correlation with etching time. The IR transparency of the CaF2 device was established using a Fourier Transform IR microscope and showed that the device could be used in the mid-IR region. Finally, utility of the device was demonstrated by following the reaction of N-methylacetamide and D2O, which results in an amide peak shift to 1625 cm(-1) from 1650 cm(-1), using an FTIR microscope. PMID:26450455

  9. Alignment nature of ZnO nanowires grown on polished and nanoscale etched lithium niobate surface through self-seeding thermal evaporation method

    SciTech Connect

    Mohanan, Ajay Achath; Parthiban, R.; Ramakrishnan, N.

    2015-08-15

    Highlights: • ZnO nanowires were grown directly on LiNbO{sub 3} surface for the first time by thermal evaporation. • Self-alignment of the nanowires due to step bunching of LiNbO{sub 3} surface is observed. • Increased roughness in surface defects promoted well-aligned growth of nanowires. • Well-aligned growth was then replicated in 50 nm deep trenches on the surface. • Study opens novel pathway for patterned growth of ZnO nanowires on LiNbO{sub 3} surface. - Abstract: High aspect ratio catalyst-free ZnO nanowires were directly synthesized on lithium niobate substrate for the first time through thermal evaporation method without the use of a buffer layer or the conventional pre-deposited ZnO seed layer. As-grown ZnO nanowires exhibited a crisscross aligned growth pattern due to step bunching of the polished lithium niobate surface during the nanowire growth process. On the contrary, scratches on the surface and edges of the substrate produced well-aligned ZnO nanowires in these defect regions due to high surface roughness. Thus, the crisscross aligned nature of high aspect ratio nanowire growth on the lithium niobate surface can be changed to well-aligned growth through controlled etching of the surface, which is further verified through reactive-ion etching of lithium niobate. The investigations and discussion in the present work will provide novel pathway for self-seeded patterned growth of well-aligned ZnO nanowires on lithium niobate based micro devices.

  10. Orientation-dependent nanostructure arrays based on anisotropic silicon wet-etching for repeatable surface-enhanced Raman scattering

    NASA Astrophysics Data System (ADS)

    Wang, C. G.; Wu, X. Z.; di, D.; Dong, P. T.; Xiao, R.; Wang, S. Q.

    2016-02-01

    Repeatable fabrication of sensitive plasmonic substrates through a simple procedure has become a major challenge for SERS-based sensing and imaging. Herein, a new class of high-performance SERS substrates, including pyramid, ridged-hexagon, and quasi-triangle nanostructures, is successfully fabricated based on the nanosphere lithography technique and anisotropic wet etching. Using the wafer-scale Cr-hole array as the etching mask, cavity-templates of various configurations are fabricated by the orientation-dependent wet etching technique, from where the nanostructure arrays are finally peeled-off. The anisotropic wet etching on (100), (110), and (111) silicon wafers has been systematically studied at the nanoscale revealing the formation mechanism of these cavity-templates. The peeled-off nanostructure arrays provide high-density tips and/or gaps (about 2.5 × 107 mm-2) and thus facilitate the generation of ``hot spots''. The distribution of the electromagnetic field is visualized by the finite difference time domain calculation. And the calculation results are validated by SERS characterization. The SERS enhancement factors of these substrates are in the order of 106-107, with the maximum enhancement factor of 1.32 × 107 yielded by the ridged-hexagon arrays. The proposed nanostructure arrays present excellent homogeneity and reproducibility (with the largest relative standard deviation of 16.43%) for the reason that the SERS-active substrates are peeled-off from an identical template. The cost-effective fabrication, high sensitivity, good homogeneity and well-performed reproducibility demonstrate that these orientation-dependent NSs are good candidates for SERS-based in vitro and in situ detection and biosensing.Repeatable fabrication of sensitive plasmonic substrates through a simple procedure has become a major challenge for SERS-based sensing and imaging. Herein, a new class of high-performance SERS substrates, including pyramid, ridged-hexagon, and quasi

  11. Orientation-dependent nanostructure arrays based on anisotropic silicon wet-etching for repeatable surface-enhanced Raman scattering.

    PubMed

    Wang, C G; Wu, X Z; Di, D; Dong, P T; Xiao, R; Wang, S Q

    2016-02-28

    Repeatable fabrication of sensitive plasmonic substrates through a simple procedure has become a major challenge for SERS-based sensing and imaging. Herein, a new class of high-performance SERS substrates, including pyramid, ridged-hexagon, and quasi-triangle nanostructures, is successfully fabricated based on the nanosphere lithography technique and anisotropic wet etching. Using the wafer-scale Cr-hole array as the etching mask, cavity-templates of various configurations are fabricated by the orientation-dependent wet etching technique, from where the nanostructure arrays are finally peeled-off. The anisotropic wet etching on (100), (110), and (111) silicon wafers has been systematically studied at the nanoscale revealing the formation mechanism of these cavity-templates. The peeled-off nanostructure arrays provide high-density tips and/or gaps (about 2.5 × 10(7) mm(-2)) and thus facilitate the generation of "hot spots". The distribution of the electromagnetic field is visualized by the finite difference time domain calculation. And the calculation results are validated by SERS characterization. The SERS enhancement factors of these substrates are in the order of 10(6)-10(7), with the maximum enhancement factor of 1.32 × 10(7) yielded by the ridged-hexagon arrays. The proposed nanostructure arrays present excellent homogeneity and reproducibility (with the largest relative standard deviation of 16.43%) for the reason that the SERS-active substrates are peeled-off from an identical template. The cost-effective fabrication, high sensitivity, good homogeneity and well-performed reproducibility demonstrate that these orientation-dependent NSs are good candidates for SERS-based in vitro and in situ detection and biosensing. PMID:26853057

  12. Ethylene Diamine Tetraacetic Acid Etched Quantum Dots as a "Turn-On" Fluorescence Probe for Detection of Trace Zinc in Food.

    PubMed

    Liu, Wei; Wei, Fangdi; Xu, Guanhong; Wu, Yanzi; Hu, Chunting; Song, Quan; Yang, Jing; Hu, Qin

    2016-06-01

    In the present paper, a simple and rapid "turn-on" fluorescence sensor for Zn2+ based on ethylene diamine tetraacetic acid (EDTA) etched CdTe quantum dots (QDs) was developed. First, the initial bright fluorescence of mercaptopropionic acid (MPA) capped CdTe QDs was effectively quenched by EDTA, and then the presence of Zn2+ could "turn on" the weak fluorescence of QDs quenched by EDTA due to the formation of ZnS passivation shell. The increase of fluorescence intensity of EDTA etched QDs was found to be linear with the concentration of Zn2+ added. Under the optimum conditions, the calibration curve of this method showed good linearity in the concentration range of 9.1-1 09.1 μM of Zn2+ with the correlation coefficient R2 = 0.998. The limit of detection (3σ/K) was 2 μM. The developed QDs-based sensor was successfully applied to detect trace zinc in zinc fortified table salts and energy drinks with satisfactory results. PMID:27427745

  13. Surface etching mechanism of carbon-doped Ge2Sb2Te5 phase change material in fluorocarbon plasma

    NASA Astrophysics Data System (ADS)

    Shen, Lanlan; Song, Sannian; Song, Zhitang; Li, Le; Guo, Tianqi; Cheng, Yan; Lv, Shilong; Wu, Liangcai; Liu, Bo; Feng, Songlin

    2016-09-01

    Recently, carbon-doped Ge2Sb2Te5 (CGST) phase change material has been widely researched for being highly promising material for future phase change memory application. In this paper, the reactive-ion etching of CGST film in CF4/Ar plasma is studied. Compared with GST, the etch rate of CGST is relatively lower due to the existence of carbon which reduce the concentration of F or CF x reactive radicals. It was found that Argon plays an important role in defining the sidewall edge acuity. Compared with GST, more physical bombardment is required to obtain vertical sidewall of CGST. The effect of fluorocarbon gas on the damage of the etched CGST film was also investigated. A Ge- and Sb-deficient layer with tens of nanometers was observed by TEM combining with XPS analysis. The reaction between fluorocarbon plasma and CGST is mainly dominated by the diffusion and consumption of reactive fluorine radicals through the fluorocarbon layer into the CGST substrate material. The formation of damage layer is mainly caused by strong chemical reactivity, low volatility of reaction compounds and weak ion bombardment.

  14. Etching of glass microchips with supercritical water.

    PubMed

    Karásek, Pavel; Grym, Jakub; Roth, Michal; Planeta, Josef; Foret, František

    2015-01-01

    A novel method of etching channels in glass microchips with the most tunable solvent, water, was tested as an alternative to common hydrogen fluoride-containing etchants. The etching properties of water strongly depend on temperature and pressure, especially in the vicinity of the water critical point. The chips were etched at the subcritical, supercritical and critical temperature of water, and the resulting channel shape, width, depth and surface morphology were studied by scanning electron microscopy and 3D laser profilometry. Channels etched with the hot water were compared with the chips etched with standard hydrogen fluoride-containing solution. Depending on the water pressure and temperature, the silicate dissolved from the glass could be re-deposited on the channel surface. This interesting phenomenon is described together with the conditions necessary for its utilization. The results illustrate the versatility of pure water as a glass etching and surface morphing agent.

  15. In-Plasma Photo-Assisted Etching

    NASA Astrophysics Data System (ADS)

    Economou, Demetre

    2015-09-01

    A methodology to precisely control the ion energy distribution (IED) on a substrate allowed the study of silicon etching as a function of ion energy at near-threshold energies. Surprisingly, a substantial etching rate was observed, independent of ion energy, when the ion energy was below the ion-assisted etching threshold (~ 16 eV for etching silicon with chlorine plasma). Careful experiments led to the conclusion that this ``sub-threshold'' etching was due to photons, predominately at wavelengths <1700 Å. Among the plasmas investigated, photo-assisted etching (PAE) was lowest in Br2/Ar gas mixtures and highest in HBr/Cl2/Ar. Above threshold etching rates scaled with the square root of ion energy. PAE rates scaled with the product of surface halogen coverage (measured by X-ray photoelectron spectroscopy) and Ar emission intensity (7504 Å). Scanning electron and atomic force microscopy (SEM and AFM) revealed that photo-etched surfaces were very rough, quite likely due to the inability of the photo-assisted process to remove contaminants from the surface. In-plasma PAE may be be a complicating factor for processes that require low ion energies, such as atomic layer etching. On the other hand PAE could produce sub-10 nm high aspect ratio (6:1) features by highly selective plasma etching to transfer nascent nanopatterns in silicon. Work supported by DOE Plasma Science Center and NSF.

  16. Fabrication of ultra-high aspect ratio silicon nanopores by electrochemical etching

    SciTech Connect

    Schmidt, Torsten; Zhang, Miao; Linnros, Jan; Yu, Shun

    2014-09-22

    We report on the formation of ultra-high aspect ratio nanopores in silicon bulk material using photo-assisted electrochemical etching. Here, n-type silicon is used as anode in contact with hydrofluoric acid. Based on the local dissolution of surface atoms in pre-defined etching pits, pore growth and pore diameter are, respectively, driven and controlled by the supply of minority charge carriers generated by backside illumination. Thus, arrays with sub-100 nm wide pores were fabricated. Similar to macropore etching, it was found that the pore diameter is proportional to the etching current, i.e., smaller etching currents result in smaller pore diameters. To find the limits under which nanopores with controllable diameter still can be obtained, etching was performed at very low current densities (several μA cm{sup −2}). By local etching, straight nanopores with aspect ratios above 1000 (∼19 μm deep and ∼15 nm pore tip diameter) were achieved. However, inherent to the formation of such narrow pores is a radius of curvature of a few nanometers at the pore tip, which favors electrical breakdown resulting in rough pore wall morphologies. Lowering the applied bias is adequate to reduce spiking pores but in most cases also causes etch stop. Our findings on bulk silicon provide a realistic chance towards sub-10 nm pore arrays on silicon membranes, which are of great interest for molecular filtering and possibly DNA sequencing.

  17. Silver ion mediated shape control of platinum nanoparticles: Removal of silver by selective etching leads to increased catalytic activity

    SciTech Connect

    Grass, Michael E.; Yue, Yao; Habas, Susan E.; Rioux, Robert M.; Teall, Chelsea I.; Somorjai, G.A.

    2008-01-09

    A procedure has been developed for the selective etching of Ag from Pt nanoparticles of well-defined shape, resulting in the formation of elementally-pure Pt cubes, cuboctahedra, or octahedra, with a largest vertex-to-vertex distance of {approx}9.5 nm from Ag-modified Pt nanoparticles. A nitric acid etching process was applied Pt nanoparticles supported on mesoporous silica, as well as nanoparticles dispersed in aqueous solution. The characterization of the silica-supported particles by XRD, TEM, and N{sub 2} adsorption measurements demonstrated that the structure of the nanoparticles and the mesoporous support remained conserved during etching in concentrated nitric acid. Both elemental analysis and ethylene hydrogenation indicated etching of Ag is only effective when [HNO{sub 3}] {ge} 7 M; below this concentration, the removal of Ag is only {approx}10%. Ethylene hydrogenation activity increased by four orders of magnitude after the etching of Pt octahedra that contained the highest fraction of silver. High-resolution transmission electron microscopy of the unsupported particles after etching demonstrated that etching does not alter the surface structure of the Pt nanoparticles. High [HNO{sub 3}] led to the decomposition of the capping agent, polyvinylpyrollidone (PVP); infrared spectroscopy confirmed that many decomposition products were present on the surface during etching, including carbon monoxide.

  18. 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.

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

    DOEpatents

    Kampwirth, Robert T.; Schuller, Ivan K.; Falco, Charles M.

    1981-01-01

    An improved method of preparing thin film superconducting electrical circuits of niobium or niobium compounds 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.

  20. Chemical etching and EDAX analysis of beryllium-free nickel-chromium ceramo-metal alloy.

    PubMed

    Atta, O M; Mosleh, I E; Shehata, M T

    1995-10-01

    A chemical etching technique is described for producing etch patterns in beryllium-free nickel chromium ceramo-metal alloy. Disc-shaped samples were chemically etched, evaluated with SEM and analysed by the EDAX technique. Scanning electron micrographs revealed, profound retentive cavities. The EDAX analysis provided a comprehensive interpretation of the etch mechanism. The obtained results show that the developed chemical etching has the potential to produce a highly retentive etched surface with less problematic and less technique sensitive than electrolytic etching.

  1. Nucleic acid interactions with pyrite surfaces

    NASA Astrophysics Data System (ADS)

    Mateo-Martí, E.; Briones, C.; Rogero, C.; Gomez-Navarro, C.; Methivier, Ch.; Pradier, C. M.; Martín-Gago, J. A.

    2008-09-01

    The study of the interaction of nucleic acid molecules with mineral surfaces is a field of growing interest in organic chemistry, origin of life, material science and biotechnology. We have characterized the adsorption of single-stranded peptide nucleic acid (ssPNA) on a natural pyrite surface, as well as the further adsorption of ssDNA on a PNA-modified pyrite surface. The characterization has been performed by means of reflection absorption infrared spectroscopy (RAIRS), atomic force microscopy (AFM) and X-ray photoemission spectroscopy (XPS) techniques. The N(1s) and S(2p) XPS core level peaks of PNA and PNA + DNA have been decomposed in curve-components that we have assigned to different chemical species. RAIRS spectra recorded for different concentrations show the presence of positive and negative adsorption bands, related to the semiconducting nature of the surface. The combination of the information gathered by these techniques confirms that PNA adsorbs on pyrite surface, interacting through nitrogen-containing groups of the nucleobases and the iron atoms of the surface, instead of the thiol group of the molecule. The strong PNA/pyrite interaction inhibits further hybridization of PNA with complementary ssDNA, contrary to the behavior reported on gold surfaces.

  2. Dry etching of metallization

    NASA Technical Reports Server (NTRS)

    Bollinger, D.

    1983-01-01

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

  3. Role of surface-reaction layer in HBr/fluorocarbon-based plasma with nitrogen addition formed by high-aspect-ratio etching of polycrystalline silicon and SiO2 stacks

    NASA Astrophysics Data System (ADS)

    Iwase, Taku; Matsui, Miyako; Yokogawa, Kenetsu; Arase, Takao; Mori, Masahito

    2016-06-01

    The etching of polycrystalline silicon (poly-Si)/SiO2 stacks by using VHF plasma was studied for three-dimensional NAND fabrication. One critical goal is achieving both a vertical profile and high throughput for multiple-stack etching. While the conventional process consists of multiple steps for each stacked layer, in this study, HBr/fluorocarbon-based gas chemistry was investigated to achieve a single-step etching process to reduce process time. By analyzing the dependence on wafer temperature, we improved both the etching profile and rate at a low temperature. The etching mechanism is examined considering the composition of the surface reaction layer. X-ray photoelectron spectroscopy (XPS) analysis revealed that the adsorption of N–H and Br was enhanced at a low temperature, resulting in a reduced carbon-based-polymer thickness and enhanced Si etching. Finally, a vertical profile was obtained as a result of the formation of a thin and reactive surface-reaction layer at a low wafer temperature.

  4. 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.

  5. 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.

  6. Deliberate modification of the behavior of n-type cadium telluride/electrolyte interfaces by surface etching: Removal of fermi level pinning

    NASA Astrophysics Data System (ADS)

    Tanaka, S.; Bruce, J. A.; Wrighton, M. S.

    1981-09-01

    Single crystal, n-type CdTe (E sub g = 1.4 eV) has been studied with respect to barrier height, E sub B, when contacting a liquid electrolyte solution containing a fast, one-electron, outer-sphere redox reagent. We approximate E sub B as equal to the photovoltage measured by cyclic voltammetry of various redox couples at illuminated n-CdTe vs. a reversible electrode. N-CdTe surfaces pretreated with an oxidizing etch give an E sub B of approximately 0.5 V + or - 0.1 V in H2O/0.1 M NaClO4 or CH3CN/0.1 M (n-Bu4N)ClO4 that is independent of the E sub 1/2 of the added redox couple. A reducing etch pretreatment gives an E sub B in either of the electrolyte solutions that depends on E sub 1/2 of the redox couple in a manner consistent with a nearly ideal semiconductor. The reduced CdTe exhibits an E sub B of up to 0.9 V for a redox couple having E sub 1/2 near 0.0V vs. SCE, whereas couples having E sub 1/2 negative of approx. -1.0 V vs. SCE give zero photovoltage. Auger and X-ray photoelectron spectroscopy of the reduced and oxidized surfaces are qualitatively different. The reduced surface exhibits signals for Cd and Te in relative intensities that are consistent with a close to stoichiometric (1/1) surface. The oxidized surface exhibits little or no detectable Cd signal and the Te signal is consistent with a thick overlayer of elemental Te.

  7. Bonding with self-etching primers--pumice or pre-etch? An in vitro study.

    PubMed

    Fitzgerald, Ian; Bradley, Gerard T; Bosio, Jose A; Hefti, Arthur F; Berzins, David W

    2012-04-01

    The purpose of this study was to compare the shear bond strengths (SBSs) of orthodontic brackets bonded with self-etching primer (SEP) using different enamel surface preparations. A two-by-two factorial study design was used. Sixty human premolars were harvested, cleaned, and randomly assigned to four groups (n = 15 per group). Teeth were bathed in saliva for 48 hours to form a pellicle. Treatments were assigned as follows: group 1 was pumiced for 10 seconds and pre-etched for 5 seconds with 37 per cent phosphoric acid before bonding with SEP (Transbond Plus). Group 2 was pumiced for 10 seconds before bonding. Group 3 was pre-etched for 5 seconds before bonding. Group 4 had no mechanical or chemical preparation before bonding. All teeth were stored in distilled water for 24 hours at 37°C before debonding. The SBS values and adhesive remnant index (ARI) score were recorded. The SBS values (± 1 SD) for groups 1-4 were 22.9 ± 6.6, 16.1 ± 7.3, 36.2 ± 8.2, and 13.1 ± 10.1 MPa, respectively. Two-way analysis of variance and subsequent contrasts showed statistically significant differences among treatment groups. ARI scores indicated the majority of adhesive remained on the bracket for all four groups. Pre-etching the bonding surface for 5 seconds with 37 per cent phosphoric acid, instead of pumicing, when using SEPs to bond orthodontic brackets, resulted in greater SBSs.

  8. 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). PMID:19363978

  9. Synergistic etch rates during low-energetic plasma etching of hydrogenated amorphous carbon

    SciTech Connect

    Hansen, T. A. R.; Weber, J. W.; Colsters, P. G. J.; Mestrom, D. M. H. G.; Sanden, M. C. M. van de; Engeln, R.

    2012-07-01

    The etch mechanisms of hydrogenated amorphous carbon thin films in low-energetic (<2 eV) high flux plasmas are investigated with spectroscopic ellipsometry. The results indicate a synergistic effect for the etch rate between argon ions and atomic hydrogen, even at these extremely low kinetic energies. Ion-assisted chemical sputtering is the primary etch mechanism in both Ar/H{sub 2} and pure H{sub 2} plasmas, although a contribution of swift chemical sputtering to the total etch rate is not excluded. Furthermore, ions determine to a large extent the surface morphology during plasma etching. A high influx of ions enhances the etch rate and limits the surface roughness, whereas a low ion flux promotes graphitization and leads to a large surface roughness (up to 60 nm).

  10. Etch Characteristics of GaN using Inductively Coupled Cl{sub 2} Plasma Etching

    SciTech Connect

    Rosli, Siti Azlina; Aziz, A. Abdul

    2008-05-20

    In this study, the plasma characteristics and GaN etch properties of inductively coupled Cl{sub 2}/Ar plasmas were investigated. It has shown that the results of a study of inductively coupled plasma (ICP) etching of gallium nitride by using Cl{sub 2}/Ar is possible to meet the requirement (anisotropy, high etch rate and high selectivity), simultaneously. We have investigated the etching rate dependency on the percentage of Argon in the gas mixture, the total pressure and DC voltage. We found that using a gas mixture with 20 sccm of Ar, the optimum etch rate of GaN was achieved. The etch rate were found to increase with voltage, attaining a maximum rate 2500 A/min at -557 V. The addition of an inert gas, Ar is found to barely affect the etch rate. Surface morphology of the etched samples was verified by scanning electron microscopy and atomic force microscopy. It was found that the etched surface was anisotropic and the smoothness of the etched surface is comparable to that of polished wafer.

  11. Damage to InP and InGaAsP surfaces resulting from CH4/H2 reactive ion etching

    NASA Astrophysics Data System (ADS)

    Hayes, Todd R.; Chakrabarti, U. K.; Baiocchi, F. A.; Emerson, A. B.; Luftman, H. S.; Dautremont-Smith, W. C.

    1990-07-01

    Structural and electrical damage imparted to InP and In0.72Ga0.28As0.6P0.4 (λg≂1.3 μm) surfaces during CH4/H2 reactive ion etching (RIE) have been examined. X-ray photoelectron spectroscopy was used to monitor changes in the surface chemistry, Rutherford backscattering spectrometry was used to measure crystallographic damage, and current-voltage and capacitance-voltage measurements were made to examine electrically active damage and its depth. Two classes of damage are observed: crystallographic damage originating from preferential loss of P (As) and/or ion bombardment-induced collision cascade mixing and, for p-type material, hydrogen passivation of Zn acceptors. Etching at 13.6 MHz, 60-90 mTorr, 10% CH4/H2, and bias voltages of ˜300 V contains gross (≳1%) damage as measured by RBS to within 40 Å and electrically active damage to within 200 Å of the surface. This is a factor of 3-6 shallower than other RIE processes operated below 10 mT with comparable or higher bias voltages. Acceptor passivation of both InP and InGaAsP, arising from the association of hydrogen with Zn sites, occurs to a depth of 2000 Å after RIE and causes a decrease in carrier concentration in this layer. The effect is reversed, however, by rapid thermal processing at temperatures between 350 and 500 °C.

  12. Tobacco etch virus infectivity in Capsicum spp. is determined by a maximum of three amino acids in the viral virulence determinant VPg.

    PubMed

    Perez, Kari; Yeam, Inhwa; Kang, Byoung-Cheorl; Ripoll, Daniel R; Kim, Jinhee; Murphy, John F; Jahn, Molly M

    2012-12-01

    Potyvirus resistance in Capsicum spp. has been attributed to amino acid substitutions at the pvr1 locus that cause conformational shifts in eukaryotic translation initiation factor eIF4E. The viral genome-linked protein (VPg) sequence was isolated and compared from three Tobacco etch virus (TEV) strains, highly aphid-transmissible (HAT), Mex21, and N, which differentially infect Capsicum genotypes encoding Pvr1(+), pvr1, and pvr1(2). Viral chimeras were synthesized using the TEV-HAT genome, replacing HAT VPg with Mex21 or N VPg. TEV HAT did not infect pepper plants homozygous for either the pvr1 or pvr1(2) allele. However, the novel chimeric TEV strains, TEVHAT(Mex21-VPg) and TEV-HAT(N-VPg), infected pvr1 and pvr1(2) pepper plants, respectively, demonstrating that VPg is the virulence determinant in this pathosystem. Three dimensional structural models predicted interaction between VPg and the susceptible eIF4E genotype in every case, while resistant genotypes were never predicted to interact. To determine whether there is a correlation between physical interaction of VPg with eIF4E and infectivity, the effects of amino acid variation within VPg were assessed. Interaction between pvr1(2) eIF4E and N VPg was detected in planta, implying that the six amino acid differences in N VPg relative to HAT VPg are responsible for restoring the physical interaction and infectivity.

  13. Ultradeep fused silica glass etching with an HF-resistant photosensitive resist for optical imaging applications

    NASA Astrophysics Data System (ADS)

    Nagarah, John M.; Wagenaar, Daniel A.

    2012-03-01

    Microfluidic and optical sensing platforms are commonly fabricated in glass and fused silica (quartz) because of their optical transparency and chemical inertness. Hydrofluoric acid (HF) solutions are the etching media of choice for deep etching into silicon dioxide substrates, but processing schemes become complicated and expensive for etching times greater than 1 h due to the aggressiveness of HF migration through most masking materials. We present here etching into fused silica more than 600 µm deep while keeping the substrate free of pits and maintaining a polished etched surface suitable for biological imaging. We utilize an HF-resistant photosensitive resist (HFPR) which is not attacked in 49% HF solution. Etching characteristics are compared for substrates masked with the HFPR alone and the HFPR patterned on top of Cr/Au and polysilicon masks. We used this etching process to fabricate suspended fused silica membranes, 8-16 µm thick, and show that imaging through the membranes does not negatively affect image quality of fluorescence microscopy of biological tissue. Finally, we realize small through-pore arrays in the suspended membranes. Such devices will have applications in planar electrophysiology platforms, especially where optical imaging is required.

  14. Acidic deposition and surface water chemistry

    NASA Astrophysics Data System (ADS)

    Church, M. R.

    A pair of back-to-back (morning and afternoon) hydrology sessions, held December 10, 1987, at the AGU Fall Meeting in San Francisco, Calif., covered “Predicting the Effects of Acidic Deposition on Surface Water Chemistry.” The combined sessions included four invited papers, 12 contributed papers, and a panel discussion at its conclusion. The gathering dealt with questions on a variety of aspects of modeling the effects of acidic deposition on surface water chemistry.Contributed papers included discussions on the representation of processes in models as well as limiting assumptions in model application (V. S. Tripathi et al., Oak Ridge National Laboratory, Oak Ridge, Tenn., and E. C. Krug, Illinois State Water Survey, Champaign), along with problems in estimating depositional inputs to catchments and thus inputs to be used in the simulation of catchment response (M. M. Reddy et al., U.S. Geological Survey, Lakewood, Colo.; and E. A. McBean, University of Waterloo, Waterloo, Canada). L. A. Baker et al. (University of Minnesota, Minneapolis) dealt with the problem of modeling seepage lake systems, an exceedingly important portion of the aquatic resources in Florida and parts of the upper U.S. Midwest. J. A. Hau and Y. Eckstein (Kent State University, Kent, Ohio) considered equilibrium modeling of two northern Ohio watersheds that receive very different loads of acidic deposition but are highly similar in other respects.

  15. Spinner For Etching Of Semiconductor Wafers

    NASA Technical Reports Server (NTRS)

    Lombardi, Frank

    1989-01-01

    Simple, inexpensive apparatus coats semiconductor wafers uniformly with hydrofluoric acid for etching. Apparatus made in part from small commercial electric-fan motor. Features bowl that collects acid. Silicon wafer placed on platform and centered on axis; motor switched on. As wafer spins, drops of hydrofluoric acid applied from syringe. Centrifugal force spreads acid across wafer in fairly uniform sheet.

  16. 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.

  17. Plasma Etching Improves Solar Cells

    NASA Technical Reports Server (NTRS)

    Bunyan, S. M.

    1982-01-01

    Etching front surfaces of screen-printed silicon photovoltaic cells with sulfur hexafluoride plasma found to increase cell performance while maintaining integrity of screen-printed silver contacts. Replacement of evaporated-metal contacts with screen-printed metal contacts proposed as one way to reduce cost of solar cells for terrestrial applications.

  18. Chemical etching of nitinol stents.

    PubMed

    Katona, Bálint; Bognár, Eszter; Berta, Balázs; Nagy, Péter; Hirschberg, Kristóf

    2013-01-01

    At present the main cause of death originates from cardiovascular diseases. Primarily the most frequent cause is vessel closing thus resulting in tissue damage. The stent can help to avoid this. It expands the narrowed vessel section and allows free blood flow. The good surface quality of stents is important. It also must have adequate mechanical characteristics or else it can be damaged which can easily lead to the fracture of the implant. Thus, we have to consider the importance of the surface treatment of these implants. In our experiments the appropriate design was cut from a 1.041 mm inner diameter and 0.100 mm wall thickness nitinol tube by using Nd:YAG laser device. Then, the stent was subjected to chemical etching. By doing so, the burr created during the laser cutting process can be removed and the surface quality refined. In our research, we changed the time of chemical etching and monitored the effects of this parameter. The differently etched stents were subjected to microscopic analysis, mass measurement and in vivo environment tests. The etching times that gave suitable surface and mechanical features were identified.

  19. Mechanisms of Hydrocarbon Based Polymer Etch

    NASA Astrophysics Data System (ADS)

    Lane, Barton; Ventzek, Peter; Matsukuma, Masaaki; Suzuki, Ayuta; Koshiishi, Akira

    2015-09-01

    Dry etch of hydrocarbon based polymers is important for semiconductor device manufacturing. The etch mechanisms for oxygen rich plasma etch of hydrocarbon based polymers has been studied but the mechanism for lean chemistries has received little attention. We report on an experimental and analytic study of the mechanism for etching of a hydrocarbon based polymer using an Ar/O2 chemistry in a single frequency 13.56 MHz test bed. The experimental study employs an analysis of transients from sequential oxidation and Ar sputtering steps using OES and surface analytics to constrain conceptual models for the etch mechanism. The conceptual model is consistent with observations from MD studies and surface analysis performed by Vegh et al. and Oehrlein et al. and other similar studies. Parameters of the model are fit using published data and the experimentally observed time scales.

  20. Comparison of acidulated phosphate fluoride gel and hydrofluoric acid etchants for porcelain-composite repair.

    PubMed

    Tylka, D F; Stewart, G P

    1994-08-01

    Hydrofluoric acid etches porcelain to produce a porous surface visible under scanning electron microscopy when compared to an acidulated phosphate fluoride gel. Some investigators have suggested the greater porosity of the hydrofluoric acid etch produces a greater composite-to-porcelain bond. This investigation tested that assumption with two common fluoride etchants. The etched surfaces were first viewed under scanning electron microscopy to ensure that a characteristic etch was achieved. Both etchants yielded bond strengths that produced cohesive failure of all samples. This suggested that the intraoral use of hydrofluoric acid is no more effective than the less dangerous acidulated phosphate fluoride gel.

  1. Alkaline etch system qualification

    SciTech Connect

    Goldammer, S.E.; Pemberton, S.E.; Tucker, D.R.

    1997-04-01

    Based on the data from this qualification activity, the Atotech etch system, even with minimum characterization, was capable of etching production printed circuit products as good as those from the Chemcut system. Further characterization of the Atotech system will improve its etching capability. In addition to the improved etch quality expected from further characterization, the Atotech etch system has additional features that help reduce waste and provide for better consistency in the etching process. The programmable logic controller and computer will allow operators to operate the system manually or from pre-established recipes. The evidence and capabilities of the Atotech system made it as good as or better than the Chemcut system for etching WR products. The Printed Wiring Board Engineering Department recommended that the Atotech system be released for production. In December 1995, the Atotech system was formerly qualified for production.

  2. Evaluation of a chemical etching solution for nickel-chromium-beryllium and chromium-cobalt alloys.

    PubMed

    Ferrari, M; Cagidiaco, M C; Borracchini, A; Bertelli, E

    1989-11-01

    Two chemical etching solutions were capable of providing micromechanical retention in two nickel-chromium-beryllium alloys and in a chromium-cobalt alloy. A resin matrix was used to verify the quality of etching on the metal surfaces. The chemical etching solutions created high microretentive surfaces in nickel-chromium-beryllium alloy but the chromium-cobalt alloy surfaces after etching were less retentive. Improved chemical etching technique should encourage expanded use of the resin-bonded retainers.

  3. LDRD final report : on the development of hybrid level-set/particle methods for modeling surface evolution during feature-scale etching and deposition processes.

    SciTech Connect

    McBride, Cory L.; Schmidt, Rodney Cannon; Musson, Lawrence Cale

    2005-01-01

    Two methods for creating a hybrid level-set (LS)/particle method for modeling surface evolution during feature-scale etching and deposition processes are developed and tested. The first method supplements the LS method by introducing Lagrangian marker points in regions of high curvature. Once both the particle set and the LS function are advanced in time, minimization of certain objective functions adjusts the LS function so that its zero contour is in closer alignment with the particle locations. It was found that the objective-minimization problem was unexpectedly difficult to solve, and even when a solution could be found, the acquisition of it proved more costly than simply expanding the basis set of the LS function. The second method explored is a novel explicit marker-particle method that we have named the grid point particle (GPP) approach. Although not a LS method, the GPP approach has strong procedural similarities to certain aspects of the LS approach. A key aspect of the method is a surface rediscretization procedure--applied at each time step and based on a global background mesh--that maintains a representation of the surface while naturally adding and subtracting surface discretization points as the surface evolves in time. This method was coded in 2-D, and tested on a variety of surface evolution problems by using it in the ChISELS computer code. Results shown for 2-D problems illustrate the effectiveness of the method and highlight some notable advantages in accuracy over the LS method. Generalizing the method to 3D is discussed but not implemented.

  4. Investigation and simulation of XeF2 isotropic etching of silicon

    NASA Astrophysics Data System (ADS)

    Bahreyni, Behraad; Shafai, C.

    2002-11-01

    Trenching and loading phenomena observed on XeF2-etched (100) silicon wafers are explained in this article. Trenching refers to deeper etching at the side of an etch feature with respect to the middle of the feature. Loading is the reduction in etch depth that adjacent etched regions impose on their respective etch profiles. These two phenomena are especially recognized at locations where the substrate is etched through large mask openings. Both phenomena were reported by other groups, but no explanation was given for them. A novel model explaining these phenomena is developed in this article, and the etching process is simulated in software. The results are compared to several etched samples with varying mask aperture size and etch depth. Good agreement is found between simulated profiles and actual measured etch profiles at given mean-free paths. Furthermore, our simulator predicts that the reaction probability between etchant and substrate molecules influences surface roughness of the etched regions.

  5. Carrier-lifetime-controlled selective etching process for semiconductors using photochemical etching

    DOEpatents

    Ashby, Carol I. H.; Myers, David R.

    1992-01-01

    The minority carrier lifetime is significantly much shorter in semiconductor materials with very high impurity concentrations than it is in semiconductor materials with lower impurity concentration levels. This phenomenon of reduced minority carrier lifetime in semiconductor materials having high impurity concentration is utilized to advantage for permitting highly selective semiconductor material etching to be achieved using a carrier-driven photochemical etching reaction. Various means may be employed for increasing the local impurity concentration level in specific near-surface regions of a semiconductor prior to subjecting the semiconductor material to a carrier-driven photochemical etching reaction. The regions having the localized increased impurity concentration form a self-aligned mask inhibiting photochemical etching at such localized regions while the adjacent regions not having increased impurity concentrations are selectively photochemically etched. Liquid- or gas-phase etching may be performed.

  6. Optimized condition for etching fused-silica phase gratings with inductively coupled plasma technology.

    PubMed

    Wang, Shunquan; Zhou, Changhe; Ru, Huayi; Zhang, Yanyan

    2005-07-20

    Polymer deposition is a serious problem associated with the etching of fused silica by use of inductively coupled plasma (ICP) technology, and it usually prevents further etching. We report an optimized etching condition under which no polymer deposition will occur for etching fused silica with ICP technology. Under the optimized etching condition, surfaces of the fabricated fused silica gratings are smooth and clean. Etch rate of fused silica is relatively high, and it demonstrates a linear relation between etched depth and working time. Results of the diffraction of gratings fabricated under the optimized etching condition match theoretical results well.

  7. Transferring resist microlenses into silicon by reactive ion etching

    NASA Astrophysics Data System (ADS)

    Eisner, Martin; Schwider, Johannes

    1996-10-01

    Reactive ion etching (RIE) is known as an effective technique for high precision anisotropic etching with a minimum loss of the critical dimensions provided by the photoresist or other masking materials. RIE can also be used to transfer continuous forms such as spherical resist microlenses into substrate materials (e.g., quartz glass or silicon). The form of the lenses can be considerably controlled by changing the etch rate ratio between resist and the substrate. This was achieved by varying the etch gas compound, especially the amount of oxygen, during the etching or by changing the applied power. Measured etch rates for silicon are given to demonstrate the possibilities of lens shaping. The surface roughness of the etched lenses was one of the main problems. The roughness could be minimized by adding helium to the etch gases for heat removal and by increasing the resist rinse time after the wet chemical development.

  8. 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.

  9. 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.

  10. Laser etching of enamel for direct bonding with an Er,Cr:YSGG hydrokinetic laser system.

    PubMed

    Uşümez, Serdar; Orhan, Metin; Uşümez, Aslihan

    2002-12-01

    Irradiation of enamel with laser energy changes the physical and chemical characteristics of the enamel surface, and these alterations hold promise for the conditioning of enamel for bonding procedures. This laboratory study examined the influence of laser irradiation of enamel at 2 different power settings with an erbium, chromium: yttrium, scandium, gallium, garnet (Er,Cr:YSGG) hydrokinetic laser system (Millennium System, Biolase Technology, Inc; San Clemente, Calif) on the shear bond strength of orthodontic appliances and compared these with that of acid-etching. The prepared surfaces of 40 noncarious, intact, extracted premolars were exposed to laser energy: 20 teeth at 2-W setting (5.6 J/cm(2)) and 20 teeth at 1-W setting (2.7 J/cm(2)) of the commercial laser unit. Twenty teeth were etched with 37% orthophosphoric acid. Brackets were bonded with an orthodontic no-mix adhesive, and shear bond strength was determined with a universal testing machine. Data were analyzed with Kruskal-Wallis and Mann-Whitney U tests. Etched and restored surfaces of an acid-etched tooth and a 2-W laser-irradiated tooth were examined with scanning electron microscopy (SEM). Laser treatment under 2 W resulted in bond strengths of 7.11 +/- 4.56 megapascals (MPa), which was not significantly different from that of acid etching (8.23 +/- 2.30 MPa). Laser irradiation at 1 W resulted in bond strengths of 5.64 +/- 3.19 MPa, which was significantly different from that of acid etching (P <.05). However, large SD and coefficient of variation values of both laser groups made reliability of this method as an enamel conditioner questionable. Scanning electron microscopy studies of the restored irradiated surfaces showed good surface characteristics, whereas the lased surface was still more irregular than the restored acid-etched sample. Although laser devices are effectively used in some other areas of dentistry, enamel conditioning with an Er,Cr:YSGG laser cannot be considered a successful

  11. Laser etching of enamel for direct bonding with an Er,Cr:YSGG hydrokinetic laser system.

    PubMed

    Uşümez, Serdar; Orhan, Metin; Uşümez, Aslihan

    2002-12-01

    Irradiation of enamel with laser energy changes the physical and chemical characteristics of the enamel surface, and these alterations hold promise for the conditioning of enamel for bonding procedures. This laboratory study examined the influence of laser irradiation of enamel at 2 different power settings with an erbium, chromium: yttrium, scandium, gallium, garnet (Er,Cr:YSGG) hydrokinetic laser system (Millennium System, Biolase Technology, Inc; San Clemente, Calif) on the shear bond strength of orthodontic appliances and compared these with that of acid-etching. The prepared surfaces of 40 noncarious, intact, extracted premolars were exposed to laser energy: 20 teeth at 2-W setting (5.6 J/cm(2)) and 20 teeth at 1-W setting (2.7 J/cm(2)) of the commercial laser unit. Twenty teeth were etched with 37% orthophosphoric acid. Brackets were bonded with an orthodontic no-mix adhesive, and shear bond strength was determined with a universal testing machine. Data were analyzed with Kruskal-Wallis and Mann-Whitney U tests. Etched and restored surfaces of an acid-etched tooth and a 2-W laser-irradiated tooth were examined with scanning electron microscopy (SEM). Laser treatment under 2 W resulted in bond strengths of 7.11 +/- 4.56 megapascals (MPa), which was not significantly different from that of acid etching (8.23 +/- 2.30 MPa). Laser irradiation at 1 W resulted in bond strengths of 5.64 +/- 3.19 MPa, which was significantly different from that of acid etching (P <.05). However, large SD and coefficient of variation values of both laser groups made reliability of this method as an enamel conditioner questionable. Scanning electron microscopy studies of the restored irradiated surfaces showed good surface characteristics, whereas the lased surface was still more irregular than the restored acid-etched sample. Although laser devices are effectively used in some other areas of dentistry, enamel conditioning with an Er,Cr:YSGG laser cannot be considered a successful

  12. Black Germanium fabricated by reactive ion etching

    NASA Astrophysics Data System (ADS)

    Steglich, Martin; Käsebier, Thomas; Kley, Ernst-Bernhard; Tünnermann, Andreas

    2016-09-01

    A reactive ion etching technique for the preparation of statistical "Black Germanium" antireflection surfaces, relying on self-organization in a Cl2 etch chemistry, is presented. The morphology of the fabricated Black Germanium surfaces is the result of a random lateral distribution of pyramidal etch pits with heights around (1450 ± 150) nm and sidewall angles between 80° and 85°. The pyramids' base edges are oriented along the <110> crystal directions of Germanium, indicating a crystal anisotropy of the etching process. In the Vis-NIR, the tapered Black Germanium surface structure suppresses interface reflection to <2.5 % for normal incidence and still to <6 % at an angle of incidence of 70°. The presented Black Germanium might find applications as low-cost AR structure in optoelectronics and IR optics.

  13. Etching reaction of methylchloride molecule on the GaAs (0 0 1)-2 × 4 surface

    NASA Astrophysics Data System (ADS)

    Ozeki, M.; Iwasa, Y.; Shimizu, Y.

    2007-04-01

    Adsorption process of methylchloride (CH 3Cl) on the GaAs (0 0 1)-2 × 4 surface was studied by a scanning tunnelling microscopy (STM) measurement. The arsenic rich 2 × 4 surface, which was prepared by molecular beam epitaxy (MBE), was exposed to a supersonic molecular beam of CH 3Cl with a kinetic energy of 0.06 eV. New bright spots appeared on the CH 3Cl exposed surface. They were largely observed at the "B-type" step edge and divided into two types according to their locations. It was suggested that new spots were due to weakly adsorbed CH 3Cl molecules without any dissociation. The adsorption mechanism of CH 3Cl molecule was also studied by an ab initio Hartree-Fock calculation, which explained the experimental results well.

  14. Time-varying wetting behavior on copper wafer treated by wet-etching

    NASA Astrophysics Data System (ADS)

    Tu, Sheng-Hung; Wu, Chuan-Chang; Wu, Hsing-Chen; Cheng, Shao-Liang; Sheng, Yu-Jane; Tsao, Heng-Kwong

    2015-06-01

    The wet cleaning process in semiconductor fabrication often involves the immersion of the copper wafer into etching solutions and thereby its surface properties are significantly altered. The wetting behavior of a copper film deposited on silicon wafer is investigated after a short dip in various etching solutions. The etchants include glacial acetic acid and dilute solutions of nitric acid, hydrofluoric acid, and tetramethylammonium hydroxide. It was found that in most cases a thin oxide layer still remains on the surface of as-received Cu wafers when they are subject to etching treatments. However, a pure Cu wafer can be obtained by the glacial acetic acid treatment and its water contact angle (CA) is about 45°. As the pure Cu wafer is placed in the ambient condition, the oxide thickness grows rapidly to the range of 10-20 Å within 3 h and the CA on the hydrophilic surface also rises. In the vacuum, it is surprising to find that the CA and surface roughness of the pure Cu wafer can grow significantly. These interesting results may be attributed to the rearrangement of surface Cu atoms to reduce the surface free energy.

  15. The isotopic composition of zinc, palladium, silver, cadmium, tin, and tellurium in acid-etched residues of the Allende meteorite

    SciTech Connect

    Loss, R.D.; Rosman, K.J.R.; De Laeter, J.R. )

    1990-12-01

    The isotopic and elemental abundances of Zn, Pd, Ag, Cd, Sn, and Te have been measured in three acid-resistant residues extracted from the Allende meteorite. High-efficiency, low-contamination ion-exchange procedures were developed to separate and purify the nanogram amounts of these elements present. Elemental-abundance determinations performed by Mass Spectrometric Isotope Dilution agree with previously published work for similarly derived residues. No isotope anomalies similar to those found for Xe (Xe-HL) in these samples were detected for any of these elements, which is consistent with the residues not being derived directly from the Xe-HL carriers. The lack of major Te-isotope anomalies does not support earlier reports of {sup 126}Te and {sup 130}Te excesses which were measured by neutron activation in similar samples. Small excesses were detected in the minor isotopes of Sn and Te, but these may be due to measurement problems associated with the small ion currents obtained for these samples. Two of the residue solutions contain Cd with up to several percent excesses for {sup 106}Cd and {sup 108}Cd. Interpretations of these results are limited by the unknown nature of the carrier minerals in the residues but may indicate the presence of a p-process component in Allende residues.

  16. Dry etching method for compound semiconductors

    DOEpatents

    Shul, Randy J.; Constantine, Christopher

    1997-01-01

    A dry etching method. According to the present invention, a gaseous plasma comprising, at least in part, boron trichloride, methane, and hydrogen may be used for dry etching of a compound semiconductor material containing layers including aluminum, or indium, or both. Material layers of a compound semiconductor alloy such as AlGaInP or the like may be anisotropically etched for forming electronic devices including field-effect transistors and heterojunction bipolar transistors and for forming photonic devices including vertical-cavity surface-emitting lasers, edge-emitting lasers, and reflectance modulators.

  17. Dry etching method for compound semiconductors

    DOEpatents

    Shul, R.J.; Constantine, C.

    1997-04-29

    A dry etching method is disclosed. According to the present invention, a gaseous plasma comprising, at least in part, boron trichloride, methane, and hydrogen may be used for dry etching of a compound semiconductor material containing layers including aluminum, or indium, or both. Material layers of a compound semiconductor alloy such as AlGaInP or the like may be anisotropically etched for forming electronic devices including field-effect transistors and heterojunction bipolar transistors and for forming photonic devices including vertical-cavity surface-emitting lasers, edge-emitting lasers, and reflectance modulators. 1 fig.

  18. Analysis methods for meso- and macroporous silicon etching baths

    NASA Astrophysics Data System (ADS)

    Nehmann, Julia B.; Kajari-Schröder, Sarah; Bahnemann, Detlef W.

    2012-07-01

    Analysis methods for electrochemical etching baths consisting of various concentrations of hydrofluoric acid (HF) and an additional organic surface wetting agent are presented. These electrolytes are used for the formation of meso- and macroporous silicon. Monitoring the etching bath composition requires at least one method each for the determination of the HF concentration and the organic content of the bath. However, it is a precondition that the analysis equipment withstands the aggressive HF. Titration and a fluoride ion-selective electrode are used for the determination of the HF and a cuvette test method for the analysis of the organic content, respectively. The most suitable analysis method is identified depending on the components in the electrolyte with the focus on capability of resistance against the aggressive HF.

  19. The Materials Chemistry of Atomic Oxygen with Applications to Anisotropic Etching of Submicron Structures in Microelectronics and the Surface Chemistry Engineering of Porous Solids

    NASA Technical Reports Server (NTRS)

    Koontz, Steve L.; Leger, Lubert J.; Wu, Corina; Cross, Jon B.; Jurgensen, Charles W.

    1994-01-01

    Neutral atomic oxygen is the most abundant component of the ionospheric plasma in the low Earth orbit environment (LEO; 200 to 700 kilometers altitude) and can produce significant degradation of some spacecraft materials. In order to produce a more complete understanding of the materials chemistry of atomic oxygen, the chemistry and physics of O-atom interactions with materials were determined in three radically different environments: (1) The Space Shuttle cargo bay in low Earth orbit (the EOIM-3 space flight experiment), (2) a high-velocity neutral atom beam system (HVAB) at Los Alamos National Laboratory (LANL), and (3) a microwave-plasma flowing-discharge system at JSC. The Space Shuttle and the high velocity atom beam systems produce atom-surface collision energies ranging from 0.1 to 7 eV (hyperthermal atoms) under high-vacuum conditions, while the flowing discharge system produces a 0.065 eV surface collision energy at a total pressure of 2 Torr. Data obtained in the three different O-atom environments referred to above show that the rate of O-atom reaction with polymeric materials is strongly dependent on atom kinetic energy, obeying a reactive scattering law which suggests that atom kinetic energy is directly available for overcoming activation barriers in the reaction. General relationships between polymer reactivity with O atoms and polymer composition and molecular structure have been determined. In addition, vacuum ultraviolet photochemical effects have been shown to dominate the reaction of O atoms with fluorocarbon polymers. Finally, studies of the materials chemistry of O atoms have produced results which may be of interest to technologists outside the aerospace industry. Atomic oxygen 'spin-off' or 'dual use' technologies in the areas of anisotropic etching in microelectronic materials and device processing, as well as surface chemistry engineering of porous solid materials are described.

  20. Chemically assisted ion beam etching of polycrystalline and (100)tungsten

    NASA Technical Reports Server (NTRS)

    Garner, Charles

    1987-01-01

    A chemically assisted ion-beam etching technique is described which employs an ion beam from an electron-bombardment ion source and a directed flux of ClF3 neutrals. This technique enables the etching of tungsten foils and films in excess of 40 microns thick with good anisotropy and pattern definition over areas of 30 sq mm, and with a high degree of selectivity. (100) tungsten foils etched with this process exhibit preferred-orientation etching, while polycrystalline tungsten films exhibit high etch rates. This technique can be used to pattern the dispenser cathode surfaces serving as electron emitters in traveling-wave tubes to a controlled porosity.

  1. Stereology of backscatter electron images of etched surfaces for characterization of particle size distributions and volume fractions: Estimation of imaging bias via Monte Carlo simulations

    SciTech Connect

    Payton, E.J. Mills, M.J.

    2011-06-15

    On metallic specimens in which a secondary phase has been selectively removed by a chemical etchant, the use of backscatter electron (BSE) imaging yields images that are more readily segmented with image processing algorithms than other modes of imaging in the scanning electron microscope. The contrast mechanisms in this imaging mode, however, produce a bias in the observation of particle sizes and volume fractions due to the effects of the electron interaction volume in the specimen. This stereological bias is quantified using Monte Carlo (MC) simulation of backscatter images. It is observed that the overprojection of features with centroids residing beneath the plane of polish is largely canceled out by the reduced segmentation size of features with centroids residing above the plane of polish. - Research Highlights: {yields} Backscatter imaging of selectively-etched surfaces can facilitate segmentation. {yields} Backscatter imaging of voids is simulated to estimate imaging/observation biases. {yields} The biases are quantified and incorporated into the stereological calculation. {yields} Systematic errors and imaging biases are observed to counteract one another. {yields} Results are illustrated using a bimodal gamma prime distribution in a Ni superalloy.

  2. Reactive Ion Etching for Randomly Distributed Texturing of Multicrystalline Silicon Solar Cells

    SciTech Connect

    ZAIDI, SALEEM H

    2002-05-01

    The quality of low-cost multicrystalline silicon (mc-Si) has improved to the point that it forms approximately 50% of the worldwide photovoltaic (PV) power production. The performance of commercial mc-Si solar cells still lags behind c-Si due in part to the inability to texture it effectively and inexpensively. Surface texturing of mc-Si has been an active field of research. Several techniques including anodic etching [1], wet acidic etching [2], lithographic patterning [3], and mechanical texturing [4] have been investigated with varying degrees of success. To date, a cost-effective technique has not emerged.

  3. Etching characteristics of LiNbO{sub 3} in reactive ion etching and inductively coupled plasma

    SciTech Connect

    Ren, Z.; Yu, S.; Heard, P. J.; Marshall, J. M.; Thomas, P. A.

    2008-02-01

    The etching characteristics of congruent LiNbO{sub 3} single crystals including doped LiNbO{sub 3} and proton-changed LiNbO{sub 3} have been studied in reactive ion etching (RIE) and inductively coupled plasma (ICP) etching tools, using different recipes of gas mixtures. The effects of parameters including working pressure, RIE power, and ICP power are investigated and analyzed by measurement of etching depth, selectivity, uniformity, etched surface state, and sidewall profile by means of focused ion beam etching, energy-dispersive x-ray analysis, secondary ion mass spectroscopy, scanning electron microscopy, and surface profilometry. The effects of a sample carrier wafer coating have also been investigated. Optimized processes with high etching rates, good mask selectivity, and a near-vertical profile have been achieved. Ridge waveguides on proton-exchanged LiNbO{sub 3} have been fabricated and optically measured.

  4. Dynamics of ion-assisted etching

    NASA Astrophysics Data System (ADS)

    Sebel, Petrus Gerardus Maria

    In this thesis a study is presented on the fundamentals of ion-assisted etching of silicon. The research was performed in the Atomic Physics and Quantum Electronics Group (AQT/B) of the Physics Department at the Eindhoven University of Technology. Etching is a key technique in the production process of integrated circuits. Industrial etching is usually done in a plasma reactor. However, to unravel the detailed mechanisms determining the etch process, a different approach was chosen. In this scheme, well defined beams of XeF2 and Ar + ions are directed towards the Si sample in an ultra-high vacuum (UHV) setup. In this way the relevant ingredients of a plasma (neutrals and ions) are simulated. The etching reaction is monitored by a quadruple mass spectrometer (QMS) which detects the desorption of non-reacted XeF2 and the main reaction products SiF4 and SiF2. We conclude that we have obtained a detailed microscopic picture of the etching of silicon by beams of neutrals and ions. However, there is still a gap between beam etching and plasma etching. To bridge this gap an ellipsometer has been added to our setup, because it is a common non-invasive diagnostic tool used in a plasma reactor. In addition, also a sample exchange mechanism was installed to facilitate the frequent exchange of samples. The first ellipsometric results of spontaneous etching show the construction of a reaction layer followed by surface roughening. The XeF2 dose needed to build the reaction layer as derived from the ellipsometric results is in good agreement with results from the mass spectrometer. Additional experiments have to be performed to obtain a full understanding of the roughening of the surface, but a first link between microscopic and macroscopic features has been established. (Abstract shortened by UMI.)

  5. 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.

  6. The adsorption of aromatic acids onto the graphite basal surface

    NASA Astrophysics Data System (ADS)

    Martin, David S.

    2003-06-01

    The adsorption of benzoic acid, toluic acid, and salicylic acid from solution onto the graphite basal surface has been studied using atomic force microscopy (AFM). A systematic study of these three related planar aromatic acids is conducted in order to observe the influence of the functional side-group upon adsorption. It is found that upon adsorption all three acids orient with the benzene ring parallel to the graphite surface. On the graphite terraces, the benzoic acid decoration follows a Stranski-Krastanov growth mode whereas toluic acid follows Volmer-Weber growth. Salicylic acid forms a fibrous aggregate network. In addition to the terraces, graphite steps and near-surface bulk defects are found to be important sites for adsorption. The AFM tip is used to create irreversible nanoscale modifications of adsorbate structures.

  7. Critical loads of acidity for surface waters in China.

    PubMed

    Duan, L; Hao, J; Xie, S; Du, K

    2000-01-31

    For further control of acid rain and sulphur dioxide pollution, the Chinese government has designated the Acid Rain Control Zone and the Sulphur Dioxide Pollution Control Zone for those areas that are, or could become, affected by acid deposition or ambient sulphur dioxide concentrations. One of the most important principles for designating the Acid Rain Control Zone is that the critical load is exceeded by the sulphur deposition. Through the steady-state water chemistry method (SSWC), critical loads of acidity for surface waters were mapped based on available data. Results show that surface waters sensitive to acid deposition, i.e. surface waters with low critical loads, are mainly found in north-east China, on the Tibetan Plateau, and in north-west China. Compared with the critical loads of soils, critical loads of surface waters are usually higher in almost all areas in China. The reason for very low critical loads of surface waters in some regions dominated by soils geologically not sensitive to acid deposition may be attributed to the low temperature, high altitude and low runoff. In contrast, surface waters in south China are not susceptible to acid deposition, and so far acidification of surface water has not been found in spite of the heavy acid rain. As can be seen from the critical load exceedance map, nearly 10% of the surface waters are subject to risk of acidification in 1995.

  8. Development of Localized Plasma Etching System for Failure Analyses in Semiconductor Devices: (3)
    Etching-Monitoring Using Quadrupole Mass Spectrometry

    NASA Astrophysics Data System (ADS)

    Takahashi, Satoshi; Horie, Tomoyuki; Shirayama, Yuya; Yokosuka, Shuntaro; Kashimura, Kenta; Hayashi, Akihiro; Iwase, Chikatsu; Shimbori, Shun'ichiro; Tokumoto, Hiroshi; Naitoh, Yasuhisa; Shimizu, Tetsuo

    Quadrupole mass spectrometry (QMS) has been applied to monitor the etching processes in a localized plasma etching system. An inward plasma was employed for etching in which the etching gas was discharged in the narrow gap between the etched sample and the entrance of an evacuating capillary tube. As the etching products are immediately evacuated through the capillary, a QMS system equipped at the capillary exit is able to analyze the products without any loss in concentration via diffusion into the chamber. Two kinds of samples, thermally grown SiO2 on Si and spin-coated polyimide film on Si, were etched, and the chemical species in the evacuated etching gas were analyzed with QMS, which enables monitoring of the composition of the surface being etched. Samples of thermal SiO2 were etched with CF4 plasma. The peak height of the SiF3+ signal during the SiO2 etching was lower than that observed during etching of the silicon substrate, leading to endpoint detection. The endpoint detection of the polyimide film etching was conducted using two etching gases: pure O2 and pure CF4. When O2 was used, the endpoint was detected by the decrease of the mass peak attributed to CO. When CF4 was employed, the plasma was able to etch both the polyimide film and Si substrate. Then the endpoint was detected by the increase of the mass peak of SiF3+ produced by the etching of the Si substrate.

  9. Effects of type of reactor, crystallinity of SiC, and NF{sub 3} gas pressure on etching rate and smoothness of SiC surface using NF{sub 3} gas plasma

    SciTech Connect

    Tasaka, A.; Yamada, H.; Nonoyama, T.; Kanatani, T.; Kotaka, Y.; Tojo, T.; Inaba, M.

    2009-11-15

    Polycrystalline {beta}-SiC and single-crystalline 4H-SiC surfaces were etched by reactive ion etching (RIE) using NF{sub 3} gas plasma. A smooth surface was obtained on the polycrystalline SiC after RIE at NF{sub 3} gas pressures of 2 and 10 Pa for 10 min, and neither spikes nor pillars were formed on it. On the other hand, some pillars were formed on the single-crystalline SiC surface by RIE at NF{sub 3} gas pressures of 2 and 10 Pa. Though the absence of carbon-rich regions and SiO{sub x} on the outermost surface before etching was confirmed by x-ray photoelectron spectroscopy and Raman analysis, x-ray diffraction analysis revealed that graphite crystallites were present in the single-crystalline SiC bulk. It was concluded that the graphite crystallites acted as masks and the pillars grew up from the graphite crystallites in the single crystalline SiC during RIE.

  10. Chemically Etched Open Tubular and Monolithic Emitters for Nanoelectrospray Ionization Mass Spectrometry

    SciTech Connect

    Kelly, Ryan T.; Page, Jason S.; Luo, Quanzhou; Moore, Ronald J.; Orton, Daniel J.; Tang, Keqi; Smith, Richard D.

    2006-11-15

    We have developed a new procedure for fabricating fused silica emitters for electrospray ionization-mass spectrometry (ESI-MS) in which the end of a bare fused silica capillary is immersed into aqueous hydrofluoric acid, and water is pumped through the capillary to prevent etching of the interior. Surface tension causes the etchant to climb the capillary exterior, and the etch rate in the resulting meniscus decreases as a function of distance from the bulk solution. Etching continues until the silica touching the hydrofluoric acid reservoir is completely removed, essentially stopping the etch process. The resulting emitters have no internal taper, making them much less prone to clogging compared to e.g. pulled emitters. The high aspect ratios and extremely thin walls at the orifice facilitate very low flow rate operation; stable ESI-MS signals were obtained for model analytes from 5-μm-diameter emitters at a flow rate of 5 nL/min with a high degree of inter-emitter reproducibility. In extensive evaluation, the etched emitters were found to enable approximately four times as many LC-MS analyses of proteomic samples before failing compared with conventional pulled emitters. The fabrication procedure was also employed to taper the ends of polymer monolith-containing silica capillaries for use as ESI emitters. In contrast to previous work, the monolithic material protrudes beyond the fused silica capillaries, improving the monolith-assisted electrospray process.

  11. Unsaturated fatty acids in alkane solution: adsorption to steel surfaces.

    PubMed

    Lundgren, Sarah M; Persson, Karin; Mueller, Gregor; Kronberg, Bengt; Clarke, Jim; Chtaib, Mohammed; Claesson, Per M

    2007-10-01

    The adsorption of the unsaturated fatty acids oleic, linoleic, and linolenic acid on steel surfaces has been investigated by means of a quartz crystal microbalance (QCM). Two different solvents were used, n-hexadecane and its highly branched isomer, viz., 2,2,4,4,6,8,8-heptamethylnonane. The area occupied per molecule of oleic acid at 1 wt % corresponds to what is needed for adsorption parallel to the surface. At the same concentration, the adsorbed amount of linoleic acid and linolenic acid indicates that they adsorb in multilayers. The chemisorbed amount estimated from static secondary ion mass spectroscopy (SIMS) measurements was found to be similar for the three unsaturated fatty acids. In the case of linolenic acid, it was found that the presence of water significantly alters the adsorption, most likely because of the precipitation of fatty acid/water aggregates. Furthermore, static SIMS results indicate that the amount of water used here inhibits the chemisorption of linolenic acid.

  12. Plasma etching in a multipolar discharge

    NASA Astrophysics Data System (ADS)

    Wicker, T. E.; Mantei, T. D.

    1985-03-01

    Etching of silicon and SiO2 has been investigated in a dc plasma discharge confined by a multipolar surface magnetic field layer. The reactive plasma is produced by primary ionizing electrons drawn from heated tungsten filaments and confined by permanent magnets. Electrical probe measurements show that a uniform high-density plasma (1010-1011 cm-3) is sustained in SF6-O2 at very low pressure (0.2-2.0×10-3 Torr). Substrates are biased independently of plasma production by a low-frequency alternating voltage (0-400 V) applied to the substrate through a blocking capacitor. Anisotropic profiles are etched into Si in SF6-20% O2 with etch rates in excess of 1 μm/min at 2×10-3 Torr. The etch rate increases with increasing primary electron current (up to 3 A) and energy (up to 60 eV), gas pressure (up to 2.0×10-3 Torr), substrate bias voltage, and the addition of up to 20% O2. For higher ionizing electron energies (>60 eV) and higher gas pressure (>2.0×10-3 Torr), etching is partially blocked by residue formation. The etch anisotropy depends mainly on substrate bias, increasing for higher values of bias voltage. The Si:SiO2 etch selectivity is typically 10-20, becoming large with decreasing substrate bias and plasma ion density.

  13. Assessment of Microshear Bond Strength: Self-Etching Sealant versus Conventional Sealant

    PubMed Central

    Biria, Mina; Ghasemi, Amir; Torabzadeh, Hassan; Shisheeian, Arash; Baghban, Alireza Akbarzadeh

    2014-01-01

    Objective Recently, self-etching fissure sealants have been introduced to reduce technical sensitivity; however, their efficacy should be assessed. The aim of this study was to assess of the microshear bond strength of self-etching and conventional fissure sealants. Materials and Methods: Thirty non-carious third molars were randomly divided into three groups (N=10). Microcylinders of Concise fissure sealant were bonded to prepared buccal and lingual surfaces using the two following procedures. In the first group, phosphoric acid was used to prepare the substrate; whereas in group two, Concise was used in combination with Prompt L-Pop. In group 3, a self-etching fissure sealant (Enamel Loc) was utilized per se. After 24 hours, the samples were subjected to 500 rounds of thermocycling and shear bond testing using a microtensile tester machine with a crosshead speed of 0.5mm/min. Data were analyzed using one-way repeated measure ANOVA and Bonferroni Post HOC tests (SPSS version 16). Results: The mean and standard deviation of microshear bond strength of the groups were as follows: Group 1: Concise+ etching (14.59 ± 1.19 MPa), Group 2: Concise+Prompt L-Pop (12.86 ± 1.98 MPa), and Group 3: Enamel Loc (5.59 ± 0.72 MPa). One-way ANOVA revealed that all the differences were significant and the conventional sealant exhibited the highest mean bond strength. Conclusion: Conventional sealant using phosphoric acid etch application prior to fissure sealant application demonstrated more bond strength in comparison with that of self-etch bonding and self-etch sealant. PMID:24910688

  14. High haze textured surface B-doped ZnO-TCO films on wet-chemically etched glass substrates for thin film solar cells

    NASA Astrophysics Data System (ADS)

    Xinliang, Chen; Jieming, Liu; Jia, Fang; Ze, Chen; Ying, Zhao; Xiaodan, Zhang

    2016-08-01

    Textured glass substrates with crater-like feature sizes of ∼5–30 μm were obtained using the chemical etching method through adjusting the treatment round (R). Pyramid-like boron-doped zinc oxide (ZnO:B) films with feature sizes of ∼300–800 nm were deposited on the etched glass substrates by the metal organic chemical deposition (MOCVD) technique using water, diethylzinc and 1%-hydrogen-diluted diborane. The ZnO:B films on the etched glass with micro/nano double textures presented a much stronger light-scattering capability than the conventional ZnO:B on the flat glass and their electrical properties changed little. Typical etched glass-3R/ZnO:B exhibited a high root mean square (RMS) roughness of ∼160 nm. The haze values at the wavelengths of 550 nm and 850 nm for etched glass-3R/ZnO:B sample were 61% and 42%, respectively. Finally, the optimized etched glass/ZnO:B was applied in the silicon (Si) based thin film solar cells. The high haze etched glass/ZnO:B substrates have potential merits for thin film solar cells. Project supported by the State Key Development Program for Basic Research of China (Nos. 2011CBA00706, 2011CBA00707), the Tianjin Applied Basic Research Project and Cutting-Edge Technology Research Plan (No. 13JCZDJC26900), the Tianjin Major Science and Technology Support Project (No. 11TXSYGX22100), the National High Technology Research and Development Program of China (No. 2013AA050302), and the Fundamental Research Funds for the Central Universities (No. 65010341).

  15. High haze textured surface B-doped ZnO-TCO films on wet-chemically etched glass substrates for thin film solar cells

    NASA Astrophysics Data System (ADS)

    Xinliang, Chen; Jieming, Liu; Jia, Fang; Ze, Chen; Ying, Zhao; Xiaodan, Zhang

    2016-08-01

    Textured glass substrates with crater-like feature sizes of ˜5-30 μm were obtained using the chemical etching method through adjusting the treatment round (R). Pyramid-like boron-doped zinc oxide (ZnO:B) films with feature sizes of ˜300-800 nm were deposited on the etched glass substrates by the metal organic chemical deposition (MOCVD) technique using water, diethylzinc and 1%-hydrogen-diluted diborane. The ZnO:B films on the etched glass with micro/nano double textures presented a much stronger light-scattering capability than the conventional ZnO:B on the flat glass and their electrical properties changed little. Typical etched glass-3R/ZnO:B exhibited a high root mean square (RMS) roughness of ˜160 nm. The haze values at the wavelengths of 550 nm and 850 nm for etched glass-3R/ZnO:B sample were 61% and 42%, respectively. Finally, the optimized etched glass/ZnO:B was applied in the silicon (Si) based thin film solar cells. The high haze etched glass/ZnO:B substrates have potential merits for thin film solar cells. Project supported by the State Key Development Program for Basic Research of China (Nos. 2011CBA00706, 2011CBA00707), the Tianjin Applied Basic Research Project and Cutting-Edge Technology Research Plan (No. 13JCZDJC26900), the Tianjin Major Science and Technology Support Project (No. 11TXSYGX22100), the National High Technology Research and Development Program of China (No. 2013AA050302), and the Fundamental Research Funds for the Central Universities (No. 65010341).

  16. Surface-active properties of humic and sulfochlorohumic acids

    SciTech Connect

    Ryabova, I.N.; Mustafina, G.A.; Akkulova, Z.G.; Satymbaeva, A.S.

    2009-10-15

    The surface tension of alkaline solutions of humic acids and their sulfochloroderivatives, which are synthesized by sulfonation of chlorohumic acids isolated from coal chlorinated by the electrochemical method, is investigated. It is established that humic compounds possess weak surface activity. Basic adsorption parameters are calculated.

  17. Si etching with reactive neutral beams of very low energy

    SciTech Connect

    Hara, Yasuhiro; Hamagaki, Manabu; Mise, Takaya; Iwata, Naotaka; Hara, Tamio

    2014-12-14

    A Si etching process has been investigated with reactive neutral beams (NBs) extracted using a low acceleration voltage of less than 100 V from CF{sub 4} and Ar mixed plasmas. The etched Si profile shows that the etching process is predominantly anisotropic. The reactive NB has a constant Si etching rate in the acceleration voltage range from 20 V to 80 V. It is considered that low-energy NBs can trigger Si etching because F radicals adsorb onto the Si surface and weaken Si–Si bonds. The etching rate per unit beam flux is 33 times higher than that with Ar NB. These results show that the low-energy reactive NB is useful for damage-free high speed Si etching.

  18. Polymer etching in the oxygen afterglow - Increased etch rates with increased reactor loading

    NASA Technical Reports Server (NTRS)

    Lerner, N. R.; Wydeven, T.

    1989-01-01

    Reactor loading has an effect on the etch rate (rate of decrease of film thickness) of films of polyvinylfluoride (Tedlar) and polyethylene exposed in the afterglow of an RF discharge in oxygen. The etch rate is found to increase with the total surface area of the polymer exposed in the reactor. The etch rates of polypyromellitimide (Kapton H) and polystyrene under these conditions are very low. However, the etch rate of these polymers is greatly enhanced by adding either Tedlar or polyethylene to the reactor. A kinetic model is proposed based on the premise that the oxygen atoms produced by the RF discharge react with Tedlar or polyethylene to produce a much more reactive species, which dominates the etching of the polymers studied.

  19. Arachidonic acid and prostaglandin E2 influence human osteoblast (MG63) response to titanium surface roughness.

    PubMed

    Dean, David D; Campbell, Casey M; Gruwell, Scott F; Tindall, John W M; Chuang, Hui-Hsiu; Zhong, Weinan; Schmitz, John P; Sylvia, Victor L

    2008-01-01

    Prior studies have shown that implant surface roughness affects osteoblast proliferation, differentiation, matrix synthesis, and local factor production. Further, cell response is modulated by systemic factors, such as 1,25(OH)2D3 and estrogen as well as mechanical forces. Based on the fact that peri-implant bone healing occurs in a site containing elevated amounts of prostaglandin E2 (PGE2), the hypothesis of the current study is that PGE2 and arachidonic acid (AA), the substrate used by cyclooxygenase to form PGE2, influence osteoblast response to implant surface roughness. To test this hypothesis, 4 different types of commercially pure titanium (cpTi) disks with surfaces of varying roughness (smooth Ti, R(a) 0.30 microm; smooth and acid etched Ti [SAE Ti], R(a) 0.40 microm; rough Ti, R(a) 4.3 microm; rough and acid etched Ti [RAE Ti], R(a) 4.15 (microm) were prepared. MG63 osteoblasts were seeded onto the surfaces, cultured to confluence, and then treated for the last 24 hours of culture with AA (0, 0.1, 1, and 10 nM), PGE2 (0, 1, 10, 25, and 100 nM), or the general cyclooxygenase inhibitor indomethacin (0 or 100 nM). At harvest, the effect of treatment on cell proliferation was assessed by measuring cell number and [3H]-thymidine incorporation, and the effect on cell differentiation was determined by measuring alkaline phosphatase (ALP) specific activity. The effect of AA and PGE2 on cell number was somewhat variable but showed a general decrease on plastic and smooth surfaces and an increase on rough surfaces. In contrast, [3H]-thymidine incorporation was uniformly decreased with treatment on all surfaces. ALP demonstrated the most prominent effect of treatment. On smooth surfaces, AA and PGE2 dose-dependently increased ALP, while on rough surfaces, treatment dose-dependently decreased enzyme specific activity. Indomethacin treatment had either no effect or a slightly inhibitory effect on [3H]-thymidine incorporation on all surfaces. In contrast, indomethacin

  20. Feasibility of hydrofluoric acid etched sand particles for enrichment and determination of polychlorinated biphenyls at trace levels in environmental water samples.

    PubMed

    Xing, Han-Zhu; Chen, Xiang-Feng; Wang, Xia; Wang, Ming-Lin; Zhao, Ru-Song

    2014-06-01

    This study aims to investigate the feasibility of etched sand particles being used as solid-phase extraction adsorbents to enrich polychlorinated biphenyls (PCBs), which are typical persistent organic pollutants in the environment, at trace levels. Gas chromatography-tandem mass spectrometry was selected to detect the compounds. Etched sand particles exhibited excellent merits on the enrichment of PCBs. Related important factors affecting extraction efficiencies were investigated and optimized in detail. Under optimized conditions, low limits of detection (0.42 to 3.69 ng L(-1)), wide linear range (10 to 1,000 ng L(-1)), and high repeatability (1.9 to 8.2%) were achieved. The developed method was validated with several real water samples, and satisfactory results were obtained. All of these findings indicate that etched sand particles would be useful for the enrichment and determination of organic pollutants at trace levels in water samples.

  1. Surface properties of superfine alumina trihydrate after surface modification with stearic acid

    NASA Astrophysics Data System (ADS)

    Liu, Gui-hua; Zhou, Bo-hao; Li, Yun-feng; Qi, Tian-gui; Li, Xiao-bin

    2015-05-01

    The surface properties of superfine alumina trihydrate (ATH) after surface modification were studied by measuring the contact angle, active ratio, oil adsorption, total organic carbon, adsorption ratio, and Fourier transform infrared (FTIR) spectrum. The contact angle increased initially and then slowly decreased with an increase of the amount of stearic acid. However, the surface free energy decreased initially and then increased. Surface modification with stearic acid or sodium stearate can benefit from elevating temperature. The base surface tension component and the free energy of Lewis acid-base both declined sharply following the surface modification. Excess stearic acid was physically adsorbed in the form of multilayer adsorption, and an interaction between oxygen on the ATH surface and hydroxyl in stearic acid was subsequently determined. Our results further indicated that the contact angle and adsorption ratio can be used as control indicators for surface modification compared with active ratio, oil adsorption and total organic carbon.

  2. 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.

  3. Solderability enhancement of copper through chemical etching

    SciTech Connect

    Stevenson, J.O.; Guilinger, T.R.; Hosking, F.M.; Yost, F.G.; Sorensen, N.R.

    1995-05-01

    Sandia National Laboratories has established a Cooperative Research and Development Agreement with consortium members of the National Center for Manufacturing Sciences (NCMS) to develop fundamental generic technology in the area of printed wiring board materials and surface finishes. Improved solderability of copper substrates is an important component of the Sandia-NCMS program. The authors are investigating the effects of surface roughness on the wettability and solderability behavior of several different types of copper board finishes. In this paper, the authors present roughness and solderability characterizations for a variety of chemically-etched copper substrates. Initial testing on six chemical etches demonstrate that surface roughness can be greatly enhanced through chemical etching. Noticeable improvements in solder wettability were observed to accompany increases in roughness. A number of different algorithms and measures of roughness were used to gain insight into surface morphologies that lead to improved solderability.

  4. Succinic acid in aqueous solution: connecting microscopic surface composition and macroscopic surface tension.

    PubMed

    Werner, Josephina; Julin, Jan; Dalirian, Maryam; Prisle, Nønne L; Öhrwall, Gunnar; Persson, Ingmar; Björneholm, Olle; Riipinen, Ilona

    2014-10-21

    The water-vapor interface of aqueous solutions of succinic acid, where pH values and bulk concentrations were varied, has been studied using surface sensitive X-ray photoelectron spectroscopy (XPS) and molecular dynamics (MD) simulations. It was found that succinic acid has a considerably higher propensity to reside in the aqueous surface region than its deprotonated form, which is effectively depleted from the surface due to the two strongly hydrated carboxylate groups. From both XPS experiments and MD simulations a strongly increased concentration of the acid form in the surface region compared to the bulk concentration was found and quantified. Detailed analysis of the surface of succinic acid solutions at different bulk concentrations led to the conclusion that succinic acid saturates the aqueous surface at high bulk concentrations. With the aid of MD simulations the thickness of the surface layer could be estimated, which enabled the quantification of surface concentration of succinic acid as a multiple of the known bulk concentration. The obtained enrichment factors were successfully used to model the surface tension of these binary aqueous solutions using two different models that account for the surface enrichment. This underlines the close correlation of increased concentration at the surface relative to the bulk and reduced surface tension of aqueous solutions of succinic acid. The results of this study shed light on the microscopic origin of surface tension, a macroscopic property. Furthermore, the impact of the results from this study on atmospheric modeling is discussed.

  5. Admittance spectroscopy of CdTe /CdS solar cells subjected to varied nitric-phosphoric etching conditions

    NASA Astrophysics Data System (ADS)

    Proskuryakov, Y. Y.; Durose, K.; Taele, B. M.; Welch, G. P.; Oelting, S.

    2007-01-01

    In this work we investigate the electric and structural properties of CdTe /CdS solar cells subjected to a nitric-phosphoric (NP) acid etching procedure, employed for the formation of a Te-rich layer before back contacting. The etching time is used as the only variable parameter in the study, while admittance spectroscopy is employed for the characterization of the cells' electric properties as well as for the analysis of the defect energy levels. Particular attention was also given to the characteristics of unetched devices and it is shown that despite the larger height of back-contact barrier such samples show well defined admittance spectra, as well as allow for extraction of as much as five defect levels in the range of 0.08-0.9eV above the valence band. In contrast, admittance characteristics of the etched samples show a decrease of the number of the detectable trap levels with increasing etching time. (Hence it is usual for only one or two trap levels to be reported in the literature for finished devices.) The latter leads to the anomalous Arrhenius energy plots as well as the breakdown of low-frequency capacitance characteristics for samples etched with times larger than 30s. The observed effects are attributed to physical thinning of the cells, the etching out of grain boundaries, and the tellurium enrichment of the CdTe surface by NP etching. We also perform analysis of the back-contact barrier height as extracted from dark I-V measurements at different temperatures. The dependence of this barrier height on NP etching time is compared with that of conversion efficiency, from which conclusions are drawn about both positive and negative effects of the nitric-phosphoric etch.

  6. Reactive ion etched substrates and methods of making and using

    DOEpatents

    Rucker, Victor C.; Shediac, Rene; Simmons, Blake A.; Havenstrite, Karen L.

    2007-08-07

    Disclosed herein are substrates comprising reactive ion etched surfaces and specific binding agents immobilized thereon. The substrates may be used in methods and devices for assaying or isolating analytes in a sample. Also disclosed are methods of making the reactive ion etched surfaces.

  7. Laser etching: A new technology to identify Florida grapefruit

    Technology Transfer Automated Retrieval System (TEKTRAN)

    Laser labeling of fruits and vegetables is an alternative means to label produce. Low energy CO2 laser beam etches the surface showing the contrasting underlying layer. These etched surfaces can promote water loss and potentially allowing for pathogen entry. The long term effects of laser labeling o...

  8. Surface-enhanced Raman spectroscopy of amino acids adsorbed on an electrochemically prepared silver surface

    NASA Astrophysics Data System (ADS)

    Stewart, S.; Fredericks, P. M.

    1999-07-01

    An electrochemically roughened silver surface, in conjunction with a Raman microprobe spectrometer, was used to obtain SER spectra of a suite of 19 L-amino acids. The spectra obtained were very different from previously reported SER spectra obtained from silver hydrosols of amino acids. Analysis of the spectra showed that adsorption of all amino acids was via the ionised carboxylate group, and that the side chain of most of the molecules was also in close proximity to the surface. The spectra also indicated that, in contrast, the amine terminus was protonated and relatively far from the surface. Sulfur-containing amino acids also interacted with the silver surface through their sulfur atoms.

  9. Effect of Acidic Agents on Surface Roughness of Dental Ceramics

    PubMed Central

    Kukiattrakoon, Boonlert; Hengtrakool, Chanothai; Kedjarune-Leggat, Ureporn

    2011-01-01

    Background: An increase in surface roughness of ceramics may decrease strength and affect the clinical success of ceramic restorations. However, little is known about the effect of acidic agents on ceramic restorations. The aim of this study was to evaluate the surface roughness of dental ceramics after being immersed in acidic agents. Methods: Eighty-three ceramic disk specimens (12.0 mm in diameter and 2.0 mm in thickness) were made from four types of ceramics (VMK 95, Vitadur Alpha, IPS Empress Esthetic, and IPS e.max Ceram). Baseline data of surface roughness were recorded by profilometer. The specimens were then immersed in acidic agents (citrate buffer solution, pineapple juice and green mango juice) and deionized water (control) at 37°C for 168 hours. One group was immersed in 4% acetic acid at 80°C for 168 hours. After immersion, surface roughness was evaluated by a profilometer at intervals of 24, 96, and 168 hours. Surface characteristics of specimens were studied using scanning electron microscopy (SEM). Data were analyzed using two-way repeated ANOVA and Tukey's multiple comparisons (α = 0.05). Results: For all studied ceramics, all surface roughness parameters were significantly increased after 168 hours immersion in all acidic agents (P < 0.05). After 168 hours in 4% acetic acid, there were significant differences for all roughness parameters from other acidic agents of all evaluated ceramics. Among all studied ceramics, Vitadur Alpha showed significantly the greatest values of all surface roughness parameters after immersion in 4% acetic acid (P < 0.001). SEM photomicrographs also presented surface destruction of ceramics in varying degrees. Conclusion: Acidic agents used in this study negatively affected the surface of ceramic materials. This should be considered when restoring the eroded tooth with ceramic restorations in patients who have a high risk of erosive conditions. PMID:22132009

  10. Experiment and Results on Plasma Etching of SRF cavities

    SciTech Connect

    Upadhyay, Janardan; Im, Do; Peshl, J.; Vuskovic, Leposova; Popovic, Svetozar; Valente, Anne-Marie; Phillips, H. Lawrence

    2015-09-01

    The inner surfaces of SRF cavities are currently chemically treated (etched or electropolished) to achieve the state of the art RF performance. We designed an apparatus and developed a method for plasma etching of the inner surface for SRF cavities. The process parameters (pressure, power, gas concentration, diameter and shape of the inner electrode, temperature and positive dc bias at inner electrode) are optimized for cylindrical geometry. The etch rate non-uniformity has been overcome by simultaneous translation of the gas point-of-entry and the inner electrode during the processing. A single cell SRF cavity has been centrifugally barrel polished, chemically etched and RF tested to establish a baseline performance. This cavity is plasma etched and RF tested afterwards. The effect of plasma etching on the RF performance of this cavity will be presented and discussed.

  11. 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.

  12. Dry Ice Etches Terrain

    NASA Technical Reports Server (NTRS)

    2007-01-01

    [figure removed for brevity, see original site] Figure 1

    Every year seasonal carbon dioxide ice, known to us as 'dry ice,' covers the poles of Mars. In the south polar region this ice is translucent, allowing sunlight to pass through and warm the surface below. The ice then sublimes (evaporates) from the bottom of the ice layer, and carves channels in the surface.

    The channels take on many forms. In the subimage shown here (figure 1) the gas from the dry ice has etched wide shallow channels. This region is relatively flat, which may be the reason these channels have a different morphology than the 'spiders' seen in more hummocky terrain.

    Observation Geometry Image PSP_003364_0945 was taken by the High Resolution Imaging Science Experiment (HiRISE) camera onboard the Mars Reconnaissance Orbiter spacecraft on 15-Apr-2007. The complete image is centered at -85.4 degrees latitude, 104.0 degrees East longitude. The range to the target site was 251.5 km (157.2 miles). At this distance the image scale is 25.2 cm/pixel (with 1 x 1 binning) so objects 75 cm across are resolved. The image shown here has been map-projected to 25 cm/pixel . The image was taken at a local Mars time of 06:57 PM and the scene is illuminated from the west with a solar incidence angle of 75 degrees, thus the sun was about 15 degrees above the horizon. At a solar longitude of 219.6 degrees, the season on Mars is Northern Autumn.

  13. Metal assisted anodic etching of silicon.

    PubMed

    Lai, Chang Quan; Zheng, Wen; Choi, W K; Thompson, Carl V

    2015-07-01

    Metal assisted anodic etching (MAAE) of Si in HF, without H2O2, is demonstrated. Si wafers were coated with Au films, and the Au films were patterned with an array of holes. A Pt mesh was used as the cathode while the anodic contact was made through either the patterned Au film or the back side of the Si wafer. Experiments were carried out on P-type, N-type, P(+)-type and N(+)-type Si wafers and a wide range of nanostructure morphologies were observed, including solid Si nanowires, porous Si nanowires, a porous Si layer without Si nanowires, and porous Si nanowires on a thick porous Si layer. Formation of wires was the result of selective etching at the Au-Si interface. It was found that when the anodic contact was made through P-type or P(+)-type Si, regular anodic etching due to electronic hole injection leads to formation of porous silicon simultaneously with metal assisted anodic etching. When the anodic contact was made through N-type or N(+)-type Si, generation of electronic holes through processes such as impact ionization and tunnelling-assisted surface generation were required for etching. In addition, it was found that metal assisted anodic etching of Si with the anodic contact made through the patterned Au film essentially reproduces the phenomenology of metal assisted chemical etching (MACE), in which holes are generated through metal assisted reduction of H2O2 rather than current flow. These results clarify the linked roles of electrical and chemical processes that occur during electrochemical etching of Si. PMID:26059556

  14. Dry-wet digital etching of Ge1-xSnx

    NASA Astrophysics Data System (ADS)

    Shang, Colleen K.; Wang, Vivian; Chen, Robert; Gupta, Suyog; Huang, Yi-Chiau; Pao, James J.; Huo, Yijie; Sanchez, Errol; Kim, Yihwan; Kamins, Theodore I.; Harris, James S.

    2016-02-01

    The development of a precise micromachining process for Ge1-xSnx has the potential to enable both the fabrication and optimization of Ge1-xSnx-based devices in photonics and microelectromechanical systems. We demonstrate a digital etching scheme for Ge0.922Sn0.078 based on a two-stage, highly selective CF4 plasma dry etch and HCl wet etch. Using X-Ray Reflectivity, we show consistent etch control as low as 1.5 nm per cycle, which is defined as one dry etch step followed by one wet etch step. The etch rate increases to 3.2 nm per cycle for a longer dry etch time due to physical sputtering contributions, accompanied by an increase in RMS surface roughness. By operating within a regime with minimal sputtering, we demonstrate that good digital etch depth control and surface quality can be achieved using this technique.

  15. Texturing a pyramid-like structure on a silicon surface via the synergetic effect of copper and Fe(III) in hydrofluoric acid solution

    NASA Astrophysics Data System (ADS)

    Cao, Ming; Li, Shaoyuan; Deng, Jianxin; Li, Yuping; Ma, Wenhui; Zhou, Yang

    2016-05-01

    An innovative approach is proposed to texture a pyramid structure on a silicon surface via Cu-catalyzed chemical etching in the HF/FeCl3 system. The surface and cross-section morphologies of the formed pyramid structure were examined by scanning electron microscopy and atomic force microscopy. The results revealed that numerous silicon pyramid-like structures with hemlines of 0.1 ∼ 3 μm and height of 0.1 ∼ 2 μm are close together, and the top angle of the pyramid structure is 90°. Additionally, the systematic study of the effects of the etching time and the concentration of FeCl3 on the pyramid-like structures by the atom configuration model of silicon crystal faces demonstrated that the etching proceeds preferentially along the <1 0 0> directions of silicon. A formation mechanism of the pyramid-like structure is proposed. The results imply that the synergetic effect of Cu nanoparticles and Fe(III) could conveniently generate a pyramid-like architecture on the surface of silicon in hydrofluoric acid solution.

  16. Oxalic acid adsorption states on the clean Cu(110) surface

    NASA Astrophysics Data System (ADS)

    Fortuna, Sara

    2016-11-01

    Carboxylic acids are known to assume a variety of configurations on metallic surfaces. In particular oxalic acid on the Cu(110) surface has been proposed to assume a number of upright configurations. Here we explore with DFT calculations the possible structures that oxalic acid can form on copper 110 at different protonation states, with particular attention at the possibility of forming structures composed of vertically standing molecules. In its fully protonated form it is capable of anchoring itself on the surface thanks to one of its hydrogen-free oxygens. We show the monodeprotonated upright molecule with two oxygens anchoring it on the surface to be the lowest energy conformation of a single oxalic molecules on the Cu(110) surface. We further show that it is possible for this configuration to form dense hexagonally arranged patterns in the unlikely scenario in which adatoms are not involved.

  17. Etching of fused silica fiber by metallic laser-induced backside wet etching technique

    NASA Astrophysics Data System (ADS)

    Vass, Cs.; Kiss, B.; Kopniczky, J.; Hopp, B.

    2013-08-01

    The tip of multimode fused silica fiber (core diameter: 550 μm) was etched by metallic laser-induced backside wet etching (M-LIBWE) method. Frequency doubled, Q-switched Nd:YAG laser (λ = 532 nm; τFWHM = 8 ns) was used as laser source. The laser beam was coupled into the fiber by a fused silica lens with a focal length of 1500 mm. The other tip of the fiber was dipped into liquid gallium metallic absorber. The etching threshold fluence was measured to be 475 mJ/cm2, while the highest fluence, which resulted etching without breaking the fiber, was 1060 mJ/cm2. The progress of etching was followed by optical microscopy, and the etch rate was measured to be between 20 and 37 nm/pulse depending on the applied laser energy. The surface morphologies of the etched tips were studied by scanning electron microscopy. A possible application of the structured fibers was also tested.

  18. Physical mechanisms for anisotropic plasma etching of cesium iodide

    SciTech Connect

    Yang Xiaoji; Hopwood, Jeffrey A.

    2004-11-01

    The physical mechanisms for the interaction between a reactive plasma and a cesium iodide surface are investigated. Under conditions of ion bombardment and elevated substrate temperature, CsI is found to sputter etch slowly (15 nm/min). If atomic fluorine, fluorocarbon radicals, of SF{sub x} radicals are present in the discharge, however, CsI is reactively etched at substantially higher rates (up to 200 nm/min). The roles of plasma radicals and energetic ion bombardment are investigated by first exposing the surface to plasma radicals and then bombarding the surface with argon ions. The optical emission from Cs and I atoms is found to correlate with the etch rate of CsI and is used as an in situ monitor of radical-enhanced etching. Small surface exposures to CF{sub x}, SF{sub x}, and F radicals are shown to enhance the etch rate of CsI. If the exposure of the CsI surface is increased, however, these same radical species act as etch inhibitors. A simple model for reactive etching of CsI is proposed, and this model is shown to compare reasonably well with experimental etch rates.

  19. Plasma etching of Hf-based high-k thin films. Part I. Effect of complex ions and radicals on the surface reactions

    SciTech Connect

    Martin, Ryan M.; Chang, Jane P.

    2009-03-15

    The effect of ion and radical compositions in BCl{sub 3}/Cl{sub 2} plasmas was assessed in this work with a focus on the formation of etch products in patterning hafnium aluminate, a potential high-k gate oxide material. The plasma composition became increasingly more complex as the percentage of boron trichloride was increased, which led to the formation of a significant amount of boron-containing species including B{sup +}, BCl{sup +}, BCl{sub 2}{sup +}, BCl{sub 3}{sup +}, B{sub 2}Cl{sub 3}{sup +}, and B{sub 2}OCl{sub 3}{sup +} in the plasma. The BCl{sub 2}{sup +} ions were found to be the dominant species in BCl{sub 3} containing plasmas at most conditions; however, increasing the pressure or decreasing the power led to an increase in the formation of higher mass ions. Several compositions of Hf{sub 1-x}Al{sub x}O{sub y} thin films ranging from pure HfO{sub 2} to pure Al{sub 2}O{sub 3} were etched in BCl{sub 3}/Cl{sub 2} plasmas as functions of ion energy and plasma composition. The etch product distributions were measured and the dominant metal-containing etch products were HfCl{sub x} and AlCl{sub x} in a Cl{sub 2} plasma and HfCl{sub x}, HfBOCl{sub 4}, and Al{sub x}Cl{sub y} in a BCl{sub 3} plasma, and their concentrations increased with increasing ion energy. Oxygen was detected removed in the form of ClO in Cl{sub 2} and as trichloroboroxin ((BOCl){sub 3}) in BCl{sub 3}. Both the etch rate and the etch product formation are enhanced in BCl{sub 3}/Cl{sub 2} plasmas, as compared to those in Cl{sub 2} plasmas, due to the change in the composition and reactivity of the dominant ions and radicals.

  20. Surface acidity of quartz: understanding the crystallographic control.

    PubMed

    Liu, Xiandong; Cheng, Jun; Lu, Xiancai; Wang, Rucheng

    2014-12-28

    We report a first principles molecular dynamics (FPMD) study of surface acid chemistry of the two growth surfaces of quartz, (101̄0) (including Alpha and Beta terminations) and (101̄1) facets. The interfacial hydration structures are characterized in detail and the intrinsic pKas of surface silanols are evaluated using the FPMD based vertical energy gap method. The calculated acidity constants reveal that every surface termination shows a bimodal acid-base behavior. It is found that all doubly-protonated forms (i.e. SiOH2) on the three terminations have pKas lower than -2.5, implying that the silanols hardly get protonated in a common pH range. The pKas of surface silanols can be divided into 3 groups. The most acidic silanol is the donor SiOH on the (101̄0)-beta surface (pKa = 4.8), the medium includes the germinal silanol on (101̄0)-alpha and the outer silanol on (101̄1) (pKa = 8.5-9.3) and the least acidic are inner silanols on the (101̄1)-facet, acceptor SiOH on (101̄0)-beta, and the secondly-deprotonated OH (i.e. Si(O-)(OH)) on (101̄0)-alpha (pKa > 11.0). With the pKa values, we discuss the implication for understanding metal cations complexing on quartz surfaces.

  1. Humic acid adsorption and surface charge effects on schwertmannite and goethite in acid sulphate waters.

    PubMed

    Kumpulainen, Sirpa; von der Kammer, Frank; Hofmann, Thilo

    2008-04-01

    In acid conditions, as in acid mine drainage waters, iron oxide particles are positively charged, attracting negatively charged organic particles present in surrounding natural waters. Schwertmannite (Fe8O8(OH)6SO4) and goethite (alpha-FeOOH) are the most typical iron oxide minerals found in mine effluents. We studied schwertmannite formation in the presence of humic acid. Further, surface charge and adsorption of humic acid on synthetic schwertmannite and goethite surfaces in pH 2-9 and in humic acid concentrations of 0.1-100 mg/L C were examined. Schwertmannite did precipitate despite the presence of humic acid, although it contained more sulphate and had higher specific surface area than ordinary schwertmannite. Specific surface area weighted results showed that schwertmannite and goethite had similar humic acid adsorption capacities. Sulphate was released from schwertmannite surfaces with increasing pH, resulting in an increase in specific surface area. Presence of sulphate in solution decreased the surface charge of schwertmannite and goethite similarly, causing coagulation. In acid conditions (pH 2-3.5), according to the zeta potential, schwertmannite is expected to coagulate even in the presence of high concentrations of humic acid (< or = 100 mg/L C). However, at high humic acid concentrations (10-100 mg/L C) with moderate acid conditions (pH>3.5), both schwertmannite and goethite surfaces are strongly negatively charged (zeta potential < -30 mV) thus posing a risk for colloid stabilization and colloidal transport. PMID:18221768

  2. Reduction of oxide microtrenching by electron beam assisted etching

    NASA Astrophysics Data System (ADS)

    Watanabe, M.; Shaw, D. M.; Collins, G. J.

    2000-10-01

    High density plasma etching of submicron wide oxide trenches often results in non-ideal etched features. For example, microtrenching is the result of higher etch rate near the side wall as compared to the center of the trench. Herein, we apply a previously reported[1] high energy (100 - 900 eV) electron beam directed at the etching wafer surface to reduce microtrenching during the etching of 0.5 micron wide silicon dioxide (SiO2) trench patterns in an inductively coupled fluorocarbon plasma. The directed electron beam neutralizes the positive charge buildup at the bottom of the trench and reduces the microtrench formation. Scanning Electron Microscopy (SEM) images of features etched with and without the electron beam show that the electron beam is effective in reducing microtrenching. [1] D. M. Shaw, M. Watanabe, G. J. Collins, and H. Sugai, Jpn. J. Appl. Phys. 38, 87 (1999).

  3. Laser-assisted dry etching of III-nitride wide band gap semiconductor materials

    NASA Astrophysics Data System (ADS)

    Leonard, Robert Tyler

    Laser assisted dry etching is a materials processing technique capable of producing highly anisotropic etch features with precise etch depth control and little contamination. The technique is simple: laser radiation is combined with a gaseous chemical etchant to remove material in pattern selected regions. The advantages of laser etching include the removal of etch products with photonic energy instead of ion bombardment, potential of projected patterning to combine growth and etching in situ without exposure to air, production of distinct sidewall etch features for device structures, and precise control of etching with a highly directional pulsed laser energy source. The use of pulsed laser radiation allows for pulsed etch depth control, ultimately resulting in atomic layer control. Laser assisted dry HCl etching of GaN, AlGaN and InGaN optical device materials was first demonstrated in our laboratory at North Carolina State University in a modified UHV vacuum chamber and ArF (193nm) excimer laser. Effective masking materials of Al and SiOsb2 were determined to be resistant to laser heating and HCl environment for laser etching. The process variables of laser intensity and HCl pressure were found to be dominant with the necessary condition that no etching occurs without both the excimer laser and HCl present. Successful laser etching of GaN, AlGaN, and InGaN was demonstrated indicating that deep etch features with distinct sidewall features are possible with this technique. Laser etching of a III-Nitride quantum well double heterostructure resulted in no degradation of the photoluminescence response. Also, reduction of etch damage with laser etching may be possible in comparison to ion etching. Finally, a proposed model for the etching mechanism includes the photothermal release of nitrogen from the GaN surface resulting in a Ga-rich surface which is removed by the HCl etchant.

  4. 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.

  5. 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.

  6. 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.

  7. Nanoscale dry etching of germanium by using inductively coupled CF4 plasma

    NASA Astrophysics Data System (ADS)

    Shim, Kyu-Hwan; Yang, Ha Yong; Kil, Yeon-Ho; Yang, Hyeon Deok; Yang, Jong-Han; Hong, Woong-Ki; Kang, Sukill; Jeong, Tae Soo; Kim, Taek Sung

    2012-08-01

    The nanoscale dry etching of germanium was investigated by using inductively coupled CF4 plasma and electron-beam lithography. The optimal dose of PMMA as E-beam lithography resist was ˜200 mC/cm2. When ICP Power was 200W, CF4 gas flow rate was 40 sccm, and process pressure was 20 mTorr, it had a smooth surface and good etch rate. The etching selectivity of Ge wafer to PMMA resist was as low as ˜1.5. Various sub-100 nm dry-etching patterns have been obtained. SEM pictures showed good profile qualities with a smooth etching sidewall and ultrasmall etching features.

  8. Chemical downstream etching of tungsten

    SciTech Connect

    Blain, M.G.; Jarecki, R.L.; Simonson, R.J.

    1998-07-01

    The downstream etching of tungsten and tungsten oxide has been investigated. Etching of chemical vapor deposited tungsten and e-beam deposited tungsten oxide samples was performed using atomic fluorine generated by a microwave discharge of argon and NF{sub 3}. Etching was found to be highly activated with activation energies approximated to be 6.0{plus_minus}0.5thinspkcal/mol and 5.4{plus_minus}0.4thinspkcal/mol for W and WO{sub 3}, respectively. In the case of F etching of tungsten, the addition of undischarged nitric oxide (NO) directly into the reaction chamber results in the competing effects of catalytic etch rate enhancement and the formation of a nearly stoichiometric WO{sub 3} passivating tungsten oxide film, which ultimately stops the etching process. For F etching of tungsten oxide, the introduction of downstream NO reduces the etch rate. {copyright} {ital 1998 American Vacuum Society.}

  9. Expanding the diversity of unnatural cell surface sialic acids

    SciTech Connect

    Luchansky, Sarah J.; Goon, Scarlett; Bertozzi, Carolyn R.

    2003-10-30

    Novel chemical reactivity can be introduced onto cell surfaces through metabolic oligosaccharide engineering. This technique exploits the substrate promiscuity of cellular biosynthetic enzymes to deliver unnatural monosaccharides bearing bioorthogonal functional groups into cellular glycans. For example, derivatives of N-acetylmannosamine (ManNAc) are converted by the cellular biosynthetic machinery into the corresponding sialic acids and subsequently delivered to the cell surface in the form of sialoglycoconjugates. Analogs of N-acetylglucosamine (GlcNAc) and N-acetylgalactosamine (GalNAc) are also metabolized and incorporated into cell surface glycans, likely through the sialic acid and GalNAc salvage pathways, respectively. Furthermore, GlcNAc analogs can be incorporated into nucleocytoplasmic proteins in place of {beta}-O-GlcNAc residues. These pathways have been exploited to integrate unique electrophiles such as ketones and azides into the target glycoconjugate class. These functional groups can be further elaborated in a chemoselective fashion by condensation with hydrazides and by Staudinger ligation, respectively, thereby introducing detectable probes onto the cell. In conclusion, sialic acid derivatives are efficient vehicles for delivery of bulky functional groups to cell surfaces and masking of their hydroxyl groups improves their cellular uptake and utilization. Furthermore, the successful introduction of photoactivatable aryl azides into cell surface glycans opens up new avenues for studying sialic acid-binding proteins and elucidating the role of sialic acid in essential processes such as signaling and cell adhesion.

  10. Surface reactions of iron - enriched smectites: adsorption and transformation of hydroxy fatty acids and phenolic acids

    NASA Astrophysics Data System (ADS)

    Polubesova, Tamara; Olshansky, Yaniv; Eldad, Shay; Chefetz, Benny

    2014-05-01

    Iron-enriched smectites play an important role in adsorption and transformation of soil organic components. Soil organo-clay complexes, and in particular humin contain hydroxy fatty acids, which are derived from plant biopolymer cutin. Phenolic acids belong to another major group of organic acids detected in soil. They participate in various soil processes, and are of concern due to their allelopathic activity. We studied the reactivity of iron-enriched smectites (Fe(III)-montmorillonite and nontronite) toward both groups of acids. We used fatty acids- 9(10),16-dihydroxypalmitic acid (diHPA), isolated from curtin, and 9,10,16-trihydroxypalmitic acid (triHPA); the following phenolic acids were used: ferulic, p-coumaric, syringic, and vanillic. Adsorption of both groups of acids was measured. The FTIR spectra of fatty acid-mineral complexes indicated inner-sphere complexation of fatty acids with iron-enriched smectites (versus outer-sphere complexation with Ca(II)-montmorillonite). The LC-MS results demonstrated enhanced esterification of fatty acids on the iron-enriched smectite surfaces (as compared to Ca(II)-montmorillonite). This study suggests that fatty acids can be esterified on the iron-enriched smectite surfaces, which results in the formation of stable organo-mineral complexes. These complexes may serve as a model for the study of natural soil organo-clay complexes and humin. The reaction of phenolic acids with Fe(III)-montmorillonite demonstrated their oxidative transformation by the mineral surfaces, which was affected by molecular structure of acids. The following order of their transformation was obtained: ferulic >syringic >p-coumaric >vanillic. The LC-MS analysis demonstrated the presence of dimers, trimers, and tetramers of ferulic acid on the surface of Fe(III)-montmorillonite. Oxidation and transformation of ferulic acid were more intense on the surface of Fe(III)-montmorillonite as compared to Fe(III) in solution due to stronger complexation on

  11. Selectively-etched nanochannel electrophoretic and electrochemical devices

    DOEpatents

    Surh, Michael P.; Wilson, William D.; Barbee, Jr., Troy W.; Lane, Stephen M.

    2004-11-16

    Nanochannel electrophoretic and electrochemical devices having selectively-etched nanolaminates located in the fluid transport channel. The normally flat surfaces of the nanolaminate having exposed conductive (metal) stripes are selectively-etched to form trenches and baffles. The modifications of the prior utilized flat exposed surfaces increase the amount of exposed metal to facilitate electrochemical redox reaction or control the exposure of the metal surfaces to analytes of large size. These etched areas variously increase the sensitivity of electrochemical detection devices to low concentrations of analyte, improve the plug flow characteristic of the channel, and allow additional discrimination of the colloidal particles during cyclic voltammetry.

  12. Selectively-etched nanochannel electrophoretic and electrochemical devices

    DOEpatents

    Surh, Michael P.; Wilson, William D.; Barbee, Jr., Troy W.; Lane, Stephen M.

    2006-06-27

    Nanochannel electrophoretic and electrochemical devices having selectively-etched nanolaminates located in the fluid transport channel. The normally flat surfaces of the nanolaminate having exposed conductive (metal) stripes are selectively-etched to form trenches and baffles. The modifications of the prior utilized flat exposed surfaces increase the amount of exposed metal to facilitate electrochemical redox reaction or control the exposure of the metal surfaces to analytes of large size. These etched areas variously increase the sensitivity of electrochemical detection devices to low concentrations of analyte, improve the plug flow characteristic of the channel, and allow additional discrimination of the colloidal particles during cyclic voltammetry.

  13. 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.

  14. Physics and chemistry of complex oxide etching and redeposition control

    NASA Astrophysics Data System (ADS)

    Margot, Joëlle

    2012-10-01

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

  15. 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.

  16. Effects of Ti surface treatments with silane and arginylglycylaspartic acid peptide on bone cell progenitors.

    PubMed

    Chen, Wen-Cheng; Lo, Yang; Chen, Hong-Sen

    2015-09-01

    Achieving optimal aesthetic appearance is a major objective in dental implant design, and the interaction between the materials and the bone cell progenitors is an important factor in the attainment of this objective. In this study, a novel concept was evaluated by varying the surface modifications on titanium (Ti). Different levels of roughness can be attained by machine grinding (M), sand blasting, and acid etching (SLA) of the samples. The behavior of bone cell progenitors (D1) on the surfaces of Ti disks with different surface modifications was investigated. The surfaces of M or SLA disks were silanized (MS or SLAS group) through treatment with silane/Gly-Arg-Gly-Asp-Ser (GRGDS) peptide (MSP or SLASP group) and anchored particles of tetracalcium phosphate (TTCP) on the specimen surfaces (SLA-TTCP group). Physicochemical analysis was performed by metallographic microscopy, scanning electron microscopy, and contact angle analysis. The proliferation and the quantitative alkaline phosphatase (ALP) production of D1 cells on the surface of different sample groups were determined. The SLASP group had a significantly larger D1 cell proliferation than the other groups after 4 and 7 d of incubation (p < 0.05). ALP expression was a very early marker of differentiation, and was the first indication of the increasing number of cells at 7 d of culture. Among the groups in the M substrate series (i.e., M, MS, and MSP) and in the SLA series (i.e., SLA, SLAS, and SLASP), the MSP and SLASP specimens exhibited superior differentiation abilities on respective cultures until day 7 and day 10. A high number of hydrophilic surfaces dominated cell proliferation in the early stage of cell attachment. However, factors affecting the pore structure and the surface morphology can improve cell proliferation and differentiation. According to analyses of proliferation and ALP expression of bone cell progenitors D1, the original SLA implant surface can be improved with surface treatment

  17. Aluminum in acidic surface waters: chemistry, transport, and effects.

    PubMed Central

    Driscoll, C T

    1985-01-01

    Ecologically significant concentrations of Al have been reported in surface waters draining "acid-sensitive" watersheds that are receiving elevated inputs of acidic deposition. It has been hypothesized that mineral acids from atmospheric deposition have remobilized Al previously precipitated within the soil during soil development. This Al is then thought to be transported to adjacent surface waters. Dissolved mononuclear Al occurs as aquo Al, as well as OH-, F-, SO4(2-), and organic complexes. Although past investigations have often ignored non-hydroxide complexes of Al, it appears that organic and F complexes are the predominant forms of Al in dilute (low ionic strength) acidic surface waters. The concentration of inorganic forms of Al increases exponentially with decreases in solution pH. This response is similar to the theoretical pH dependent solubility of Al mineral phases. The concentration of organic forms of Al, however, is strongly correlated with variations in organic carbon concentration of surface waters rather than pH. Elevated concentrations of Al in dilute acidic waters are of interest because: Al is an important pH buffer; Al may influence the cycling of important elements like P, organic carbon, and trace metals; and Al is potentially toxic to aquatic organisms. An understanding of the aqueous speciation of Al is essential for an evaluation of these processes. PMID:3935428

  18. Aluminum in acidic surface waters: chemistry, transport, and effects.

    PubMed

    Driscoll, C T

    1985-11-01

    Ecologically significant concentrations of Al have been reported in surface waters draining "acid-sensitive" watersheds that are receiving elevated inputs of acidic deposition. It has been hypothesized that mineral acids from atmospheric deposition have remobilized Al previously precipitated within the soil during soil development. This Al is then thought to be transported to adjacent surface waters. Dissolved mononuclear Al occurs as aquo Al, as well as OH-, F-, SO4(2-), and organic complexes. Although past investigations have often ignored non-hydroxide complexes of Al, it appears that organic and F complexes are the predominant forms of Al in dilute (low ionic strength) acidic surface waters. The concentration of inorganic forms of Al increases exponentially with decreases in solution pH. This response is similar to the theoretical pH dependent solubility of Al mineral phases. The concentration of organic forms of Al, however, is strongly correlated with variations in organic carbon concentration of surface waters rather than pH. Elevated concentrations of Al in dilute acidic waters are of interest because: Al is an important pH buffer; Al may influence the cycling of important elements like P, organic carbon, and trace metals; and Al is potentially toxic to aquatic organisms. An understanding of the aqueous speciation of Al is essential for an evaluation of these processes.

  19. Aspect-ratio-dependent etching of polymers as interlayer dielectrics

    NASA Astrophysics Data System (ADS)

    Kim, Gusung

    2000-08-01

    The reactive ion etching of the polymer has been studied in CF4-O2, SF6, and N2 plasmas to understand the contributions of aspect-ratio dependent etching (ARDE), an anisotropic etch profiles, and the etch rate for one of low-k polymers, Divinyl bis-benzocyclobutene (BCB, silicon containing spin-on polymer). A new experimental process (Type B) was implemented to determine the ARDE in which the AR remains constant during the entire experiment. These samples showed the uniform etch rate for all trenches. However, in conventional structure (Type A), using a SiO2 hardmask for patterning, ARDE phenomena can be observed. In the range of 30--35% CF4 in O2, BCB shows the maximum etch rate, and this coincides with the maximum in the oxygen concentration. Complete anisotropic profiles can be obtained at low pressure where the fluorine atom concentration is low. The highest etch rates are achieved at the higher pressures where fluorine and oxygen atom concentrations are high, but with an increase in the amount of profile tapering in Type A. In Type B samples, etching gives increased undercutting and bowing with an increase in pressure. At low pressure, the sidewall profile is vertical regardless of the aspect ratio of the pattern. No oxide is exposed to the CF4-O2 plasma and undercutting occurs with an increase of fluorine concentration. In large trenches, polymer residue and micromasking phenomena were observed in both cases. Specifically, the surface roughness of etched BCB in CF 4-O2 was much higher than in SF6 and N2. Lateral etching of the BCB, mask erosion and faceting of the hardmask were more prominently observed with SF6. SF6 produces a very clean surface and no residue at the bottom of a trench. In N2 plasma, the etch rate of BCB is very low due to physical ion bombardment and trenches are formed by mask erosion and micro-trenching.

  20. Patterning of platinum (Pt) thin films by chemical wet etching in Aqua Regia

    NASA Astrophysics Data System (ADS)

    Köllensperger, P. A.; Karl, W. J.; Ahmad, M. M.; Pike, W. T.; Green, M.

    2012-06-01

    The chemical and physical properties of platinum (Pt) make it a useful material for microelectromechanical systems and microfluidic applications such as lab-on-a-chip devices. Platinum thin-films are frequently employed in applications where electrodes with high chemical stability, low electrical resistance or a high melting point are needed. Due to its chemical inertness it is however also one of the most difficult metals to pattern. The gold standard for patterning is chlorine RIE etching, a capital-intensive process not available in all labs. Here we present simple fabrication protocols for wet etching Pt thin-films in hot Aqua Regia based on sputtered Ti/Pt/Cr and Cr/Pt/Cr metal multilayers. Chromium (Cr) or titanium (Ti) is used as an adhesion layer for the Pt. Cr is used as a hard masking layer during the Pt etch as it can be easily and accurately patterned with photoresist and withstands the Aqua Regia. The Cr pattern is transferred into the Pt and the Cr mask later removed. Only standard chemicals and cleanroom equipment/tools are required. Prior to the Aqua Regia etch any surface passivation on the Pt is needs to be removed. This is usually achieved by a quick dip in dilute hydrofluoric acid (HF). HF is usually also used for wet-etching the Ti adhesion layer. We avoid the use of HF for both steps by replacing the HF-dip with an argon (Ar) plasma treatment and etching the Ti layer with a hydrogen peroxide (H2O2) based etchant.

  1. Surface interactions of cesium and boric acid with stainless steel

    SciTech Connect

    Grossman-Canfield, N.

    1995-08-01

    In this report, the effects of cesium hydroxide and boric acid on oxidized stainless steel surfaces at high temperatures and near one atmosphere of pressure are investigated. This is the first experimental investigation of this chemical system. The experimental investigations were performed using a mass spectrometer and a mass electrobalance. Surfaces from the different experiments were examined using a scanning electron microscope to identify the presence of deposited species, and electron spectroscopy for chemical analysis to identify the species deposited on the surface. A better understanding of the equilibrium thermodynamics, the kinetics of the steam-accelerated volatilizations, and the release kinetics are gained by these experiments. The release rate is characterized by bulk vaporization/gas-phase mass transfer data. The analysis couples vaporization, deposition, and desorption of the compounds formed by cesium hydroxide and boric acid under conditions similar to what is expected during certain nuclear reactor accidents. This study shows that cesium deposits on an oxidized stainless steel surface at temperatures between 1000 and 1200 Kelvin. Cesium also deposits on stainless steel surfaces coated with boric oxide in the same temperature ranges. The mechanism for cesium deposition onto the oxide layer was found to involve the chemical reaction between cesium and chromate. Some revaporization in the cesium hydroxide-boric acid system was observed. It has been found that under the conditions given, boric acid will react with cesium hydroxide to form cesium metaborate. A model is proposed for this chemical reaction.

  2. 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.

  3. Experimental investigation of photoresist etching by kHz AC atmospheric pressure plasma jet

    NASA Astrophysics Data System (ADS)

    Wang, Lijun; Zheng, Yashuang; Wu, Chen; Jia, Shenli

    2016-11-01

    In this study, the mechanism of the photoresist (PR) etching by means of a kHz AC atmospheric pressure plasma jet (APPJ) is investigated. The scanning electron (SEM) and the polarizing microscope are used to perform the surface analysis, and the mechanical profilometry is applied to diagnose the etch rate. The results show that granulated structure with numerous microparticles appears at the substrate surface after APPJ treatment, and the etch rate in the etch center is the fastest and gradually slows down to the edge of etch region. In addition, the pin-ring electrode APPJ has the highest etch rate at but easy to damage the Si wafer, the double-ring APPJ is the most stable but requires long time to achieve the ideal etch result, and the etch rate and the etch result of the multi-electrode APPJ fall in between. Ar APPJ had much higher PR etch rate and more irregular etch trace than He APPJ. It is speculated that Ar APPJ is more energetic and effective in transferring reactive species to the PR surface. It is also observed that the effective etch area initially increases and then decreases as plasma jet outlet to the PR surface distance increases.

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

    NASA Astrophysics Data System (ADS)

    Zhu, Weiye; Sridhar, Shyam; Liu, Lei; Hernandez, Eduardo; Donnelly, Vincent M.; Economou, Demetre J.

    2014-05-01

    Cl2, Br2, HBr, Br2/Cl2, and HBr/Cl2 feed gases diluted in Ar (50%-50% by volume) were used to study etching of p-type Si(100) in a rf inductively coupled, Faraday-shielded plasma, with a focus on the photo-assisted etching component. Etching rates were measured as a function of ion energy. Etching at ion energies below the threshold for ion-assisted etching was observed in all cases, with Br2/Ar and HBr/Cl2/Ar plasmas having the lowest and highest sub-threshold etching rates, respectively. Sub-threshold etching rates scaled with the product of surface halogen coverage (measured by X-ray photoelectron spectroscopy) and Ar emission intensity (7504 Å). Etching rates measured under MgF2, quartz, and opaque windows showed that sub-threshold etching is due to photon-stimulated processes on the surface, with vacuum ultraviolet photons being much more effective than longer wavelengths. Scanning electron and atomic force microscopy revealed that photo-etched surfaces were very rough, quite likely due to the inability of the photo-assisted process to remove contaminants from the surface. Photo-assisted etching in Cl2/Ar plasmas resulted in the formation of 4-sided pyramidal features with bases that formed an angle of 45° with respect to ⟨110⟩ cleavage planes, suggesting that photo-assisted etching can be sensitive to crystal orientation.

  5. 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.

  6. Low Temperature Silicon Surface Cleaning by HF Etching/Ultraviolet Ozone Cleaning (HF/UVOC) Method (I)—Optimization of the HF Treatment—

    NASA Astrophysics Data System (ADS)

    Suemitsu, Maki; Kaneko, Tetsuya; Miyamoto, Nobuo

    1989-12-01

    Several variations of fluoric acid (HF) treatments of silicon substrates were examined for their adaptability as a pretreatment method for a silicon epitaxy process. Treatments with and without distilled, deionized (DI) water rinse, of different HF concentrations, and of different methods of HF supply were tested and their residual carbonic impurity contents were measured using RHEED. As a result, HF treatments by themselves were found to be insufficient in passivating the surface dangling bonds irrespective of the method of HF supply: dipping into the solution or exposure to the vapor. The optimum procedure of HF treatment thus proposed is a succession of (a) HF dipping, (b) DI-water rinsing, (c) nitrogen-gas blowing, and (d) UV-ozone cleaning.

  7. Surface characteristic changes of dental ceramics after cyclic immersion in acidic agents and titratable acidity.

    PubMed

    Junpoom, Peerapong; Kukiattrakoon, Boonlert; Hengtrakool, Chanothai

    2010-12-01

    The potential erosive effect of acidic food, sour fruits and drinks on all-ceramic restorations used in dentistry has not been clearly documented. Surface characteristic changes have been evaluated and compared for disc-shaped specimens (diameter 12.0 mm and thickness 2.0 mm) of fluorapatite-leucite and fluorapatite ceramics using various storage agents (deionized water, citrate buffer solution, pineapple juice, green mango juice, cola soft drink and 4% acetic acid). Immersion in pineapple juice, green mango juice, cola soft drink and 4% acetic acid for 16 hours produce significant increases in surface roughness for both types of ceramics investigated.

  8. Focused electron-beam-induced etching of silicon dioxide

    SciTech Connect

    Randolph, S.J.; Fowlkes, J.D.; Rack, P.D.

    2005-08-01

    Focused electron-beam (FEB)-induced etching of silicon dioxide with xenon difluoride has been investigated as a selective nanoscale etching technique. In order to gain an understanding of the parameters that control etch rate and etch efficiency, the effects of beam current, beam energy, and scan rate conditions on the FEB process were examined. High etch rates were obtained for low beam energy, high beam current, and high scan rates. Experimental results also indicated that the FEB etch process is governed by the electron-stimulated desorption of oxygen from the SiO{sub 2} matrix, and subsequently rate limited by XeF{sub 2} availability. Based on experimental evidence and existing literature, a simple, two-step model was introduced to qualitatively describe the etch mechanism. The model involves a cyclical process, which is initiated by the reduction of a surface layer of SiO{sub 2} to elemental silicon. The exposed silicon surface is then removed by a chemical-mediated etch reaction.

  9. Focused electron-beam-induced etching of silicon dioxide

    NASA Astrophysics Data System (ADS)

    Randolph, S. J.; Fowlkes, J. D.; Rack, P. D.

    2005-08-01

    Focused electron-beam (FEB)-induced etching of silicon dioxide with xenon difluoride has been investigated as a selective nanoscale etching technique. In order to gain an understanding of the parameters that control etch rate and etch efficiency, the effects of beam current, beam energy, and scan rate conditions on the FEB process were examined. High etch rates were obtained for low beam energy, high beam current, and high scan rates. Experimental results also indicated that the FEB etch process is governed by the electron-stimulated desorption of oxygen from the SiO2 matrix, and subsequently rate limited by XeF2 availability. Based on experimental evidence and existing literature, a simple, two-step model was introduced to qualitatively describe the etch mechanism. The model involves a cyclical process, which is initiated by the reduction of a surface layer of SiO2 to elemental silicon. The exposed silicon surface is then removed by a chemical-mediated etch reaction.

  10. Hydrothermal Etching Treatment to Rutile TiO2 Nanorod Arrays for Improving the Efficiency of CdS-Sensitized TiO2 Solar Cells.

    PubMed

    Wan, Jingshu; Liu, Rong; Tong, Yuzhu; Chen, Shuhuang; Hu, Yunxia; Wang, Baoyuan; Xu, Yang; Wang, Hao

    2016-12-01

    Highly ordered TiO2 nanorod arrays (NRAs) were directly grown on an F:SnO2 (FTO) substrate without any seed layer by hydrothermal route. For a larger surface area, the second-step hydrothermal treatment in hydrochloric acid was carried out to the as-prepared TiO2 NRAs. The results showed that the center portion of the TiO2 nanorods were dissolved in the etching solution to form a nanocave at the initial etching process. As the etching time extended, the tip parts of the nanocave wall split into lots of nanowires with a reduced diameter, giving rise to a remarkable increase of specific surface area for the TiO2 NRAs. The TiO2 films after etching treatment were sensitized by CdS quantum dots (QDs) to fabricate quantum dot-sensitized solar cells (QDSSCs), which exhibited a significant improvement in the photocurrent density in comparison with that of the un-treated device, this mainly attributed to the enhancement of QD loading and diffused reflectance ability. Through modifying the etching TiO2 films with TiCl4, a relatively high power conversion efficiency (PCE) of 3.14 % was obtained after optimizing the etching time.

  11. Hydrothermal Etching Treatment to Rutile TiO2 Nanorod Arrays for Improving the Efficiency of CdS-Sensitized TiO2 Solar Cells

    NASA Astrophysics Data System (ADS)

    Wan, Jingshu; Liu, Rong; Tong, Yuzhu; Chen, Shuhuang; Hu, Yunxia; Wang, Baoyuan; Xu, Yang; Wang, Hao

    2016-01-01

    Highly ordered TiO2 nanorod arrays (NRAs) were directly grown on an F:SnO2 (FTO) substrate without any seed layer by hydrothermal route. For a larger surface area, the second-step hydrothermal treatment in hydrochloric acid was carried out to the as-prepared TiO2 NRAs. The results showed that the center portion of the TiO2 nanorods were dissolved in the etching solution to form a nanocave at the initial etching process. As the etching time extended, the tip parts of the nanocave wall split into lots of nanowires with a reduced diameter, giving rise to a remarkable increase of specific surface area for the TiO2 NRAs. The TiO2 films after etching treatment were sensitized by CdS quantum dots (QDs) to fabricate quantum dot-sensitized solar cells (QDSSCs), which exhibited a significant improvement in the photocurrent density in comparison with that of the un-treated device, this mainly attributed to the enhancement of QD loading and diffused reflectance ability. Through modifying the etching TiO2 films with TiCl4, a relatively high power conversion efficiency (PCE) of 3.14 % was obtained after optimizing the etching time.

  12. Reactive ion etching (RIE) technique for application in crystalline silicon solar cells

    SciTech Connect

    Yoo, Jinsu

    2010-04-15

    Saw damage removal (SDR) and texturing by conventional wet chemical processes with alkali solution etch about 20 micron of silicon wafer on both sides, resulting in thin wafers with which solar cell processing is difficult. Reactive ion etching (RIE) for silicon surface texturing is very effective in reducing surface reflectance of thin crystalline silicon wafers by trapping the light of longer wavelength. High efficiency solar cells were fabricated during this study using optimized RIE. Saw damage removal (SDR) with acidic mixture followed by RIE-texturing showed the decrease in silicon loss by {proportional_to}67% and {proportional_to}70% compared to conventional SDR and texturing by alkaline solution. Also, the crystalline silicon solar cells fabricated by using RIE-texturing showed conversion efficiency as high as 16.7% and 16.1% compared with 16.2%, which was obtained in the case of the cell fabricated with SDR and texturing with NaOH solution. (author)

  13. Surface acidity and degree of carburization of modified silver catalysts

    SciTech Connect

    Pestryakov, A.N.; Belousova, V.N.; Roznina, M.I.

    1993-11-10

    The effect has been studied of some compounds as modifying additives on the surface acidity, degree of carburization, aggregation and silver entrainement of silver-pumice catalysts for methanol oxidation. Catalyst samples have been tested in an industrial reactor. The probable mechanism of modifying action of the additives is discussed.

  14. Optical diagnostic instrument for monitoring etch uniformity during plasma etching of polysilicon in a chlorine-helium plasma

    SciTech Connect

    Hareland, W.A.; Buss, R.J.

    1993-06-01

    Nonuniform etching is a serious problem in plasma processing of semiconductor materials and has important consequences in the quality and yield of microelectronic components. In many plasmas, etching occurs at a faster rate near the periphery of the wafer, resulting in nonuniform removal of specific materials over the wafer surface. This research was to investigate in situ optical diagnostic techniques for monitoring etch uniformity during plasma processing of microelectronic components. We measured 2-D images of atomic chlorine at 726 nm in a chlorine-helium plasma during plasma etching of polysilicon in a parallel-plate plasma etching reactor. The 3-D distribution of atomic chlorine was determined by Abel inversion of the plasma image. The experimental results showed that the chlorine atomic emission intensity is at a maximum near the outer radius of the plasma and decreases toward the center. Likewise, the actual etch rate, as determined by profilometry on the processed wafer, was approximately 20% greater near the edge of the wafer than at its center. There was a direct correlation between the atomic chlorine emission intensity and the etch rate of polysilicon over the wafer surface. Based on these analyses, 3-D imaging would be a useful diagnostic technique for in situ monitoring of etch uniformity on wafers.

  15. 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

  16. Chlorine-based dry etching of β-Ga2O3

    NASA Astrophysics Data System (ADS)

    Hogan, Jack E.; Kaun, Stephen W.; Ahmadi, Elaheh; Oshima, Yuichi; Speck, James S.

    2016-06-01

    Reactive ion etching (RIE) and inductively coupled plasma (ICP) etching techniques were used to determine the optimal dry etch conditions for β-Ga2O3. RF power and chamber pressure were examined to study their effects on etch rate and surface roughness for three crystallographic planes, i.e., (100); (010); and (\\bar{2}01) by RIE. BCl3 etch rate calibrations were performed on all β-Ga2O3 planes studied, in comparison to Cl2. RIE yielded moderate etch rates (<20 nm min‑1), and surface roughness showed no clear trend with RF power. Moreover, the effect of bias power, plasma power, and the choice of etchant were studied using ICP. The etches performed by ICP were shown to be superior to RIE in both etch rate and surface roughness, due to the much higher plasma densities and uniformities possible with plasma powers beyond those realized in RIE. The maximum etch rate of 43.0 nm min‑1 was achieved using BCl3 in ICP. SF6/BCl3 mixtures, which yield high GaN etch rates, were also studied. However, in contrast to GaN etching, SF6/BCl3 was found to be far less effective than pure BCl3 in etching β-Ga2O3.

  17. Rapid recipe formulation for plasma etching of new materials

    NASA Astrophysics Data System (ADS)

    Chopra, Meghali; Zhang, Zizhuo; Ekerdt, John; Bonnecaze, Roger T.

    2016-03-01

    A fast and inexpensive scheme for etch rate prediction using flexible continuum models and Bayesian statistics is demonstrated. Bulk etch rates of MgO are predicted using a steady-state model with volume-averaged plasma parameters and classical Langmuir surface kinetics. Plasma particle and surface kinetics are modeled within a global plasma framework using single component Metropolis Hastings methods and limited data. The accuracy of these predictions is evaluated with synthetic and experimental etch rate data for magnesium oxide in an ICP-RIE system. This approach is compared and superior to factorial models generated from JMP, a software package frequently employed for recipe creation and optimization.

  18. Metal-assisted chemical etch porous silicon formation method

    DOEpatents

    Li, Xiuling; Bohn, Paul W.; Sweedler, Jonathan V.

    2004-09-14

    A thin discontinuous layer of metal such as Au, Pt, or Au/Pd is deposited on a silicon surface. The surface is then etched in a solution including HF and an oxidant for a brief period, as little as a couple seconds to one hour. A preferred oxidant is H.sub.2 O.sub.2. Morphology and light emitting properties of porous silicon can be selectively controlled as a function of the type of metal deposited, Si doping type, silicon doping level, and/or etch time. Electrical assistance is unnecessary during the chemical etching of the invention, which may be conducted in the presence or absence of illumination.

  19. Surface Behavior of Boronic Acid-Terminated Silicones.

    PubMed

    Mansuri, Erum; Zepeda-Velazquez, Laura; Schmidt, Rolf; Brook, Michael A; DeWolf, Christine E

    2015-09-01

    Silicone polymers, with their high flexibility, lie in a monolayer at the air-water interface as they are compressed until a critical pressure is reached, at which point multilayers are formed. Surface pressure measurements demonstrate that, in contrast, silicones that are end-modified with polar groups take up lower surface areas under compression because the polar groups submerge into the water phase. Boronic acids have the ability to undergo coordination with Lewis bases. As part of a program to examine the surface properties of boronic acids, we have prepared boronic acid-modified silicones (SiBAs) and examined them at the air-water interface to better understand if they behave like other end-functional silicones. Monolayers of silicones, aminopropylsilicones, and SiBAs were characterized at the air-water interface as a function of end functionalization and silicone chain length. Brewster angle and atomic force microscopies confirm domain formation and similar film morphologies for both functionalized and non-functionalized silicone chains. There is a critical surface pressure (10 mN m(-1)) independent of chain length that corresponds to a first-order phase transition. Below this transition, the film appears to be a homogeneous monolayer, whose thickness is independent of the chain length. Ellipsometry at the air-water interface indicates that the boronic acid functionality leads to a significant increase of film thickness at low molecular areas that is not seen for non-functionalized silicone chains. What differentiates the boronic acids from simple silicones or other end-functionalized silicones, in particular, is the larger area occupied by the headgroup when under compression compared to other or non-end-functionalized silicones, which suggests an in-plane rather than submerged orientation that may be driven by boronic acid self-complexation. PMID:26263385

  20. Optimum inductively coupled plasma etching of fused silica to remove subsurface damage layer

    NASA Astrophysics Data System (ADS)

    Jiang, Xiaolong; Liu, Ying; Liu, Zhengkun; Qiu, Keqiang; Xu, Xiangdong; Hong, Yilin; Fu, Shaojun

    2015-11-01

    In this work, we introduce an optimum ICP etching technique that successfully removes the subsurface damage (SSD) layer of fused silica without causing plasma induced surface damage (PISD) or lateral etching of SSD. As one of the commonest PISD initiators, metal contamination from reactor chamber is prevented by employing a simple isolation device. Based on this device, a unique low-density pitting damage is discovered and subsequently eliminated by optimizing the etching parameters. Meanwhile etching anisotropy also improves a lot, thus preventing the lateral etching of SSD. Using this proposed technique, SSD layer of fused silica is successfully removed with a surface roughness of 0.23 nm.

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

    NASA Astrophysics Data System (ADS)

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

    2016-04-01

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

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

    PubMed

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

    2016-12-01

    Friction-induced selective etching provides a convenient and practical way for fabricating protrusive nanostructures. A further understanding of this method is very important for establishing a controllable nanofabrication process. In this study, the effect of etching temperature on the formation of protrusive hillocks and surface properties of the etched silicon surface was investigated. It is found that the height of the hillock produced by selective etching increases with the etching temperature before the collapse of the hillock. The temperature-dependent selective etching rate can be fitted well by the Arrhenius equation. The etching at higher temperature can cause rougher silicon surface with a little lower elastic modulus and hardness. The contact angle of the etched silicon surface decreases with the etching temperature. It is also noted that no obvious contamination can be detected on silicon surface after etching at different temperatures. As a result, the optimized condition for the selective etching was addressed. The present study provides a new insight into the control and application of friction-induced selective nanofabrication. PMID:27119157

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

    PubMed

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

    2016-08-15

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

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

    PubMed

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

    2016-08-15

    A combination of scanning electrochemical cell microscopy (SECCM) and atomic force microscopy (AFM) is used to quantitatively study the acid-induced dissolution of dental enamel. A micron-scale liquid meniscus formed at the end of a dual barrelled pipette, which constitutes the SECCM probe, is brought into contact with the enamel surface for a defined period. Dissolution occurs at the interface of the meniscus and the enamel surface, under conditions of well-defined mass transport, creating etch pits that are then analysed via AFM. This technique is applied to bovine dental enamel, and the effect of various treatments of the enamel surface on acid dissolution (1mM HNO3) is studied. The treatments investigated are zinc ions, fluoride ions and the two combined. A finite element method (FEM) simulation of SECCM mass transport and interfacial reactivity, allows the intrinsic rate constant for acid-induced dissolution to be quantitatively determined. The dissolution of enamel, in terms of Ca(2+) flux ( [Formula: see text] ), is first order with respect to the interfacial proton concentration and given by the following rate law: [Formula: see text] , with k0=0.099±0.008cms(-1). Treating the enamel with either fluoride or zinc ions slows the dissolution rate, although in this model system the partly protective barrier only extends around 10-20nm into the enamel surface, so that after a period of a few seconds dissolution of modified surfaces tends towards that of native enamel. A combination of both treatments exhibits the greatest protection to the enamel surface, but the effect is again transient. PMID:27209395

  5. Influence of preliminary etching on the stability of bonds created by one-step self-etch bonding systems.

    PubMed

    Taschner, Michael; Nato, Fernando; Mazzoni, Annalisa; Frankenberger, Roland; Falconi, Mirella; Petschelt, Anselm; Breschi, Lorenzo

    2012-06-01

    We evaluated the effects of preliminary etching of dentine on the stability of the bond created by one-step self-etch adhesives under different storage conditions. Adper Easy Bond (3M ESPE) and iBond Self-Etch (iBond SE; Heraeus Kulzer) were applied with an etch-and-rinse (i.e. after preliminary phosphoric acid etching for 15 s) or a self-etch approach. Resin-dentine bonded specimens were sectioned perpendicularly to the adhesive interface according to the 'non-trimming technique'. Beams were stored in artificial saliva for 24 h, 6 months, or 1 yr at 37°C, or in 10% NaOCl for 5 h at room temperature, and then stressed until failure; the microtensile bond strengths were calculated. Interfacial nanoleakage of additional teeth was evaluated using light microscopy or transmission electron microscopy. Adper Easy Bond showed higher bond strength than iBond SE, regardless of the dentine treatment. Similar microtensile bond strength results were obtained for teeth subjected to artificial ageing in 10% NaOCl for 5 h at room temperature and for teeth stored in artific