• Title/Summary/Keyword: Hydrofluoric Acid Etching Treatment

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

  • Kursoglu, Pinar;Karagoz Motro, Pelin Fatma;Yurdaguven, Haktan
    • The Journal of Advanced Prosthodontics
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    • v.5 no.2
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    • pp.98-103
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    • 2013
  • 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 ($5mm{\times}5mm{\times}2mm$) 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 $37^{\circ}C$ 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 (${\alpha}$=0.05). RESULTS. Adhesion was significantly stronger in Group 2 ($3.88{\pm}1.94$ MPa) and Group 3 ($3.65{\pm}1.87$ MPa) than in Control group ($1.95{\pm}1.06$ MPa), in which bonding values were lowest (P<.01). No significant difference was observed between Group 4 ($3.59{\pm}1.19$ MPa) and Control group. Shear bond strength was highest in Group 1 ($8.42{\pm}1.86$ 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.

Influence of different surface treatments on bond strength of novel CAD/CAM restorative materials to resin cement

  • Komurcuoglu, Meltem Bektas;Sagirkaya, Elcin;Tulga, Ayca
    • The Journal of Advanced Prosthodontics
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    • v.9 no.6
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    • pp.439-446
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    • 2017
  • PURPOSE. To evaluate the effects of different surface treatments on the bond strength of novel CAD/CAM restorative materials to resin cement by four point bending test. MATERIALS AND METHODS. The CAD/CAM materials under investigation were e.max CAD, Mark II, Lava Ultimate, and Enamic. A total of 400 bar specimens ($4{\times}1.2{\times}12mm$) (n=10) milled from the CAD/CAM blocks underwent various pretreatments (no pretreatment (C), hydrofluoric acid (A), hydrofluoric acid + universal adhesive (Scotchbond) (AS), sandblasting (Sb), and sandblasting + universal adhesive (SbS)). The bars were luted end-to-end on the prepared surfaces with a dual curing adhesive resin cement (Variolink N, Ivoclar Vivadent) on the custom-made stainless steel mold. Ten test specimens for each treatment and material combination were performed with four point bending test method. Data were analyzed using ANOVA and Tukey's test. RESULTS. The surface treatment and type of CAD/CAM restorative material showed a significant effect on the four point bending strength (FPBS) (P<.001). For LDC, AS surface treatment showed the highest FPBS results ($100.31{\pm}10.7MPa$) and the lowest values were obtained in RNC ($23.63{\pm}9.0MPa$) for control group. SEM analyses showed that the surface topography of CAD/CAM restorative materials was modified after treatments. CONCLUSION. The surface treatment of sandblasting or HF acid etching in combination with a universal adhesive containing MDP can be suggested for the adhesive cementation of the novel CAD/CAM restorative materials.

Fabrication and Characterization of Dodecyl-derivatized Silicon Nanowires for Preventing Aggregation

  • Shin, Donghee;Sohn, Honglae
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3451-3455
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    • 2013
  • Single-crystalline silicon nanowires (SiNWs) were fabricated by using an electroless metal-assisted etching of bulk silicon wafers with silver nanoparticles obtained by wet electroless deposition. The etching of SiNWs is based on sequential treatment in aqueous solutions of silver nitrate followed by hydrofluoric acid and hydrogen peroxide. SEM observation shows that well-aligned nanowire arrays perpendicular to the surface of the Si substrate were produced. Free-standing SiNWs were then obtained using ultrasono-method in toluene. Alkyl-derivatized SiNWs were prepared to prevent the aggregation of SiNWs and obtained from the reaction of SiNWs and dodecene via hydrosilylation. Optical characterizations of SiNWs were achieved by FT-IR spectroscopy and indicated that the surface of SiNWs is terminated with hydrogen for fresh SiNWs and with dodecyl group for dodecyl-derivatized SiNWs, respectively. The main structures of dodecyl-derivatized SiNWs are wires and rods and their thicknesses of rods and wire are typically 150-250 and 10-20 nm, respectively. The morphology and chemical state of dodecyl-derivatized SiNWs are characterized by scanning electron microscopy, transmission electron microscopy, and X-ray photoelectron spectroscopy.

EFFECTS OF SURFACE TREATMENTS AND STORAGE CONDITIONS ON TARGIS/DENTIN BOND STRENGTH (Targis 표면처리가 상아질과의 전단결합강도에 미치는 영향)

  • Oh, Young-Taek;Hwang, Su-Jin;Lee, Se-Joon;Lee, Kwang-Won
    • Restorative Dentistry and Endodontics
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    • v.25 no.2
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    • pp.262-271
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    • 2000
  • The purpose of this study was to estimate shear bond strength according to difference in Targis surface treatment and storage condition. 140 non-carious extracted human molars and Targis D210(Ivoclar, Liechtenstein) were used in the present study and were divided into 7 experimental groups respectively according to surface treatment of Targis. Group 1 ; No treatment, Group 2 ; $50{\mu}m$ aluminium oxide blasting, Group 3 ; 4% HF etching for 3 minutes, Group 4 ; 4% HF etching after blasting, Group 5 ; silane treatment after blasting, Group 6 ; silane treatment after 4% HF etching, Group 7 ; silane treatment after blasting and 4% HF etching. In Each group, one half of 20 specimens was stored in distilled water at $37^{\circ}C$ for 24 hours and the other half was stored at atmosphere for 24 hours respectively. Dentin surface was etched with 10% $H_3PO_4$ for 15 seconds and luting cement(Variolink II, Vivadent, Liechtenstein) was applied by manufacturer's recommendation. Shear bond strength for each group was then measured. To examine the failure patterns after shear bond test and to observe the change after surface treatment of Targis. Specimens were fabricated and observed under the SEM. Statistical analysis was performed by One Way ANOVA test and t-test. The results were as follows ; 1. The shear bond strength of the groups stored in water significantly lower than that of groups stored at atmosphere (P<0.05). 2. There was no significant difference in shear bond strength in groups stored in water (P>0.05). 3. The shear bond strength without surface treatment of Targis were lowest among all experimental groups in atmosphere condition(P<0.05). 4. There was no significant difference in bond strength between groups using the silane or not(P>0.05). 5. The groups treated by blasting, hydrofluoric acid and silane sequentially showed highest bond strength than that of other groups in atmosphere condition, but there was no significant difference(P>0.05). 6 The proportions of the specimens showing the mixed fracture failure were 20% in HF etching group and blasting + HF group, 40% in blasting + HF + silane group in atmosphere condition. All the specimens stored in water showed adhesive fracture failure.

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Wet Etching Characteristics of Cu Surface for Cu-Cu Pattern Direct Bonds (Cu-Cu 패턴 직접접합을 위한 습식 용액에 따른 Cu 표면 식각 특성 평가)

  • Park, Jong-Myeong;Kim, Yeong-Rae;Kim, Sung-Dong;Kim, Jae-Won;Park, Young-Bae
    • Journal of the Microelectronics and Packaging Society
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    • v.19 no.1
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    • pp.39-45
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    • 2012
  • Three-dimensional integrated circuit(3D IC) technology has become increasingly important due to the demand for high system performance and functionality. In this work, BOE and HF wet etching of Cu line surfaces after CMP were conducted for Cu-Cu pattern direct bonding. Step height of Cu and $SiO_2$ as well as Cu dishing after Cu CMP were analyzed by the 3D-Profiler. Step height increased and Cu dishing decreased with increasing BOE and HF wet etching times. XPS analysis of Cu surface revealed that Cu surface oxide layer was partially removed by BOE and HF wet etching treatment. BOE treatment showed not only the effective $SiO_2$ etching but also reduced dishing and Cu surface oxide rather than HF treatment, which can be used as an meaningful process data for reliable Cu-Cu pattern bonding characteristics.

The effect of silane applied to glass ceramics on surface structure and bonding strength at different temperatures

  • Yavuz, Tevfik;Eraslan, Oguz
    • The Journal of Advanced Prosthodontics
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    • v.8 no.2
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    • pp.75-84
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    • 2016
  • PURPOSE. To evaluate the effect of various surface treatments on the surface structure and shear bond strength (SBS) of different ceramics. MATERIALS AND METHODS. 288 specimens (lithium-disilicate, leucite-reinforced, and glass infiltrated zirconia) were first divided into two groups according to the resin cement used, and were later divided into four groups according to the given surface treatments: G1 (hydrofluoric acid (HF)+silane), G2 (silane alone-no heat-treatment), G3 (silane alone-then dried with $60^{\circ}C$ heat-treatment), and G4 (silane alonethen dried with $100^{\circ}C$ heat-treatment). Two different adhesive luting systems were applied onto the ceramic discs in all groups. SBS (in MPa) was calculated from the failure load per bonded area (in $N/mm^2$). Subsequently, one specimen from each group was prepared for SEM evaluation of the separated-resin-ceramic interface. RESULTS. SBS values of G1 were significantly higher than those of the other groups in the lithium disilicate ceramic and leucite reinforced ceramic, and the SBS values of G4 and G1 were significantly higher than those of G2 and G3 in glass infiltrated zirconia. The three-way ANOVA revealed that the SBS values were significantly affected by the type of resin cement (P<.001). FIN ceramics had the highest rate of cohesive failure on the ceramic surfaces than other ceramic groups. AFM images showed that the surface treatment groups exhibited similar topographies, except the group treated with HF. CONCLUSION. The heat treatment was not sufficient to achieve high SBS values as compared with HF acid etching. The surface topography of ceramics was affected by surface treatments.

Preparation and Characterization of Surface Modified Mica by Microwave-enhanced Wet Etching (마이크로웨이브로 증폭된 습식 에칭에 의한 표면 개질 마이카의 제조와 특성)

  • Jeon, Sang-Hoon;Kwon, Sun-Sang;Kim, Duck-Hee;Shim, Min-Kyung;Choi, Young-Jin;Han, Sang-Hoon
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.34 no.4
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    • pp.269-274
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    • 2008
  • In this study we successfully altered the structural characteristics of the mica surface and were able to control oil-absorption by using the microwave enhanced etching (MEE) technique, which has originally been used in semiconductor industry. When microwave energy is applied to the mica, the surface of the mica is etched in a few minutes. As the result of etching, oil-absorption of the mica was enhanced and surface whiteness was improved by modifying the silicon dioxide layer. Additionally, the high whiteness was maintained even though the etched mica absorbed the sebum or sweat. The surface modification of mica was performed by microwave irradiation after the treatment of hydrofluoric acid. The degree of etching was regulated by acid concentration, irradiation time, the amount of energy and slurry concentration. The surface morphology of the etched mica appears to be the shape of the 'Moon'. The characteristics of surface area and roughness were examined by Brunauer-Emmett-Teller (BET) surface area analysis, atomic force microscopy (AFM), scanning electron microscopy (SEM), spectrophotometer and goniophotometer.

The Study of Nano-texturing Process for Crystalline Silicon Solar Cell Using Ag Catalyst Layer (결정질 실리콘 태양전지의 Ag 촉매층을 이용한 나노 텍스쳐링 공정에 관한 연구)

  • Oh, Byoung-Jin;Yeo, In-Hwan;Kim, Min-Young;Lim, Dong-Gun
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.25 no.1
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    • pp.58-61
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    • 2012
  • In our report a relatively simple process for fast nano-texturing of p-type(100) CZ- silicon surface using silver catalyzed wet chemical etching in aqueous hydrofluoric acid (HF) and hydrogen peroxide solution($H_2O_2$) at room temperature. The wafers were saw-damaged by NaOH(6 wt%) at $60^{\circ}C$ for 150s. To obtain a nano-structured black surface, a thin layer of silver with thickness of 1 - 10 nm was deposited on the surfaces by evaporation system. After this process the samples were etched in HF : $H_2O_2$ : $H_2O$ = 1:5:10 at room temperature for 80s - 220s. Due to the local catalytic of the Ag clusters, this treatment results in the nano-scale texturing on the surface. This resulted in average reflectance values less than 9% after the silver on the surface of the wafers were removed.

Fabrication Technology of Glass Micro-framework by Photolithographic Process (사진식각 공정에 의한 유리 미세구조물 제작 기술)

  • O, Jae-Yeol;Jo, Yeong-Rae;Kim, Hui-Su;Jeong, Hyo-Su
    • Korean Journal of Materials Research
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    • v.8 no.9
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    • pp.871-875
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    • 1998
  • High aspect ratio microstructures were fabricated by photolithography. The material for the microstructure was photosensitive glass which has good mechanical and electrical insulation properties. The photosensitive glass was exposed to ultraviolet light at 312nm through a chromium mask in which the structures are drawn. After heat treatment process over $500^{\circ}C$, the photosensitive glass was etched in a 10% hydrofluoric acid solution with ultrasonic conditions. Final dimension of the micro-framework was greatly dependent on the thickness of photosensitive glass, mask pattern, ultraviolet light exposure and etching conditions. The maximum aspect ratio of the micro-framework obtained from this work was over 30.

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Comparison on the Physical & Chemical Characteristics in Surface of Polished Wafer and Epi-Layer Wafer (Polished Wafer와 Epi-Layer Wafer의 표면 처리에 따른 표면 화학적/물리적 특성)

  • Kim, Jin-Seo;Seo, Hyungtak
    • Korean Journal of Materials Research
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    • v.24 no.12
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    • pp.682-688
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    • 2014
  • Physical and chemical changes in a polished wafer and in $2.5{\mu}m$ & $4{\mu}m$ epitaxially grown Si layer wafers (Epilayer wafer) after surface treatment were investigated. We characterized the influence of surface treatment on wafer properties such as surface roughness and the chemical composition and bonds. After each surface treatment, the physical change of the wafer surface was evaluated by atomic force microscopy to confirm the surface morphology and roughness. In addition, chemical changes in the wafer surface were studied by X-ray photoemission spectroscopy measurement. Changes in the chemical composition were confirmed before and after the surface treatment. By combined analysis of the physical and chemical changes, we found that diluted hydrofluoric acid treatment is more effective than buffered oxide etching for $SiO_2$ removal in both polished and Epi-Layer wafers; however, the etch rate and the surface roughness in the given treatment are different among the polished $2.5{\mu}m$ and $4{\mu}m$ Epi-layer wafers in spite of the identical bulk structural properties of these wafers. This study therefore suggests that independent surface treatment optimization is required for each wafer type, $2.5{\mu}m$ and $4{\mu}m$, due to the meaningful differences in the initial surface chemical and physical properties.