• Title/Summary/Keyword: HF Etching

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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.

AN EXPERIMENTAL STUDY ON THE BOND STRENGTH OF THE LIGHT ACTIVATED COMPOSITE RESIN BONDED TO THE ETCHED PORCELAIN (부식된 도재와 광중합성 수지와의 접합강도에 관한 실험적연구)

  • Lee, June-Kyu;Kay, Kee-Sung
    • The Journal of Korean Academy of Prosthodontics
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    • v.25 no.1
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    • pp.363-378
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    • 1987
  • 도재소부전장관에서 금속이 노출되지 않고 도재만이 파절시, 구강내에서 직접 행할 수 있는 심미적 수복 방법으로서 복합성 수지를 이용한 수복 방법이 널리 이용되고 있는데 본실험의 목적은 도재와 광중합성 수지간의 접합강도를 비교 측정코저 함에 있다. 본 실험에서는 주사전자 현미경을 사용하여 도재의 부식액 (5% 불화수소산용액, Excelco's porcelain etching gel) 및 부식 시간(2.5분, 5분, 10분, 20분)에 따른 부식양상을 먼저 관찰하였다. 그다음 각기 다른 시간에서 부식 처리된 도재와 대조군으로서 미부식 처리된 도재에 광중합성 수지를 부착시킬시, 첫째 Silane coupling agent(Scotch-Prime)도포후 광중합성 수지를 결합 시켰고 둘째 bonding agent(Scotch bond)도포후 광중합성 수지를 결합시켰으며 셋째 Silane coupling agent(Scotch-Prime)에 bonding agent(Scotch bond)를 도포후 광중합성 수지로 결합 시킨후, 인장강도 측정기 (Shimadzu universal testing machine)를 사용하여 결합력을 측정한 결과 다음과 같은 결론을 얻었다. 1. 부식처리된 도재가 미부식 처리된 도재 보다 결합력이 높았다. (p<0.05, P<0.001) 2. 부식 처리된 도재나 미부식 처리된 도재에 있어서 silane coupling agent 도포후 bonding agent로 처치한 경우 가장 결합력이 높았으며 그다음 silane coupling agent로 처치한 경우, bonding agent로 처치한 경우의 순이었다. 3. 도재부식 시간의 증가에 따른 결합력의 차이는 5% HF용액으로 부식 처리된 도재와 Excelco로 부식 처리된 도재에 있어서 5분 정도 까지는 결합력의 증가를 보였으나 그 후에는 결합력에 있어서 거의 증가하지 않는 양상을 보였다. 4. Excelco로 부식 처리된 도재와 5% HF 용액으로 부식처리된 도재간의 결합력 차이에 있어서 bonding agent만으로 처치한 경우에는 두결합력 사이에 서로 유의한 차이를 보이지 않았으나 (P>0.5) silane coupling agent만으로 처치한 경우와 silane coupling agent 도포후 bonding agent로 처치한 경우에는 두결합력 사이에 서로 유의한 차이를 보였다. (P<0.05, P<0.001) 5. Excelco로 부식처리된 도재가 5% HF 용액으로 부식처리된 도재보다 부식정도가 더 현저하였다.

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Fabrication of Microwire Arrays for Enhanced Light Trapping Efficiency Using Deep Reactive Ion Etching

  • Hwang, In-Chan;Seo, Gwan-Yong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2014.02a
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    • pp.454-454
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    • 2014
  • Silicon microwire array is one of the promising platforms as a means for developing highly efficient solar cells thanks to the enhanced light trapping efficiency. Among the various fabrication methods of microstructures, deep reactive ion etching (DRIE) process has been extensively used in fabrication of high aspect ratio microwire arrays. In this presentation, we show precisely controlled Si microwire arrays by tuning the DRIE process conditions. A periodic microdisk arrays were patterned on 4-inch Si wafer (p-type, $1{\sim}10{\Omega}cm$) using photolithography. After developing the pattern, 150-nm-thick Al was deposited and lifted-off to leave Al microdisk arrays on the starting Si wafer. Periodic Al microdisk arrays (diameter of $2{\mu}m$ and periodic distance of $2{\mu}m$) were used as an etch mask. A DRIE process (Tegal 200) is used for anisotropic deep silicon etching at room temperature. During the process, $SF_6$ and $C_4F_8$ gases were used for the etching and surface passivation, respectively. The length and shape of microwire arrays were controlled by etching time and $SF_6/C_4F_8$ ratio. By adjusting $SF_6/C_4F_8$ gas ratio, the shape of Si microwire can be controlled, resulting in the formation of tapered or vertical microwires. After DRIE process, the residual polymer and etching damage on the surface of the microwires were removed using piranha solution ($H_2SO_4:H_2O_2=4:1$) followed by thermal oxidation ($900^{\circ}C$, 40 min). The oxide layer formed through the thermal oxidation was etched by diluted hydrofluoric acid (1 wt% HF). The surface morphology of a Si microwire arrays was characterized by field-emission scanning electron microscopy (FE-SEM, Hitachi S-4800). Optical reflection measurements were performed over 300~1100 nm wavelengths using a UV-Vis/NIR spectrophotometer (Cary 5000, Agilent) in which a 60 mm integrating sphere (Labsphere) is equipped to account for total light (diffuse and specular) reflected from the samples. The total reflection by the microwire arrays sample was reduced from 20 % to 10 % of the incident light over the visible region when the length of the microwire was increased from $10{\mu}m$ to $30{\mu}m$.

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Etching Property of the TaN Thin Film using an Inductively Coupled Plasma (유도결합플라즈마를 이용한 TaN 박막의 식각 특성)

  • Um, Doo-Seung;Woo, Jong-Chang;Kim, Dong-Pyo;Kim, Chang-Il
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2009.06a
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    • pp.104-104
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    • 2009
  • Critical dimensions has rapidly shrunk to increase the degree of integration and to reduce the power consumption. However, it is accompanied with several problems like direct tunneling through the gate insulator layer and the low conductivity characteristic of poly-silicon. To cover these faults, the study of new materials is urgently needed. Recently, high dielectric materials like $Al_2O_3$, $ZrO_2$ and $HfO_2$ are being studied for equivalent oxide thickness (EOT). However, poly-silicon gate is not compatible with high-k materials for gate-insulator. To integrate high-k gate dielectric materials in nano-scale devices, metal gate electrodes are expected to be used in the future. Currently, metal gate electrode materials like TiN, TaN, and WN are being widely studied for next-generation nano-scale devices. The TaN gate electrode for metal/high-k gate stack is compatible with high-k materials. According to this trend, the study about dry etching technology of the TaN film is needed. In this study, we investigated the etch mechanism of the TaN thin film in an inductively coupled plasma (ICP) system with $O_2/BCl_3/Ar$ gas chemistry. The etch rates and selectivities of TaN thin films were investigated in terms of the gas mixing ratio, the RF power, the DC-bias voltage, and the process pressure. The characteristics of the plasma were estimated using optical emission spectroscopy (OES). The surface reactions after etching were investigated using X-ray photoelectron spectroscopy (XPS) and auger electron spectroscopy (AES).

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Effect of hydrofluoric acid-based etchant at an elevated temperature on the bond strength and surface topography of Y-TZP ceramics

  • Yu, Mi-Kyung;Lim, Myung-Jin;Na, Noo-Ri;Lee, Kwang-Won
    • Restorative Dentistry and Endodontics
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    • v.45 no.1
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    • pp.6.1-6.8
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    • 2020
  • Objectives: This study investigated the effects of a hydrofluoric acid (HA; solution of hydrogen fluoride [HF] in water)-based smart etching (SE) solution at an elevated temperature on yttria-stabilized tetragonal zirconia polycrystal (Y-TZP) ceramics in terms of bond strength and morphological changes. Materials and Methods: Eighty sintered Y-TZP specimens were prepared for shear bond strength (SBS) testing. The bonding surface of the Y-TZP specimens was treated with 37% phosphoric acid etching at 20℃-25℃, 4% HA etching at 20℃-25℃, or HA-based SE at 70℃-80℃. In all groups, zirconia primers were applied to the bonding surface of Y-TZP. For each group, 2 types of resin cement (with or without methacryloyloxydecyl dihydrogen phosphate [MDP]) were used. SBS testing was performed. Topographic changes of the etched Y-TZP surface were analyzed using scanning electron microscopy and atomic force microscopy. The results were analyzed and compared using 2-way analysis of variance. Results: Regardless of the type of resin cement, the highest bond strength was measured in the SE group, with significant differences compared to the other groups (p < 0.05). In all groups, MDP-containing resin cement yielded significantly higher bond strength values than MDP-free resin cement (p < 0.05). It was also shown that the Y-TZP surface was etched by the SE solution, causing a large change in the surface topography. Conclusions: Bond strength significantly improved when a heated HA-based SE solution was applied to the Y-TZP surface, and the etched Y-TZP surface was more irregular and had higher surface roughness.

Congruent LiNbO3 Crystal Periodically Poled by Applying External Field (외부전계 인가에 의한 조화용융조성 LiNbO3 결정의 주기적 분극반전)

  • Kwon, Soon-Woo;Yang, Woo-Seok;Lee, Hyung-Man;Kim, Woo-Kyung;Lee, Han-Young;Yoon, Dae-Ho;Song, Yo-Seung
    • Journal of the Korean Ceramic Society
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    • v.42 no.11 s.282
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    • pp.749-752
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    • 2005
  • When an electric field higher than a characteristic coercive field is applied to a ferroelectric such as $LiNbO_3$, the orientation of the spontaneous polarization is reversed, which causes the reversal of the sign of odd-rank tensor properties such as electro-optic and nonlinear optic coefficients. A fabrication process of insulator and periodic external field assisted poling of a z-cut $LiNbO_3$ have been optimized for a periodic $180^{\circ}$ phase inversion along z-axis. The poling jig and the poling control system, fully controlled by a computer, for high quality and reproducible PPLN fabrication have been devised. Periodically polarization reversed PPLN was adjusted based on the fabricated thickness of insulator. The poling structure of PPLN was observed under a microscope after etching PPLN samples by an etching solution ($HF:HNO_3$ = 1 : 2) for about 15 min.

STI Top Profile Improvement and Gap-Fill HLD Thickness Evaluation (STI의 Top Profile 개선 및 Gap-Fill HLD 두께 평가)

  • Seong-Jun, Kang;Yang-Hee, Joung
    • The Journal of the Korea institute of electronic communication sciences
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    • v.17 no.6
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    • pp.1175-1180
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    • 2022
  • STI has been studied a lot as a process technology for wide area planarization according to miniaturization and high integration of semiconductor devices. In this study, as methods for improving the STI profile, wet etching of pad oxide using hydrofluorine solution and dry etching of O2+CF4 after STI dry etching were proposed. This process technology showed improvement in profile imbalance and leakage current between patterns according to device density compared to the conventional method. In addition, as a result of measuring the HLD thickness after CMP for a device having the same STI depth and HLD deposition, the measured value was different depending on the device density. It was confirmed that this was due to the difference in the thickness of the nitride film according to the device density after CMP and the selectivity of the slurry.

Recovery of Silicon Wafers from the Waste Solar Cells by H3PO4-NH4HF2-Chelating Agent Mixed Solution (인산-산성불화암모늄-킬레이트제 혼합용액에 의한 폐태양전지로부터 실리콘웨이퍼의 회수)

  • Koo, Su-Jin;Ju, Chang-Sik
    • Korean Chemical Engineering Research
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    • v.51 no.6
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    • pp.666-670
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    • 2013
  • Recovery method of silicon wafer from defective products generated from manufacturing process of silicon solar cells was studied. The removal effect of the N layer and antireflection coating (ARC) of the waste solar cell were investigated at room temperature ($25^{\circ}C$) by variation of concentration of $H_3PO_4$, $NH_4HF_2$, and concentration and types of chelating agent. Removal efficiency was the best in the conditions; 10 wt% $H_3PO_4$ 2.0 wt% $NH_4HF_2$, 1.5 wt% Hydantoin. Increasing the concentration of $H_3PO_4$, the surface contamination degree was increased and the thickness of the silicon wafe became thicker than the thickness before surface treatment because of re-adsorption on the silicon wafer surface by electrostatic attraction of the fine particles changed to (+). The etching method by mixed solution of $H_3PO_4$-$NH_4HF_2$-chelating agents was expected to be great as an alternative to conventional RCA cleaning methods and as the recycle method of waste solar cells, because all processes are performed at room temperature, the process is simple, and less wastewater, the removal efficiency of the surface of the solar cell was excellent.

Growth of Highly Purified Carbon Nanotubes by Thermal Chemical Vapor Deposition (열화학기상증착법에 의한 고순도 탄소나노튜브의 성장)

  • Yu, Jae-Geun;Park, Jeong-Hun;Kim, Dae-Un;Lee, Cheol-Jin;Son, Gwon-Hui;Sin, Dong-Hyeok;Mun, In-Gi
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.49 no.12
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    • pp.649-653
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    • 2000
  • We have grown carbon nanotubes by thermal chemical vapor deposition of $C_{2}H_{2}$ on catalytic metal deposited on silicon oxide substrates. Highly purified carbon nanotubes are uniformly grown on a large area of the silicon oxide substrates. It is observed that surface modification of catalytic metals deposited on substrates by either etching with dipping in a HF solution and/or $NH_{3}$ pretreatment is a crucial step for the nanotube growth prior to the reaction of $C_{2}H_{2}$ gas. The diameters of carbon naotubes could be controlled by applying the different catalytic metals.

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A Study on the Wet Etching of CoNbZr/Cu/CoNbZr Multi-Layer Films (CoNbZr/Cu/CoNbZr 다층막의 습식 식각에 관한 연구)

  • 김현식;민복기;송재성;이영생;오영우
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 1997.04a
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    • pp.141-145
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    • 1997
  • 스퍼터링법으로 제조한 CoNbZr/Cu/CoNbZr 다층막에 대해 습식 식각법으로 패턴을 형성하기 위해 새로운 식각 용액을 제조하여 이 용액의 최적의 식각 조건에 대해 연구하였다. 염기성 수용액은 농도에 관계없이 Cu만을 선택적으로 식각하며 CoNbZr 비정질 박막은 식각하지 않았다. 그러나, 본 연구에서 제조 한 17.5 mol%의 염기성 수용액에 HF를 20 mol% 혼합한 식각 용액으로 CoNbZr/Cu/CoNbZr 다층막을 동시에 식각할 수 있었다. 또한 이 식각 용액은 CoNbZr/Cu/CoNbZr 다층막을 3단계로 식각하고 식각된 단면은 이방성 구조를 가지며, 매우 우수한 식각 특성을 나타내었다.

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