• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2007.06a
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• pp.85-85
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• 2007

최근 귀금속중의 하나인 Ruthenium(Ru)은 높은 일함수, 누설전류에 대한 높은 저항성등의 톡성으로 인해 캐패시터의 하부전극으로 각광받고 있다. 하부전극으로 증착된 Ru은 일반적으로 각 캐패시터의 분리와 평탄화를 위해 건식식각이 이루어진다. 하지만, 건식식각 공정중 유독한 $RUO_4$ 가스가 발생할 수 있으며, 불균일한 캐패시터 표면을 유발할 수 있다. 이러한 문제점들을 해결하기 위해 CMP 공정이 필요하게 되었다. 하지만, Ru은 화학적으로 매우 안정하기 때문에 Ru CMP 슬러리에 대한 연구가 필요하게 되었으며, 이에 대한 연구가 활발히 진행되고 있다. 본 연구에서는 Ru CMP 공정에서 Chemical A가 에칭제 및 산화제로 사용된 슬러리의 pH 변화와 pH 적정제에 따른 영향을 살펴보았다. Ru wafer를 이용하여 static etch rate, passivation film thickness와 wettability를 pH와 pH 적정제에 따라 비교해 보았다. 또한, pH 적정제로 $NH_4OH$와 TMAH를 이용하여 pH별 슬러리를 제작하고 CMP 공정을 실시하여 Ru의 removal rate을 측정하였다. $NH_4OH$와 TMAH의 경우 각각 130. 100 nm/min의 연마율이 측정된 pH 6에서 가장 높은 연마률을 보였으며, TMAH의 경우가 pH 전 구간에서 $NH_4OH$에 비해 낮은 연마율이 측정되었다. TEOS 에 대한 Ru의 선택비를 측정해 본 결과, $NH_4OH$의 경우 pH 8~9. TMAH의 경우 pH 6~7에서 높은 selectivity를 얻을 수 있었다.

• Proceedings of the Korean Vacuum Society Conference
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• 2010.02a
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• pp.261-261
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• 2010

본 연구에서는 PBMS (Particle Beam Mass Spectrometer)와 ISPM (In-Situ Particle Monitor)을 연계하여 BPSG (Borophosphosilicate Glass) 및 PSG (Phosphosilicate Glass) 박막 증착을 위한 CVD (chemical vapor deposition) 공정 중 발생하는 오염입자 발생특성에 대해 비교 평가하였다. 소스는 TEB (Triethylborate), TEPO (Triethylphosphate) 및 TEOS (Tetraethoxysilane)를 사용하였고, 운반가스 및 반응가스로 He과 $O_2$ 및 $O_3$를 사용하였다. 증착온도와 압력은 각각 $450^{\circ}C$, 200 Torr 이었다. 반응기의 배기라인에 PBMS와 ISPM을 설치하고 500 nm 이하의 입자에 대해 공정단계별 시간에 따른 모니터링 결과 전 공정에 걸쳐 동일한 패턴의 입자발생분포를 보였으며, 특히 PBMS의 경우 ISPM의 입자측정한계인 260 nm 이하의 입자크기도 측정할 수 있었다. 입자발생이 안정적으로 일어나는 증착공정 중 PBMS를 통하여 입자크기를 측정한 결과 BPSG의 경우 약 110 nm, PSG의 경우 약 80 nm의 분포를 나타내었다. 이를 통해 TEB 소스가 배제된 PSG의 경우 BPSG의 경우보다 입자의 성장이 지체됨을 확인하였다. 측정에 대한 신뢰성을 확보하기 위해 PBMS 내의 TEM (Transmission Electron Microscopy) grid를 이용하여 입자를 샘플링 하였고, TEM 분석을 실시한 결과 PBMS 측정결과와 잘 일치하였다. 또한 EDS (Energy Dispersive Spectroscopy) 분석을 통하여 입자성분에 대해 검증하였다.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2007.04a
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• pp.71-72
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• 2007

In this study, we investigated the fabrication of MLR (multi-layer resist) with a very thin diamond-like carbon (DLC) layer. ArF PR/$SiO_2$/DLC MLR structure was investigated and etching characteristics of the DLC layer was patterned using $SiO_2$ hard-mask by varying the process parameters such as different high-frequency/low-frequency combination ($f_{LF}/f_{HF}$), HF/LF power ratio ($P_{HF}/P_{LF}$), $O_2$ flow and $N_2$ flow rate in $O_2/N_2$/Ar plasmas. The results indicated an increased etch rate of DLC for the higher $f_{LF}/f_{HF}$ combination and for the increased low-frequency power ($P_{LF}$). And the etch rate of DLC was decreased with increasing the $N_2$ flow rate in $O_2/N_2$/Ar plasmas. In order to confirm the application of DLC MLR for the etching process of silicon oxide, the stack of ArF PR/BARC/$SiO_2$/DLC/TEOS/Si was investigated.

• Journal of Microbiology and Biotechnology
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• v.31 no.3
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• pp.419-428
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• 2021

To efficiently recycle GH78 thermostable rhamnosidase (TpeRha) and easily separate it from the reaction mixture and furtherly improve the enzyme properties, the magnetic particle Fe3O4-SiO2-NH2-Cellu-ZIF8 (FSNcZ8) was prepared by modifying Fe3O4-NH2 with tetraethyl silicate (TEOS), microcrystalline cellulose and zinc nitrate hexahydrate. FSNcZ8 displayed better magnetic stability and higher-temperature stability than unmodified Fe3O4-NH2 (FN), and it was used to adsorb and immobilize TpeRha from Thermotoga petrophilea 13995. As for properties, FSNcZ8-TpeRha showed optimal reaction temperature and pH of 90℃ and 5.0, while its highest activity approached 714 U/g. In addition, FSNcZ8-TpeRha had better higher-temperature stability than FN. After incubation at 80℃ for 3 h, the residual enzyme activities of FSNcZ8-TpeRha, FN-TpeRha and free enzyme were 93.5%, 63.32%, and 62.77%, respectively. The organic solvent tolerance and the monosaccharides tolerance of FSNcZ8-TpeRha, compared with free TpeRha, were greatly improved. Using naringin (1 mmol/l) as the substrate, the optimal conversion conditions were as follows: FSNcZ8-TpeRha concentration was 6 U/ml; induction temperature was 80℃; the pH was 5.5; induction time was 30 min, and the yield of products was the same as free enzyme. After repeating the reaction 10 times, the conversion of naringin remained above 80%, showing great improvement of the catalytic efficiency and repeated utilization of the immobilized α-L-rhamnosidase.

• Korean Journal of Materials Research
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• v.33 no.7
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• pp.265-272
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• 2023

In this study, the synthesis of nitrobenzene was carried out using sulfated silica catalyst. The study delved into H₂SO₄/SiO₂ as a solid acid catalyst and the effect of its weight variation, as well as the use of a microwave batch reactor in the synthesis of nitrobenzene. SiO₂ was prepared using the sol-gel method from TEOS precursor. The formed gel was then refluxed with methanol and calcined at a temperature of 600 ℃. SiO₂ with a 200-mesh size was impregnated with 98 % H₂SO₄ by mixing for 1 h. The resulting 33 % (w/w) H₂SO₄/SiO₂ catalyst was separated by centrifugation, dried, and calcined at 600 ℃. The catalyst was then used as a solid acid catalyst in the synthesis of nitrobenzene. The weights of catalyst used were 0.5; 1; and 1.5 grams. The synthesis of nitrobenzene was carried out with a 1:3 ratio of benzene to nitric acid in a microwave batch reactor at 60 ℃ for 5 h. The resulting nitrobenzene liquid was analyzed using GC-MS to determine the selectivity of the catalyst. Likewise, the use of a microwave batch reactor was found to be appropriate and successful for the synthesis of nitrobenzene. The thermal energy produced by the microwave batch reactor was efficient enough to be used for the nitration reaction. Reactivity and selectivity tests demonstrated that 1 g of H₂SO₄/SiO₂ could generate an average benzene conversion of 40.33 %.

• Membrane Journal
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• v.25 no.2
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• pp.115-122
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• 2015

$SiO_2{\cdot}B_2O_3$ was prepared by trimethylborate (TMB)/tetraethylorthosilicate (TEOS) mole ratio 0.01 at $800^{\circ}C$. PDMS[poly(dimethysiloxane)]-$SiO_2{\cdot}B_2O_3$ composite membranes were prepared by adding porous $SiO_2{\cdot}B_2O_3$ to PDMS. To investigate the characteristics of PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane, we observed PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane using TG-DTA, FT-IR, BET, X-ray, and SEM. PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane was studied on the permeabilities of $H_2$ and $N_2$ and the selectivity ($H_2/N_2$). Following the results of TG-DTA, BET, X-ray, FT-IR, $SiO_2{\cdot}B_2O_3$ was the amorphous porous $SiO_2{\cdot}B_2O_3$ with $247.6868m^2/g$ surface area and $37.7821{\AA}$ the mean of pore diameter. According to the TGA measurements, the thermal stability of PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane was enhanced by inserting $SiO_2{\cdot}B_2O_3$. SEM observation showed that the size of dispersed $SiO_2{\cdot}B_2O_3$ in the PDMS-$SiO_2{\cdot}B_2O_3$ composite membrane was about $1{\mu}m$. The increasing of $SiO_2{\cdot}B_2O_3$ content in PDMS leaded the following results in the gas permeation experiment: the permeability of both $H_2$ and $N_2$ was increased, and the permeability of $H_2$ was higher than $N_2$, but the selectivity($H_2/N_2$) was decreased.

• Journal of the Microelectronics and Packaging Society
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• v.28 no.1
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• pp.39-46
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• 2021

The quantitative measurement of interfacial adhesion energy (Gc) of multilayer thin films for Cu interconnects was investigated using a double cantilever beam (DCB) and 4-point bending (4-PB) test. In the case of a sample with Ta diffusion barrier applied, all Gc values measured by the DCB and 4-PB tests were higher than 5 J/㎡, which is the minimum criterion for Cu/low-k integration without delamination. However, in the case of the Ta/Cu sample, measured Gc value of the DCB test was lower than 5 J/㎡. All Gc values measured by the 4-PB test were higher than those of the DCB test. Measured Gc values increase with increasing phase angle, that is, 4-PB test higher than DCB test due to increasing plastic energy dissipation and roughness-related shielding effects, which matches well interfacial fracture mechanics theory. As a result of the 4-PB test, Ta/Cu and Cu/Ta interfaces measured Gc values were higher than 5 J/㎡, suggesting that Ta is considered to be applicable as a diffusion barrier and a capping layer for Cu interconnects. The 4-PB test method is recommended for quantitative adhesion energy measurement of the Cu interconnect interface because the thermal stress due to the difference in coefficient of thermal expansion and the delamination due to chemical mechanical polishing have a large effect of the mixing mode including shear stress.

• Journal of Adhesion and Interface
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• v.24 no.4
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• pp.136-142
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• 2023

In this study, TEOS was used as a silica source, and a triblock copolymer (P123) was used as a template to produce mesoporous silica with a well-ordered hexagonal mesopore array through a self-assembly method and hydrothermal process under acidic condition. (Surfactant-extracted SBA-15). Surfactant-extracted SBA-15 showed the particle shape of a short rod with a size of approximately 980 nm. The surface area and pore diameter were 730 m²g^-1 and 70.8 Å, respectively. Meanwhile, aminosilane (3-aminopropyltriethoxysilane, APTES) was grafted into the mesopores using a post-synthesis method. Mesoporous silica (APTES-SBA-15) modified with aminosilane had a well-ordered pore structure (p6mm) and well-maintained the particle shape of short rods. The surface area and pore diameter of APTES-SBA-15 decreased to 350 m²g^-1 and 60.7 Å, respectively. APTES-modified mesoporous silica was treated with a solution of rare earth metal ions (Eu³⁺, Tb³⁺) to synthesize a mesoporous silica material in which rare earth metal complexes were introduced into the mesopores. (Eu/APTES-SBA-15, Tb/APTES-SBA-15) These materials exhibited characteristic photoluminescence spectra by λ_ex=250 nm. (⁵D₄→⁷F₅ (543.5 nm), ⁵D₄→⁷F₄ (583.5 nm), ⁵D₄→⁷F₃ (620.2 nm) transitions for Tb/APTES-SBA-15; ⁵D₀→⁷F₀ (577.7 nm), ⁵D₀→⁷F₁ (592.0 nm), ⁵D₀→⁷F₂ (614.9 nm), ⁵D₀→⁷F₃ (650.3 nm) and ⁵D₀→⁷F₄ (698.5 nm) transitions for Eu/APTES-SBA-15)

• Journal of the Korean Chemical Society
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• v.61 no.4
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• pp.179-184
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• 2017

In this paper, a $ZnO/SiO_2$ nano-composite was prepared by a simple chemical method at room temperature. For the synthesis of ZnO nanoparticles (NPs), a sonochemical method was used, and $SiO_2$ NPs were prepared by precipitation method. The formation of $ZnO/SiO_2$ NCs was characterized by X-ray diffractometer (XRD) and confirmed by field-emission scanning electron microscopy (FE-SEM) and Fourier transform infra-red spectroscopy(FT-IR). The photocatalytic properties of $ZnO/SiO_2$ NCs formed at different concentrations of $SiO_2$ were evaluated by rhodamine-B dye. It was confirmed that increasing $SiO_2$ concentration resulted in an increase in the photocatalytic property. In addition, the antibacterial activity of $ZnO/SiO_2$ NCs was conducted against Escherichia coli (E. coli) and Staphylococcus aureus (S. aureus). As a result, the antibacterial activities of E.coli and S. aureus were increased in the presence of thick SiO NPs layer.

• Proceedings of the Korean Vacuum Society Conference
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• 2013.02a
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• pp.416-417
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• 2013

최근 질화물계 발광다이오드(light emitting diode, LED) 소자는 핸드폰, 스마트 TV 등의 디스플레이 분야와 실내외조명, 감성조명, 특수조명 등의 조명분야에 그 응용분야가 급속히 확대되고 있다. 이러한 LED 소자는 에너지 절감과 친환경에 장점을 가지고, 가까운 미래에 조명시장을 대체할 것으로 예상된다. 이를 만족하기 위해서는 현재보다 더 높은 효율을 갖는 LED 개발이 요구되어지고 있는 상황이다. 일반적으로 질화물계 LED 소자의 효율은 내부양자 효율, 광추출 효율 등으로 나타낼 수 있다. 내부 양자효율은 성장된 결정의 질의 개선 및 다층의 이종접합 또는 다중양자우물 구조와 같이 활성층의 캐리어 농도를 높이는 접합구조로 설계되어 80% 이상의 효율을 나타낸다. 그러나 광추출 효율은 이에 미치지 못하고 있다. 이는 반도체 재료의 높은 굴절률로 인하여 빛이 외부로 탈출하지 못하고 내부로 반사되거나 물질 안에서 흡수가 일어나기 때문이다. 따라서 이러한 문제를 해결하기 위해 많은 연구 그룹들은, 표면에 패턴 형성하여 빛의 전반사를 줄여 그 효율을 올리는 연구결과를 보고하고 있다. 대표적인 방법으로는 wet etching, 전자빔 리소그라피, 나노임프린트 리소그라피, 레이저 홀로 리그라피, 나노스피어 리소그라피 등이 사용되고 있다. 이 중, 나노스피어 리소그라피는 폴리스틸렌 혹은 실리카 등과 같은 나노 크기의 bead를 사용하여 반도체 기판 표면에 단일층으로 고르게 코팅한 마스크로 사용하여 패턴을 주는 방법이다. 이 방법의 장점으로는 대면적에 균일한 패턴을 형성할 수 있고, 공정비용이 저렴하여 양산하기에 적합하다는 특징이 있다. 나노스피어 리소그라피를 통해서 표면에 생성된 패턴 모양의 각도에 따라서, 식각되는 깊이에 변화에 따라 실험한 결과들은 있지만, 아직까지 크기가 다른 나노입자들의 마스크 이용하여 형성된 패턴 밀도에 따른 광 추출 효과에 대한 연구가 많이 미흡하다. 따라서 본 연구에서는 다양한 크기의 실리카로 패턴을 형성시켜 패턴 밀도에 대한 광추출 효율의 효과에 대해서 조사하였다. 실험 방법으론, DI, 에탄올, TEOS, 암모니아의 순서대로 그 혼합 비율을 조정하여 100, 250, 500 nm 크기의 나노입자를 합성하였고 이것을 질화물계 LED의 표면 위에 단일층으로 스핀코팅 방법을 통해 코팅을 하였다. 그 후 ICP-RIE 방법으로 필라 패턴을 형성하였는데, 그 결과 100 nm SiO2 입자를 이용한 경우 $4.5{\times}10^9$/$cm^2$, 250 nm의 경우 $1.4{\times}10^9$/$cm^2$, 500 nm의 경우 $0.4{\times}10^9$/$cm^2$의 패턴의 밀도를 보여주었다(Fig. 1). 패턴의 밀도에 따라 전계광학적 특성을 확인하여 보았는데, 그 결과는 평평한 표면과 비교하였을 때 100 nm에서 383%, 250 nm에서는 320%, 500 nm에서는 244% 상승하는 결과를 보여주었다(Fig. 2). 이번 실험을 통해서 LED의 광추출 효율은 표면 모양과 깊이 뿐 아니라 밀도가 커질수록 그 효율이 올라간다는 사실을 알 수 있었다.