• Title/Summary/Keyword: 열처리 공정

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A Study on Oxygen Evolution Activity of Co3O4 with different morphology prepared by Ultrasonic Spray Pyrolysis for Water Electrolysis (분무열분해로 합성한 수전해용 Co3O4의 입자형태에 따른 산소발생 활성에 관한 연구)

  • Kim, Ingyeom;Nah, In Wook;Park, Sehkyu
    • Korean Chemical Engineering Research
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    • v.54 no.6
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    • pp.854-862
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    • 2016
  • As the demand for a clean energy to replace fossil fuel being depleted increases, hydrogen energy is considered as a promising candidate for future energy source. Water electrolysis which produces hydrogen has high energy efficiency and stability but still has a large overpotential for oxygen evolution reaction (OER). In this study, $Co_3O_4$ catalysts with different morphology were prepared by spray pyrolysis from solutions which contain Co precursor and various organic additives (urea, sucrose, and citric acid), followed by post heat treatment. For the catalysts synthesized, X-ray diffraction (XRD) measurements were performed to identify their crystal structure. Morphology and surface shape of the catalysts were observed by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). Surface area and pore volume were examined by nitrogen adsortpion & desorption tests and X-ray photoelectron spectroscopy (XPS) was conducted to confirm nitrogen doping. Linear sweep voltammetry (LSV) was carried out to investigate OER activity of $Co_3O_4$ catalysts. As a result, bare-$Co_3O_4$ which has high surface area and small particle size determined by spray pyrolysis showed high activity toward OER.

Improvement of Calcium Phosphate Forming Ability of Titanium Implant by Thermal Oxidation Method (열산화법에 의한 티타늄 임플란트의 인산칼슘 결정의 형성 능력 증진)

  • Hwang, Kyu-Seog;An, Jun-Hyung;Lee, Seon-Ok;Yun, Yeon-Hum;Kang, Bo-An;Oh, Jeong-Sun;Kim, Sang-Bok
    • Journal of the Korean Ceramic Society
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    • v.39 no.5
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    • pp.460-466
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    • 2002
  • Titanium oxide film was deposited on the commercially pure titanium (cp-Ti) by thermal oxidation method for its medical application. The cp-Ti disks were cleaned and then heat-treated at the temperatures of 500, 550, 600, 650, and 700${\circ}C$, respectively, for 10 min in air or Ar. To test the ability of calcium phosphate formation, the specimens were immersed in the Eagle's minimum essential medium solution at 36.5${\circ}C$ for 15 days. The morphology and chemical composition of the surfaces before and after soaking were analyzed by using FE-SEM and EDS. The in-vitro formation of carbonated calcium phosphate on the thin films containing nano-sized $TiO_2$ crystals was identified.

Hydrothermal Synthesis of Ultra-fine SrAl2O4:Eu Powders and Investigation of their Photoluminescent Characteristics (수열합성법에 의한 SrAl2O4:Eu 초미세 분말 합성공정 및 형광 특성)

  • 박우식;김선재;김정식
    • Journal of the Korean Ceramic Society
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    • v.41 no.5
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    • pp.370-374
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    • 2004
  • Sr$_{l-x}$Ba$_{x}$Al$_2$O$_4$:Eu (x = 0, 0.1, 0.2, and 0.3 mol) phosphor was synthesized by the hydrothermal method and its properties of photoluminescence and long-afterglow were investigated. The mixtures of Sr(NO$_3$)$_2$, Al(NO$_3$)$_3$9$H_2O$, and Eu(NO$_3$)$_3$$.$6$H_2O$ salts dissolved in distilled water, after controlling their pH by NH$_4$OH solution, put into an Autoclave reactor with high temperature and pressure to react. Such synthesized SrAl$_2$O$_4$:Eu powders showed homogeneous and ultra-fine particles of sub-micron size. In order to have the photoluminescence characteristic, powders were heat treated at 1100 -140$0^{\circ}C$ for 2 h in Ar/H$_2$ reduction atmosphere. Photoluminescence spectra showed a excitation along the wide wavelength of 250 ∼ 450 nm, and broaden emission with maxima peak at 520 nm. Also, it showed a good long afterglow with decaying over 1000 sec after excitation illumination for 10 min. In addition, the microstructure and crystal structure of SrAl$_2$O$_4$:Eu powders were investigated by an SEM and XRD, respectively.

A Study on the Electric and Ferroelectric Properties of PZT(30/70) Thick Film Prepared by Using 1,3-Propanediol (1, 3-Propanediol 을 이용해 제작된 PZT(30/70) 후막의 전기적 및 강유전 특성에 관한 연구)

  • 송금석;장동훈;강성준;윤영섭
    • Journal of the Institute of Electronics Engineers of Korea SD
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    • v.40 no.9
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    • pp.631-637
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    • 2003
  • We have evaluated structural and electric, ferroelectric properties of PZT(30/70) thick film prepared by using 1,3-propanediol based sol-gel method on Pt/Ti/SiO$_2$/Si substrates. Rapid thermal annealing (RTA) is used to reduce the thermal stress and final furnace annealing is processed at $650^{\circ}C$. As the results of SEM analysis, we find that we get 350 nm in thickness for one coating and 1 $\mu$m for three times of coating. In the results of C-D analysis at 1 kHz, dielectric constant ($\varepsilon$$_{r}$) and dissipation factor were 886 and 0.03, respectively. C-V curve is shaped as a symmetrical butterfly. Leakage current density at 200 kV/cm is 1.23${\times}$10$^{-5}$ A/cm$^2$ and in the results of hysteresis loops measured at 150 kV/cm, the remnant polarization (P$_{r}$) and the coercive field (E$_{c}$) are 33.8 $\mu$C/cm$^2$ and 56.9 kV/cm, respectively. PZT(30/70) thick film exhibits relatively good ferroelectric, electric properties.s..

Characteriatics of Single Cell Suspension of Garlic, Red Pepper and Cucumber Prepared by Protopectin Hydrolytic Enzymes (펙틴분해효소를 이용한 마늘, 고추와 오이의 단세포화물의 제조)

  • Baek, Ku-Hyoun;Kim, Sung-Soo;Lee, Young-Chun
    • Korean Journal of Food Science and Technology
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    • v.38 no.3
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    • pp.369-377
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    • 2006
  • Protopectinase (PPase) from Bacillus subtilis was used to investigate enzymatic maceration of vegetable tissues. Optimum concentration and pH of PPase were 0.75, 0.75, and 0.5%, and 5.0, 8.0, 7.0 for red pepper, garlic, and cucumber, respectively. Optimum shaking-rate, reaction time, and temperature of PPase were 250 rpm, 150 min, and $37^{\circ}C$, respectively. Yields of mechanically macerated red pepper, garlic, and cucumber were 45.8, 47.5, and 82.1%, whereas those treated with PPase were 81.8, 84, and 98%. Over 40% Vitamin C, the most unstable component during mechanical maceration, remained intact for 12 days after enzymatic treatment. Color differences $({\Delta}E)$ of mechanically macerated red pepper, garlic, and cucumber were 1.16, 2.86, and 3.27, whereas those of PPase-treated ones were 2.87, 7.68, and 5.22 after heat treatment at $100^{\circ}C$ for 20 min. Capsaicin content of mechanically macerated red pepper was 0.4 mg/100 g, whereas that treated with PPase was 1.32 mg/100 g. Viscosity of PPase-treated vegetable decreased slowly with increasing storage period, whereas that of mechanically macerated vegetable sharply decreased. These results indicate PPase treatment of vegetable could be better choice for preparation of high-values and functionally processed food and for extending preservation period.

Recovery of Palladium (Pd) from Spent Catalyst by Dry and Wet Method and Re-preparation of Pd/C Catalyst from Recovered Pd (폐촉매로부터 Pd회수 및 이를 이용한 Pd/C 촉매 재제조 기술 개발)

  • Kim, Ji Sun;Kwon, Ji Soo;Baek, Jae Ho;Lee, Man sig
    • Applied Chemistry for Engineering
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    • v.29 no.4
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    • pp.376-381
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    • 2018
  • The purpose of this study is to investigate and optimize an effectiveness process for the recovery of Pd from the spent Pd/C catalyst by the process of hydrogenation of maleic anhydride over Pd/C. Pd solution recovered from Pd/C catalyst was used to prepare Pd/C catalysts. Their characteristics were compared to those of Pd/C catalyst prepared by using a reagent grade precursor solution. Pd in the spent catalyst was leached by the modified process with dry and wet methods to obtain the high recovery ratio of Pd. The burn-out of carbon in the spent Pd/C catalyst was carried out in the rage of $600-900^{\circ}C$. Pd content of carbonized catalyst was confirmed by XRF and ICP. Pd was extracted from carbonized spent catalysts with acid solutions of 1,2 and 4 M HCl at a leaching temperature of $90^{\circ}C$ for 2 h. The high recovery ratio of Pd was shown as 92.4% that leached in 4 M HCl. Also Pd/C catalysts were prepared by using the leached solution and the reagent grade of $H_2PdCl_4$ as a precursor solution and the characteristics were analyzed by XRD, CO-chemisorption and FE-TEM. As a result, the dispersion of the catalyst prepared by using the leached solution was 34.6%, which was found to be equal to or more than that of the Pd/C catalyst prepared by the reagent grade precursor solution.

LPCVD로 성장된 텅스텐 게이트의 물리.전기적 특성 분석

  • 노관종;윤선필;황성민;노용한
    • Proceedings of the Korean Vacuum Society Conference
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    • 1999.07a
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    • pp.151-151
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    • 1999
  • 금속-산화막-반도체(MOS) 소자를 이용하는 집적회로의 발전은 게이트 금속의 규격 감소를 필요로 한다. 규격감소에 따른 저항 증가가 중요한 문제점으로 대두되었으며, 그동안 여러 연구자들에 의하여 금속 게이트에 관련된 연구가 진행되어 왔다. 특히 저항이 낮으며 녹는점이 매우 높은 내화성금속(refractory metal)인 텅스텐(tungsten, W)이 차세대 MOS 소자의 유력한 대체 게이트 금속으로 제안되었다. 텅스텐은 스퍼터링(sputtering)과 화학기상 증착(CVD) 방식을 이용하여 성장시킬 수 있다. 스퍼터링에 의한 텅스텐 증착은 산화막과의 접착성은 우수한 반면에 증착과정 동안에 게이트 산화막(SiO2)에 손상을 주어 게이트 산화막의 특성을 열화시킬 수 있다. 반면, 화학기상 증차에 의한 텅스텐 성장은 스퍼터링보다 증착막의 저항이 상대적으로 낮으나 산화막과의 접착성이 좋지 않은 문제를 해결하여야 한다. 본 연구에서는 감압 화학기상 증착(LPCVD)방식을 이용하여 텅스텐 게이트 금속을 100~150$\AA$ 두께의 게이트 산화막(SiO2 또는 N2O 질화막)위에 증착하여 물리 및 전기적 특성을 분석하였다. 물리적 분석을 위하여 XRD, SEM 및 저항등이 증착 조건에 따라서 측정되었으며, 텅스텐 게이트로 구성된 MOS 캐패시터를 제작하여 절연 파괴 강도, 전하 포획 메커니즘 등과 같은 전기적 특성 분석을 실시하였다. 특히 텅스텐의 접착성을 증착조건의 변화에 따라서 분석하였다. 텅스텐 박막의 SiO2와의 접착성은 스카치 테이프 테스트를 실시하여 조사되었고, 증착시의 기판의 온도에 민감하게 반응하는 것을 알 수 있었다. 또한, 40$0^{\circ}C$ 이상에서 안정한 것을 볼 수 있었다. 텅스텐 박막은 $\alpha$$\beta$-W 구조를 가질 수 있으나 본 연구에서 성장된 텅스텐은 $\alpha$-W 구조를 가지는 것을 XRD 측정으로 확인하였다. 성장된 텅스텐 박막의 저항은 구조에 따라서 변화되는 것으로 알려져 있다. 증착조건에 따른 저항의 변화는 SiH4 대 WF6의 가스비, 증착온도에 따라서 변화하였다. 특히 온도가 40$0^{\circ}C$ 이상, SiH4/WF6의 비가 0.2일 경우 텅스텐을 증착시킨 후에 열처리를 거치지 않은 경우에도 기존에 발표된 저항률인 10$\mu$$\Omega$.cm 대의 값을 얻을 수 있었다. 본 연구를 통하여 산화막과의 접착성 문제를 해결하고 낮은 저항을 얻을 수 있었으나, 텅스텐 박막의 성장과정에 의한 게이트 산화막의 열화는 심각학 문제를 야기하였다. 즉, LPCVD 과정에서 발생한 불소 또는 불소 화합물이 게이트의 산화막에 결함을 발생시킴을 확인하였다. 향후, 불소에 의한 게이트 산화막의 열화를 최소화시킬 수 있는 공정 조건의 최저고하 또는 대체게이트 산화막이 적용될 경우, 개발된 연구 결과를 산업체로 이전할 수 있는 가능성이 높을 것을 기대된다.

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Process technology and the formation of the TiN barrier metal by physical vapor deposition (PVD 방법에 의한 TiN barrier metal 형성과 공정개발)

  • 최치규;강민성;박형호;염병렬;서경수;이종덕;김건호;이정용
    • Journal of the Korean Vacuum Society
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    • v.6 no.3
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    • pp.255-262
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    • 1997
  • Titanium nitride (TiN) films were prepared by reactive sputter deposition in mixed gas of Ar+$N_2$. The volume percentage of $N_2$ in the working gas was chosen so as to grow stoichiometric TiN films and the substrate temperature during film growth was set from room temperature to $700^{\circ}C$. Stoichiometric $Ti_{0.5}N){0.5}$ films with (111) texture were grown at temperatures over $600^{\circ}C$, while films prepared at temperatures below $600^{\circ}C$ showed N-rich TiN. The composition X and y in the $Ti_xN_y$ films determined by XPS and RBS varied within 5% with the substrate temperature. The sheet resistance of the TiN films decreases as the substrate temperature increased. TiN film prepared at $600^{\circ}C$ showed 14.5$\Omega\Box$, and it decreased to 8.9$\Omega\Box$ after the sample was annealed at $700^{\circ}C$, 30 sec in Ar-gas ambient by RTA. By far, high quality stoichiometric TiN films by reactive sputtering in the mixed gas ambient could be prepared at substrate temperature over $600^{\circ}C$.

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Wafer Level Hermetic Sealing Characteristics of RF-MEMS Devices using Non-Conductive Epoxy (비전도성 에폭시를 사용한 RF-MEMS 소자의 웨이퍼 레벨 밀봉 실장 특성)

  • 박윤권;이덕중;박흥우;송인상;김정우;송기무;이윤희;김철주;주병권
    • Journal of the Microelectronics and Packaging Society
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    • v.8 no.4
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    • pp.11-15
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    • 2001
  • In this paper, hermetic sealing technology was studied for wafer level packaging of the RF-MEMS devices. With the flip-chip bonding method. this non-conductive B-stage epoxy sealing will be profit to the MEMS device sealing. It will be particularly profit to the RF-MEMS device sealing. B-stage epoxy can be cured by 2-step and hermetic sealing can be obtained. After defining 500 $\mu\textrm{m}$-width seal-lines on the glass cap substrate by screen printing, it was pre-baked at $90^{\circ}C$ for about 30 minutes. It was, then, aligned and bonded with device substrate followed by post-baked at $175^{\circ}C$ for about 30 minutes. By using this 2-step baking characteristic, the width and the height of the seal-line could be maintained during the sealing process. The height of the seal-line was controlled within $\pm$0.6 $\mu\textrm{m}$ in the 4 inches wafer and the bonding strength was measured to about 20MPa by pull test. The leak rate, that is sealing characteristic of the B-stage epoxy, was about $10^{-7}$ cc/sec from the leak test.

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InSb 적외선 감지 소자용 $Si_3N_4$, $SiO_2$ 절연막 계면 특성 연구

  • Park, Se-Hun;Lee, Jae-Yeol;Kim, Jeong-Seop;Kim, Su-Jin;Seok, Cheol-Gyun;Yang, Chang-Jae;Park, Jin-Seop;Yun, Ui-Jun
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.08a
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    • pp.163-163
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    • 2010
  • 중적외선 영역 ($3{\sim}5\;{\mu}m$)은 공기 중에 존재하는 이산화탄소나 수증기에 의해 흡수가 일어나지 않기 때문에 군사적으로 중요한 파장 영역이며, 야간에 적을 탐지하는데 응용되고 있다. InSb는 77 K에서 중적외선 파장 흡수에 적합한 밴드갭 에너지 (0.228 eV)를 갖고 있으며, 다른 화합물 반도체와 달리 전하 수송자 이동도 (전자: $10^6\;cm^2/Vs$, 정공: $10^4\;cm^2/Vs$)가 매우 빠르기 때문에 적외선 화상 감지기 재료로 매우 적합하다. 또한 현재 중적외선 영역대에서 널리 사용되는 HgCdTe (MCT)와 대등한 소자 성능을 나타냄과 동시에 낮은 기판 가격, 소자의 제작 용이성 때문에 MCT를 대체할 물질로 주목 받고 있다. 하지만, 기판과 절연막의 계면에 존재하는 결함 때문에 에너지 밴드갭 내에 에너지 준위를 형성하여 높은 누설 전류 특성을 보인다. 따라서 InSb 적외선 소자의 구현을 위하여 고품질의 절연막의 연구가 필수적이라고 할 수 있겠다. 절연막의 특성을 알아보기 위해, n형 InSb 기판에 플라즈마 화학 기상 증착법 (PECVD)을 이용하여 $SiO_2$, $Si_3N_4$를 증착하였으며, 증착 온도를 $120^{\circ}C$에서 $240^{\circ}C$까지 $40^{\circ}C$ 간격으로 변화하여 증착온도가 미치는 영향에 대하여 알아보았다. 절연막과 기판의 계면 특성을 분석하기 위하여 77 K에서 커패시턴스-전압 (C-V) 분석을 하였으며, 계면 트랩 밀도는 Terman method를 이용하여 계산하였다 [1]. $Si_3N_4$를 증착하였을 경우, $120{\sim}240^{\circ}C$의 증착 온도에서 $2.4{\sim}4.9{\times}10^{12}\;cm^{-2}eV^{-1}$의 계면 트랩 밀도를 가졌으며, 증착 온도가 증가할수록 계면 트랩 밀도가 증가하는 경향을 보였다. 또한 모든 증착 온도에서 flat band voltage가 음의 전압으로 이동하였다. $SiO_2$의 경우 $120{\sim}200^{\circ}C$의 증착온도에서 $7.1{\sim}7.3{\times}10^{11}\;cm^{-2}eV^{-1}$의 계면 트랩 밀도 값을 보였으나, $240^{\circ}C$ 이상에서 계면 트랩밀도가 $12{\times}10^{11}\;cm^{-2}eV^{-1}$로 크게 증가하였다. $SiO_2$ 절연막을 사용함으로써, $Si_3N_4$ 대비 약 25% 정도 낮은 계면 트랩 밀도를 얻을 수 있었으며, 모든 증착 온도에서 양의 전압으로 flat band voltage가 이동하였다. 두 절연막에 대한 계면 트랩의 원인을 분석하기 위하여 XPS 측정을 진행하였으며, 깊이에 따른 조성 분석을 하였다. 본 실험에서 최적화된 $SiO_2$ 절연막을 이용하여 InSb 소자의 pn 접합 연구를 진행하였다. Be+ 이온 주입을 진행하고, 급속열처리(RTA) 공정을 통하여 p층을 형성하였다. -0.1 V에서 16 nA의 누설 전류 값을 보였으며, $2.6{\times}10^3\;{\Omega}\;cm^2$의 RoA (zero bias resistance area)를 얻을 수 있었다.

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