• Title/Summary/Keyword: Vacuum pyrolysis

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Aerosol Jet Deposition of $CuInS_2$ Thin Films

  • Fan, Rong;Kong, Seon-Mi;Kim, Dong-Chan;Chung, Chee-Won
    • Proceedings of the Korean Vacuum Society Conference
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    • 2011.02a
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    • pp.159-159
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    • 2011
  • Among the semiconductor ternary compounds in the I-III-$VI_2$ series, $CulnS_2$ ($CulnSe_2$) are one of the promising materials for photovoltaic applications because of the suitability of their electrical and optical properties. The $CuInS_2$ thin film is one of I-III-$VI_2$ type semiconductors, which crystallizes in the chalcopyrite structure. Its direct band gap of 1.5 eV, high absorption coefficient and environmental viewpoint that $CuInS_2$ does not contain any toxic constituents make it suitable for terrestrial photovoltaic applications. A variety of techniques have been applied to deposit $CuInS_2$ thin films, such as single/double source evaporation, coevaporation, rf sputtering, chemical vapor deposition and chemical spray pyrolysis. This is the first report that $CuInS_2$ thin films have been prepared by Aerosol Jet Deposition (AJD) technique which is a novel and attractive method because thin films with high deposition rate can be grown at very low cost. In this study, $CuInS_2$ thin films have been prepared by Aerosol Jet Deposition (AJD) method which employs a nozzle expansion. The mixed fluid is expanded through the nozzle into the chamber evacuated in a lower pressure to deposit $CuInS_2$ films on Mo coated glass substrate. In this AJD system, the characteristics of $CuInS_2$ films are dependent on various deposition parameters, such as compositional ratio of precursor solution, flow rate of carrier gas, stagnation pressure, substrate temperature, nozzle shape, nozzle size and chamber pressure, etc. In this report, $CuInS_2$ thin films are deposited using the deposition parameters such as the compositional ratio of the precursor solution and the substrate temperature. The deposited $CuInS_2$ thin films will be analyzed in terms of deposition rate, crystal structure, and optical properties.

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A Study on the molecular structure and molecular weight control of styrene films by plasma polymerization (플라즈마 중합법에 의한 스티렌 박막의 분자 구조 및 분자량 제어에 관한 연구)

  • 김종택;최충양;박종관;박응춘;이덕출
    • Journal of the Korean Vacuum Society
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    • v.6 no.3
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    • pp.213-219
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    • 1997
  • The plasma polymerized styrene films were prepared by using an inter-electrode capacitively coupled gas-flow-type reactor, and the effects of plasma polymerization condition on the molecular weight distribution were investigated by Fourier Transform Infrared (FT-IR), Pyrolysis Gas Chromatography(PyGC), Differential Scanning Calorimetry(DSC) and Gel Permeation Chromatography(GPC). From the above results, the very cross-linked films different from chemical characteristics of the starting monomer were taken out, and it is realized that the molecular structure, cross linking density, and molecular weight distribution could be controlled by changing the parameters such as deposition pressure, deposition power and gas flow rate. Accordingly, it is suggested that plasma polymerization method performed by inter-electrode capacitively coupled gas-flow-type reactor has good characteristics for manufacturing the functional organic thin films which can be applied in sensors, opto-electric device, photo-resist by changing the polymerization parameters.

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Synthesis of functional ZnO nanoparticles and their photocatalytic properties

  • Nam, Sang-Hun;Kim, Myoung-Hwa;Lee, Sang-Duck;Kim, Min-Hee;Boo, Jin-Hyo
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.54-54
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    • 2010
  • Zinc oxide is metal oxide semiconductor with the 3.37 eV bandgap energy. Zinc oxide is very attractive materials for many application fields. Zinc Oxide has many advantages such as high conductivity and good transmittance in visible region. Also it is cheaper than other semiconductor materials such as indium tin oxide (ITO). Therefore, ZnO is alternative material for ITO. ZnO is attracting attention for its application to transparent conductive oxide (TCO) films, surface acoustic wave (SAW), films bulk acoustic resonator (FBAR), piezoelectric materials, gas-sensing, solar cells and photocatalyst. In this study, we synthesized ZnO nanoparticles and defined their physical and chemical properties. Also we studied about the application of ZnO nanoparticles as a photocatalyst and try to find a enhancement photocatalytic activity of ZnO nanorticles.. We synthesized ZnO nanoparticles using spray-pyrolysis method and defined the physical and optical properties of ZnO nanoparticles in experiment I. When the ZnO are exposed to UV light, reduction and oxidation(REDOX) reaction will occur on the ZnO surface and generate ${O_2}^-$ and OH radicals. These powerful oxidizing agents are proven to be effective in decomposition of the harmful organic materials and convert them into $CO_2$ and $H_2O$. Therefore, we investigated that the photocatalytic activity was increased through the surface modification of synthesized ZnO nanoparticles. In experiment II, we studied on the stability of ZnO nanoparticles in water. It is well known that ZnO is unstable in water in comparison with $TiO_2$. $Zn(OH)_2$ was formed at the ZnO surface and ZnO become inactive as a photocatalyst when ZnO is present in the solution. Therefore, we prepared synthesized ZnO nanoparticles that were immersed in the water and dried in the oven. After that, we measured photocatalytic activities of prepared samples and find the cause of their photocatalytic activity changes.

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RF magnetron sputtering에 의해 제작된 $SnO_2$ 투명전극의 구조적 및 광학적 특성

  • Im, Jeong-U;Lee, Dong-Hun;Yu, Jae-Su
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.205-205
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    • 2010
  • 투명 전극(transparent conducting oxide, TCO)은 높은 전기전도도 및 낮은 비저항 ($10^{-4}{\sim}10^{-3}\;{\Omega}cm$)과 가시광영역에서의 우수한 광투과도(> 80%) 특성을 가지며, 주로 디스플레이, 태양전지, 가스 센서 소자 등에 쓰인다. 투명전극으로 쓰이는 대표적인 물질로서는 ITO, ZnO, $SnO_2$ 등이 있으며, ITO는 전기적 특성이 우수하여 널리 사용되고 있으나 가격이 비싸고 화학적으로 불안정하고, ZnO는 ITO에 비해 가격이 저렴하지만 고온에서 불안정한 특성을 가지고 있다. 반면, $SnO_2$는 ITO와 ZnO에 비해 전기적 특성은 떨어지지만, 우수한 열적, 화학적 안정성 및 높은 내마모성을 가지고 제조단가가 저렴하여 TCO 재료로 많은 연구가 진행되고 있다. TCO 박막을 증착시키는 방법으로 CVD, ion plating, sputtering, spray pyrolysis 등이 있으며, 이 중 sputtering 방법은 균일한 입자로 균질의 박막을 입힐 수 있고 우수한 재현성과 낮은 온도에서도 증착이 가능하여 박막 제조 방법으로 널리 이용되고 있다. 본 연구에서는 $SnO_2$ 박막을 실리콘 (100) 및 글라스 (Eagle 2000) 기판 위에 RF magnetron sputtering 방법을 사용하여 제작하였다. 박막 증착을 위해 99.99%의 2 인치 un-doped $SnO_2$ 타겟을 사용하였고, 기판은 20 rpm 으로 회전시켜 균일한 박막이 형성될 수 있도록 하였으며, 초기 진공도는 $1{\times}10^{-6}\;Torr$가 되도록 하였다. 증착 변수로 기판-타겟간 거리, RF 파워, $O_2/(Ar+O_2)$ 비, 공정압력, 기판 온도 등을 각각 변화 시키며 $SnO_2$ 박막을 증착하였다. 증착된 박막의 구조적 및 광학적 특성을 분석하기위해 FE-SEM, AFM, XRD, UV/VIS spectrophotometer, Photoluminescence 등을 사용하였다.

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열분해법을 이용한 실리콘 나노입자 형성과정 수치해석 연구

  • U, Dae-Gwang;Ha, Su-Hyeon;Kim, Myeong-Jun;Hang, Zhang;Kim, Tae-Seong
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.117-117
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    • 2010
  • 나노입자 제조 기술이 점차 발전하면서 금속산화물, 반도체용 및 태양전지용, 신소재 등 다양한 응용분야에 사용하고 있다. 따라서 이와 같은 나노입자 제조방법으로는 펄스 레이저 용사법(pulsed laser ablation), 플라즈마 아크 합성법(plasma arc synthesis), 열분해법(pyrolysis), plasma-enhanced chemical vapor deposition (PECVD)법 등과 같은 기상공정이 많이 사용되고 있다. 기상공정은 기존의 공정에 비해 고순도 입자의 대량 생산, 다성분 입자의 화학적 균질성 유지, 비교적 간단하고 깨끗한 공정 등의 장점을 가지고 있다. 기상공정에서 일반적인 입자 형성 메커니즘은 기체 상태의 화학 물질이 물리적 공정 혹은 화학 반응에 의해 과포화상태에 도달하게 되며, 이 때 동질 핵생성(homogeneous nucleation)이 일어나고 생성된 핵(nuclei)에 기체가 응축되고 충돌, 응집하면서 입자는 성장하게 된다. 열분해법은 실리콘 나노입자를 생산하는 기상공정 중 하나이다. 일반적으로 열분해 공정은 지속적으로 열이 가해지는 반응기 내에 반응기체인 $SiH_4$을 주입하고, 운반기체는 He, $H_2$, Ar, $N_2$ 등을 사용하였을 때, 높은 열로 인해 $SiH_4$가 분해되며, 이 때 가스-입자 전환 현상(gas to particle conversion)이 일어나 실리콘 입자가 형성된다. 그러나 입자 형성과정은 $SiH_4$ 농도, 유량, 작동 압력, 온도 등 매우 다양한 요소에 영향을 받는다. 고, 복잡한 화학반응 메커니즘에 의해 명확히 규명되지는 못하고 있다. 이에 본 연구에서는 복잡한 화학반응을 해석하는 상용코드 CHEMKIN 4.1.1을 이용하여 열분해 반응기 내에서의 실리콘 입자 형성, 성장, 응집, 전송 모델을 만들고 이를 수치해석하였다. 표면 반응, 응집, 전송에 의한 입자 성장 메커니즘을 포함하고 있는 aerosol dynamics model을 method of moment법으로 해를 구하였으며, 이를 실험 결과와 비교하여 모델링을 검증하였다. 또한 반응기의 온도, 압력, 가스 농도, 유량 등의 요소를 고려하여 실리콘 나노입자를 형성하는 최적의 조건을 연구하였다.

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Synthesis and Microstructural Changes of Nanostructured Tungsten Carbide Powder by Chemical Vapor Condensation Process (화학기상응축법에 의한 나노구조 텅스텐카바이드 분말의 제조와 미세구조 변화)

  • ;;;;O.V.Tolochko
    • Journal of Powder Materials
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    • v.9 no.3
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    • pp.174-181
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    • 2002
  • Nanosized tungsten carbide powders were synthesized by the chemical vapor condensation(CVC) process using the pyrolysis of tungsten hexacarbonyl($W(CO)_6$). The effect of CVC parameters on the formation and the microstructural change of as-prepared powders were studied by XRD, BET and TEM. The loosely agglomerated nanosized tungsten-carbide($WC_{1-x}$) particles having the smooth rounded tetragonal shape could be obtained below $1000^{\circ}C$ in argon and air atmosphere respectively. The grain size of powders was decreased from 53 nm to 28 nm with increasing reaction temperature. The increase of particle size with reaction temperature represented that the condensation of precursor vapor dominated the powder formation in CVC reactor. The powder prepared at $1000^{\circ}C$ was consisted of the pure W and cubic tungsten-carbide ($WC_{1-x}$), and their surfaces had irregular shape because the pure W was formed on the $WC_{1-x}$ powders. The $WC_{1-x}$ and W powders having the average particles size of about 5 nm were produced in vacuum.

Nano-sized $Gd_{2}O_{3}:Eu$ phosphor particles of high brightness

  • Lee, Chang-Hee;Roh, Hyun-Sook;Kang, Yun-Chan;Park, Hee-Dong;Park, Seung-Bin
    • 한국정보디스플레이학회:학술대회논문집
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    • 2003.07a
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    • pp.791-794
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    • 2003
  • To synthesize $Gd_{2}O_{3}:Eu$ phosphor powder of nano size and high luminescence efficiency under UV (ultraviolet) and VUV (vacuum ultraviolet) light, organic additives such as citric acid and ethylene glycol and $Na_{2}CO_{3}$ flux were introduced in large-scale spray pyrolysis and critical conditions for forming nano-sized particles were investigated. The $Gd_{2}O_{3}:Eu$ phosphor particles prepared from solutions with organic additives such as citric acid and ethylene glycol had micron size and spherical shape. However, the particles prepared from polymeric precursor solution with $Na_{2}CO_{3}$ flux had nano size and non-aggregation characteristics. The as-prepared spherical particles with micron size turned into nano-sized particles during post-treatment by recrystallization process. The nano-sized $Gd_{2}O_{3}:Eu$ phosphor particles showed higher brightness than the commercial $Y_2O_3:Eu$ phosphor product under both UV light of 254nm and VUV light of 147 nm.

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High Permeability, High Selectivity Carbon-Silica Membranes for Gas Separation (기체분리용 고투과선택성 탄소-실리카막)

  • 이영무;박호범
    • Membrane Journal
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    • v.12 no.2
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    • pp.107-119
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    • 2002
  • Carbon-silica ($C-SiO_2$) membranes can be easily prepared by the pyrolysis of two-phase copolymers containing an aromatic imide block and a siloxane block and remarkably high permselectivities of $He/N_2, O_2/N_2,$ and $CO_2/N_2$. The pyrolysis of the imide-siloxane block copolymers was carried out at different final temperatures, $600^{\circ}C, 800^{\circ}C,$ and $1000^{\circ}C$ under an inert atmosphere, and is the first reported case of the precursors being used for the preparation of carbon membrane. The polymeric precursors were synthesized in a wide range of siloxane content and different final morphology, and the pyrolozed membranes were tested with a high vacuum time-lag method at $25^{\circ}C$ and 76cmHg of feed pressure. In experiments with He, $CO_2, O_2 \;and \;N_2$, the membranes were found to have good $O_2/N_2$ selectivity up to 32.2 and $O_2$ permeability on the order of $10-8/cm^2(STP)cm/cm^2seccmHg.$.

$Cu_2ZnSnS_4$ Thin Film Absorber Synthesized by Chemical Bath Deposition for Solar Cell Applications

  • Arepalli, Vinaya Kumar;Kumar, Challa Kiran;Park, Nam-Kyu;Nang, Lam Van;Kim, Eui-Tae
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2011.10a
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    • pp.35.1-35.1
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    • 2011
  • New photovoltaic (PV) materials and manufacturing approaches are needed for meeting the demand for lower-cost solar cells. The prototypal thin-film photovoltaic absorbers (CdTe and $Cu(In,Ga)Se_2$) can achieve solar conversion efficiencies of up to 20% and are now commercially available, but the presence of toxic (Cd,Se) and expensive elemental components (In, Te) is a real issue as the demand for photovoltaics rapidly increases. To overcome these limitations, there has been substantial interest in developing viable alternative materials, such as $Cu_2ZnSnS_4$ (CZTS) is an emerging solar absorber that is structurally similar to CIGS, but contains only earth abundant, non-toxic elements and has a near optimal direct band gap energy of 1.4~1.6 ev and a large absorption coefficient of ${\sim}10^4\;cm^{-1}$. The CZTS absorber layers are grown and investigated by various fabrication methods, such as thermal evaporation, e-beam evaporation with a post sulfurization, sputtering, non-vacuum sol-gel, pulsed laser, spray-pyrolysis method and electrodeposition technique. In the present work, we report an alternative method for large area deposition of CZTS thin films that is potentially high throughput and inexpensive when used to produce monolithically integrated solar panel modules. Specifically, we have developed an aqueous chemical approach based on chemical bath deposition (CBD) with a subsequent sulfurization heat treatment. Samples produced by our method were analyzed by scanning electron microscopy, X-ray diffraction, transmission electron microscopy, absorbance and photoluminescence. The results show that this inexpensive and relatively benign process produces thin films of CZTS exhibiting uniform composition, kesterite crystal structure, and good optical properties. A preliminary solar cell device was fabricated to demonstrate rectifying and photovoltaic behavior.

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Study on the response surface optimization of online upgrading of bio-oil with MCM-41 and catalyst durability analysis

  • Liu, Sha;Cai, Yi-xi;Fan, Yong-sheng;Li, Xiao-hua;Wang, Jia-jun
    • Environmental Engineering Research
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    • v.22 no.1
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    • pp.19-30
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    • 2017
  • Direct catalysis of vapors from vacuum pyrolysis of biomass was performed on MCM-41 to investigate the effects of operating parameters including catalyzing temperature, catalyzing bed height and system pressure on the organic yields. Optimization of organic phase yield was further conducted by employing response surface methodology. The statistical analysis showed that operating parameters have significant effects on the organic phase yield. The organic phase yield first increases and then decreases as catalyzing temperature and catalyzing bed height increase, and decreases as system pressure increases. The optimal conditions for the maximum organic phase yield were obtained at catalyzing temperature of $502.7^{\circ}C$, catalyzing bed height of 2.74 cm and system pressure of 6.83 kPa, the organic phase yield amounts to 15.84% which is quite close to the predicted value 16.19%. The H/C, O/C molar ratios (dry basis), density, pH value, kinematic viscosity and high heat value of the organic phase obtained at optimal conditions were 1.287, 0.174, $0.98g/cm^3$, 5.12, $5.87mm^2/s$ and 33.08 MJ/kg, respectively. Organic product compositions were examined using gas chromatography/mass spectrometry and the analysis showed that the content of oxygenated aromatics in organic phase had decreased and hydrocarbons had increased, and the hydrocarbons in organic phase were mainly aliphatic hydrocarbons. Besides, thermo-gravimetric analysis of the MCM-41 zeolite was conducted within air atmosphere and the results showed that when the catalyst continuously works over 100 min, the index of physicochemical properties of bio-oil decreases gradually from 1.15 to 0.45, suggesting that the refined bio-oil significantly deteriorates. Meanwhile, the coke deposition of catalyst increases from 4.97% to 14.81%, which suggests that the catalytic activity significantly decreases till the catalyst completely looses its activity.