• Title/Summary/Keyword: Electro chemical deposition

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Development of a Silicon Carbide Large-aperture Optical Telescope for a Satellite (SiC를 이용한 대구경 위성용 망원경 제작)

  • Bae, Jong In;Lee, Haeng Bok;Kim, Jeong Won;Lee, Kyung Mook;Kim, Myung-Whun
    • Korean Journal of Optics and Photonics
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    • v.33 no.2
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    • pp.74-83
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    • 2022
  • The entire process, from the raw material to the final system qualification test, has been developed to fabricate a large-diameter, lightweight reflective-telescope system for a satellite observation. The telescope with 3 anastigmatic mirrors has an aperture of 700 mm and a total mass of 66 kg. We baked a silicon carbide substrate body from a carbon preform using a reaction sintering method, and tested the structural and chemical properties, surface conditions, and crystal structure of the body. We developed the polishing and coating methods considering the mechanical and chemical properties of the silicon carbide (SiC) body, and we utilized a chemical-vapor-deposition method to deposit a dense SiC thin film more than 170 ㎛ thick on the mirror's surface, to preserve a highly reflective surface with excellent optical performance. After we made the SiC mirrors, we measured the wave-front error for various optical fields by assembling and aligning three mirrors and support structures. We conducted major space-environment tests for the components and final assembly by temperature-cycling tests and vibration-shock tests, in accordance with the qualifications for the space and launch environment. We confirmed that the final telescope achieves all of the target performance criteria.

Photoemission Electron Micro-spectroscopic Study of the Conductive Layer of a CVD Diamond (001)$2{\times}1$ Surface

  • Kono, S.;Saitou, T.;Kawata, H.;Goto, T.
    • Proceedings of the Korean Vacuum Society Conference
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    • 2010.02a
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    • pp.7-8
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    • 2010
  • The surface conductive layer (SCL) of chemical vapor deposition (CVD) diamonds has attracting much interest. However, neither photoemission electron microscopic (PEEM) nor micro-spectroscopic (PEEMS) information is available so far. Since SCL retains in an ultra-high vacuum (UHV) condition, PEEM or PEEMS study will give an insight of SCL, which is the subject of the present study. The sample was made on a Ib-type HTHP diamond (001) substrate by non-doping CVD growthin a DC-plasma deposition chamber. The SCL properties of the sample in air were; a few tens K/Sq. in sheet resistance, ${\sim}180\;cm^2/vs$ in Hall mobility, ${\sim}2{\times}10^{12}/cm^2$ in carrier concentration. The root-square-mean surface roughness (Rq) of the sample was ~0.2nm as checked by AFM. A $2{\times}1$ LEED pattern and a sheet resistance of several hundreds K/Sq. in UHV were checked in a UHV chamber with an in-situ resist-meter [1]. The sample was then installed in a commercial PEEM/S apparatus (Omicron FOCUS IS-PEEM) which was composed of electro-static-lens optics together with an electron energy-analyzer. The presence of SCL was regularly monitored by measuring resistance between two electrodes (colloidal graphite) pasted on the two ends of sample surface. Figure 1 shows two PEEM images of a same area of the sample; a) is excited with a Hg-lamp and b) with a Xe-lamp. The maximum photon energy of the Hg-lamp is ~4.9 eV which is smaller that the band gap energy ($E_G=5.5\;eV$) of diamond and the maximum photon energy of the Xe-lamp is ~6.2 eV which is larger than $E_G$. The image that appear with the Hg-lamp can be due to photo-excitation to unoccupied states of the hydrogen-terminated negative electron affinity (NEA) diamond surface [2]. Secondary electron energy distribution of the white background of Figs.1a) and b) indeed shows that the whole surface is NEA except a large black dot on the upper center. However, Figs.1a) and 1b) show several features that are qualitatively different from each other. Some of the differences are the followings: the two main dark lines A and B in Fig.1b) are not at all obvious and the white lines B and C in Fig.1b) appear to be dark lines in Fig.1a). A PEEMS analysis of secondary electron energy distribution showed that all of the features A-D have negative electron affinity with marginal differences among them. These differences can be attributed to differences in the details of energy band bending underneath the surface present in SCL [3].

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Cu2ZnSn(S,Se)4 Thin Film Solar Cells Fabricated by Sulfurization of Stacked Precursors Prepared Using Sputtering Process

  • Gang, Myeng Gil;Shin, Seung Wook;Lee, Jeong Yong;Kim, Jin Hyeok
    • Proceedings of the Korean Vacuum Society Conference
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    • 2013.08a
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    • pp.97-97
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    • 2013
  • Recently, Cu2ZnSn(S,Se)4 (CZTSS), which is one of the In- and Ga- free absorber materials, has been attracted considerable attention as a new candidate for use as an absorber material in thin film solar cells. The CZTSS-based absorber material has outstanding characteristics such as band gap energy of 1.0 eV to 1.5 eV, high absorption coefficient on the order of 104 cm-1, and high theoretical conversion efficiency of 32.2% in thin film solar cells. Despite these promising characteristics, research into CZTSS based thin film solar cells is still incomprehensive and related reports are quite few compared to those for CIGS thin film solar cells, which show high efficiency of over 20%. I will briefly overview the recent technological development of CZTSS thin film solar cells and then introduce our research results mainly related to sputter based process. CZTSS thin film solar cells are prepared by sulfurization of stacked both metallic and sulfide precursors. Sulfurization process was performed in both furnace annealing system and rapid thermal processing system using S powder as well as 5% diluted H2S gas source at various annealing temperatures ranging from $520^{\circ}C$ to $580^{\circ}C$. Structural, optical, microstructural, and electrical properties of absorber layers were characterized using XRD, SEM, TEM, UV-Vis spectroscopy, Hall-measurement, TRPL, etc. The effects of processing parameters, such as composition ratio, sulfurization pressure, and sulfurization temperature on the properties of CZTSS absorber layers will be discussed in detail. CZTSS thin film solar cell fabricated using metallic precursors shows maximum cell efficiency of 6.9% with Jsc of 25.2 mA/cm2, Voc of 469 mV, and fill factor of 59.1% and CZTS thin film solar cell using sulfide precursors shows that of 4.5% with Jsc of 19.8 mA/cm2, Voc of 492 mV, and fill factor of 46.2%. In addition, other research activities in our lab related to the formation of CZTS absorber layers using solution based processes such as electro-deposition, chemical solution deposition, nano-particle formation will be introduced briefly.

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Electrochemical properties of heat-treated multi-walled carbon nanotubes (열처리된 탄소나노튜브 상대전극의 전기화학적 특성 연구)

  • Lee, S.K.;Moon, J.H.;Hwang, S.H.;Kim, G.C.;Lee, D.Y.;Kim, D.H.;Jeon, M.H.
    • Journal of the Korean Vacuum Society
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    • v.17 no.1
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    • pp.67-72
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    • 2008
  • We have studied the effect of heat treatment of multi-walled carbon nanotubes (MWNTs) as a counter electrode on the electro-chemical properties of dye-snsitized solar cells. MWNTs on the p-type Si substrate were synthesized by thermal chemical vapor deposition (CVD) using Fe catalysts. We prepared the two types of MWNTs samples with the different diameters. The rapid thermal annealing (RTA) treatment for the MWNTs was carried out at the growth temperature ($900^{\circ}C$) for 1 minute with $N_2$ gas atmosphere. The structural, electrical and electrochemical properties of MWNTs were investigated by field-emission scanning electron microscopy (FE-SEM), Raman spectroscopy, 2-point probe station and electrochemical impedance spectroscopy (EIS). The I(D)/I(G) ratio of heat-treated MWNTs in Raman spectra was considerably decreased. It was also found that the heat-treated MWNTs showed better redox reaction of iodide at the interface between MWNTs surface and electrolyte than that of as-grown MWNTs. The redox resistance value of heat-treated electrodes was measured to be much lower than that of as-grown electrode at the interface. As a result, the counter electrode using the heat-treated MWNTs showed better electrochemical properties.

Effects of hydrogen and ammonia partial pressure on MOCVD $Co/TaN_x$ layer for Cu direct electroplating

  • Park, Jae-Hyeong;Mun, Dae-Yong;Han, Dong-Seok;Yun, Don-Gyu;Park, Jong-Wan
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2012.05a
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    • pp.84-84
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    • 2012
  • 소자가 고집적화 됨에 따라, 비저항이 낮고 electro migration (EM), Stress Migration (SM) 특성이 우수한 구리(Cu)를 배선재료로서 사용하고 있다. 그러나, 구리는 Si과 $SiO_2$의 내부로 확산이 빠르게 일어나, Si 소자 내부에 deep donor level을 형성하고, 누설 전류를 증가시키는 등 소자의 성능을 저하시킬 수 있는 문제점을 가지고 있다. 그러나, electroplating 을 이용하여 증착한 Cu 박막은 일반적으로 확산 방지막으로 쓰이는 TiN, TaN, 등의 물질과의 접착 (adhesion) 특성이 나쁘다. 따라서, Cu CMP 에서 증착된 Cu 박막의 벗겨지거나(peeling), EM or SM 저항성 저하 등의 배선에서의 reliability 문제를 야기하게된다. 따라서 Cu 와 접착 특성이 좋은 새로운 확산방지막 또는 adhesion layer의 필요성이 대두되고 있다. 본 연구에서는 이러한 Cu 배선에서의 접착성 문제를 해결하고자 Metal organic chemical vapor deposition (MOCVD)을 이용하여 제조한 코발트(Co) 박막을 $Cu/TaN_x$ 사이의 접착력 개선을 위한 adhesion layer로 적용하려는 시도를 하였다. Co는 비저항이 낮고, Cu 와 adhesion이 좋으며, Cu direct electroplating 이 가능하다는 장점을 가지고 있다. 하지만, 수소 분위기에서 $C_{12}H_{10}O_6(Co)_2$ (dicobalt hexacarbonyl tert-butylacetylene, CCTBA) 전구체에 의한 MOCVD Co 박막의 경우 탄소, 산소와 같은 불순물이 다량 함유되어 있어, 비저항, surface roughness 가 높아지게 된다. 따라서 구리 전착 초기에 구리의 핵 생성(nucleation)을 저해하고 핵 생성 후에도 응집(agglomeration)이 발생하여 연속적이고 얇은 구리막 형성을 방해한다. 이를 해결하기 위해, MOCVD Co 박막 증착 시 수소 반응 가스에 암모니아를 추가로 주입하여, 수소/암모니아의 분압을 1:1, 1:6, 1:10으로 변화시켜 $Co/TaN_x$ 박막의 특성을 비교 분석하였다. 각각의 수소/암모니아 분압에 따른 $Co/TaN_x$ 박막을 TEM (Transmission electron microscopy), XRD (X-ray diffraction), AES (Auger electron spectroscopy)를 통해 물성 및 조성을 분석하였고, AFM (Atomic force microscopy)를 이용하여, surface roughness를 측정하였다. 실험 결과, $Co/TaN_x$ 박막은 수소/암모니아 분압 1:6에서 90 ${\mu}{\Omega}-cm$의 낮은 비저항과 0.97 nm 의 낮은 surface roughness 를 가졌다. 뿐만 아니라, MOCVD 에 의해 증착된 Co 박막이4-6 % concentration 의 탄소 및 산소 함량을 가지는 것으로 나타났고, 24nm 크기의 trench 기판 위에 약 6nm의 $Co/TaN_x$ 박막이 매우 균일하게 형성된 것을 확인 할 수 있었다. 이러한 결과들은, 향후 $Co/TaN_x$ 박막이 Cu direct electroplating 공정이 가능한 diffusion barrier로서 성공적으로 사용될 수 있음을 보여준다.

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Defect Inspection and Physical-parameter Measurement for Silicon Carbide Large-aperture Optical Satellite Telescope Mirrors Made by the Liquid-silicon Infiltration Method (액상 실리콘 침투법으로 제작된 대구경 위성 망원경용 SiC 반사경의 결함 검사와 물성 계수 측정)

  • Bae, Jong In;Kim, Jeong Won;Lee, Haeng Bok;Kim, Myung-Whun
    • Korean Journal of Optics and Photonics
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    • v.33 no.5
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    • pp.218-229
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    • 2022
  • We have investigated reliable inspection methods for finding the defects generated during the manufacturing process of lightweight, large-aperture satellite telescope mirrors using silicon carbide, and we have measured the basic physical properties of the mirrors. We applied the advanced ceramic material (ACM) method, a combined method using liquid-silicon penetration sintering and chemical vapor deposition for the carbon molded body, to manufacture four SiC mirrors of different sizes and shapes. We have provided the defect standards for the reflectors systematically by classifying the defects according to the size and shape of the mirrors, and have suggested effective nondestructive methods for mirror surface inspection and internal defect detection. In addition, we have analyzed the measurements of 14 physical parameters (including density, modulus of elasticity, specific heat, and heat-transfer coefficient) that are required to design the mirrors and to predict the mechanical and thermal stability of the final products. In particular, we have studied the detailed measurement methods and results for the elastic modulus, thermal expansion coefficient, and flexural strength to improve the reliability of mechanical property tests.

Reaction Gas Composition Dependence on the Properties of SnO2 Films on PET Substrate by ECR-MOCVD (반응가스조성이 PET기판위에 ECR 화학증착법에 의해 제조된 SnO2 박막특성에 미치는 영향)

  • Kim, Yun-Seok;Lee, Joong-Kee
    • Journal of the Korean Electrochemical Society
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    • v.8 no.3
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    • pp.139-145
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    • 2005
  • [ $SnO_x$ ] films on the flexible substrate of PET film were prepared at ambient temperature under a $(CH_3)_4Sn(TMT: tetra-methyl tin)-H_2-O_2$ atmosphere in order to obtain transparent conductive polymer by using ECR-MOCVD(Electro Cyclotron Resonance Metal Organic Chemical Yfpor Deposition) system. The prepared $SnO_x$ thin films show generally over $90\%$ of optical transmittance at wavelength range of 380-780nm and about $1\times10^{-2\~3}ohm{\cdot}cm$ of electrical resistivity. In the present study, effects of $O_2/TMT\;and\;H_2/TMT$ mole ratio on the properties of $SnO_x$ films are investigated and the other process parameters such as microwave power, magnetic current power, substrate distance and working pressure are fixed. Based on our experimental results, the $SnO_x$ film composition ratio of Sn and O directly influences on the electrical and optical properties of the films prepared. The $SnO_x$ film with low electric resistivity and high transmittance could be obtained by controlling the process parameters such as $O_2/TMT\;and\;H_2/TMT$ mole ratio, which play an important role to change the composition ratio between Sn and O. An increase of $O_2/TMT$ mole ratio brought on the increases 0 content in the $SnO_x$ film. On the other hand, an increase of $H_2/TMT$ mole ratio lead to decreases the oxygen content in the film. The optimized composition ratio of oxygen : tin Is determined as 2.4: 1 at $O_2/TMT$ of 80 and $H_2/TMT$ of 40 mole ratio, respectively.

Optical Properties of SiNx Thin Films Grown by PECVD at 200℃ (200℃의 저온에서 PECVD 기법으로 성장한 SiNx 박막의 열처리에 따른 광학적 특성 변화 규명)

  • Lee, Kyung-Su;Kim, Eun-Kyeom;Son, Dae-Ho;Kim, Jeong-Ho;Yim, Tae-Kyung;An, Seung-Man;Park, Kyoung-Wan
    • Journal of the Korean Vacuum Society
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    • v.20 no.1
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    • pp.42-49
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    • 2011
  • We deposited $SiN_x$ thin films by using PECVD technique at $200^{\circ}C$ with various flow ratios of the $SiH_4/N_2$ gases. The photoluminescence measurements revealed that the maximum emission wavelength shifted to long wavelength as the ratio increased, however, positions of the several peak wavelengths, such as 1.9, 2.2, 2.4, and 3.1 eV, were independent on the ratio. Changes of the photoluminescence spectra were measured in the $N_{2}-$, $H_{2}-$, and $O_2$-annealed films. The luminescence intensities increased after the annealing process. In particular, the maximum emission wavelength shifted to short wavelength after $H_{2}-$ or $O_2$-annealing. But there were still several peaks on the spectra of all annealed films, several peak positions remained to be unchanged after the annealing. As for the light emission mechanism, we have considered the defect states of the Si- and N- dangling bonds in the $SiN_x$ energy gap, so that the energy transitions from/to the conduction/valence bands and the defect states in the gap were attributed to the light emission in the $SiN_x$ films. The experimental results point to the possibility of a Si-based light emission materials for flexible Si-based electro-optic devices.