Proceedings of the Korean Institute of Surface Engineering Conference (한국표면공학회:학술대회논문집)
The Korean Institute of Surface Engineering
- Semi Annual
Domain
- Materials > Thermal/Surface Treatment
2001.11a
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21세기의 신물질로 알려져 있는 플라즈마는 기체에 에너지를 가해 형성되는 높은 에너지(수십만도)의 이옹화된 기체의 집합체로 최근 이러한 플라즈마를 이용하여 고부가가치의 신기 능 제품개발에 널리 활용되고 있다. 플라즈마를 이용한 신기능 표면처리 기술개발이 가속 화됨에 따라 자동차, 기계, 전자, 에너지, 환경 산엽둥 전 산업 분야에 그 응용범위가 광범위 하게 확대 되고 있으며 이에 따른 핵심 연구개발도 최근 매우 중요시 되고 있다. 본 발표에서는 이라한 최끈 플라즈마 기술의 발전동향, 응용현황 및 향후 기술 확산을 위한 핵심 연구 방향에 대해 고찰하고저 한다.
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Two companies plating baths were selected for plating on phenol and epoxy resin boards as well as on flexible p polyimide boards. After plating, deposited i&IIk&.ness al1d physical properties, as well as solder wettabilities by aging with
$150^{\circ}C$ heating and 100% humidity were compared. After plating and aged with two different tin baths, deposited thickness and physical properties were not so great differences, but solder wettabilities were superior used polymer catalyst than the other. Furthermore depend upon the compactness and fineness of metallic sturctures of the base copper, the amounts of the plated copper were big differel1lces. These differences seems to be inherited from the kind and amount of additives. as well as current densities, which are influences upon structures of Copper layers. Generally the tin thickness are hetween 0.5 to$1.0\mu\textrm{m}$ and thicker the solder wettabilities are the better, and also me compact structures of deposits showed gooo soidierabiiities. In this study, with our own deveiotaedl plating equipment could get more than$0.5\mu\textrm{m}$ of till thickness and piating speed was$0.1\mu\textrm{m}$ per minutes. -
In this paper, initial depositing process of electroless Ni-Cu-P alloy was investigated by means of SEM, TEM and AES. The results show that the initial deposition is inhomogeneous and there exist different transition layers between different coatings and substrates, which are decided by the structures and compositions of the bath. For Ni-P binary alloy, its deposition takes place superiorly at grain boundary and on some grains with beneficial texture, the thickness of transition layer composed of Ni-Fe-P reaches 2000 angstrom. But during initiation of Ni-Cu-P trinary alloy, only at grain boundary is prIor to be deposited electrolessly, transited layer contains Ni-Fe-Cu-P and is decreased to about 500 angstrom. The structures of the films of Ni-P and Ni-Cu-P are crystalline at the initial depositing stage. The mechanisms of the process are put forward in this paper.
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$TiCl_44,{\;}AICl_3,{\;}H_2,{\;}Ar,{\;}NH_3$ 기체를 사용하여 플라즈마 화학 증착법으로$(Ti_{1-x}AI_x)N$ 피막을 증착한 후 진공열처리 실험을 통해 열처리 전후에 나타나는 피막의 가계적 특성 변화 및 상변화 양상에 대해 연구하였다. 기판으로는 M2 고속도강과 알루미나(${\alpha}-Al_2O_3$ )를 사용하였으며, 열처리 실험은 진공 열처리로를 이용하여$800$ ~$1100^{\circ}C$ 에서 진행하였다. M2 고속도강 위에 증착한$(Ti_{1-x}AI_x)N$ 피막은 모두 (200) 우선 방위를 갖고 있었으며, AI의 함량이 높아짐에 따라 입자의 크기가 미세해져$(Ti_{0.2}AI_{0.8})N$ 의 경우 수 nm의 업자들로 이루어져 있었다. 열처리 시간을 일정하게 하고, 그 온도를 증가시킬 경우 비교적 낮은 온도 영역($~900^{\circ}C$ )에서는 경도 증가를 나타내지만, 열처리가 더욱 진행됨에 따라 다시 경도가 감소하는 양상을 나타내었으며, 열처리 온도를 일정하게 하고 열처리 시간을 변화 시킬 경우에도 초기에 경도가 증가하다가 열처리가 진행됨에 따라 경도가 다시 감소하는 현상을 관찰 하였다. 이때 경도증가 정도는 Al 함량이 높을 수록 뚜렷하고 오래 지속되었으며,$(Ti_{0.2}AI_{0.8})N$ 피막의 경우 열처리 전$2000HK_{0.01}$ 에서 열처리 후$4500HK_{0.01}$ 로, 매우 큰 경도 증가를 나타내었다. 이와 같은 열처리 전후의 기계적 특성 변화는 준 안정상의$(Ti_{1-x}AI_{x})N$ 피막에서, 열처리가 진행됨에 따라 미세한 AlN 업자가 석출되면서 나타나는 현상으로, 고분해능 전자현미경(HRTEM) 분석을 통해 경도가 증가한 시편의 경우 석출상의 크기가 5nm 이하로 매우 작고 대체로 기지와 연속적인 계면을 형성하나, 열처리가 진행될수록 석 출상의 크기가 커지고 임계크기 이상에 이르면 연속적인 계면은 거의 발견되지 않고, 대부 분 불연속적이고 확연한 계면을 형성함을 관찰 할 수 있었다. 알루미나(${\alpha}-Al_2O_3$ ) 기판 위에 증착한$(Ti_{1-x}AI_{x})N$ 피막은 마찬가지로 (200) 우선 방위를 나타내었으나, 그 입자의 크기가 수십 nm로 고속도강위에 증착한 피막에 비해 상당히 크게 형성되었다. 또한 열처리 후에 AIN의 석출이 진행됨에도 불구하고 경도 증가는 나타나지 않고, 열처리가 진행됨에 따라 경도가 감소하는 양상만을 나타내었다. 결국$(Ti_{1-x}AI_{x})N$ 피막이 열처리 전후에 보아는 기계적 특성의 변화 양상은 열역학적으로 안정한 Wurzite-AlN의 석출에 따른 것으로 AlN 석출상의 크기에 의존하며, 또한 이러한 영향은$(Ti_{1-x}AI_{x})N$ 피막에 존재하는 AI의 함량이 높고, 초기에 증착된 막의 업자 크기가 작을 수록 클 것으로 여겨진다. -
This paper presents some results of plasma nitriding on hard chromium deposit. The substrates were C45 steel and
$30~50{\;}\mu\textrm{m}$ of chromium deposit by electroplating was formed. Plasma nitriding was carried out in a plasma nitriding system with$95NH_3{\;}+{\;}SCH_4$ atmosphere at the pressure about 600 Pa and different temperature from$450^{\circ}C{\;}to{\;}720^{\circ}C$ for various time. Optical microscopy and X-ray diffraction were used to evaluate the characteristics of surface nitride layer formed by nitrogen diffusion from plasma atmosphere inward iCr coating and interface carbide layer formed by carbon diffusion from substrate outward Cr coating. The microhardness was measured using microhareness tester at the load of 100 gf. Corrosion resistance was evaluated using the potentiodynamic measurement in 3.5% NaG solution. A saturated calomel electrode (SiCE) was used as the reference electrode. Fig.1 shows the typical microstructures of top surface and cross-section for nitrided and unnitrided samples. Aaer plasma nitriding a sandwich structure was formed consisting of surface nitride layer, center chromium layer and interface carbide layer. The thickness of nitride and carbide layers was increased with the increase of processing temperature and time. Hardness reached about 1000Hv after nitriding while 900Hv for unnitrided hard chromium deposit. X-ray diffraction indicated that surface nitrided layer was a mixture of$Cr_2N$ and CrN at low temperature and erN at high temperature (Fig.2). Anodic polarization curves showed that plasma nitriding can greatly improve the corrosion resistance of chromium e1ectrodeposit. After plasma nitriding, the corrosion potential moved to noble direction and passive current density was lower by 1 to 4 orders of magnitude compared with chromium deposit(Fig.3). -
Recently, many of the current development in surface modification engineering are focused on multilayered coatings. Multilayered coatings have the potential to improve the tribological and corrosion properties of tools and components. By using cathodic arc deposition,
$WC-Ti_{1-x}Al_xN$ multilayers were deposited on steel substrates. Wear tests of four multiplayer coatings were performed using a ball-on-disc configuration with a linear sliding speed of 0.1m/s, 5N load. The tests were carried out at room temperature in airby employing AISI 52100 steel ball ($H_v=848N$ ) of 11mm in diameter. Electrochemical tests were performed using the potentiodynamic and electrochemical impedance spectroscopy (EIS) measurements. The surface morphology and topography of the wear scars of tribo-element and the corroded specimen have been determined by using scanning electron spectroscopy (SEM). Also, wear mechanism was determined by using SEM coupled with EDS. Results have showed an improved wear resistance and corrosion resistance of the$WC-Ti_{1-x}Al_xN$ coatings. -
agnesium Oxide (MgO) with a NaCI structure is well known to exhibit high secondary electron emission, excellent high temperature chemical stability, high thermal conductance and electrical insulating properties. For these reason MgO films have been widely used for a buffer layer of high
$T_c$ superconducting and a protective layer for AC-plasma display panels to improve discharge characteristics and panel lifetime. Up to now MgO films have been synthesized by lE-beam evaporation, Molecular Beam Epitaxy (MBE) and Metalorganic Chemical Vapor Deposition (MOCVD), however there have been some limitations such as low film density and micro-cracks in films. Therefore magnetron sputtering process were emerged as predominant method to synthesis high density MgO films. In previous works, we designed and manufactured unbalanced magnetron source with high power density for the deposition of high quality MgO films. The magnetron discharges were sustained at the pressure of O.lmtorr with power density of$110W/\textrm{cm}^2$ and the maximum deposition rate was measured at$2.8\mu\textrm{m}/min$ for Cu films. In this study, the syntheses of MgO films were carried out by unbalanced magnetron sputtering with various$O_2$ partial pressure and specially target power densities, duty cycles and frequency using pulsed DC power supply. And also we investigated the plasma states with various$O_2$ partial pressure and pulsed DC conditions by Optical Emission Spectroscopy (OES). In order to confirm the relationships between plasma states and film properties such as microstructure and secondary electron emission coefficient were analyzed by X-Ray Diffraction(XRD), Transmission Electron Microscopy(TEM) and${\gamma}-Focused$ Ion Beam (${\gamma}-FIB$ ). -
TiN coatings were applied for VarIOUS application fields, because of a good wear-resistance and a high hardness. Typically, TiN thin films show the hardness of 25GPa and friction coefficient of 0.6. However, in many field, one is looking for a more improved tool which has low friction coefficient and high wear resistance. The main motivation of this study is to characterize the influence of copper dopant content on TiN thin films. Ti-Cu-N thin films were deposited onto D2 steel substrates by PVD processing with various magnetron current densities (Cu contents). In this work, we synthesized titanium nitride films similar with reported typical titanium nitride films and synthesized Ti-Cu-N thin films with the addition of elemental copper which is measured improved hardness more than pure TiN films with copper content variables. This films has preferred oriented films of (111) direction. In addition, It was found that there is a strong correlation between content of various metal and film characteristics such as preferred orientation, grain size, hardness and friction coefficient and so, in future study, improved mechanical properties of TiN films can be controlled by change in target current density. The Ti-Cu-N film will show apparent hardness improvement and mechanical properties enhancement, when doping element is added onto TiN thin films. Film structure, chemical composition, mechanical properties were investigated by means of X-ray diffraction(XRD), scanning electron microscopy(SEM), transmission electron microscopy (TEM), energy dispersive spectroscopy(EDS), wear resistance tester and nanohardness tester.
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포항가속기의 초고진공 세정기술은 초고진공 영역에서의 기체방출을 최소화하기 위한 것으로 발생한 오염원을 추적하여 큰 오염원 부터 시작하여 단계적으로 진행해 미세한 오염원 을 제거해 나가는 방법을 적용하고 있다. 이러한 극청정한 진공표면을 얻기 위해서는 표면과 오염물질 사이의 결합에너지를 극복해야 한다. 오염물 제거 방법으로는 물리.전기.화학적인 방법을 모두 적용하며 그리스 및 절삭유를 비롯해 흡착된 탄화수소와 불순물 성분 또는 산소나 황과 같은 반응성 원소와의 화합물 등을 효과적으로 제거한다. 또한, 세정 과정 에서 생성될 수 있는 수소, 불규칙한 산화물, 질화물, 염화물, 그리고 탄수화물을 최소화하여 초고진공 영역에 도달할 수 있는 방법을 제공한다. 본 논문에서는 포항가속기 연구소의 초고진공 환경을 확보하기 위한 화학세정 설비 및 응용기술, 주요 진공 구성재료의 표면 분석 결과를 소개하고자 한다.
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Ni-W alloy deposit is one of the best alternatives to hard chromium plating because of its good mechanical properties (high hardness, high strength, and good wear resistance). Ni-W alloy is deposited from weakly acidic or alkaline electrolytic bath with nickel sulfate, sodium tungstate or APT, and some kinds of organic hydroxy-acid complex and ammonia salts. W content of the deposit can be changed from 0 to 5Owt% and the coating with high W content is more attracted. But, meanwhile, the deposited layers are always found high internal stress, which cause them to become brittle and to bond insufficiently with the substrate. On the second hand, as the W content is incresed, the current efficiency reduced, which results in large quantities of hydrogen evolution and then produces bubbles on surface and pitting appearance In this paper, the influence of some additives on Ni-W alloy electroplating was investigated by means of compositional analysis and SEM. The initial results showed that 2-butyne-1,4-diol was the best brightener for Ni-W plating process. It could brighten and level deposit, but decreased the cathodic current efficiency. Its optimum concentration range is from O.lgjL to 0.5gjL. Besides, three kinds of additives including 2-butyne-1,4-diol were examined with Dagguchi method.
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As a new approach to substitute for a hard alloy of stellite 6B containing Co which is radioactive in nuclear system, a hard-phase coating of CrN will be applicable to protect 12Cr steel from erosion at leading edge on steam turbine blade. The CrN coating was prepared by arc ion plating on 12 Cr steel and was undertaken in liquid impact test at the velocity of 35Om/sec, which simulate the environment in the last stage of blade. The erosion resistance of coating was evaluated by optical observation on damaged surface. The threshold number of impact was closely related with surface hardness. And thus, it was confirmed that surface hardening improves the life time of steam turbine blade.
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The structure zone model has been used to provide an overview of the relationship between the microstructure of the films deposited by PVD and the most prominent deposition condition.s. B.AMovchan and AV.Demchishin have proposed it firstls such model. They concluded that the general features of the resulting structures could be correlated into three zones depending on
$T/T_m$ . Here T m is the melting point of the coating material and T is the substrate temperature in kelvines. Zone 1 ($T/Tm_ ) is dominated by tapered macrograins with domed tops, zone 2 ( $O.3 ) by columnar grains with denser boundaries and zone 3 ( $T/T_m>O.5$ ) by equiaxed grains formed by recrystallization. J.AThomton has extended this model to include the effect of the sputtering gas pressure and found a fourth zone termed zone T(transition zone) consisting of a dense array of poorly defined fibrous grains. R.Messier found that the zone I-T boundary (fourth zone of Thorton) varies in a fashion similar to the film bias potential as a function of gas pressure. However, there has not nearly enough model for explaining the change in morphology with crystal orientation of the films. The structure zone model only provide an information about the morphology of the deposited film. In general, the nucleation and growth mechanism for granular and fine structure of the deposited films are very complex in an PVD technique because the morphology and orientation depend not only on the substrate temperature but also on the energy of deposition of the atoms or ions, the kinetic mechanism between metal atoms and argon or nitrogen gas, and even on the presence of impurities. In order to clarify these relationship, AI and Mg thin films were prepared on SPCC steel substrates by PVD techniques. The influence of gas pressures and bias voltages on their crystal orientation and morphology of the prepared films were investigated by SEM and XRD, respectively. And the effect of crystal orientation and morphology of the prepared films on corrosion resistance was estimated by measuring polarization curves in 3% NaCI solution. -
Thin films of polycrystalline silicon (poly-Si) is a promising material for use in large-area electronic devices. Especially, the poly-Si can be used in high resolution and integrated active-matrix liquid-crystal displays (AMLCDs) and active matrix organic light-emitting diodes (AMOLEDs) because of its high mobility compared to hydrogenated _amorphous silicon (a-Si:H). A number of techniques have been proposed during the past several years to achieve poly-Si on large-area glass substrate. However, the conventional method for fabrication of poly-Si could not apply for glass instead of wafer or quartz substrate. Because the conventional method, low pressure chemical vapor deposition (LPCVD) has a high deposition temperature (
$600^{\circ}C-1000^{\circ}C$ ) and solid phase crystallization (SPC) has a high annealing temperature ($600^{\circ}C-700^{\circ}C$ ). And also these are required time-consuming processes, which are too long to prevent the thermal damage of corning glass such as bending and fracture. The deposition of silicon thin films on low-cost foreign substrates has recently become a major objective in the search for processes having energy consumption and reaching a better cost evaluation. Hence, combining inexpensive deposition techniques with the growth of crystalline silicon seems to be a straightforward way of ensuring reduced production costs of large-area electronic devices. We have deposited crystalline poly-Si thin films on soda -lime glass and SiOz glass substrate as deposited by PVD at low substrate temperature using high power, magnetron sputtering method. The epitaxial orientation, microstructual characteristics and surface properties of the films were analyzed by TEM, XRD, and AFM. For the electrical characterization of these films, its properties were obtained from the Hall effect measurement by the Van der Pauw measurement. -
We report a study of the nitriding of the martensitic grade of stainless steel AKSK 420 in a low-pressure rl discharge using pure nitrogen. Much studied samples of the austenitic grade AISI 304 were treated at the same time to provide a comparison. With a treatment time of 4.0 h at
$400^{\circ}C$ , the nitrogen-rich layer on MSK 420 is 20pm thick and has a hardness about 4.3 times higher than that of the untreated material. The layer thickness is much greater than that obtained on AISI 304 under identical treatment conditions, reflecting the different Cr content of the two alloys. The alloy AlISI 420 is more susceptible than AISI 304 to the formation of CrN and ferrite, and this has a deleterious effect on the hardnes, gain. Below the temperature at which CrN forms, the treated layer retains its martensitic structure, but with a larger lattice parameter than the bulk, a phase that we term expanded martensite, by analogy with the situation with austenitic stainless steel. The fact that the treated layer retains a martensitic structure is interesting in view of previous evidence that nitrogen is an austenite stabilizer. -