• Title/Summary/Keyword: $TiCl_3$

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Effect of Microstructure on Corrosion Behavior of TiN Hard Coatings Produced by Two Grid-Attached Magnetron Sputtering

  • Kim, Jung Gu;Hwang, Woon Suk
    • Corrosion Science and Technology
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    • v.5 no.1
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    • pp.15-22
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    • 2006
  • The introduction of two-grid inside a conventional process system produces a reactive coating deposition and increases metal ion ratio in the plasma, resulting in denser and smoother films. The corrosion behaviors of TiN coatings were investigated by electrochemical methods, such as potentiodynamic polarization test and electrochemical impedance spectroscopy (EIS) in deaerated 3.5% NaCl solution. Electrochemical tests were used to evaluate the effect of microstructure on the corrosion behavior of TiN coatings exposed to a corrosive environment. The crystal structure of the coatings was examined by X-ray diffractometry (XRD) and the microstructure of the coatings was investigated by scanning electron microscopy (SEM) and transmission electron spectroscopy (TEM). In the potentiodynamic polarization test and EIS measurement, the corrosion current density of TiN deposited by two grid-attached magnetron sputtering was lower than TiN deposited by conventional magnetron type and also presented higher Rct values during 240 h immersion time. It is attributed to the formation of a dense microstructure, which promotes the compactness of coatings and yields lower porosity.

Characterizations of Ti-Al-V-N Films Deposited by DC and RF Reactive Magnetron Sputtering (직류 및 고주파 마그네트론 스퍼터링법으로 증착한 Ti-Al-V-N 박막의 특성)

  • Sohn, Yong-Un;Chung, In-Wha;Lee, Young-Ki
    • Journal of the Korean Society for Heat Treatment
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    • v.13 no.6
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    • pp.398-404
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    • 2000
  • The Ti-Al-V-N films have been deposited on various substrates by d.c and r.f reactive magnetron sputtering from a Ti-6Al-4V alloy target in mixed $Ar-N_2$ discharges. The films were investigated by means of XRD, AES, SEM/EDX, microhardness, TG and scratch test. The XRD and SEM results indicated that the films were of single B1 NaCl phase having dense columnar structure with the (111) preferred orientation. The composition of Ti-Al-V-N film was the Ti-7.1Al-4.3V-N(wt%) films. Adhesion and microhardness of Ti-Al-V-N films deposited by r.f magnetron sputtering method were better than those deposited by d.c magnetron sputtering method. The anti-oxidation properties of Ti-Al-V-N films were also superior to that of Ti-N film deposited by the same deposition conditions.

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The microstructure and adhesive characteristics of Ti-Al-V-N films prepared by reactive magnetron sputtering (반응성 마그네트론 스퍼터링법으로 제조한 Ti-Al-V-N 박막의 미세조직 및 부착특성에 관한 연구)

  • Sohn, Yong-Un;Lee, Young-Ki
    • Journal of the Korean Society for Heat Treatment
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    • v.12 no.3
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    • pp.199-205
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    • 1999
  • The quaternary Ti-Al-V-N films have been grown on glass substrates by reactive dc and rf magnetron sputter deposition from a Ti-6Al-4V target in mixed Ar-$N_2$ discharges. The Ti-Al-V-N films were investigated by means of X-ray diffraction(XRD), electron probe microanalysis(EPMA) and scratch tester. Both XRD and EPMA results indicated that the Ti-Al-V-N films were of single B1 NaCl phase having columnar structure with the (111) preferred orientation. Scratch tester results showed that the adhesion strength of Ti-Al-V-N films which treated with substrate heating and vacuum annealing was superior to that of as-deposited film. The good adhesion strength was also achieved in the double-layer structure of Ti-Al-V-N/Ti-Al-V/Glass.

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Evaluation of Self-cleaning Property by Measuring Brightness of Tio2 Coating Ceramic Tile under Outdoor Exposure Test (옥외폭로시험 Tio2 코팅 세라믹 타일의 명도측정에 의한 방오특성 평가)

  • Shin, Dae-Yong;Kim, Kyung-Nam
    • Journal of the Korean Ceramic Society
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    • v.45 no.6
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    • pp.345-349
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    • 2008
  • $TiO_2$ coating ceramic tile for self-cleaning purpose was prepared by the precipitant dropping method using $TiCl_4$ as a precursor. $TiO_2$ film was formed on the ceramic tile by spray-coating technique and heat-treated at $500^{\circ}C$ for 1 h. The size and crystalline structure of $TiO_2$ particles were 15.3 nm and anatase phase. The outdoor exposure tests were conducted and the effects of outdoor exposure test conditions, such as exhaust concentration of contamination materials (test places), the UV light intensity (irradiation direction) and coating amounts of $TiO_2$ on the self-cleaning properties were investigated by the brightness measurements. As a results, self-cleaning property of $TiO_2$ coating tile was affected by the coating amount of $TiO_2$ however, not affected by the UV light intensity included in sun's ray (irradiation direction). $TiO_2$ coating ceramic tile can be utilized for exterior finishing materials because of self-cleaning property of $TiO_2$ coating tile.

Wear and corrosion coatings by MO-PACVD and dual plasma processes (MO-PACVD 및 복합 플라즈마 공정에 의한 내마모 내식성 코팅)

  • 김선규
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 1999.10a
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    • pp.3-4
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    • 1999
  • 최근 산업이 고속도화, 고능률화 및 고정멸화의 추세로 발전함에 따라 우수한 내마모성, 인성, 고온 안정성 및 내구성을 갖는 공구 및 금형을 요구하게 되었다. 그러나 이와같은 성질들은 어떤 단일 재료에서는 얻을 수 없으며 적당한 기판공구나 금혈위에 내마모성 보호피막을 coating함으로 비교적 저렴하게 얻을 수 있다. 화학증착법으로 TiC, TiN등을 증착시킬때에는 $1000^{\circ}C$정도의 반응온도가 필요하며 이러한 증착온도는 모재가 초경합금일때는 문제가 안되나 강재일 경우 모재의 연화와 칫수변화의 문제를 야기시킨다. 최근에는 플라즈마를 사용하여 증착반응온도를 $550^{\circ}C$ 이하로 낮추는 플라즈마 화학 증착볍(PACVD)이 대두되고 있다. 그러나 이 방법어서 는 뚱착하려는 금속원소가 TiCl4의 형태로 공급되고 있으므로 생성된 층이 염소를 포함하고 있다. 이 층에 잔존하는 염소는 층의 기계적 성질을 저하시키고 층내의 stress를 유발시킨다. 또한 HCI개스의 생성으로 인하여 펌프 및 장비의 부식이 촉진 된다 이러한 결점을 극복하기 위하여 금속유기화합물 전구체(metallo-organic precursor)로 $TiCl_4$를 대체하고자 하는 연구가 활발하게 진행되고 있으며 본 연구실에서 이에 대하여 연구한 결과를 소개하고자 한다. diethylamino titanium을 전구체로 사용하여 $H_2,\;N_2,\;Ar$분위기하에서 pulsed d.c.를 사용하는 MO-PACVD에 의하여 $150~250^{\circ}C$의 저온에서 Al 2024 기판에 TiCN층 형 성을 하였다. 전구체 증발온도는 $74~78^{\circ}C$의 온도범위어야 하며 고경도의 코탱층은 54% duty, 14.2kHz, 450V의 조건에서 얻어졌으며 duty, 주파수, 전압이 증가함에 따라 경도는 저하되었다. 이때의 표면 morphology를 SEM으로 조사한바 dome structure가 크게 발달되었음을 알 수 있었다. 본 실험의 온도 범위내에서 얻은 TiCN 증착반응의 활성화에너지는 7.5Kcal/mol이었다. 증착된 TiCN층은 우수한 내마모섣을 나타내었으며 스크래치테스트 결과 17N의 엄계하중을 나타내었다. 본 연구에서 변화 시킨 duty, 주파수, 전압의 범위에서는 층의 밀착력은 크게 변화하지 않았다. titanium isopropoxide를 전구체로 사용하여 Hz, Nz 분위기하에서 d.c.를 사용하는 MO-PACVD에 의하여 Ti(NCO) 코팅층을 SKDll, SKD61, SKH9 공구강에 형성시키는 공정을 개발하였다. 최적의 Ti(NCO) 코탱층을 얻기 위해 유입전구체 부피%의 양은 향착압력의 5%를 넘지 않아야 되고 수소와 젤소 가스비가 1:1일 때 가장 높은 코팅층의 경도값을 나타내었다. 수소와 질소 가스비가 3:7일 때 TiFeCr(NCO)의 복화합물 코팅층이 형성됨을 알 수 있었고 500t의 증착온도에서 얻은 Ti(NCO) 코팅층이 높은 경도값과 좋은 내식성을 나타내었다. 또한 이와같은 Ti(NCO) 코팅공정과 본 실험실에서 개발한 확산층만 형성시키는 plsma nitriding 공정을 결합하여 복합코탱층을 형성하였는데 이 복합코팅층은 고경도와 우수한 내마모성, 내식성 뿐만 아니라 10)N 이상의 뛰어난 밀착력을 나타내었다. 현재 많이 사용되고 있는 PVD법은 step coverage가 좋지 않은 점과 cost intensive p process라는 단점이 있다. MO-PACVD법은 이러한 문제를 해결할 수 있는 방법으로서 앞으로 지속적인 도전이 요구되는 분야이다.

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Color Removal of Rhodamine B by Photoelectrochemical Process using Powder TiO$_2$ (분말 광촉매를 이용한 광전기화학 공정에서 Rhodamine B의 색 제거)

  • Kim, Dong-Seog;Park, Young-Seek
    • Journal of Korean Society of Environmental Engineers
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    • v.30 no.8
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    • pp.823-830
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    • 2008
  • The feasibility study for the application of the photoelectrocatalytic decolorization of Rhodamine B(RhB) was performed in the slurry photoelectrochemical reactor with powder TiO$_2$. The photoelectrocatalytic process was consisted of powder TiO$_2$, Pt electrode and three 8 W UV-C lamps. The effects of operating conditions, such as current, electrolyte, air flow rate and electrode material were evaluated. The experimental results showed that optimum TiO$_2$ dosage and current in photoelectrocatalytic process were 0.4 g/L and 0.02 A, respectively. It was found that the RhB could be degraded more efficiently by this photoelectrocatalytic process than the sum of the two individual oxidation processes(photocatalytic and electrolytic process). It demonstrated a synergetic effect between the photo- and electrochemical catalysis. Photoelectrocatalytic process was affected to air flow rate and optimum air flow rate was 2 L/min. The electrode material and NaCl effect of decolorization of RhB were not significant within the experiment conditions.

Effect of Surface Treatment on Hydrogen Production of Cadmium Sulfide Particulate Film Electrodes (수소제조용 CdS 입자막 전극의 표면처리 효과)

  • Jang, Jum-Suk;Chang, Hye-Young;So, Won-Wook;Rhee, Young-Woo;Moon, Sang-Jin
    • Journal of Hydrogen and New Energy
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    • v.11 no.3
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    • pp.119-125
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    • 2000
  • To improve the photochemical energy conversion efficiency and the stability of CdS particulate film electrode which is used to produce hydrogen from the aqueous $H_2S$ solution photoelectrochemically, surface treatment of this film was carried out using $TiCl_4$ solution. CdS particles for preparation of the films were synthesized by precipitation reaction of $Cd({NO_3})_2{\cdot}9H_2O$ and $Na_2S{\cdot}4H_2O$. Then, the CdS sol was hydrothermally treated for 12hr in an autoclave with the variation of treatment temperature to control the crystalline phase of particles. CdS film electrode was thus prepared by annealing at $400^{\circ}C$ for 12hr of the wet-film cast at room temperature, and subsequently surface treated with $TiCl_4$ solution. The electrodes were characterized using XRD, SEM, and the photocurrent meter. The photocurrents of Cds film electrodes prepared with surface treatment were up to two times higher than the electrodes without surface treatment, indicating about $4.0mA/cm^2$. Hydrogen production rate in a continuous flow system using photoelectrochemical or photochemical cells prepared with surface treatment also increased in proportion to the increase of photocurrents.

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Generation of Free Chlorine Using $RuO_2$/ Ti Electrode with Various Amount of Ru (Ru 코팅량에 따른 $RuO_2$/Ti 전극의 염소 발생)

  • Lee, JunCheol;Pak, DaeWon
    • Journal of Korean Society of Environmental Engineers
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    • v.34 no.11
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    • pp.715-719
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    • 2012
  • We investigated the effects of electrochemical characteristics and generation of chlorine by the different amount of Ru coating which was prepared for $RuO_2$/Ti electrode coated with 1.5 mg, 2.5 mg, 5.5 mg, 8.5 mg Ru per unit area ($cm^2$). As a Result of the cycle voltammetry experiments, chlorine overvoltage of Ru-coated electrodes showed to be the nearly sustained value of approximately 1.15V (vs. Ag/AgCl). By contrary, According to the results of the AC impedance spectroscopy and potentiodynamic polarization tests, the amount of Ru per unit area ($cm^2$) included 2.5 mg, 3.5 mg as $RuO_2$/Ti offered the highest levels of durability which was electrode resistance and corrosion rate appeared to be $0.4582{\Omega}$, $0.5267{\Omega}$ and 0.082 mm/yr, 0.058 mm/yr, respectively. It was also observed that generation of chlorine coated with 3.5 mg per unit area ($cm^2$) was the highest value of 15.2 mg/L.

AN ESR STUDY OF AMINO ACID AND PROTEIN FREE RADICALS IN SOLUTION PART I. Reaction Mechanism of Free Radical Production in the Ti-$H_2O_2$ Flow System (용액에서의 아미노산 및 단백질 자유기에 관한 ESR 연구 제1보 ; Ti-$H_2O_2$ Flow System에서 자유기를 만드는 반응기구)

  • Hong Sun-Joo;L. H. Piette
    • Journal of the Korean Chemical Society
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    • v.15 no.1
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    • pp.37-44
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    • 1971
  • The reaction of amino acids and the reactive hydroxyl radical generated by $Ti^{3+}-H_2O_2$ system was studied using fast flow techniques coupled with ESR. Upon adding methionine to the 0.2M $H_2O_2$ solution (0.05M methionine after addition) and mixing with 0.01M $TiCl_3$, the low field component of the two incompletely resolved peaks, in the spectrum of $Ti^{3+}-H_2O_2$ system alone, vanished completely whereas the high field component remained almost constant and superimposed on the secondary spectrum of the methionine free radical. Similar results were obtained for other amino acids and proteins. The results strongly demonstrate that the $T^{3+}-H_2O_2$ flow system generates two different radical species, only one of which, giving rise to the low field component, is alone responsible for abstracting hydrogen atoms from substrate molecules. The effects of HCl, $H_2SO_4$ and NaOH on the system were also studied with widely varying results.

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Photodegradation of Halogen Derivatives of Aliphatic Hydrocarbon in Aqueous Photocatalytic Suspensions (지방족 탄화수소의 할로겐 유도체 수용액의 광촉매-광분해)

  • Jun, Jin;Jung, Hak-Jin;Kim, Hae-Jin;Kim, Sam-Hyeok
    • Journal of Environmental Science International
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    • v.6 no.1
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    • pp.75-88
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    • 1997
  • The rates of photodegradation, reactivities, and mechanisms of photooxidation for the aqueous solution containing with halogen derivatives of aliphatic hydrocarbons have been discussed with respect to the kinds of photocatalysts, concentration of photocatalytlc suspensions, strength of radiant power, time of illumination, changes of pH of substrate solution, wavelength of radiation, and pressure of oxygen gas saturated In the solution. These aqueous solutions suspended with 0.5 $gL^{-1}$ $TiO_2$ powder have been photodecomposed in the range of 100 and 93.8% per 1 hour if it is illuminated with wavelength (λ $\geq$ 300nm) produced from Xe-lamp(450W). The photocatalytic abilities have been increased In the order of $Fe_2O_3$ < CdS < $CeO_2$ < Y_2O_3$ <$TiO_2$, and rates of photodegradation for the solution have maldmum values in the condition of pH 6 ~ 8 and 3 psi-$O_2$ gL^{-1}$. These rates for the Photoolddation Per 1 hour were dependent on the size of molecular weight and chemical bonding for organic halogen compounds and the rates of photodegadation were increased in the order of $C_2H_5Br$ < CH_2Br_2$ < C_5H_11Cl C_2H_4Cl_2$ < tracts-$C_2H_2Cl_2$ < cis-C_2H_2Cl_2$ The T_{1/2}$ and t99% for these solutions were 5~21 and 40~90 minutes. respectively, and these values were coincided with Initial reaction kinetics(ro). It was found that reaction of photodegradation has the pseudo first-order kinetics controlled by the amount of $h^+_{VB}$ diffused from a surface of photocatalysts.

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