• Journal of the Korean institute of surface engineering
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• v.47 no.2
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• pp.86-92
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• 2014

The purpose of this comparative study was to investigate the properties of chromium nitride coatings deposited by asymmetric bipolar pulsed DC sputtering and DC sputtering system. Oscilloscope traces of the I-V waveforms indicate high power and high current density outputs during the asymmetric bipolar pulsed mode. The grain size decreases with decreasing duty cycle. The duty cycle has a strong influence not only on the microstructural properties but also on the mechanical properties of chromium nitride coatings. Comparing with the continuous DC sputtering, the chromium nitride coatings prepared by pulsed DC asymmetric bipolar process also exhibit better surface roughness.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 2000.07a
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• pp.573-576
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• 2000

The physical, electrical and piezoresitive characteristics of CrN(chromium nitride) thin-films on silicon substrates have been investigated for use as strain gauges. The thin-film depositions have been carried out by DC reactive magnetron sputtering in an argon-nitrogen atmosphere(Ar-(5∼25 %)Na$_2$). The deposited CrN thin-films with thickness of 3577${\AA}$ and annealing conditions(300$^{\circ}C$, 48 hr) in Ar-10 % N$_2$deposition atmosphere have been selected as the ideal piezoresistive material for the strain gauges. Under optimum conditions, the CrN thin-films for the strain gauges is obtained a high electrical resistivity, $\rho$=1147.65 ${\mu}$$\Omega$cm, a low temperature coefficient of resistance, TCR=-186 ppm/$^{\circ}C$ and a high temporal stability with a good longitudinal gauge factor, GF=11.17.

• Journal of the Korean Society for Heat Treatment
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• v.14 no.1
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• pp.8-16
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• 2001

The effects of gas composition, pressure, temperature and time on the case thickness, hardness and nitride formation in the surface of tool steels(STD11 and STD61) have been studied by micro-pulse plasma nitriding. External compound layer and internal diffusion layer and the diffusion layer were observed in the nitrided case of tool steels. The relative amounts and kind of phases formed in the nitrided case changed with the change of nitriding conditions. Generally, only nitride phases such as ${\gamma}(Fe_4N)$, ${\varepsilon}(Fe_{2-3}N)$, or $Cr_{1.75}V_{0.25}N_2$ phases were detected in the compound layer, while nitride and carbide phases such as ${\varepsilon}-nitride(Fe_{2-3}N)$, $(Cr,Fe)_{\gamma}C_3$ or $Fe_3C$ were detected in the diffusion layer by XRD analysis. The thickness of compound layer increased with the increase of nitrogen content in the gas composition. Maximum case depth was obtained at gas pressure of 200Pa.

• Korean Journal of Materials Research
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• v.20 no.4
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• pp.187-193
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• 2010

Chromium nitride (CrN) samples with two different layer structures (multilayer and single layer) were coated on bipolar plates of polymer electrolyte membrane fuel cells (PEMFC) using the reactive sputtering method. The effects with respect to layer structure on corrosion resistance and overall cell performance were investigated. A continuous and thin chromium nitride layer ($Cr_{0.48}\;N_{0.52}$) was formed on the surface of the SUS 316L when the nitrogen flow rate was 10 sccm. The electrochemical stability of the coated layers was examined using the potentiodynamic and potentiostatic methods in the simulated corrosive circumstances of the PEMFC under $80^{\circ}C$. Interfacial contact resistance (ICR) between the CrN coated sample and the gas diffusion layer was measured by using Wang's method. A single cell performance test was also conducted. The test results showed that CrN coated SUS316L with multilayer structure had excellent corrosion resistance compared to single layer structures and single cell performance results with $25\;cm^2$ in effective area also showed the same tendency. The difference of the electrochemical properties between the single and multilayer samples was attributed to the Cr interlayer layer, which improved the corrosion resistance. Because the coating layer was damaged by pinholes, the Cr layer prevented the penetration of corrosive media into the substrate. Therefore, the CrN with a multilayer structure is an effective coating method to increase the corrosion resistance and to decrease the ICR for metallic bipolar plates in PEMFC.

• Applied Chemistry for Engineering
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• v.17 no.5
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• pp.451-457
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• 2006

We synthesized phase pure CrN having surface areas up to $47m^2/g$ starting from $CrCl_{3}$ with $NH_{3}$. Thermal Gravimetric Analysis coupled with X-ray diffraction was carried out to identify solid state transition temperatures and the phase after each transition. In addition, the BET surface areas, pore size distributions, and crystalline diameters for the synthesized materials were analyzed. Space velocity influenced a little to the surface areas of the prepared materials, while heating rate did not. We believe it is due to the fast removal of reaction by-products from the system. Temperature programmed reduction results revealed that the CrN was hardly passivated by 1% $O_{2}$. Molecular nitrogen was detected from CrN at 700 and $950^{\circ}C$, which may be from lattice nitrogen. In temperature programmed oxidation with heating rate of 10 K/min in flowing air, oxidation started at or higher than $300^{\circ}C$ and resulting $Cr_{2}O_{3}$ phase was observed with XRD at around $800^{\circ}C$. However the oxidation was not completed even at $900^{\circ}C$. CrN catalysts were highly active for n-butane dehydrogenation reaction. Their activity is even higher than that of a commercial $Pt-Sn/Al_{2}O_{3}$ dehydrogenation catalyst in terms of volumetric reaction rate. However, CrN was not active in pyridine hydrodenitrogenation.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2009.05a
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• pp.177-181
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• 2009

Compositional gradient CrNx coatings were fabricated using arc ion plating in Ar/$N_2$ gaseous mixture by gradually increasing $N_2$ flux rate from 0 to 120 SCCM. The effect of negative substrate bias on the film microstructure and mechanical properties were systematically investigated with XRD, GDOES, and SEM. The results show that substrate bias has an important influence on film growth and microstructure of gradient CrNx coatings. The coatings mainly crystallized in the mixture of hexagonal $Cr_{2}N$ and fcc CrN phases. By increasing substrate bias, film microstructure evolved from an apparent columnar structure to an equiaxed one. With increasing substrate bias, deposition rate first increased, and then decreased. The maximum of deposition rate was 15 nm/min obtained at a bias of -50V.

• Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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• 1999.05a
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• pp.692-695
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• 1999

This paper presents annealing characteristics of CrN thin-film strain gauges, which were deposited on glass by DC reactive magnetron sputtering in an argon-nitrogen atmosphere)Ar-(5-~25%)$N_2$. The physical and electrical characteristics of these films investigated with the thickness range 3500$\AA$ of CrN thin films, annealing temperature (100~30$0^{\circ}C$) and annealing time (24-72hr) . The optimized condition of CrN thin-film strain gauges were thickness range of 3500$\AA$ and annealing condition(30$0^{\circ}C$ , 48hr) in Ar-10%$N_2$ deposition atmosphere. Under optimum conditions, the CrN thin-films for strain gauge is obtained a high resistivity, $\rho$=1147.65$\Omega$cm a low temperature coefficient of 11.17. And change in resistance after annealing for the CrN thin film were quitely linear and stable.

• Journal of the Korean Ceramic Society
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• v.45 no.3
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• pp.161-166
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• 2008

The multi-films of a metallic film and a transparent conducting oxide (TCO, indium-tin oxide, ITO) film were formed on the stainless steel 316 and 304 plates by a sputtering method and an E-beam method and then the external metallic region of the stainless steel bipolar plates was converted into the metal nitride films through an annealing process. The multi-film formed on the stainless steel bipolar plates showed the XRD patterns of the typical indium-tin oxide, the metallic phase and the metal substrate and the external nitride film. The XRD pattern of the thin film on the bipolar plates modified showed two metal nitride phases of CrN and $Cr_2N$ compound. Surface microstructural morphology of the multi-film deposited bipolar plates was observed by AFM and FE-SEM. The metal nitride film formed on the stainless steel bipolar plates represented a microstructural morphology of fine columnar grains with 10 nm diameter and 60nm length in FE-SEM images. The electrical resistivity of the stainless steel bipolar plates modified was evaluated.

• Proceedings of the Korean Society for Technology of Plasticity Conference
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• 2006.05a
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• pp.421-424
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• 2006

High nitrogen steels (HNS) exhibit both high strength and ductility during tensile deformation. In the present study the Fe-18Cr-14Mn-4Ni-0.9N high nitrogen steel was heat treated at $1000^{\circ}C$ and $1100^{\circ}C$ to produce $Cr_2N$ precipitates in austenite matrix and full austenite microstructures, respectively. Tensile tests of the heat treated specimens were performed at two different strain rates of 0.05/sec and 0.00005/sec. Each tensile curve of the specimens could be well characterized by the the modified Ludwik equation. Plastic deformation of the steel was adequately represented by the four parameters of the modified Ludwik equation. At 0.05/s strain rate, the specimen with the $Cr_2N$ precipitate exhibited higher strength than the full austenite specimen, while the full austenite specimen showed better mechanical properties at 0.00005/s strain rate. It was found that the $Cr_2N$ precipitates influences deformation behavior of the high nitrogen steel significantly.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2001.11a
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• pp.29-30
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• 2001

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).