• 열처리공학회지
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• 제17권2호
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• pp.87-93
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• 2004

Nitrocarburizing was carried out with various $CH_4$ gas composition with 4 torr gas pressure at $570^{\circ}C$ for 3 hours and post oxidation was carried out with 100% $O_2$ gas atmosphere with 4 torr at different temperatures for various time. In the case of plasma nitrocarburizing, It is that the ratio of ${\varepsilon}-Fe_{2-3}$(N, C) and ${\gamma}^{\prime}-Fe_4$(C, N), which comprise the compound layer phase, depend on concentrations of $N_2$ gas and $CH_4$ such that when the concentration of $N_2$ and $CH_4$ increased, the ratio of ${\gamma}^{\prime}-Fe_4$(C, N) decreased, but the ratio of ${\varepsilon}-Fe_{2-3}$(N, C) increased. The thickness of compound layer consistently increased as gas concentration increased regardless of $N_2$ and $CH_4$ expect when the concentration of $CH_4$ was 3.5 volume%, it decreased insignificantly. When oxidizing for 15min in the temperature range of $460{\sim}570{^\circ}C$, the study found small amount of $Fe_3O_4$ at the temperature of $460{^\circ}C$ and also found that amounts of $Fe_2O_3$. and $Fe_3O_4$ on the surface and amount of ${\gamma}^{\prime}-Fe_4$(C, N) in the compound layer increased as the increased over $460^{\circ}C$, but the thickness of the compound layer decreased. Corrosion resistance was influenced by oxidation times and temperature.

• 한국표면공학회지
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• 제32권3호
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• pp.312-316
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• 1999

The interfacial structure of duplex treated AISI 4140 consisting of iron nitride and TiN layer was characterized by optical microscope, SEM and XRD. A black layer was formed from the decomposition of iron nitride during Ti ion bombardment. The black layer was characterized as an a-Fe phase transformed from the iron nitride by XRD. In order to identify the formation mechanism of the black layer, a thermal analysis of iron nitride undertaken by DSC method. As an iron nitride was mostly consisted of ${\gamma}$'-Fe$_4$N and $\varepsilon$-$Fe_3$N phase after plasma nitriding, in this study, a ${\gamma}$'$-Fe_4$N and $\varepsilon$-$Fe_3$N powders were separately prepared by the different processing conditions of gas nitriding of iron powder in the fluidized bed. From the DSC thermal analysis, the phase transformation of ${\gamma}$'$-Fe_4$N, $\varepsilon$-$Fe_3$N was followed the path of transformation; $ \Upsilon{'}-Fe_4$Nlongrightarrow${\gamma}$-Felongrightarrowa-Fe and of $\varepsilon$-$Fe_3$Nlongrightarrow$\varepsilon$-$Fe_{2.5}$ /N+${\gamma}$'$-Fe_4$Nlongrightarrow${\gamma}$'-Fe$_4$Nlongrightarrow${\gamma}$longrightarrowFelongrightarrowalongrightarrowFe, respectively. It explains the reason why the $\varepsilon$ $-Fe_3$N phase disappeared in the first time and then ${\gamma}$'-Fe$_4$N in the formation of the black layer in the duplex coating.

• 한국표면공학회지
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• 제31권3호
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• pp.142-150
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• 1998

Stainless steel is being used widely for various purposes due to its good corrosion resistance. There has been much research to produce colored stainless steel by several methods such as anodizing and ion plating. In this experiment, we coated TiN(C,O,H)films SUS304 substraate with the DC magnetron spttering system made by Leybold Heraeus and studied the interlater structure and abhesive strength of the films as a function of additional gases, acetylene, hydrogen and oxygen. When the acetylene gas was added into the chamber, the specimen with the interlayer phase had good adhesion due to the toughness of the $\gamma'-Fe_4N$ plase induced from a solid solution of carbon atoms, while low adhesion appeared on the specimen of the non interlayer phase. The formation of the interlayer phase($\gamma'-Fe_4N$) was due to hydrogen embrittlement and internal stress induced by $\gamma'-Fe_4N$ formation in the interlayer. We could fine the interlayer phase ($\gamma'-Fe_4N$) at the interface between the film and the substrate of the TEM image when $\gamma'-Fe_4N$ was detected by the X-ray duffraction metheod.

• 열처리공학회지
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• 제12권1호
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• pp.9-20
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• 1999

The effect of post oxidation, water-quenched after holding in air for 5~420 seconds or cooling or furnace cooling, on corrosion resistance and phase formation characteristics of the surface layer of SM20C and SM45C carbon steels after gas nirtrocarbursing in the $NH_3-5%CO_2-N_2$ gas atmosphere at $580^{\circ}C$ for 3hours is studied. The compound layers of two steels consist of ${\varepsilon}-Fe_{2-3}N$, ${\gamma}^{\prime}-Fe_4N$ and $Fe_3O_4$, phases, however, the quantity of ${\gamma}^{\prime}-Fe_4N$ phase increases for the furnace cooled specimen compared to that of air cooling specimen. With increasing $NH_3$ content in the gas mixture and also increasing the keeping time in the air after gas nitrocarburising, the ${\varepsilon}-Fe_{2-3}N$ phase of compound layer increases, while the decreased current density recognizing the improvement of corrosion resistance are shown. the passive current density of SM45C steel is lower than that of SM20C steel at the same nitrocarburising conditions.

• 한국표면공학회지
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• 제40권6호
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• pp.250-253
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• 2007

Plasma nitrocarburizing and plasma oxidizing treatments were performed to improve the wear and corrosion resistance of SKD 11 steel. Plasma nitrocarburizing was conducted for 12 h at $520^{\circ}C$ in the nitrogen, hydrogen and methane atmosphere to produce the $\varepsilon-Fe_{2-3}(N,C)$ phase. It was found that the compound layer produced by plasma nitrocarburising was predominantly composed of $\varepsilon-phase$, with a small proportion of $\gamma'-Fe_4(N,C)$ phase. The thickness of the compound layer was about $5{\mu}m$ and the diffusion layer was about $150{\mu}m$ in thickness, respectively. Plasma post oxidation was performed on the nitrocarburized samples with various oxygen/hydrogen ratio at constant temperature of $500^{\circ}C$ for 1 hour. The very thin magnetite($Fe_3O_4$) layer $1-2{\mu}m$ in thickness on top of the compound layer was obtained by plasma post oxidation. It was confirmed that the corrosion characteristics of the nitrocarburized compound layer could be further improved by the application of the superficial magnetite layer.

• 한국세라믹학회지
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• 제29권12호
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• pp.942-948
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• 1992

Ultrafine iron oxide powder, {{{{ gamma }}-Fe2O3 and $\alpha$-Fe2O3, were prepared by the thermal decomposition of organometallic compounds. The formation process of powder includes the thermal decomposition and oxidation of the organometallic precursors, Fe(N2H3COO)2(N2H4)2 (A) and N2H5Fe(N2H3COO)3.H2O (B). The organometallic precursors, A and B, were synthesized by the reaction of ferrous ion with hydrazinocarboxylic acid, and characterized by quantitative analysis and infrared spectroscopy. The mechanistic study for the thermal decomposition was performed by DAT-TG. The iron oxide powder was obtained by the heat treatment of the precursors at 20$0^{\circ}C$ and $600^{\circ}C$ for half an hour in air. The phases of the resulting product were proved {{{{ gamma }}-Fe2O3 and $\alpha$-Fe2O3 respectively. The particle shape was equiaxial and the particle size was less than 0.1 ${\mu}{\textrm}{m}$. Magnetic properties of the {{{{ gamma }}-Fe2O3 powder obtained from A and B was 234 Oe of coercivity, 64.26 emu/g of saturation magnetization, 23.59 emu/g of remanent magnetization and 24.1 Oe, 47.27 emu/g, 3.118 emu/g respectively. The value of $\alpha$-Fe2O3 powder was 1.494 Oe, 0.4862 emu/g, 0.1832 emu/g and 1,276 Oe, 0.4854 emu/g, 0.1856 emu/g respectively.

• 열처리공학회지
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• 제8권4호
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• pp.289-301
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• 1995

The effect of Air/$C_3H_8$ gas addition on the compound layer growth of steels nitrocarburised in $NH_3+Air+C_3H_8$ mixed gas atmospheres was investigated. It is considered that amount of residual $NH_3$ was varied according to alternation of Air/$C_3H_8$ mixing ratio and volume content. The compound layer formed from nitrocarburising was composed of ${\varepsilon}-Fe_{2-3}$(C, N) and ${\gamma}^{\prime}-Fe_4$(C, N). According as Air/$C_3H_8$ mixing ratio increased, the superficial content of ${\gamma}^{\prime}-Fe_4$(C, N) within the compound layer was increased, at the same time the growth rate of compound layer and porous layer was increased. In the case of alloy steel at the fixed gas composition, the growth rate of compound layer and porous layer was worse than carbon steel and compound layer phase composition structure primarily consisted of E phase. As the carbon content of materials was increasing in the given gas atmospheres, the growth rate of compound layer and porous layer was increased and the superficial content of ${\varepsilon}-Fe_{2-3}$(C, N) within the compound layer was increased.

• 열처리공학회지
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• 제7권3호
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• pp.206-218
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• 1994

In 50%$NH_3+Air+N_2$ atmospheres, the effect of air additions on the growth characteristics of the compound layer during oxynitriding at $570^{\circ}C$ for 2hr in carbon and alloy steels has been investigated. The ammount of apparent residual ammonia during oxynitriding has shown to be increased with air additions(9~36 Vol. %) and X-ray diffraction analysis of case oxynitreded has shown that the compound layer consist of ${\varepsilon}-Fe_{2-3}$(N, C) phase and ${\gamma}^{\prime}-Fe_4$(N,C) phase. In the case of carbon steels, the thickness of oxide layer, compound layer and porous layer and the amount of ${\varepsilon}-Fe_{2-3}$(N,C) phase in the compound layer were increased with additions of air in 50%$NH_3+N_2$ atmospheres. At the same gas composition, the thickenss of oxide layer, compound layer and porous layer in alloy steels showed slightly thin layer thickness compared to those of carbon steels and the ${\gamma}^{\prime}-Fe_4$(N,C) phase in the compound layer of alloy steels was found barely. Therefore, the most obvious effect of air addition in the gas nitriding atmosphere has been found to in crease further kinetics of nitriding reaction.

• 열처리공학회지
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• 제12권2호
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• pp.117-128
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• 1999

This study was carried out to investigate the surface characteristics of SCM440 steel nitrided with various nitrogen contents for 7 hours at $520^{\circ}C$ by using micro-pulse plasma nitriding apparatus of hot wall type. The effects of oxidation treatment was also investigated on plasma nitrided in 30% nitrogen and post oxidized SCM440 steel at $500^{\circ}C$ in $H_2O$ atmosphere. The ${\gamma}^{\prime}-Fe_4N$ and ${\varepsilon}-Fe_{2-3}N$ phases were detected in compound layer of the nitrided steel. As the content of nitrogen in plasma gas increased with 30, 50, 70% on the micro-pulse plasma nitriding for SCM440 steel, the thickness of compound, diffusion layer and the surface hardness were increased. From the wear test results, the best wear resistance was appeared in the condition of ductile ${\gamma}^{\prime}-Fe_4N$ phase formed specimen at 30% nitrogen, whereas that of the treated with 50% and 70% nitrogen decreased owing to the exfoliation of brittle ${\varepsilon}-Fe_{2-3}N$ phase in the compound layer. On the nitrided and subsequently oxidized SCM440 steel, the surface layer consisted of $Fe_3O_4$, ${\gamma}^{\prime}-Fe_4N$, and ${\varepsilon}-Fe_{2-3}N$ phases. In these treatments, the dissolution of nitrides affect hardness and hardening depth in compound and diffusion layers. For the nitrided in 30% nitrogen and post oxidized specimen at $500^{\circ}C$ for 1 hour, the wear resistance was lower than that of the only nitrided one in 30% nitrogen but higher than those of the nitrided ones in 50 and 70% nitrogen.

• 열처리공학회지
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• 제15권5호
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• pp.219-227
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• 2002

This study has been performed to investigate the effect of $CO_2$ content on the growth characteristics of the compound layer, porous layer and corrosion characteristics of carbon steels after gaseous nitrocarburizing in $70%-NH_3-CO_2-N_2$ at $580^{\circ}C$ for 2.5 hrs. The results obtained from the experiment were the thickness of the compound and porous layers increased with increasing $CO_2$ contents. At the same fixed gas composition the thickness of the compound and porous layer increased with increasing carbon content of the specimens. X-ray diffraction analysis showed that compound layer was mainly consisted of ${\varepsilon}-Fe_{2-3}(N,C)$ and ${\gamma}^{\prime}-Fe_4N$ as the increased with $CO_2$ contents in atmosphere, compound layer was chiefly consisted of ${\varepsilon}-Fe_{2-3}(N,C)$ phase. With increasing $CO_2$ content and total flow rate in gaseous nitrocarburizing, the amount of ${\varepsilon}-Fe_{2-3}(N,C)$ phase in the compound layer was increased. The current density of passivity decreased with increasing $CO_2$ content due to the development of porous layer at the out most surface of ${\varepsilon}-Fe_{2-3}(N,C)$.