• Journal of the Korean Society for Heat Treatment
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• v.19 no.1
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• pp.3-9
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• 2006

The phase changes, nitride precipitation and hardness variations of 14%Cr-6.7Ni-0.65Mo-0.26Nb-0.05V-0.03C super martensitic stainless steel were investigated after nitrogen permeation heat treatment at a temperature range between $1050^{\circ}C$ and $1150^{\circ}C$. The nitrogen-permeated surface layer was transformed into austenite. The rectangular type NbN, NbCrN precipitates and fine round type precipitate were coexisted in the surface austenite layer, while the interior region that was free from nitrogen permeation kept the martensitic phase. The hardness of surface austenite showed 280 Hv, while the interior region of martensite phase represented 340 Hv. When tempering the nitrogen-permeated steel at $450^{\circ}C$, a maximum hardness of 433 Hv was appeared, probably this is attributed to the secondary hardening effect of the precipitates. The nitrogen concentration decreased gradually with increasing depth below the surface after showing a maximum of 0.3% at the outmost surface. The strong affinity between nitrogen and Cr enabled the substitutional element Cr to move from interiors to the surface when nitrogen diffuse form surface to the interior. Corrosion resistance of nitrogen permeated steel was superior to that of solution-anneaed steel in the solution of 1N $H_2SO_4$.

• Journal of the Korean Society for Heat Treatment
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• v.19 no.2
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• pp.83-89
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• 2006

The surface phase changes, the hardness variations, the nitrogen contents and the corrosion resistances of 17-4 PH stainless steel have been investigated after nitrogen permeation(solution nitriding) at a temperature ranges from $1050^{\circ}C$ to $1150^{\circ}C$ The phases appeared at the nitrogen-permeated surface layer were shown to martensite plus austenite and austenite, depending on the variation of nitrogen and chromium contents. And the surface hardness was also depended on the phases appeared at the surface layer from 370 Hv to 220 Hv. The precipitates exhibited at the nitrogen-permeated surface layer were niobium nitride, niobium chromium nitride and carbo-nitride in the austenite and martensite matrices. The surface nitrogen contents were followed by the Cr contents of the surface layers, representing 0.55% at the temperatures of $1050^{\circ}C$ and $1150^{\circ}C$ respectively, and 0.96% at $1100^{\circ}C$ at the distances of $60{\mu}m$ from the outmost surface. From the comparison of the corrosion resistances between nitrogen-permeated and solution-annealed steels, nitrogen permeation remarkably improved the corrosion resistance in the solution of 1 N $H_2SO_4$ due to the increase of nitrogen content in the surface austenite phase.

• Journal of the Korean Society for Heat Treatment
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• v.12 no.3
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• pp.221-230
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• 1999

The surface nitrogen permeation of Al alloyed 0.14%C-13%Cr stainless steels was investigated after heat treating at $1050^{\circ}C{\sim}1150^{\circ}C$ in the nitrogen gas atmosphere. The strong affinity between Al and nitrogen permeates the nitrogen through the interior of the steels. Two precipitates of round type and needle type are observed at the surface layer. These precipitates mainly consist of AlN containing plenty of aluminum. The surface layer of 0.53%Al alloyed specimen shows ferrite phase, while the surface layers of 1.65%Al and 2.27%Al alloyed specimens appear ${\gamma}$ plus ${\alpha}$ phases. The depth of nitrogen permeation depends upon the Al content and microstructure of the matrix. The 1.65%Al alloyed specimen representing ${\alpha}+{\gamma}$ matrix phases at the nitrogen permeation temperature shows the maximum case depth in this experiment. Although the surface hardness increases by raising the Al content of the specimen owing to the increase of nitride precipitation density, the nitride precipitation deteriorates the corrosion resistance in the solution of HCl, $H_2SO_4$, and $FeCl_3$.

• Journal of the Korean Society for Heat Treatment
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• v.13 no.3
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• pp.151-157
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• 2000

This study aims to investigate the effect of carbon content on the surface nitrogen permeation of 13%Cr-1.8%Al alloyed stainless steels. The surface nitrogen permeation was performed at $1050^{\circ}C{\sim}1200^{\circ}C$ in the $1kg/cm^2$ nitrogen gas atmosphere. The nitrogen permeated surface layer of the specimen containing 0.03%C consists of AlN, martensite and retained austenite phases. while the surface layer of the specimen containing 0.14%C appears the $AlFe_3C_x$ phase including former three phases. The specimen containing 0.14%C shows lower total case depth than that containing 0.03%C at the nitrogen permeation temperatures of $1050^{\circ}C$ and $1100^{\circ}C$, while the total case depth of the specimen containing 0.14%C is remarkably increased at the temperature of $1150^{\circ}C$ and $1200^{\circ}C$ due to the increase in the retained austenite content. Martensitic phase, AlN and $AlFe_3C_x$ precipitate of the nitrogen permeated surface layer cause to increase the surface hardness of 550~600Hv.

• Journal of the Korean Society for Heat Treatment
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• v.15 no.2
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• pp.57-64
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• 2002

The 22%Cr-5%Ni-3%Mo duplex and 18%Cr-8%Ni austenitic stainless steels have been nitrogen permeated under the $1Kg/cm^2$ nitrogen gas atmosphere at the temperature range of $1050^{\circ}C{\sim}1150^{\circ}C$. The nitrogen-permeated duplex and austenitic stainless steels showed the gradual decrease in hardness with increasing depth below surface. The duplex stainless steel showed nitrogen pearlite at the outmost surface and austenite single phase in the center after nitrogen permeation treatment, while the obvious microstructural change was not observed for the nitrogen-permeated austenitic stainless steel. After solution annealing the nitrogen-permeated stainless steels(NPSA treatment) at $1200^{\circ}C$ for 10 hours, the hardness of the duplex and austenitic stainless steels was constant through the 2 mm thickness of the specimen, and the ${\alpha}+{\gamma}$ phase of duplex stainless steel changed to austenite single phase. Tensile strengths and elongations of the NPSA-treated duplex stainless steel remarkably increased compared to those of solution annealed (SA) duplex stainless steel due to the solution strengthening effect of nitrogen and the phase change from a mixture of ferrite and austenite to austenite single phase, while the NP-treated austenitic stainless steel displayed the lowest value in elongation due to inhomogeneous deformation by the hardness difference between surface and interior.

• Journal of the Korean Society for Heat Treatment
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• v.26 no.3
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• pp.105-112
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• 2013

The microstructural changes of Fe-20Mn-12Cr-1Cu alloy have been studied during high temperature gas nitriding (HTGN) at the range of $1000^{\circ}C{\sim}1150^{\circ}C$ in an atmosphere of nitrogen gas. The mixed microstructure of austenite and ${\varepsilon}$-martensite of as-received alloy was changed to austenite single phase after HTGN treatment at the nitrogen-permeated surface layer, however the interior region that was not affected nitrogen permeation remained the structure of austenite and ${\varepsilon}$-martensite. With raising the HTGN treatment temperature, the concentration and permeation depth of nitrogen, which is known as the austenite stabilizing element, were increased. Accordingly, the depth of austenite single phase region was increased. The outmost surface of HTGN treated alloy at $1000^{\circ}C$ appeared Cr nitride. And this was in good agreement with the thermodynamically calculated phase diagram. The grain growth was delayed after HTGN treatment temperature ranges of $1000^{\circ}C{\sim}1100^{\circ}C$ due to the grain boundary precipitates. For the HTGN treatment temperature of $1150^{\circ}C$, the fine grain region was shown at the near surface due to the grain boundary precipitates, however, owing to the depletion of grain boundary precipitates, coarse grain was appeared at the depth far from the surface. This depletion may come from the strong affinity between nitrogen and substitutional element of Al and Ti leading the diffusion of these elements from interior to surface. Because of the nitrogen dissolution at the nitrogen-permeated surface layer by HTGN treatment, the surface hardness was increased above 150 Hv compared to the interior region that was consisted with the mixed microstructure of austenite and ${\varepsilon}$-martensite.

• Journal of the Korean Society for Heat Treatment
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• v.25 no.3
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• pp.115-120
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• 2012

It has been known that the ferritic stainless steel can be changed to martensitic stainless steel when nitrogen is added. However the high hardness of martensitic stainless steel prevents the plastic deformation. In this study, instead of martensite, the surface microstructure was changed into nitrogen pearlite to increase the plastic deformation easily by isothermal heat treatment after high temperature gas nitriding (HTGN) the AISI 430 ferritic stainless steel. The isothermal treatment was carried out at $780^{\circ}C$ for 4, 6, and 10 hrs, respectively, after HTGN treatment at $1100^{\circ}C$ for 10 hrs. The surface layer of isothermal-treated steel appeared nitrogen pearlite composed with fine chromium nitride and ferrite. Hence, the interior region that was not affected by nitrogen permeation exhibited ferrite phase. When quenching the isothermal treated steel at 1100oC, martensitic phase formed at the surface layer. The hardness of surface layer of isothermal-treated steel and quenched steel measured the value of 150~240 Hv and 630 Hv, respectively.

• Journal of the Korean Society for Heat Treatment
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• v.20 no.2
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• pp.84-93
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• 2007

Microstructural changes during tempering at the temperature range of $300^{\circ}C{\sim}700^{\circ}C$ for the nitrogen-permeated STS 410 and 410L martensitic stainless steels has been investigated. After nitrogen permeation at temperature between 1050 and $1150^{\circ}C$, the surface layer appeared fine $Cr_2N$ of square and rod types in the martensite matrices. Hardness of the nitrogen-permeated surface layer represented 680Hv and 625Hv, respectively, for 410 and 410L steels. It is considered that the fine homogeneously dispersive effect of precipitates by nitrogen caused the increased hardness. Due to the counter current effect of carbon from interior to surface during nitrogen diffusion from surface to interior, the 0.1%C alloyed 410 steel showed the low nitrogen content of 0.025% compared with 0.045% of 410L steel at the distance of $100{\mu}m$ from the surface. Tempering of nitrogen-alloyed 410 and 410L showed the maximum hardness at $450^{\circ}C$. This maximum hardness was considered to be the secondary hardening effect of very fine carbide and nitride. The decrease in hardness at $700^{\circ}C$ was the softening effect of the matrix due to the precipitation of many needle-shaped $Cr_2N$ for 410 steel and the precipitation of coarse nitride of $Cr_2N$ in line with the spherical precipitates with directionality for 410L steel. For 410 steel, the corrosion resistance of nitrogen permeated surface in the solution of 1 N $H_2SO_4$ were nearly unchanged, however the superior corrosion resistance was obtained for nitrogen permeated 410L steel compared to the solution annealed condition.

• Journal of Surface Science and Engineering
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• v.37 no.5
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• pp.243-248
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• 2004

A palladium-nikel(Pd-Ni) alloy composite membrane has been fabricated on microporous nickel support formed with nickel powder. Plasma surface treatment process is introduced as pre-treatment process instead of HCI activation. Pd coating layer was prepared by dc magnetron sputtering deposition after $H_2$ plasma surface treatment. Palladium-nickel alloy composite layer had a fairly uniform and dense surface morphology. The membrane was characterized by permeation experiments with hydrogen and nitrogen gases at temperature of 773 K and pressure of 2.2psi. The hydrogen permeance was 6 ml/minㆍ$\textrm{cm}^2$ㆍatm and the selectivity was 120 for hydrogen/nitrogen($H_2$/$N_2$) mixing gases at 773 K.

• Journal of Surface Science and Engineering
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• v.37 no.5
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• pp.289-295
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• 2004

A dense palladium-nikel (Pd-Ni) alloy composite membrane has been fabricated on microporous nickel support mixed with submicron/micron nickel powder instead of mesoporous stainless steel support. Plasma treatment process is introduced as pre-treatment process instead of HCI activation. Pd-Ni alloy composite membrane prepared by electro plating was fairly a uniform and dense surface morphology. The membrane was characterized by permeation experiments with hydrogen and nitrogen gases at temperature 773 K and pressure 2.2 psi. The results showed that hydrogen ($H_2$) permeance was 27 ml/$\textrm{cm}^2$ㆍatmㆍmin and hydrogen/ nitrogen ($_H2$$N_2$) selectivity was 8 at 773 K.