• Journal of the Korean Chemical Society
• /
• v.38 no.2
• /
• pp.92-100
• /
• 1994

Ultrafine cobalt-substituted iron oxide particles were prepared by the thermal decomposition and oxidation of the new organometallic precursor, $Co_xFe_{1-x}(N_2H_3COO)_2(N_2H_4)_2$ (x = 0, 0.01, 0.02, 0.03, 0.05, 0.10, 1.00). The organometallic precursors were synthesized by the reaction of Co(II) and Fe(II) ion in a mole ratio of x : 1-x with hydrazinocarboxylic acid, and characterized by quantitative analysis, elemental analysis and infrared spectroscopy. The mechanistic study on the thermal decomposition of the organometallic precursors was performed by TG-DTG and DSC. The cobalt-substituted iron oxide particles were obtained by the heat treatment of the precursors at $350^{\circ}C$ and $450^{\circ}C$ for six hours in air. The prepared iron oxide was found to have two phases such as ${\gamma}-Fe_2O_3$ and a mixture of ${\gamma}-Fe_2O_3\;and\;{\alpha}-Fe_2O_3$ at $350^{\circ}C$ and $450^{\circ}C$ respectively. The particle shape was equiaxial and the particle size was less than 0.05 ${\mu}m.$ The coercivity and squareness of the cobalt substituted iron oxide particles increased with increasing cobalt content. Both coercivity and squareness showed higher values at $450^{\circ}C.$

• Journal of the Korean Society for Heat Treatment
• /
• v.8 no.4
• /
• pp.279-288
• /
• 1995

To investigate the characteristics of nitrocarburizing for high carbon chromium bearing steel, it was undertaken 4 hours holding at $850^{\circ}C$ in the atmosphere containing 60% endothermic gas and 40% ammonia. The microstructure of nitrocarburized surface consists of ${\varepsilon}-Fe_{2-3}N$, ${\gamma}^{\prime}-Fe_4N$, $Fe_3C$ and $Fe_3$(C,N), and the ${\varepsilon}$-nitride was rich in the surface-internal part. The nitrocarburized surface contains a larger volume fraction of primary carbonitrides and has more retained austenite and is slightly harder than the interior.

• Korean Journal of Materials Research
• /
• v.14 no.4
• /
• pp.265-269
• /
• 2004

Plasma nitrocarburising and post oxidation were performed on SCM435 steel by a pulsed plasma ion nitriding system. Plasma oxidation resulted in the formation of a very thin ferritic oxide layer 1-2 $\mu\textrm{m}$ thick on top of a 15～25 $\mu\textrm{m}$ $\varepsilon$-F $e_{2-3}$(N,C) nitrocarburized compound layer. The growth rate of oxide layer increased with the treatment temperature and time. However, the oxide layer was easily spalled from the compound layer either for both oxidation temperatures above $450^{\circ}C$, or for oxidation time more than 2 hrs at oxidation temperature $400^{\circ}C$. It was confirmed that the relative amount of $Fe_2$$O_3$, compared with $e_3$$O_4$, increased rapidly with the oxidation temperature. The amounts of ${\gamma}$'-$Fe_4$(N,C) and $\theta$-$Fe_3$C, generated from dissociation from $\varepsilon$-$Fe_{2-3}$ /(N,C) phase during $O_2$ plasma sputtering, were also increased with the oxidation temperature.e.

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

• Journal of the Korean Magnetics Society
• /
• v.22 no.3
• /
• pp.79-84
• /
• 2012

Nano-magnetic materials such as iron-nitrides have been actively studied as an alternative to the application of high density, high performance needs for next generation information storage and also alternative to the rare earth and neodymium magnet. $Fe_4N$ is the basic materials for magnetic storage media and is one of the important magnetic materials in focus because of its higher magnetic recording density and chemical stability. Single phase ${\gamma}^{\prime}-Fe_4N$ nanoparticles have been prepared by a PAD (Plasma Arc Discharge) method and nitriding in a $NH_3-H_2$ mixed gases at temperature, $400^{\circ}C$ for 4 hrs. Also $Fe_{17}Sm_2N_x$ powders were synthesized by nitriding after reduction/diffusion of $Fe_{17}Sm_2$ to compare the magnetic properties with nano-sized $Fe_4N$ particles. The saturation magnetization of $Fe_4N$ and $Fe_{17}Sm_2N_x$ were 149 and 117 emu/g, respectively, but the coercive force was considerably smaller than that of bulk or acicular $Fe_4N$.

• Journal of Surface Science and Engineering
• /
• v.38 no.5
• /
• pp.202-206
• /
• 2005

Nitriding treatments were conducted on tool steel (SKD 61) at a temperature of $500^{\circ}C$ for 5 hr using high vacuum direct current (DC) plasma, with ammonia and argon as source gases. The structural and compositional changes produced in the nitrided layers by applying different ratios of Ar to $NH_{3}\;(n_{Ar}/n_{NH3}) were investigated using glancing x-ray diffraction (GXRD), optical microscopy, atomic force microscopy (AFM), micro-Vickers hardness testing, and pin-on-disc type tribometer. Nitriding case depths of around of $50{\mu}m$ were produced, varying slightly with different ratios of $n_{Ar}/n_{NH3}. It was found that the specimen surface hardness was 1150 Hv with $n_{Ar}/n_{NH3}=1, increasing to a maximum value of 1500 Hv with $n_{Ar}/n_{NH3}=5. With a further increase in ratio to $n_{Ar}/n_{NH3}=10, the surface hardness of the specimen reduced slightly to a value of 1370 Hv. These phenomena were caused by changes of the crystallographic structure of the nitride layers, i.e the $\gamma'-Fe_{4}N$ phase only was observed in the sample treated with $n_{Ar}/n_{NH3}$=1, and the intensity of the $\gamma'-Fe_{4}N$ phase were reduced but new phase of $\varepsilon'-Fe_{3}N$, which was known as a high hardness, with increasing $n_{Ar}/n_{NH3}. Also, the relative weight loss of counterface of the pin-on-disc with unnitrided steel was 0.2. And that of nitrided steel at a gas mixture ($n_{Ar}/n_{NH3}) of 1, 5, 7, and 10 was 0.4, 0.7, 0.6, and 0.5 mg, respectively. This means that the wear resistance of the nitrided samples could be increased by a factor of 2 at least than that of unnitrided steel.

• Journal of Surface Science and Engineering
• /
• v.44 no.4
• /
• pp.149-154
• /
• 2011

Martensitic stainless steel STS 431 has been nitrided by active screen ion nitriding under the various temperature and time. The thickness of diffusion layer, case depth, hardness and composition phases were investigated using field emission scanning electron microscopy (FE-SEM), micro-Vickers hardness tester, X-ray diffraction (XRD) and glow discharge spectroscopy (GDS). It was observed that the thickness of diffusion layer depends strongly on the treatment temperature and time. A sample, which was nitrided at $450^{\circ}C$ for 8hours, was a maximum hardness of Hv0.01 1558 and nitride layer of $70{\mu}m$. As shown in XRD patterns, $\varepsilon(Fe_{2-3}N)$ and expanded martensite (${\alpha}_N$) phases which was saturated with nitrogen solid solution were in the nitrided layer treated at $450^{\circ}C$ for 2 hours. Composition phases of $\varepsilon$ $(Fe_{2-3}N)$ and ${\gamma}'$ ($Fe_4N$) were observed after active screen nitriding at $450^{\circ}C$ for 8 hours.

• Journal of the Korean Society for Heat Treatment
• /
• v.11 no.4
• /
• pp.305-314
• /
• 1998

This study has been performed to investigate into some effects of various amounts of $CO_2$ and CO gas added to the $50%NH_3-N_2$ based gas atmosphere on microstructure, hardness, chemical analysis and residual stress in the compound and diffusion layer of AISI H13 treated by gaseous nitrocarburising process. The compound layer formed in the surface is composed of mainly ${\varepsilon}-Fe_3$(N,C) and small amount of ${\gamma}^{\prime}-Fe_4N$ and cementite. The maximum hardness value obtainable from H13 steel is shown to be 1200 Hv and the effecvtive hardening depth increases with increasing CO content from 1% to 4%. In the case of CO content over 4%, however, it decreases with increasing CO content. The composition profiles of nitrogen and carbon are found to be within the ${\varepsilon}$-phase field located above the ${\varepsilon}+{\gamma}^{\prime}$ phase field in the Fe-N-C diagram. It is shown that the maximum value of compressive residual stress of H13 steel treated in atmospheres of $50%NH_3-(2,4)%CO_2-N_2-CO$ gas mixture is $48kg/mm^2$ and the depth to which residual stress is in Compressive state is $90{\mu}m$ for the atmosphere $50%NH_3-45%N_2-4%CO_2-1%CO$ gas mixture. It is consequently important to control the maximum value and size of compressive residual stress region in order to obtain desirable mechanical properties.

• Korean Journal of Materials Research
• /
• v.16 no.2
• /
• pp.85-91
• /
• 2006

The fraction of $\varepsilon\;and\;\gamma$'-iron nitride in compound layer is predicted by x-ray diffraction using direct comparison method. The validity of formulation models was checked by comparing calculated results with metallographic analysis of iron nitride compound layer grown on steel S45C by gas nitriding. The fraction of $\varepsilon$ calculated by the three phase model, porous-$Fe_3N$/ dense-$Fe_3N$/ mixed layer with $Fe_3N\;and\;Fe_4N$, is 80 percent of that analyzed by etching technique. The $\varepsilon$ fraction predicted by mixed layer model is 122 percent of that measured by microscope.

• Journal of Power System Engineering
• /
• v.9 no.1
• /
• pp.76-81
• /
• 2005

The effect of micro-pulse plasma nitriding temperature and time on the case thickness, hardness and nitride formation in the surface of Fe-12Cr-22Mn-X alloy with 3% Co and 1% Ti alloys elements investigated. External compound layer and internal diffusion layer was constituted in plasma nitride case of Fe-12Cr-22Mn-X alloys and formed nitride phase such as ${\gamma}'-Fe4N\;and\;{\varepsilon}-Fe2-3N$. Case depth increased with increasing the plasma nitriding temperature and time. Surface hardness of nitrided Fe-12Cr-22Mn-X alloys obtained the above value of Hv 1,600 and case depth obtained the above value of $45{\mu}m$ in Fe-12Cr-22Mn-3Co alloy and $60{\mu}m$ in Fe-12Cr-22Mn-1Ti alloy. Wear-resistance increased with increasing plasma nitriding time and showing the higher value in Fe-12Cr-22Mn-1Ti alloy than Fe-12Cr-22Mn-3Co alloy.