• 한국분말재료학회지
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• 제21권6호
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• pp.422-428
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• 2014

In this study, the reduction kinetics and behaviors of oxides in the water-atomized iron powder have been evaluated as a function of temperature ranging $850-1000^{\circ}C$ in hydrogen environment, and compared to the reduction behaviors of individual iron oxides including $Fe_2O_3$, $Fe_3O_4$ and FeO. The water-atomized iron powder contained a significant amount of iron oxides, mainly $Fe_3O_4$ and FeO, which were formed as a partially-continuous surface layer and an inner inclusion. During hydrogen reduction, a significant weight loss in the iron powder occurred in the initial stage of 10 min by the reduction of surface oxides, and then further reduction underwent slowly with increasing time. A higher temperature in the hydrogen reduction promoted a high purity of iron powder, but no significant change in the reduction occurred above $950^{\circ}C$. Sequence reduction process by an alternating environment of hydrogen and inert gases effectively removed the oxide scale in the iron powder, which lowered reduction temperature and/or shortened reduction time.

• 한국분말재료학회지
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• 제11권1호
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• pp.50-54
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• 2004

Nanoparticles of iron oxides have been prepared by the levitational gas condensation (LGC) method, and their structural and magnetic properties were studied by XRD, TEM and Mossbauer spectroscopy. Fe clusters were evaporated from a surface of the levitated liquid Fe droplet and then condensed into nanoparticles of iron oxide with particle size of 14 to 30 nm in a chamber filled with mixtures of Ar and $O_2$ gases. It was found that the phase transition from both $\gamma$-$Fe_2O_3$ and $\alpha$-Fe to $Fe_3O_4$, which was evaluated from the results of Mossbauer spectra, strongly depended on the $O_2$ flow rate. As a result, $\gamma$-$Fe_2O_3$ was synthesized under the $O_2$ flow rate of 0.1$\leq$$Vo_2$(Vmin)$\leq$0.15, whereas $Fe_3O_4$ was synthesized under the $O_2$, flow rate of 0.15$\leq$$Vo_2$(Vmin)$\leq$0.2.

• 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.

• 한국주조공학회지
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• 제10권2호
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• pp.154-161
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• 1990

The microstructures of sintered products of $Fe_2O_3$or $Fe_3O_4$-Oxide added cast iron powder was investigated. And the effects of particle size distribution was investigated too. As the result, the structures of sintered products did not related to the species of Fe-Oxide. Th porosity of sintered products was decreased in size and spherodized with increasing sintering temperature, decreasing Fe-Oxide quantity. Fe-Oxide itself did not hinder sintering of cast iron powder particularly, therefore sintering could be occurred without termination of reduction of it. And the sintered products of finer particle size distribution had finer and more spherodized porosity, and had minimized the deviation of size and shape of porosity.

• 한국분말재료학회지
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• 제26권6호
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• pp.481-486
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• 2019

Iron oxides currently attract considerable attention due to their potential applications in the fields of lithiumion batteries, bio-medical sensors, and hyperthermia therapy materials. Magnetite (Fe₃O₄) is a particularly interesting research target due to its low cost, good biocompatibility, outstanding stability in physiological conditions. Hydrothermal synthesis is one of several liquid-phase synthesis methods with water or an aqueous solution under high pressure and high temperature. This paper reports the growth of magnetic Fe₃O₄ particles from iron powder (spherical, <10 ㎛) through an alkaline hydrothermal process under the following conditions: (1) Different KOH molar concentrations and (2) different synthesis time for each KOH molar concentrations. The optimal condition for the synthesis of Fe₃O₄ using Fe powders is hydrothermal oxidation with 6.25 M KOH for 48 h, resulting in 89.2 emu/g of saturation magnetization at room temperature. The structure and morphologies of the synthesized particles are characterized by X-ray diffraction (XRD, 2θ = 20°-80°) with Cu-kα radiation and field emission scanning electron microscopy (FE-SEM), respectively. The magnetic properties of magnetite samples are investigated using a vibrating sample magnetometer (VSM). The role of KOH in the formation of magnetite octahedron is observed.

• Journal of Magnetics
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• 제15권4호
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• pp.179-184
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• 2010

We have investigated the effects of post annealing on iron oxide nanoparticles synthesized by the novel hydrothermal synthesis method with the $FeSO_4{\cdot}7H_2O$. To investigate the post annealing effect, the as-synthesized iron oxide nanoparticles were annealed at different temperatures in a vacuum chamber. The morphological, structural and magnetic properties of the iron oxide nanoparticles were investigated with high resolution X-ray powder diffraction (XRD), high resolution transmission electron microscopy (HRTEM), Mossbauer spectroscopy, and vibrating sample magnetometer analysis. According to the XRD and HRTEM analysis results, as-synthesized iron oxide nanoparticles were only magnetite ($Fe_3O_4$) phase with face-centered cubic structure but post annealed iron oxide nanoparticles at $700^{\circ}C$ were mainly magnetite phase with trivial maghemite ($\gamma-Fe_2O_3$) phase which was induced in the post annealing treatment. The crystallinity of the iron oxide nanoparticles is enhanced by the post annealing treatment. The particle size of the as-synthesized iron oxide nanoparticles was about 5 nm and the particle shape was almost spherical. But the particle size of the post annealed iron oxide nanoparticles at $700^{\circ}C$ was around 25 nm and the particle shape was spherical and irregular. The as-synthesized iron oxide nanoparticles showed superparamagnetic behavior, but post annealed iron oxide nanoparticles at $700^{\circ}C$ did not show superparamagnetic behavior due to the increase of particle size by post annealing treatment. The saturation of magnetization of the as-synthesized nanoparticles, post annealed nanoparticles at $500^{\circ}C$, and post annealed nanoparticles at $700^{\circ}C$ was found to be 3.7 emu/g, 6.1 emu/g, and 7.5 emu/g, respectively. The much smaller saturation magnetization value than one of bulk magnetite can be attributed to spin disorder and/or spin canting, spin pinning at the nanoparticle surface.

• 한국분말야금학회:학술대회논문집
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• 한국분말야금학회 2006년도 Extended Abstracts of 2006 POWDER METALLURGY World Congress Part2
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• pp.971-972
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• 2006

Mechanochemical synthesis of zinc ferrite, $ZnFe_2O_4$, was attempted from a powder mixture of iron (III) oxide, alpha-$Fe_2O_3$ and zinc (II) oxide, ZnO. Nanocrystalline zinc ferrite, $ZnFe_2O_4$ powders were successfully synthesized only bymilling for 30 hours. Evidence of the $ZnFe_2O_4$ formation was absent for the powders milled for 10 and 20 hours; the milling lowered the crystallinity of the starting materials. Heating after milling enhanced the formation of $ZnFe_2O_4$, crystal growth of $ZnFe_2O_4$ and the unreacted starting materials. The unreacted starting materials decreased their amounts by heating at higher temperatures.

• 한국분말재료학회지
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• 제30권4호
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• pp.297-304
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• 2023

Iron oxide (Fe₂O₃) nanoclusters exhibit significant potential in the biomedical and pharmaceutical fields due to their strong magnetic properties, stability in solutions, and compatibility with living systems. They excel in magnetic separation processes, displaying high responsiveness to external magnetic fields. In contrast to conventional Fe2O3 nanoparticles that can aggregate in aqueous solutions due to their ferrimagnetic properties, these nanoclusters, composed of multiple nanoparticles, maintain their magnetic traits even when scaled to hundreds of nanometers. In this study, we develop a simple method using solvothermal synthesis to precisely control the size of nanoclusters. By adjusting precursor materials and reducing agents, we successfully control the particle sizes within the range of 90 to 420 nm. Our study not only enhances the understanding of nanocluster creation but also offers ways to improve their properties for applications such as magnetic separation. This is supported by our experimental results highlighting their size-dependent magnetic response in water. This study has the potential to advance both the knowledge and practical utilization of Fe₂O₃ nanoclusters in various applications.

• 대한금속재료학회지
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• 제49권1호
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• pp.52-57
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• 2011

Nickel ferrite ($NiFe_2O_4$) powder was prepared through the ceramic route by calcination of a stoichiometric mixture of nickel oxide (NiO) and iron oxide ($Fe_2O_3$). The pressed pellets of $NiFe_2O_4$ were isothermally reduced in pure hydrogen at 800, 900, 1000 and $1100^{\circ}C$. Based on thermogravimetric analysis, the reduction behavior and the kinetic reaction mechanisms of the synthesized ferrite were studied. The initial ferrite powder and various reduction products were characterized by XRD, SEM, reflected light microscope and VSM to reveal the effect of hydrogen reduction on the composition, microstructure, magnetic properties and reaction kinetics of the produced Fe-Ni alloy. Complete reduction of the $NiFe_2O_4$ was achieved with synthesis of homogeneous nanocrystalline Fe-Ni alloys. Arrhenius equation with the approved mathematical formulations for a gas-solid reaction was applied for calculating the activation energy ($E_a$) values and detecting the controlling reaction mechanism.

• 대한화학회지
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• 제38권2호
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• pp.92-100
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• 1994

초미립 코발트 치환 산화철 분말을 새로운 유기금속 전구체인 $Co_xFe_{1-x}(N_2H_3COO)_2(N_2H_4)_2$ (x = 0, 0.01, 0.02, 0.03, 0.05, 0.10, 1.00)을 열분해화 산화과정으로 제조하였다.유기금속 전구체는 몰비 x : 1-x인 Co(II)와 Fe(II)를 hydrazinocarboxylic acid와 반응시켜서 합성하였고, 합성을 정량분석, 및 적외선분광기를 사용하며, 합성을 정량분석, 원소분석 및 적외선분광기를 사용하여 확인하였다. 유기금속 전구체의 열분해 과정은 TG-DTG 와 DSC로 살펴보았다. 코발트치환 산화철 분말은 유기금속 전구체를 대기 중에서 $350^{\circ}C$ 와 $450^{\circ}C$에서 6시간 열처리하여 제조하였다. 산화철의 결정상은 각각 ${\gamma}-Fe_2O_3$ 및 ${\gamma}-Fe_2O_3$ 와 ${\alpha}-Fe_2O_3$의 혼합상이었다. 입자의 형태는 구형에 가까운 모양이었고 크기는 $0.05{\mu}m$ 이하의 초미립이었다. 코발트 치환 산화철의 보자력과 각형비는 코발트 함량 또는 열처리 온도가 높아질 수록 증가하였다.