• 한국자기학회지
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• 제15권3호
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• pp.172-176
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• 2005

화학기상응축법(CVC)에 의한 제조된 네 개의 나노-Fe 입자 시료들이 뫼스바우어, XRD, BET와 TEM에 의하여 조사되었다. 네 개의 시료들은 고순도 이송가스와 분해온도에 의해 구성이 되었다. 각 시료를 구성하고 있는 입자들은 2 또는 3층구조로 형성되었음을 TEM분석으로 알 수 있었다. 평균입도의 경우에는 분해온도에 정비례하는 특성을 보여 주었다. 분해온도가 $500^{\circ}C$일 경우에, 이송가스를 CO로 사용하게 되면 $Fe_3C$의 형성이 $CH_4$보다 용이한 것으로 나타났다. 그러나 $1,100^{\circ}C$의 경우에는, CO와 $CH_4$모두에서 $Fe_3C$의 형성이 대부분을 차지하고 있는 것으로 나타났다.

• Environmental Engineering Research
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• 제10권4호
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• pp.165-173
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• 2005

Nano-sized iron particles were synthesized by reduction of $Fe^{3+}$ in aqueous solution under two reaction conditions, aerobic and anaerobic, and the reactivity of iron was tested by reaction with trichloroethene (TCE) using a batch system. Results showed that iron produced under anoxic condition for both synthesis and drying steps gave rise to iron with higher reduction reactivity, indicating the presence of oxygen is not favorable for production of nano-sized iron deemed to accomplish reactivity enhancement from particle sized reduction. Nano-sized iron sample obtained from the anoxic synthesis condition was further characterized using various instrumental measurements to identity particle morphology, composition, surface area, and particle size distribution. The scanning electron microscopic (SEM) image showed that synthesized particles were uniform, spherical particles (< 100 nm), and aggregated into various chain structures. The effects of other synthesis conditions such as solution pH, initial $Fe^{3+}$ concentration, and reductant injection rate on the reactivity of nano-sized iron, along with standardization of the synthesis protocol, are presented in the companion paper.

• 한국자기학회지
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• 제17권2호
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• pp.76-80
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• 2007

화학기상응축공정법으로 세 가지 분해온도에서 제조된 나노 Fe-N 시료들을 뫼스바우어 분광기, XRD와 BET를 이용하여 자기적 특성의 변화를 연구하였다. 분해온도가 낮을수록 ${\gamma}'-Fe_4N$의 형성이 용이하였으며, 중간온도에서의 ${\epsilon}-Fe_{2.12}N$을 거쳐 높은 분해온도에서는 ${\gamma}-Fe$가 주로 형성되었다. 높은 분해온도에서는 Fe와 N이 서로 잘 결합되지 못하였는데, 이는 Fe와 N을 결합시키기 위해서는 분해온도를 낮게 하는 것이 바람직하다는 것을 의미한다.

• Journal of Magnetics
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• 제13권4호
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• pp.149-152
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• 2008

In this report, we present the results of a study on the effects of the particle size on the properties of the Prussian blue (PB) analog $Na_xMn_y[Fe(CN){_6}]$. A novel synthesis method of the $Na_xMn_y[Fe(CN){_6}]$ nano-particles using an organic solvent, formamide, is employed. The size of the PB particles is found to be 100-150 nm for the samples prepared in the formamide solvent, which is much smaller than that of the samples prepared using water only. The broadening of the X-ray diffraction peaks of the nano-sized PB samples is attributed to the lattice disorder and a dramatic reduction in the particle size. The compositions of the samples are confirmed by an energy-dispersive X-ray analysis (EDAX), and the result proves that the samples are actually $Na_xMn_y[Fe(CN){_6}]$ Prussian blue. The UV-vis spectra show a broad intervalence charge-transfer (CT) band in the visible region between 400 and 700 nm, and the absorption decreases abruptly in the green region for the nano-sized PB sample. A divergence between the field cooled (FC) and zero field cooled (ZFC) magnetization curves is observed for the nano-sized PB sample at 11 K, indicating that nanoparticles in the sample are single domain superparamagnets with a blocking temperature of 11 K. Our results reveal that the nano-sized PB samples show significantly different optical and magnetic properties than those of the bulk PB samples.

• 한국재료학회지
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• 제20권10호
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• pp.508-512
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• 2010

The optimum route to fabricate nano-sized Fe-50 wt% Co and hydrogen-reduction behavior of calcined Fe-/Conitrate was investigated. The powder mixture of metal oxides was prepared by solution mixing and calcination of Fe-/Co-nitrate. A DTA-TG and microstructural analysis revealed that the nitrates mixture by the calcination at $300^{\circ}C$ for 2 h was changed to Fe-oxide/$Co_3O_4$ composite powders with an average particle size of 100 nm. The reduction behavior of the calcined powders was analyzed by DTA-TG in a hydrogen atmosphere. The composite powders of Fe-oxide and Co3O4 changed to a Fe-Co phase with an average particle size of 40 nm in the temperature range of $260-420^{\circ}C$. In the TG analysis, a two-step reduction process relating to the presence of Fe3O4 and a CoO phase as the intermediate phase was observed. The hydrogen-reduction kinetics of the Fe-oxide/Co3O4 composite powders was evaluated by the amount of peak shift with heating rates in TG. The activation energies for the reduction, estimated by the slope of the Kissinger plot, were 96 kJ/mol in the peak temperature range of $231-297^{\circ}C$ and 83 kJ/mol of $290-390^{\circ}C$, respectively. The reported activation energy of 70.4-94.4 kJ/mol for the reduction of Fe- and Co-oxides is in reasonable agreement with the measured value in this study.

• 한국분말재료학회지
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• 제10권5호
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• pp.333-336
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• 2003

The purpose of this study is the fabrication of nano-sized Fe-Co alloy powders with soft magnetic properties by the slurry mixing and hydrogen reduction (SMHR) process. $FeCl_2$0 and $CoCl_2$ powders with 99.9% purities were used for synthesizing nanostructured Fe-Co alloy powder. Nano-sized Fe-Co alloy powders were successfully fabricated using SMHR, which was performed at 50$0^{\circ}C$ for 1 h in H$_2$ atmosphere. The fabricated Fe-Co alloy powders showed $\alpha$' phase (ordered body centered cubic) with the average particle size of 45 nm. The SMHR powder exhibited low coercivity force of 32.5 Oe and saturation magnetization of 214 emu/g.

• 한국입자에어로졸학회지
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• 제8권2호
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• pp.83-88
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• 2012

The electrical wire explosion process in liquid media is promising for nano-sized metal and/or alloy particles. The hybrid Pt/Fe-Cr-Al and Pt/Ni-Cr-Fe nanoparticles for exhaust emission control system are synthesized by electrical wire explosion process in liquid media. The alloy powders have spherical shape and nanometer size. According to the wire component, while Pt/Fe-Cr-Al nanoparticles are shown the well dispersed Pt on the Fe-Cr-Al core particle, Pt/Ni-Cr-Fe nanoparticles are shown the partially separated Pt on the Ni-Cr-Fe core particle. Morphologies and component of two kinds of hybrid nano catalyst particles were characterized by transmission electron microscope and energy dispersive X-ray spectroscopy analysis.

• Environmental Engineering Research
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• 제10권4호
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• pp.174-180
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• 2005

Nano-sized iron was synthesized using borohydride reduction of $Fe^{3+}$ in aqueous solution. A wide range of synthesis conditions including varying concentrations of reagents, reagent feeding rate, and solution pH was applied in an aqueous system under anaerobic condition. The reactivity of nano-sized iron from each synthesis was evaluated by reacting the iron with TCE in batch systems. Evidence obtained from this study suggest the reactivity of iron is strongly dependent on the synthesis solution pH. The iron reactivity increased as solution pH decreased. More rapid TCE reduction was observed for iron samples synthesized from higher initial $Fe^{3+}$ concentration, which resulted in lower solution pH during the synthesis reaction. Faster feeding of $BH_4^-$ solution to the $Fe^{3+}$ solution resulted in lower synthesis solution pH and the resultant iron samples gave higher TCE reduction rate. Lowering the pH of the solution after completion of the synthesis reaction significantly increased reactivity of iron. It is presumed that the increase in the reactivity of iron synthesized at lower pH is due to less precipitation of iron (hydr)oxides or less surface passivation of iron.

• Journal of Magnetics
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• 제21권1호
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• pp.40-45
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• 2016

Nickel substituted nano-sized ferrite powders, $Co_{1-x}Ni_xFe_2O_4$, $Mn_{1-x}Ni_xFe_2O_4$ and $Mn_{1-2x}Zn_xNi_xFe_2O_4$ ($0.0{\leq}x{\leq}0.2$), were fabricated using a sol-gel method, and their crystallographic and magnetic properties were subsequently compared. The lattice constants decreased as quantity of nickel substitution increased, while the particle size decreased in $Co_{1-x}Ni_xFe_2O_4$ ferrite but increased for the $Mn_{1-x}Ni_xFe_2O_4$ and $Mn_{1-2x}Zn_xNi_xFe_2O_4$ ferrites. For the $Co_{1-x}Ni_xFe_2O_4$ and $Mn_{1-x}Ni_xFe_2O_4$ ($0.0{\leq}x{\leq}0.2$) ferrite powders, the $M{\ddot{o}}ssbauer$ spectra could be fitted as the superposition of two Zeeman sextets due to the tetrahedral and octahedral sites of the $Fe^{3+}$ ions. However, the $M{\ddot{o}}ssbauer$ spectrum of $Mn_{0.8}Zn_{0.1}Ni_{0.1}Fe_2O_4$ consisted of two Zeeman sextets and one single quadrupole doublet due to the ferrimagnetic and paramagnetic behavior. The area ratio of the $M{\ddot{o}}ssbauer$ spectra could be used to determine the cation distribution equation, and we also explain the variation in the $M{\ddot{o}}ssbauer$ parameters by using this cation distribution equation, the superexchange interaction and the particle size. The saturation magnetization decreased in the $Co_{1-x}Ni_xFe_2O_4$ and $Mn_{1-2x}Zn_xNi_xFe_2O_4$ ferrites but increased in the $Mn_{1-x}Ni_xFe_2O_4$ ferrite with nickel substitution. The coercivity decreased in the $Co_{1-x}Ni_xFe_2O_4$ and $Mn_{1-2x}Zn_xNi_xFe_2O_4$ ferrites but increased in the $Mn_{1-x}Ni_xFe_2O_4$ ferrite with nickel substitution. These variations could thus be explained by using the site distribution equations, particle sizes and spin magnetic moments of the substituted ions.

• 한국세라믹학회지
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• 제49권5호
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• pp.454-460
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• 2012

The nano-sized zirconia powders were synthesized in an impregnation method using pulp and $ZrOCl_2{\cdot}8H_2O$ as an initial material. The synthesized powders were characterized by XRD and FE-SEM. The particle size of the powder was controlled by preparation conditions, such as drying temperature and time. As a result of the various drying and calcination conditions, 30~50 nm sized homogeneous zirconia particles were obtained at $800^{\circ}C$ for 1 h. Crystallization and the rapid growth of particles were accelerated with increasing calcination temperature and time. Tetragonal phase generated below $800^{\circ}C$ were transferred to monoclinic phase with increasing calcination temperature and time. Moreover, above $800^{\circ}C$, heat treatment time had very large influence on the particle growth, and the change of drying condition also had large influence on the growth of a crystal.