• 한국세라믹학회지
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• 제50권3호
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• pp.231-237
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• 2013

Thermodynamic modeling of the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ complex ferrite system has been adopted as a rational approach to establish routes to better synthesis conditions for pure phase $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ complex ferrite. Quantitative analysis of the different reaction equilibria involved in the precipitation of $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ from aqueous solutions has been used to determine the optimum synthesis conditions. The spinel ferrites, such as magnetite and substitutes for magnetite, with the general formula $MFe_2O_4$, where M= $Fe^{2+}$, $Co^{2+}$, and $Ni^{2+}$ are prepared by coprecipitation of $Fe^{3+}$ and $M^{2+}$ ions with a stoichiometry of $M^{2+}/Fe^{3+}$= 0.5. The average particle size of the as synthesized $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$, measured by transmission electron microscopy (TEM), is 14.2 nm, with a standard deviation of 3.5 nm the size when calculated using X-ray diffraction (XRD) is 16 nm. When $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ ferrite is annealed at elevated temperature, larger grains are formed by the necking and mass transport between the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ ferrite nanoparticles. Thus, the grain sizes of the $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ gradually increase as heat treatment temperature increases. Based on the results of Thermogravimetric Analysis (TGA) and Differential Scanning Calorimeter (DSC) analysis, it is found that the hydroxyl groups on the surface of the as synthesized ferrite nanoparticles finally decompose to $Ni_{0.5}Zn_{0.4}Cu_{0.1}Fe_2O_4$ crystal with heat treatment. The results of XRD and TEM confirmed the nanoscale dimensions and spinel structure of the samples.

• 대한전자공학회:학술대회논문집
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• 대한전자공학회 2001년도 The 6th International Symposium of East Asian Resources Recycling Technology
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• pp.106-110
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• 2001

Formation of stoichiometric lithium-, nickel-, and zinc- ferrites by calcining organo-metallic precursors a temperature below 40$0^{\circ}C$ is examined using DTA/TG, and XRD techniques. It attempts to simulate th immobilization of metal ions in industrial liquid influents (waste) through the synthesis of stoichiometric spinel ferrites (SSF). Two steps of the SSF formation during thermal treatments are noted. The transformation of magnetite to ${\gamma}$ - Fe$_2$O$_3$and subsequent first formation of SSF were observed at temperatures ranging from 200 to 45$0^{\circ}C$. Th formation of cation-containing ${\gamma}$-Fe$_2$O$_3$and subsequent second formation of the ferrite occurred at temperature ranges of < 45$0^{\circ}C$ and 500 to $650^{\circ}C$, depending on the heating rate used. Then the temperature range of 200t 45$0^{\circ}C$ is critical to the performance of the technique, because a calcination at the range would lead to a complete formation of SSF, avoiding the occurrences of ${\gamma}$-Fe$_2$O$_3$and ion-containing ${\gamma}$-Fe$_2$O$_3$. If not, so $\alpha$-Fe$_2$O$_3$would occur. And annealing at temperature above $650^{\circ}C$ must be employed by which solid-state reactio of $\alpha$-Fe$_2$O$_3$with metal ions (possibly metal oxides) to form SSF can be conducted.

• 한국재료학회지
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• 제32권8호
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• pp.354-360
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• 2022

In this study, an Co/Fe coated porcelain using a cobalt and ferrous sulfate was sintered at 1,250 ℃. The specimens were investigated by HR-XRD, FE-SEM (EDS), Dilatometer, and UV-vis spectrophotometer. The surface of the porcelain was uniformly fused with the pigment, and white ware and celadon body specimens were densely fused to a certain thickness from the surface. Other new compounds were produced by the chemical reaction of cobalt/ferrous sulfate with the porcelain body during the sintering process. These compounds were identified as cobalt ferrite spinel phases for white ware and white mixed ware, and an andradite phase for the celadon body, and the amorphous phase, respectively. As for the color of the specimens coated with cobalt and ferrous mixed pigments, it was found that the L^* value was greatly affected by the white ware, and the a^* and b^* values were significantly changed in the celadon body. The L^* values of the specimens fired with pure white ware, celadon body, and white mix ware were 72.1, 60.92, 82.34, respectively. The C7F3 pigment coated porcelain fired at 1,250 ℃ had L^* values of 39.91, 50.17, and 40.53 for the white ware, celadon body, and white mixed ware, respectively; with a^* values of -1.07, -2.04, and -0.19, and at b^* values of 0.46 and 6.01, it was found to be 4.03. As a new cobalt ferrite spinel phase was formed, it seemed to have had a great influence on the color change of the ceramic surface.

• 한국자기학회지
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• 제19권5호
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• pp.180-185
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• 2009

Sol-gel 법을 이용하여 Fe$_3$O$_4$ 분말을 합성하였으며, 합성한 분말의 구조적 특성, 입자의 모양 및 크기, 자기적 특성에 관하여 연구하였다. 두 가지의 다른 성분비 (Fe$^{2+}$와 Fe$^{3+}$의 몰 당량비를 1 : 2와 Fe$^{2+}$ 만을 사용)와 2-methoxyethanol 용매를 사용하여 refluxing한 후, 질소 분위기에서 200$\sim$600$^{\circ}C$로 열처리하여 페라이트 분말을 합성할 수 있었다. X-선 회절기를 이용하여 합성한 시료의 결정구조를 확인한 결과 두 경우 모두 250$^{\circ}C$ 이상의 열처리로 단일상의 spinel 페라이트가 만들어짐을 확인할 수 있었다. 전계방출 주사전자현미경을 이용하여 관측한 결과에 의하면 열처리 온도가 높아짐에 따라 입자의 크기 증가를 관측할 수 있었다. Mossbauer 분광 실험에서 입자의 크기 변화에 따른 상자성체에서 준강자성체로의 전이를 관측할 수 있었다. 몰 당량비를 1 : 2의 비율로 혼합 후 250$^{\circ}C$에서 열처리한 분말은 크기가 상자성체와 준강자성체의 경계에 위치하며 이중 78%의 시료는 준강자성체의 특성을 22%의 분말은 상자성체의 특성을 가짐을 알 수 있었다. Fe$^{2+}$ 이온만을 사용하는 만든 Fe$_3$O$_4$ 분말은 200$^{\circ}C$의 열처리로 spinel 구조를 가지나 입자의 크기가 작아서 상자성체의 특성을 지닌다. 250$^{\circ}C$ 이상에서 열처리한 시료는 준비 방법에 무관하게 전형적인 Fe$_3$O$_4$ 분말의 연자성 특성을 보이고 있으며, 열처리 온도가 높아감에 따라 포화자화가 증가하고 보자력 또한 증가하는 것을 확인할 수 있었다.

• Journal of Magnetics
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• 제19권3호
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• pp.210-214
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• 2014

The effects of manganese substitution on the crystallographic and magnetic properties of Li-Zn-Cu ferrite, $Li_{0.5}Zn_{0.2}Cu_{0.4}Mn_xFe_{2.1-x}O_4$ ($0.0{\leq}x{\leq}0.8$), were investigated. Ferrites were synthesized via a conventional ceramic method. We confirmed the formation of crystallized particles using X-ray diffraction, field emission scanning electron microscopy and $M{\ddot{o}}ssbauer$ spectroscopy. All of the samples showed a single phase with a spinel structure, and the lattice constants linearly decreased as the substituted manganese content increased, and the particle size of the samples also somewhat decreased as the doped manganese content increased. All the $M{\ddot{o}}ssbauer$ spectra can be fitted with two Zeeman sextets, which are the typical spinel ferrite spectra of $Fe^{3+}$ with A- and B-sites, and one doublet. The cation distribution was determined from the variation of the $M{\ddot{o}}ssbauer$ parameters and of the absorption area ratio. The magnetic behavior of the samples showed that an increase in manganese content led to a decrease in the saturation magnetization, whereas the coercivity was nearly constant throughout. The maximum saturation magnetization was 73.35 emu/g at x = 0.0 in $Li_{0.5}Zn_{0.2}Cu_{0.4}Mn_xFe_{2.1-x}O_4$.

• 한국자기학회지
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• 제10권6호
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• pp.285-290
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• 2000

본 연구에서는 Hexagonal Barium Ferrite(BaM) 박막을 RF magnetron sputtering system을 이용하여 상온에서 증착한후, 85$0^{\circ}C$에서 열처리하여 결정화하였다. XRD pattern을 통해 BaM 박막의 working pressure 10 mTorr에 대한 산소분압(Po$_2$)을 0~3 mTorr가지 변화하여 알아본 결과, 1 mTorr 이하의 산소분압(Po$_2$)에서는 spinel 상과 BaM 상이 함께 형성되었으나, 1 mTorr 이상의 높은 산소분압(Po$_2$)에서는 BaM 상만이 형성되는 것을 알 수 있었다. BaM 박막의 자기적특성을 VSM을 통하여 알아본 결과 산소분압(Po$_2$)이 증가함에 따라 수직보자력은 일정하게 감소를 하였으나 포화자화값은 1 mTorr가지 증가하다 감소하였다. 열처리 시간에 따른 결정화 정도와 특성을 알아본 결과 열처리를 시작한 뒤 10분 이내에 대부분의 특성변화가 일어났으며, 그 이상의 온도에서는 커다란 변화를 일으키지 않음을 알 수 있었다.

• Journal of Magnetics
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• 제21권3호
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• pp.308-314
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• 2016

Cobalt-, zinc-, and nickel-zinc-substituted nano-size manganese ferrite powders, $MnFe_2O_4$, $Mn_{0.8}Co_{0.2}Fe_2O_4$, $Mn_{0.8}Zn_{0.2}Fe_2O_4$ and $Mn_{0.8}Ni_{0.1}Zn_{0.1}Fe_2O_4$, were fabricated using a sol-gel method, and their crystallographic and magnetic properties were subsequently studied. The $MnFe_2O_4$ ferrite powder annealed at temperatures above 523 K exhibited a spinel structure, and the particle size increased as the annealing temperature increased. All ferrites annealed at 773 K showed a single spinel structure, and the lattice constants and particle size decreased with the substitution of Co, Zn, and Ni-Zn. The $M{\ddot{o}}ssbauer$ spectrum of the $MnFe_2O_4$ ferrite powder annealed at 523 K only showed a doublet due to its superparamagnetic phase, and the $M{\ddot{o}}ssbauer$ spectra of the $MnFe_2O_4$, $Mn_{0.8}Co_{0.2}Fe_2O_4$, and $Mn_{0.8}Zn_{0.2}Fe_2O_4$ ferrite powders annealed at 773 K 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 the $Mn_{0.8}Ni_{0.1}Zn_{0.1}Fe_2O_4$ ferrite powder annealed at 773 K consisted of two Zeeman sextets and one quadrupole doublet due to its 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 explained the variation in the $M{\ddot{o}}ssbauer$ parameters by using this cation distribution equation, the superexchange interaction and the particle size. Relative to pure $MnFe_2O_4$, the saturation magnetizations and coercivities were larger in $Mn_{0.8}Co_{0.2}Fe_2O_4$ and smaller in $Mn_{0.8}Zn_{0.2}Fe_2O_4$, and $Mn_{0.8}Ni_{0.1}Zn_{0.1}Fe_2O_4$. These variations could be explained using the site distribution equations, particle sizes and magnetic moments of the substituted ions.

• 폴리머
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• 제29권2호
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• pp.156-160
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• 2005

Octamethylcyclotetrasiloxane$(D_4)$과 1,3,5-trimethyl-1,3,5-triphenylcyclotrisiloxane$(D_3^{Me,Ph)$을 1,1,3,3-tetramethyl-1,3-divinyldisiloxane(MVS)과 평형중합시켜 실리콘의 Si원자에 dimethyl 및 methylphenyl기가 도입된 $\alpha,\omega-vinyl$ poly(dimethyl-methylphenyl) siloxane prepolymer(VPMPS)를 제조하였으며, 또한 $D_4$와 1,3,5-trimethylcyclotrisiloxane$(D_3^:Me,H})$을 1,1,3,3-tetramethyldisiloxane(MS)와 평형중합시켜 Si원자에 dimethyl 및 methylhydrogen기가 도입된 $\alpha,\omega-hydrogen$ poly (dimethyl-methyl) siloxane prepolymer(HPDMS)를 제조하였다. Poly(acrylic acid)(PAA)을 chelating agent로 하여 nickel(II) nitrate와 iron(III) nitrate를 솔-젤 방법으로 PAA 금속염을 제조하고 이틀을 소결시켜 nickel ferrite 나노 입자를 제조하였다. 제조한 nickel ferrite는 XRD 패턴으로 확인하고 입자의 크기를 TEM으로 측정하였다 1,3-Divinyltetramethyldisilazane(VMS)으로 표면처리한 나노 실리카, nickel ferrite, VPMPS, HPDMS 및 촉매를 고속 교반기에 가하고 $130^{\circ}C$에서 컴파운딩하여 poly(organosiloxane) rubber nanocomposites를 제조하였다. Nickel ferrite 함유한 nanocomposite, POX-30과 POX-50을 각각 제조하였으며 이들의 기계적 및 열전도 특성 그리고 체적 저항을 측정하였다.

• 한국재료학회지
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• 제12권10호
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• pp.791-795
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• 2002

We studied the physical properties of $Co_3$$O_4$-added Ni-Zn ferrite which were sintered at 1050~110$0^{\circ}C$ for 2 hours. X-ray diffraction showed a spinel structure, and optical microscopy showed grain sizes of 5 to 10 $\mu\textrm{m}$. As the sintering temperature was increased from $1050^{\circ}C$ to $1070^{\circ}C$, the initial permeability and magnetic induction increased, and both of the loss factor and the coercive force decreased. The Curie temperatures were about $^234~245{\circ}C$ with added $Co_3$$O_4$. The initial permeability was 350 to 420 and maximum magnetic induction density and coercive force 4870G to 4980G and 0.15 Oe to 0.21 Oe, respectively which were similar to those of Ni-Zn ferrite synthesized in the conventional process. The frequency of specimen was in the range of 1MHz to 300MHz. In the plot of initial permeability vs. frequencies, a $180^{\circ}C$ rotation of the magnetic domain could be perceived in a broad band of microwave before and after the resonance frequency.

• 한국자기학회지
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• 제18권2호
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• pp.63-66
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• 2008

초상자성 코발트 페라이트 나노입자를 제조하여 자화 및 자기엔트로피 변화를 조사하였다. 제조된 시료는 전형적인 입방 스피넬 구조를 띠고 있었다. 5K와 300K에서의 최대 자화는 덩어리 상태에서의 최대 자화보다 작은 값을 가졌다. 시료의 초상자성적 거동은 M vs. H/T 곡선의 겹침에 의해 확인되었다. 열역학적 이론을 바탕으로 자기엔트로피의 변화에 대한 온도 의존성을 도출한 결과, 온도가 높을수록 자기엔트로피의 변화는 더 크게 감소하는 것으로 나타났다.