• 전기화학회지
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• 제9권4호
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• pp.158-169
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• 2006

The present article is concerned with the overview of the chemically/surface modified cubic spinel $LiMn_2O_4$ as a cathode electrode far lithium ion secondary batteries. Firstly, this article presented a comprehensive survey of the cubic spinel structure and its correlated electrochemical behaviour of $LiMn_2O_4$. Subsequently, the various kinds of the chemically/surface modified $LiMn_2O_4$ and their electrochemical characteristics were discussed in detail. Finally, this article reviewed our recent research works published on the mechanism of lithium transport through the chemically/surface modified $Li_{1-\delta}Mn_2O_4$ electrode from the kinetic view point by the analyses of the experimental potentiostatic current transients and ac-impedance spectra.

• 한국자기학회지
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• 제15권2호
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• pp.96-99
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• 2005

Phase transition from normal- to inverse-spinel structure has been observed for $Fe_xCo_{3-x}O_4$ thin films as the Fe composition (x) increases from 0 to 2. The samples were fabricated as thin films by sol-gel method on Si(100) substrates. X-ray diffraction measurements revealed a coexistence of two phases, normal and inverse spinel, for $0.76{\le}x{\le}0.93$. The normal-spinel phase is dominant for $x{\le}0.55$ while the inverse-spinel phase for $x{\ge}l.22$. The cubic lattice constant of the inverse-spinel phase is larger than that of the normal-spinel phase. For both phases the lattice constant increases with increasing x. X-ray photoelectron spectroscopy measurements revealed that both $Fe^{2+}$ and $Fe^{3+}$ ions exist with similar strength in the x=0.93 sample. Conversion electron $M\ddot{o}ssbauer$ spectra measured on the same sample showed that $Fe^{2+}$ ions prefer the octahedral $Co^{3+}$ sites, indicating the formation of the inverse-spinel phase. Analysis on the measured optical absorption spectra for the samples by spectroscopic ellipsometry indicates the dominance of the normal spinel phase for low x in which $Fe^{3+}$ ions tend to substitute the octahedral sites.

• 한국결정성장학회지
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• 제25권5호
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• pp.225-229
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• 2015

본 연구에서는 Mn-Co-Ni 삼성분계로 이루어진 NTC 서미스터의 cubic 스핀넬 결정구조의 변화를 고찰하고자 하였다. Mn, Co, Ni로 이루어진 산화물 원재료 분말들을 혼합하고 건조한 후 In-situ XRD 장비를 이용하여 공기분위기에서 상온부터 $1400^{\circ}C$까지 가열하면서 발생하는 결정구조 변화를 분석하였다. In-situ XRD 분석 결과 cubic 스핀넬 구조는 $900^{\circ}C$부터 존재하는 것을 확인할 수 있었으나, 온도가 $1300^{\circ}C$ 이상으로 올라갔을 때는 스핀넬 결정구조로부터 NiO의 상분리 현상이 발생하기 시작함을 관찰할 수 있었다. 이러한 NiO 상의 분리가 고온에서의 NTC 서미스터의 결정성 감소의 원인임을 알 수 있었으며, 제작된 NTC 서미스터의 표면을 FE-SEM을 이용하여 관찰하여 양품과 불량품의 차이를 분석하였다.

• 한국재료학회지
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• 제9권7호
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• pp.657-662
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• 1999

기판온도 $320^{\circ}C$에서 알루미나 기판 위에 형성한 NTC 써미스터용 Mn-Ni계 산화물 박막의 산소가스 농도 변화와 막 형성 후 열처리에 따른 미세구조, 결정상 비저항, B정수 변화에 관하여 연구하였다. 미세구조는 주상 구조(columnar structure)를 지녔으며 열처리 온도가 증가함에 따라 $700^{\circ}C$ 부근에서 등축 결정립 (equiaxed grain) 형태의 미세구조로 바뀌기 시작하였다. 박막의 결정상은 대부분 입방 스피넬 (cubic spinel) 상과 입방 $Mn_2$$O_3$, 상이 공존하였으며 산소농도 0.16%~0.7%의 경우 $800^{\circ}C$에서 열처리하였을 때 입방 스피넬 상만이 존재하였다. 분위기 산소의 농도가 증가함에 따라 비저항과 B정수도 급격하게 감소하다가 다소 증가하였으며, $600^{\circ}C$-$700^{\circ}C$ 로 열처리할 경우 이 값들이 대체로 낮고 안정된 특성을 보였다.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2001년도 하계학술대회 논문집
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• pp.455-458
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• 2001

Spinel $LiMn_{2-y}$$M_{y}$ $O_4$powder was prepared solid-state method by calcining the mixture of LiOH - $H_2O$, Mn $O_2$, ZnO and MgO at 80$0^{\circ}C$ for 36h. To investigate the effect of substitution with Mg, Zn cation, charge-discharge experiments and initial impedance spectroscopy performed. The structure of $LiMn_{2-y}$$M_{y}$ $O_4$crystallites was analyzed from powder X-ray diffraction data as a cubic spinel, space group Fd3m. all cathode material showed spinel phase based on cubic phase in X-ray diffraction. Ununiform which calculated by (111) face and (222) face was constant in spite of the change of y value, except PUf\ulcorner LiM $n_2$ $O_4$. The discharge capacities of the cathode for the cation subbstitUtes $LiMn_{2-y}$$M_{y}$ $O_4$/Li cell at the 1st cycle and at the 40th cycle were about 120~124 and 108~112mAh/g except LiM $n_{1.9}$Z $n_{0.1}$ $O_4$/Li cell, respectively. This cell capacity is retained by 93% after 40th cycle. AC impedance of $LiMn_{2-y}$$M_{y}$ $O_4$/Li cells revealed the similar resistance of about 65~110$\Omega$ before cycling. before cycling.g.g.

• 한국결정학회지
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• 제14권2호
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• pp.110-114
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• 2003

LiAl/sub 0.24/Mn/sub 1.76/O/sub 4-y/S/sub y/ (y=0, 0.02) were synthesized by the sol-gel method. Both structures were refined by Rietveld method, its structure refined as a cubic spinel, space group Fd-3m, a=8.17937(30) Å and 8.18331(19) Å respectively. Though it has been made a charge/discharge experiment above 20 times, there was no change of 3 V/4 V capacity degradation. It was considered that the volume change of MnO/sub 6/ octahedron induced by sulfur substitution plays a key role in keeping the 3 V/4 V capacity. The refined composition of the compound could be confirmed with the ICP analysis.

• 한국재료학회지
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• 제15권6호
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• pp.393-398
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• 2005

The crystal structure and magnetic properties of the $Mg_{1-x}Zn_xFeAlO_4\;(0{\leq}x\leq1.0)$ have been investigated by means of x-ray diffractometry and $M\ddot{o}ssbauer$ spectroscopy. The samples$(0{\leq}x\leq1.0)$ have been prepared by the ceramic sintering method. The x-ray diffraction pattern shows that the crystal structure of the samples is a cubic spinel type. The lattice constant has been found by extrapolation using the Nelson-Riley function and it increases slightly from $8.3496\AA\;to\;8.4128\AA$ with Zn concentration. The $M\ddot{o}ssbauer$ spectra for x<0.4 show a superposition of two sextets ana a paramagnetic doublet at room temperature. The superparamagnetic doublet for x<0.4 seems to be due to Al ion in tetrahedral site by the superparamagnetic clustering effect.

• 한국세라믹학회지
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• 제39권12호
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• pp.1119-1123
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• 2002

Nanostructured spinel NiZn ferrites were prepared by the sol-gel method from metal nitrate raw materials. Analyses by X-ray diffraction and scanning electron microscopy showed the average particle size of NiZn ferrite was under 50 nm. The single phase of NiZn ferrites was obtained by firing at 250${\circ}C$, resulting in nanoparticles exhibiting normal ferrimagnetic behavior. The nanostructured $Ni_{1-X}Zn_XFe_2O_4$ (x=0.0∼1.0) were found to have the cubic spinel structure of which the lattice constants ${\alpha}_2$ increases linearly from 8.339 to 8.427 ${\AA}$ with increasing Zn content x, following Vegard's law, approximately. The saturation magnetization $M_s$ was 48 emu/g for x=0.4 and decreased to 8.0 emu/g for higher Zn contents suggesting the typical ferrimagnetism in mixed spinel ferrites. Pure NiZn ferrite phase substituted by Cu was observed before using the additive but hematite phase was partially appeared at $Ni_{0.2}Zn_{0.2}Cu_{0.6}Fe_2O_4$. On the other hand, the hematite phase in this NiZn Cu ferrite was disappeared after using the additive of acethyl aceton with small amount. The saturation magnetization Ms of $Ni_{0.2}Zn_{0.8-y}Cu_yFe_2O_4$(y=0.2∼0.6) as measured was about 51 emu/g at 77K and 19 emu/g at room temperature, respectively.

• 한국재료학회지
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• 제8권5호
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• pp.424-428
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• 1998

RF magnetron sputter로 알루미나 기판 위에 증착한 NTC 써미스터용 Mn-Ni계 산화물 박막의 기판온도 변화와 열처리에 따른 미세구조, 결정상, 비저항, B정수 변화에 관하여 연구하였다. 미세구조는 $178^{\circ}C$이하에서 증착한 막의 경우 fibrous microcrystalline이었고, $320^{\circ}C$와 $400^{\circ}C$에서는 columnar grain 구조로 바뀌었다. 또한, 90$0^{\circ}C$에서 열처리한 박막의 경우 equiaxed grain 형태의 미세구조를 나타내었다. 박막의 결정상은 대부분 입방 스피넬(cubic spinel)상과 $Mn_{2}$$O_{3}$ 상이 공존하였고, $400^{\circ}C$에서 증착한 경우 $700^{\circ}C$이상에서 열처리하면 입방 스피넬의 단상으로 바뀌었다. 기판온도가 증가함에 따라 비저항과 B정수도 급격하게 감소하였으며, $600^{\circ}C$~$700^{\circ}C$로 열처리할 경우 이 값들이 대체로 낮고 안정된 특성을 보였다. 본 연구의 박막 시편들은 모두 NTC 써미스터의 특성을 나타내었다.

• 한국전기전자재료학회논문지
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• 제14권4호
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• pp.309-315
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• 2001

Crystallized $LiMn_{2-y}Mg_{y}O_4$ powder was prepared by calcing the mixture of LiOH.$H_2O$, $MnO_2$ and MgO at $800^{\circ}C$ for 36h in an air atmosphere. The structure of $LiMn_{2-y}Mg_{y}O_4$ crystallites was analyzed from powder X-ray diffraction data as a cubic spinel, space group Fd3m. Though all cathode material showed spinel phase based on cubic phase in X-ray diffraction, other peaks gradually exhibited and became intense with increasing y value in $LiMn_{2-y}Mg_{y}O_4$. However, ununiform which calculated by (111) face and (222) face was constant in spite of the increase of y value, except pure $LiMn_2O_4$. AC impedance of Li/$LiMn_{2-y}Mg_{y}O_4$ cells revealed the similar resistance of about $70\Omega$ before cycling. In addition, The impedance of Li/$LiMn_{1.9}Mg_{0.1}O_4$ cell changed during charge and discharge or after cycling.