• Journal of the Korean Physical Society
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• 제73권10호
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• pp.1535-1540
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• 2018

In this study, we prepared and characterized Nb-doped $Li_7La_3Zr_{2-x}O_{12}$ (LLZNO) powder and pellets with a cubic garnet structure by using a modified sol-gel synthesis and hot pressing. LLZNO powder with a very small grain size and cubic structure without secondary phases could be obtained by using a synthesis method in which Li and La sources in a propanol solvent were mixed together with Zr and Nb sources in 2-methoxy ethanol. A pure cubic phase LLZNO pellet could be fabricated from the prepared LLZNO and an additional 6-wt% of $Li_2CO_3$ powder by hot pressing at $1050^{\circ}C$ and 15.8 MPa. The hot-pressed LLZNO pellet with a relative density of 99% exhibited a very dense surface morphology. The total Li ionic conductivity of the hot-pressed LLZNO was $7.4{\times}10^{-4}S/cm$ at room temperature, which is very high level compared to other reported values. The activation energy for ionic conduction was estimated to be 0.40 eV.

• 한국세라믹학회지
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• 제56권2호
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• pp.111-129
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• 2019

Recently, all-solid-state batteries (ASSBs) have attracted increasing interest owing to their higher energy density and safety. As the core material of ASSBs, the characteristics of the solid electrolyte largely determine the performance of the battery. Thus far, a variety of inorganic solid electrolytes have been studied, including the NASICON-type, LISICON-type, perovskite-type, garnet-type, glassy solid electrolyte, and so on. The garnet Li₇La₃Zr₂O₁₂ (LLZO) solid electrolyte is one of the most promising candidates because of its excellent comprehensively electrochemical performance. Both, experiments and theoretical calculations, show that cubic LLZO has high room-temperature ionic conductivity and good chemical stability while contacting with the lithium anode and most of the cathode materials. In this paper, the crystal structure, Li-ion transport mechanism, preparation method, and element doping of LLZO are introduced in detail based on the research progress in recent years. Then, the development prospects and challenges of LLZO as applied to ASSBs are discussed.

• 한국광물학회지
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• 제2권1호
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• pp.26-36
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• 1989

Clinopyroxene in the Geodo mine belongs to diopside-hedenbergite series. It is widely distributed throughout the mine area together with garnet and is also closely related with Fe-mineralization. Clinopyroxenes in the Geodo mine including two samples from the sangdong and Ulchin Mines are studied using polarized microscope, EPMA, XRD, and IR spectroscopy for occurrence, chemistry, structure, and crystal chemistry. Especially, variations in unit-cell parameters are examined in relation with the substitution scheme between Fe and Mg cations. Clinopyroxenes in the Geodo mine occur in both endoskarn and exoskarn zone. It is mostly anhedral to subhedral with fine- to medium-grained in texture, but some have bigger crystals of short prismatic or columnar habits. Clinopyroxene occurs as monomineralic or is associated with mostly garnet and sometimes with actinolite, magnetite, epidote, and chlorite. Chemical analysis reveals that the Geodo clinopyroxene is diopsidic in composition (Di: 65-96%). This fact is in good contrast with garnet chemistry showing mostly andraditic (An: 41-82%). Especially, clinopyroxene coexisting with magnetite belongs to nearly end member diopside (Di: 97-99%). Thus, diopside-andradite pair indicates that Geodo skarns were formed under the reduced environment. X-ray diffraction analysis shows unit-cell parameters vary with increase of Fe contents: a = 9.765-9.838$\AA$, b = 8.943-9.020$\AA$, c= 5.240-5.253$\AA$.$\beta$ = 105.70-104.83$^{\circ}$, and V =440.64-448.19$\AA$3. It is noted from the least square regression that a, b and V increase linearly with increase of Fe content, while $\beta$ slightly decreases and c remains nearly unchanged as change in Fe content. These trends are to difference between synthetic and natural clinopyroxenes. This fact is also recognized in IR spectra which show a slight shift of several absorption bands toward lower wavenumber region with increasing Fe content.

• Journal of Magnetics
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• 제13권3호
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• pp.110-113
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• 2008

In this study, heavy rare earth garnet $Tb_2Bi_1Ga_1Fe_4O_{12}$ powders were fabricated by a sol-gel and vacuum annealing process. The crystal structure was found to be single-phase garnet with a space group of Ia3d. The lattice constant $a_0$ was determined to be 12.465 ${\AA}$. From the analysis of the vibrating sample magnetometer (VSM) hysteresis loop at room temperature, the saturation magnetization and coercivity of the sample are 7.64 emu/g and 229 Oe, respectively. The N$\acute{e}$el temperature($T_N$) was determined to be 525 K. The M$\ddot{o}$ssbauer spectrum of $Tb_2Bi_1Ga_1Fe_4O_{12}$ at room temperature consists of 2 sets of 6 Lorentzians, which is the pattern of single-phase garnet. From the results of the M$\ddot{o}$ssbauer spectrum at room temperature, the absorption area ratios of Fe ions on 24d and 16a sites are 74.7% and 25.3%(approximately 3:1), respectively. These results show that all of the non-magnetic Ga atoms occupy the 16a site by a vacuum annealing process. Absorption area ratios of Fe ions are dependent not only on a sintering condition but also on the temperature of the sample. It can then be interpreted that the Ga ion distribution is dependent on the temperature of the sample. The M$\ddot{o}$ssbauer measurement was carried out in order to investigate the atomic migration in $Tb_2Bi_1Ga_1Fe_4O_{12}$.

• 한국자기학회지
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• 제16권5호
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• pp.245-248
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• 2006

Sol-gel법을 이용하여 단일상을 갖는 $Tb_{3-x}Bi_xFe_5O_{12}$ 분말 시료를 제조하였으며, 그 결정학적 및 자기적 특성을 x-선 회절법(XRD), 진동 시료 자화율 측정법(VSM), $M\"{o}ssbauer$ 분광법으로 연구하였다. XRD 분석 결과 결정구조는 Ia3d의 공간그룹을 갖는 cubic 구조임을 알 수 있었고, Bismuth의 치환량이 x=0.5, 0.75, 1.0 및 1.25로 증가할수록 격자상수가 각각 $a_0=12.466{\AA},\;12.487{\AA},\;12.499{\AA},\;12.518{\AA}$으로 선형적으로 증가함을 확인할 수 있었다. VSM을 이용한 온도에 따른 자기모멘트 측정 결과 Bismuth의 치환량이 증가하면 $N\'{e}el$ 온도는 증가하며 compensation 온도는 감소함을 확인할 수 있었다. 또한 field cooled 조건에서 비정상적인 음의 자화값이 관측되었다. $M\"{o}ssbauer$ 스펙트럼은 4.2 K에서부터 $N\'{e}el$ 온도까지 측정하였으며, 분석 결과 상온에서 모든 시료의 이성질체 이동치의 값은 평균적으로 0.27mm/s로 철의 이온상태가 +3가 임을 확인할 수 있었다.

• 한국재료학회지
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• 제13권1호
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• pp.48-52
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• 2003

The substituted yttrium iron garnet systems $Y_{ 3-x}$/Gd$_{x}$X$0.2_{0.2}$ $Fe_{4.8}$ $O _{12}$ (x = 0.2, 0.4, 0.6) have been investigated by means of X-ray diffraction, Mossbauer spectroscopy and SQUID. The X-ray diffraction patterns at room temperature confirm the samples to have a single phase of the garnet structure over the whole composition range. The lattice constants of all the samples linearly change with increasing x due to the size of substituted ions in the dodecahedral sites. $Y_{3-x}$ $Gd_{x}$ X$Fe_{4.8}$ $In_{0.2}$ $O_{12}$ system which $Y_{3-x}$ ions are substituted with Gd$^{ 3＋}$ ions, the Mossbauer spectrum consists of three Zeeman sextets at room temperature, one due to the $Fe^{3＋}$ ions on the octahedral(a-) sites and the others due to the $Fe^{3＋}$ ions on the tetrahedral(d-, d'-) sites, respectively. From the hysteresis loop measured by means of SQUID over the whole composition range, the saturation magnetization $M_{s}$ and magnetic moments $\mu_{ B}$ per unit cell have been obtained. The increment of Gd-ion content causes $M_{s}$ and $\mu_{B}$ decrease while the increment of In-ion content does not.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2006년도 추계학술대회 논문집 Vol.19
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• pp.322-323
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• 2006

The nano-sized Ce-doped YAG(Yttrium Aluminum Garnet, $Y_3Al_5O_{12}$) phosphor powders were prepared by combustion method from a mixed aqueous solution of metal nitrates, using citric acid as a fuel. The luminescence formation process and structure of phosphor powders were investigated by means of XRD, SEM and PL. The XRD patterns show that YAG phase can form at all of the $Ce^{3+}$ concentration. However, when $Ce^{3+}$ concentration is over 2.0mol%, XRD patterns show $CeO_2$ peak between (321) peak and (400) peak. The pure crystalline YAG:Ce with uniform size of 30nm was obtained at 0.6mol% of the $Ce^{3+}$ concentration. The crystalline YAG:Ce powders showed broad emission peaks in the range 475~630nm and had maximum intensity at 526nm.

• 한국전기전자재료학회:학술대회논문집
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• 한국전기전자재료학회 2006년도 하계학술대회 논문집 Vol.7
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• pp.489-490
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• 2006

The Ce-doped YAG(Yttrium Aluminum Garnet, $Y_3Al_5O_{12}$) phosphor powders were synthesized by Sol-gel method. The luminescence, formation process and structure of phosphor powders were investigated by means of XRD, SEM and PL. The XRD patterns show that YAG phase can form through sintering at $1000^{\circ}C$ for 2h. This temperature is much lower than that required to synthesize YAG phase via the conventional solid state reaction method. There were no intermediate phases such as YAP(Yttrium Aluminum Perovskite, $YAlO_3$) and YAM(Yttrium Aluminum Monoclinic, $Y_4Al_2O_9$) observed in the sintering process. The powders absorbed excitation energy in the range 410~510nm. Also, the crystalline YAG:Ce showed broad emission peaks in the range 480~600nm and had maximum intensity at 528nm.

• Nuclear Engineering and Technology
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• 제54권7호
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• pp.2579-2585
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• 2022

Ceramics of quaternary garnets (Gd,Y)₃Al₂Ga₃O₁₂ doped with Ce, Tb have been fabricated and evaluated as prospective materials for indirect energy converters of α-and β-voltaic. Samples were characterized at excitation with an X-ray source and an intense 150 keV electron beam and showed good temperature stability of their emission and tolerance to irradiation. The role of X-rays accompanied the α-particle emitting in the increase of the conversion efficiency is clarified. The garnet-type structure of the matrix in the developed materials allows the production of quality crystalline mass with a light yield exceeding that of the commonly used YAG: Ce scintillator by a factor of two times.

• 자원환경지질
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• 제38권2호
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• pp.187-196
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• 2005

석류석 구조에서, 양이온이 점할 수 있는 구조적 위치는 사면체, 팔면체 및 이들과 능을 공유하고 있는 배위다면체의 중심 등이다. 이들 중, 사면체의 자리를 차지하는 양이온의 크기는 석류석의 단위포의 크기와 밀접한 관계를 가진다. 따라서 4-배위 자리에 비교적 이온반경이 큰 철을 함유하고 있는 석류석은 방사성 폐기물 내에 함유된 비교적 이온반경이 큰 악티나이드 원소를 고정시키기 위한 유망한 매트릭스로써 고려될 수 있다. 따라서 본 연구에서는 $Ca_{1.5}GdCe_{0.5}ZrFeFe_3O_{12}$인 조성을 가진 석류석을 합성하여 이들의 상평형 관계 및 특성을 연구하였다. 혼합된 시료는 $200{\~}400{\cal}kg/{\cal}cm^2$의 압력으로 성형한 후, $1100{\~}1400^{\circ}C$ 범위에서 온도 및 분위기를 변화시키면서 소결하였으며, 합성된 시료는 XRD 및 SEM/EDS를 사용하여 상분석과 정량분석을 실시하였다. 실험결과, 석류석은 소결온도 $1300^{\circ}C$에서 최적의 합성상을 얻을 수 있었지만, 미량의 페로브스카이트 및 미지의 상이 공존하였다. 석류석과 페로브스카이트의 화학조성은 각각 $[Ca_{l.2-1.8}Gd_{0.9-1.4}Ce_{0.3-0.5}]^{VIII}[Zr_{0.8-1.3}Fe_{0.7-1.2}]^{VI}[Fe_{2.9-3.1}]^{IV}O_{12}$ 및 $Ca_{0.1-0.5}Gd_{0.0-0.8}Ce_{0.1-0.5}\;Zr_{0.0-0.2}Fe_{0.9-1.1}O_3$ 이었다. 특히 화학양론적 조성과 비교 시, 합성된 석류석의 8-배위 자리를 점하고 있는 Ca의 초과 및 Ce의 결핍된 양상을 보였다. 이는 6-배위 자리에서의 Zr 및 Fe의 화학조성과 밀접한 관계를 지닌다.