• 한국결정성장학회지
• /
• 제7권2호
• /
• pp.253-258
• /
• 1997

반도체화 첨가제인 $Y_2O_3$와 $Nb_2O_5$ 첨가랑 변화에 따른 PTCR $BaTiO_3$ 세라믹스의 결정구조 해석과 상전이 특성을 연구하기 위하여 ($Ba_{0.85}Ca_{0.15})TiO_3$ ＋ X m/o $Nb_2O_5$(Y m/o $Y_2O_3$) ＋ 0.08 w/o $Mn(NO_3)_2$ㆍ$6H_2O$ ＋ 0.25 w/o $SiO_2$ 계에서 X는 0.1 ~ 0.4로 Y는 0.2 ~ 0.4로 각각 변화시켜 실험을 수행하였다. $Nb_2O_5$의 첨가시 B-site 치환에 따라서 격자상수가 선형적으로 변화하다가 0.3 mol% 이상 치환할 경우 c 축의 격자상수가 급격히 감소함을 알 수 있었다. 이는 octahedron distortion둥의 원인으로 판단되며, 이러한 격자상수 변화는 상전이 온도 결과와도 잘 일치함을 확인할 수 있었다. 또한 $Y_2O_3$ 첨가의 경우 0.3 mol%가지는 A, B-site를 각각 치환하며 그 이상부터는 A-site 이온을 주로 치환하는 것을 격자상수 변화와 상전이 온도결과를 통해 알 수 있었으며, Rietveld 해석결과 $Y^{3+}$가 A-site 치환시 $Ba^{2＋}$와 $Ca^{2＋}$를 같은 비율로 치환한다는 것을 알 수 있었다.

• 한국세라믹학회지
• /
• 제36권2호
• /
• pp.136-144
• /
• 1999

텅스템브론즈형 고주파 유전체의 $BaORe_2O_3TiO_2$(BLT)와 $BaO(Nd({0.77}Y_{0.23})_2O_34TiO_2(B(NY)T)$의 결정구조를 Rietveld 정밀화법으로 분석하였다. 양이온은 X-선 데이터로부터, 산소이온은 중성자 데이터로부터 정밀화한 'combined법'에 의해 가장 신뢰성이 높은 결정구조분석 결과를 얻었다. Mateeva 등이 처음 제시한 결정구조의 결정학적 모순점을 해결하였다. BaORe2O34TiO2(Re=La, Nd, Y) 유전체는 $3\times2$개의 페롭스카이트 블록과 이 블록사이에 형성된 4개의 pentagon-channel로 이뤄진다. Ti-O6팔면체는 tilted 및 변형된 구조를 갖고 있고, 이에 의해 같은 z-층에 있는 Ba 및 Re 이온의 변위되어 초격자(c$\approx$ 7.6$\AA$)를 형성된다. Re 이온반경이 작은 B(NY)T의 Ti-O6 팔면체가 tilting 및 변형이 큰 것으로 나타났다. 유전상수 $\varepsilon_{\gamma}$과 온도계수 $au_\varepsilon$은 BLT의 경우 각각 $109.5, -180 ppm/^{\circ}C$였고, B(NY)T 경우 $76, +40ppm/^{\circ}C$이었다. Re 이온 크기가 작은 시료의 $\tau$$\varepsilon$이 +값을 나타내었다. 복합 페롭스카이트에서 관찰되는 $\tau_\varepsilon$과 팔면체 tilting과의 관계를 본 텅스텐 브론즈 구조재료에서 고찰하였다.

• Applied Microscopy
• /
• 제34권2호
• /
• pp.113-120
• /
• 2004

복합페로브스카이트 (1-x) $(Li_{1/2}Sm_{1/2})TiO_3-x (Na_{1/2}Sm_{1/2})TiO_3$ (LNST)의 미세구조를 TEM으로 관찰하였다. $0.0{\leq}x{\leq}0.6$ LNST에서는 A-site 양이온의 결핍에 의한 1/2 (001) 초격자 회절점을 형성하는 vacancy ordering을 갖고 있으며 이는 APB로 확인할 수 있었다. 그러나 x가 증가함에 따라 Li 이온의 양이 적어져서 vacancy ordering 을 만들기 어렵게 된다. $0.8{\leq}x{\leq}1.0$ 조성의 LNST의 미세구조에서도 APB가 관찰되었는데 이는 A-site에서 Na와 Sm 이온간의 1:1 chemical ordering에 의한 것으로 사료된다. LNST 전 조성에서 산소팔면체의 anti-phase tilting과 in-phase tilting 그리고 A-site 양이온의 antiparallel shift가 관찰되었는데, 이들은 ferroelastic domain으로 확인할 수 있었다.

• Bulletin of the Korean Chemical Society
• /
• 제21권10호
• /
• pp.1041-1043
• /
• 2000

We present the effects of temperature (between 10 K and 298 K) and of hole concentration on the frequency and intensity of characteristic phonons in polycrystalline $La_2CuO_4-related$ compounds using FT-IR spectros-copy. The influences of the concentration of carrier doped on the phonon modes are prominent in the IR spectra of $La_2CuO_4-related$ compounds. For $La_2-xSrxCuO_4({\chi}=$ 0.00, 0.03, 0.07, 0.10, and 0.15) and electrochemically (or chemically) oxidized $La_2CuO_4$, the intensities of the transverse oxygen mode around 680cm $-^1$ which cor-responds mainly to Cu-O(1) stretching vibration in the basal plane of CuO6 octahedron, are decreased and dis-appeared depending on the Sr-substitution rate and the amount of excess oxygen, while the longitudinal oxygen mode around 510 cm $-^1$ corresponding to the Cu-O(2) stretching in the basal plane of CuO6 octahedron are near-ly invariable. In particular, after two cycles of cooling-heating between 10 K and 298 K for these sample, the phonons around 680 cm $-^1$ are blue shif 13-15 cm $-^1$, while the phonons around 510 cm $-^1$ are nearly constant. The introduction of the charge carrier by doping would give rise to the small contraction of CuO6 oc-tahedron as Cu $^3+$ requires a smaller site than Cu $^2+$, which results in the shortening of the Cu-O(1) bond length and Cu-O(2) bond length with the increased La-O(2) bond length. These results in the frequency shift of the characteristic phonons. The IR spectra of $La_2Li0.5Cu0.5O_4$ which exhibits an insulator behavior despite the $Cu^3+$ of nearly 100%, corroborate our IR interpretations. The mode around 710 cm $-^1$ corresponding to Cu-O(1) stretching vibration is still strongly remained even at low temperature (10 K). Thus, we conclude that the con-duction electrons formed within $CuO_2$ planes of $La_2CuO_4-related$ superconductors screen more effectively the transverse oxygen breathing mode around 680 $cm-^1$ depending on the concentration of the doped charge carrier in $La_2CuO_4-related$ compounds, which might use as a superconductivity probe.

• Bulletin of the Korean Chemical Society
• /
• 제25권7호
• /
• pp.977-982
• /
• 2004

The reaction of $cis-[Cr([14]-decane)(OH_2)_2]^+$ ([14]-decane = rac-5,5,7,12,12,14-hexamethyl-1,4,8,11-teraazacyclotetradecane) with auxiliary ligands {$L_a$ = benzoate(bz) or chlorobenzoate(cbz)} leads to a new compound $[Cr([14]-decane)(bz)_2]ClO_4$ or $[Cr([14]-decane)(cbz)_2]ClO_4$. These complexes have been characterized by a combination of elemental analysis, conductivity, IR and Vis spectroscopy, mass spectrometry, and X-ray crystallography. The crystal structure of $[Cr([14]-decane)(cbz)_2]^+$ was determined. The complex shows a distorted octahedral coordination environment with the macrocycle adopting a folded cis-V conformation. The angle $N_{axial}-Cr-N_{axial}$ deviates by $14.5^{\circ}$ from the ideal value of $180^{\circ}$for a perfect octahedron. The bond angle cis-O-Cr-O between the Cr(III) ion and the two carboxylate oxygen atoms of the monodentate p-chlorobenzoate ligands is close to 90$^{\circ}$. The FAB mass spectra of the $cis-[Cr([14]-decane)(La)_2]ClO_4$ display peaks due to the molecular ions $[Cr([14]-decane)(bz)_2-H]^\;,\;[Cr([14]-decane)(cbz)_2-2H]^$ at m/z 578, 646, respectively.

• 한국재료학회지
• /
• 제9권1호
• /
• pp.81-85
• /
• 1999

Polarization and strain induced by unipolar electric field (P\ulcorner, S\ulcorner), those induced by bipolar electric field (P, S) and remanent polarization (P\ulcorner) were investigated in 0.9Pb(Mg\ulcornerNb\ulcorner)O$_3$-$0.1PbTiO_3$relaxor ferroelectric ceramics in the temperature range of $-50^{\circ}C$~$90^{\circ}C$. From the temperature dependence of polarization and strain, the transition from predominantly paraelectric (electrostrictive) to partially ferroelectric (piezoelectric) is visualized. Under the given temperature, the P\ulcorner/P\ulcorner is always larger than the S\ulcorner/S\ulcorner and the difference between them becomes larger ass the temperature decrease. The S\ulcorner/P\ulcorner increases as the temperature decreased below phase transition temperature. It was suggested that these experimental results might be explained with a simple rigid ion model concentrating on BO\ulcorner octahedron.

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

• 한국전기전자재료학회:학술대회논문집
• /
• 한국전기전자재료학회 1995년도 추계학술대회 논문집
• /
• pp.217-220
• /
• 1995

By substituting Cd$\^$2+/ into both A-site and B-site in PNN-PZ-PT ternary perovskite material, it is possible to determine the effects of the substitution site of Cd$\^$2+/ on sintering behavior. Sintering was performed in the temperature range from 1000$^{\circ}C$ to 1300$^{\circ}C$. The substitution site of Cd$\^$2+/ is identified by XPS spectra. Although Cd$\^$2+/ is substituted into both A-site and B-site in PNN-PZ-PT, Cd$\^$2+/ prefers A-site to B-site. The density is influenced by substitution site of Cd$\^$2+/. If Cd$\^$2+/ replaces Pv$\^$2+/, weight gain is observed during sinterig process. On the contrary, if Cd$\^$2+/ replaces Ni$\^$2+/, weight loss is promoted during sintering. From these weight changes, it is believed that Cd$\^$2+/ changes the bonding strength between B-site cation and oxygen of octahedron in perovskite structure. The changes of lattice parameters as a function of Cd$\^$2+/ content were consistent with those of the bonding strength. The densities of A-site-doped compositions were higher than those of B-site-doped composition.

• 한국결정학회지
• /
• 제10권1호
• /
• pp.88-93
• /
• 1999

The complex [Ni(L)](ClO4)2 (1) (L=2,13-bis(2-pyridylmethyl)-3,14-dimethyl-2,6,13,17-tetraazatricyclo[14,4,01.1807.12]docosane) has been synthesized and characterized by X-ray crystallography. (1) crystallizes in the triclinic, space group P, with a=10.948(2), b=10.948(2), c=14.911(4) , α=93.73(2), β=93.77(2), γ=99.29(2)o, V=1754.8(7) 3, Z=2, R1(wR2) for 5217 observed reflections of [I>2σ(I)] was 0.048(0.099). The coordination environment around nickel(II) ion shows a distorted octahedron with four secondary and tertially amines of the macrocycle and two nitrogen atoms of pyridylmethyl groups.

• 한국세라믹학회지
• /
• 제30권6호
• /
• pp.499-509
• /
• 1993

Structures of hematite(${\alpha}$-Fe2O3), Ba-ferrite(BaFe12O19) and Zn2Y(Ba2Zn2Fe12O22) were studied by powder X-ray diffraction(XRD) method. Powder XRD patterns of the ferrites were analyzed with the Rietveld method, and the final refined R-factors were RWP<0.01 and RI<0.03. The lattice parameters refined with hexagonal crystal system were a=5.0342${\AA}$, c=13.746${\AA}$ for hematite, a=5.8928${\AA}$, c=23.201${\AA}$ for Ba-ferrite, and a=5.8763${\AA}$, c=43.567${\AA}$ for Zn2Y. In the hematite, the oxygen parameter is 0.3072 and the Fe-O distances in FeO6octahedron are 1.941${\AA}$ and 2.118${\AA}$, close to the single crystal data of Blake et al.. In the Ba-ferrite, the Fe atom in oxygen trigonal bipyramid is displaced 0.155${\AA}$ away from the BaO3 mirror plane into 4e position. In the Zn2Y, 75% of Zn is located at the oxygen terahedral site in S-block.