• 한국결정성장학회지
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• 제13권2호
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• pp.56-62
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• 2003

졸-겔법을 이용하고 금속 나프테네이트를 출발원료로 사용하여 $SrTiO_3$(100), $LaA1O_3$(100) 및 MgO(100) 기판 위에 에피탁샬 $Bi_4Ti_3O_{12}$ 박막을 제조하였다. 코팅된 전구막은 $500^{\circ}C$에서 10분간 전열처리 하였고, $750^{\circ}C$에서 30분간 최종 열처리를 행하였다. 박막의 결정화도는 X-선회절 분석법 ($\theta$-2$\theta$ 스캔과 $\beta$ 스캔)으로 조사하였고, 표면 미세구조와 거칠기를 field emission-scanning electron microscope와 atomic force microscope를 이용하여 각각 분석하였다. MgO(100) 기판 위에 제조한 박막은 모든 기판 중에서 가장 낮은 결정화도와 면내 배향성을 보였다. 가장 낮은 결정화도와 배향성을 보인 MgO(100) 기판위의 박막은 침상 형태로 성장한 반면, 결정성과 배향성이 좋은 $LaA1O_3$(100)과 $SrTiO_3$(100) 기판위의 박막들은 원형의 입자 성장 형태를 보이고 있었다.

• 한국결정성장학회지
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• 제7권4호
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• pp.555-559
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• 1997

lead acetate, scandium acetate, niobium isopropoxide를 전구체로 사용한 솔-젤법으로 $Pb(Sc_{1/2}Nb_{1/2})O_3$ 분말을 제조하였다. 젤 분말에 대한 결정화 거동과 상변화가 연구되었다. 솔-젤법을 이용하여 $700^{\circ}C$에서 1시간 동안 열처리를 행하여 97 % 이상의 매우 순수한 $Pb(Sc_{1/2}Nb_{1/2})O_3$ 상을 얻을 수 있었으며 0.2 $\mu \textrm{m}$ 이하의 평균 입자 크기를 가진 매우 미세한 분말의 제조가 가능하다.

• 한국자기학회지
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• 제13권1호
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• pp.36-40
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• 2003

D $y_{x}$B $i_{3-x}$F $e_{5}$ $O_{12}$(x=0.5,1.0,1.5,2.0) 가네트 박막을 sol-gel법의 일종인 Pechini법의 이용하여 $Al_2$ $O_3$, G $d_3$G $a_{5}$ $O_{12}$ (111) 평면에 성장시켰다. 단일 조성의 D $y_{x}$B $i_{3-x}$F $e_{5}$ $O_{12}$ 박막을 얻기 위한 열처리 온도는 기판의 종류에 의존하며, 박막과 같은 구조의 G $d_3$G $a_{5}$ $O_{12}$ (111) 기판의 경우 A1$_2$ $O_3$ 기판을 사용한 경우에 비해 단일 조성을 얻기 위한 열처리 온도가 약 5$0^{\circ}C$ 감소함을 알 수 있었다. G $d_3$G $a_{5}$ $O_{12}$ (111) 기판 위에 성장된 가네트 박막의 낟알들은 대부분 기판과 같은 [111] 방향으로 정렬하며, 이 경우 박막의 자기 이력 곡선은 5000 Oe 이상에서도 포화 자기화에 도달하지 못하는 것으로 확인되었다. 이러한 현상의 원인으로 회전 자기화 과정 (rotation magnetization process)에 의한 것으로 추정하였다. Pechini 법으로 성장시킨 D $y_{x}$B $i_{3-x}$F $e_{5}$ $O_{12}$ 박막에서 단위 세포 당 최대 Bi 이온의 양은 2.0 이하임을 처음으로 확인하였고, 이는 LPE법에 의해 성장된 단결정 가네트의 경우에 알려진 최대 Bi이온의 양 2.3보다 작은 값이다.에 알려진 최대 Bi이온의 양 2.3보다 작은 값이다.은 값이다.

• 산업기술연구
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• 제20권A호
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• pp.247-256
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• 2000

Precursor gels with the composition of $xZrO_2{\cdot}(100-x)SiO_2$ systems (x=10, 20 and 30 mol%) were prepared by the sol-gel method. Kinetic parameters, such as activation energy, Avrami's exponent, n, and dimensionality crystal growth value, m, have been simultaneously calculated from the DTA data using Kissinger and Matusita equations. The crystallite size dependence on tetragonal to monoclinic transformation of $ZrO_2$ was investigated using XRD, in relation to the fracture toughness. The crystallization of tetragonal $ZrO_2$ occurred through 3-dimensional diffusion controlled growth(n=m=2) and the activation energy for crystallization was calculated using Kissinger and Matusita equations, as about $310{\sim}325{\pm}10kJ/mol$. The growth of $t-ZrO_2$, in proportion to the cube of radius, increased with increasing heating temperature and heat-treatment time. It was suggested that the diffusion of Zr4+ions by Ostwald ripening was rate-limiting process for the growth of $t-ZrO_2$ crystallite size. The fracture toughness of $xZrO_2{\cdot}(100-x)SiO_2$ systems glass ceramics increased with increasing crystallite size of $t-ZrO_2$. The fracture toughness of $30ZrO_2{\cdot}70SiO_2$ system glass ceramics heated at $1,100^{\circ}C$ for 5 h was $4.84Mpam^{1/2}$ at a critical crystaliite size of 40 nm.

• Journal of Magnetics
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• 제8권4호
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• pp.138-141
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• 2003

$Ni_{0.65}Zn_{0.35}Fe_2O_4$thin films were prepared by using a sol-gel method. Their crystallographic, dielectric and magnetic properties were investigated as a function of Cu contents by means of an X-ray diffractometer (XRD), X-ray reflectivity, LCZ meter (NF2232), a vibrating sample magnetometer (VSM), and an atomic force microscope (AFM). From typical C-V measurements for $Ni_{0.65}Zn_{0.35}Fe_2O_4$ thin films on p-type silicon substrate, the surface charge density was calculated as 1.4 ${\mu}$C/$m^2$. The dielectric constant evaluated from the capacitance at the accumulation state was 28. The high $H_{c}$ and low $M_{sat}$ at x=0.0 and 0.1 were due to the growth of the ${\alpha}$-$Fe_2O_3$ phase having antiferromagnetic properties. The rapidly decreased $H_{c}$ and increased $M_{sat}$ at x=0.2 and 0.3 can be explained that the ${\alpha}$-$Fe_2O_3$ phases have completely disappeared at x=0.3 and so, non-magnetic defects are minimized. The $M_{sat}$ was slightly decreased and the $H_{c}$ was increased above at x=0.3 because the increase of grain boundary due to smaller grain size acts as defects during magnetization process.

• The Korean Journal of Ceramics
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• 제2권2호
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• pp.102-110
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• 1996

The Mg-PSZ/$Al_2O_3$ fibers were fabricated by the sol-gel method. The added $Al_2O_3$ amounts were varied from 5 to 20 mol%. The phase transformation studies of a drawn Mg-PSZ/$Al_2O_3$ fibers were investigated by use of X-ray diffraction, IR and Raman spectroscopy. Microstructure and tensile strength of fibers were subjected to scanning electron microscopy and tensile strength tester. When $Al_2O_3$ was added to the Mg-PSZ fibers, it was found out from the analysis of XRD patterns and Raman spectra that a small amount of crystalline spinel($MgAl_2O_4$) started to form due to the reaction between $Al_2O_3$ and MgO, at $1000^{\circ}C$, and the phase transformation temperature of $ZrO_2$ crystal phase at different sintering temperatures increased. Also, the rapid grain growth with average size of 2.0 ${\mu}m$ shown in Mg-PSZ fiber at $1500^{\circ}C$ was considerably suppressed to 0.39 ${\mu}m$ by adding $Al_2O_3$ at the same temperature. When the Mg-PSZ/$Al_2O_3$ fibers containing 5 mol% $Al_2O_3$ were sintered $800^{\circ}C$ for 1 hr, average tensile strength of fibers was 0.9 GPs at diameters of 20 to 30 ${\mu}m$, but as the sintering temperatures was increased to $1000^{\circ}C$ for 1 hr, average tensile strength of fibers increased to 1.2 GPa in the same diameter range.

• 한국재료학회지
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• 제24권5호
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• pp.259-265
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• 2014

$ZrO_2$ films were coated on aluminum etching foil by the sol-gel method to apply $ZrO_2$ as a dielectric material in an aluminum(Al) electrolytic capacitor. $ZrO_2$ films annealed above $450^{\circ}C$ appeared to have a tetragonal structure. The withdrawal speed during dip-coating, and the annealing temperature, influenced crack-growth in the films. The $ZrO_2$ films annealed at $500^{\circ}C$ exhibited a dielectric constant of 33 at 1 kHz. Also, uniform $ZrO_2$ tunnels formed in Al etch-pits $1{\mu}m$ in diameter. However, $ZrO_2$ film of 100-200 nm thickness showed the withstanding voltage of 15 V, which was unsuitable for a high-voltage capacitor. In order to improve the withstanding voltage, $ZrO_2$-coated Al etching foils were anodized at 300 V. After being anodized, the $Al_2O_3$ film grew in the directions of both the Al-metal matrix and the $ZrO_2$ film, and the $ZrO_2$-coated Al foil showed a withstanding voltage of 300 V. However, the capacitance of the $ZrO_2$-coated Al foil exhibited only a small increase because the thickness of the $Al_2O_3$ film was 4-5 times thicker than that of $ZrO_2$ film.

• 한국세라믹학회지
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• 제31권12호
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• pp.1475-1482
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• 1994

Compositionally triphasic boehmite-silica-zirconia composite gels were prepared by a multiphasic sol-gel route. Phase-formation characteristics and densification behavior of the gel compacts were examined with and without $\alpha$-Al2O3 seeding. In the unseeded triphasic gels, both $\alpha$-Al2O3 and mullite crystallize simultaneously at 130$0^{\circ}C$. On the other hand, the $\alpha$-Al2O3 seeding selectively induces the formation of corundum phase ($\alpha$-Al2O3) at a significantly lower temperature (~110$0^{\circ}C$) and facilitates an epitaxial growth of $\alpha$-Al2O3 between 1100~130$0^{\circ}C$. The densification of alumina-mullite-zirconia composite (derived from the triphasic gels) was also enhanced by the $\alpha$-Al2O3 seeding, and this was attributed to the delayed crystallization of mullite in the $\alpha$-Al2O3 seeded gel.

• 한국세라믹학회지
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• 제47권4호
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• pp.343-352
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• 2010

A zirconia gel/polymer hybrid nanofiber was produced in a nonwoven fabric mode by electrospinning a sol derived from hydrolysis of zirconium butoxide with a polyvinyl butyral. Results indicated that the hydroxyl groups on the vinyl alcohol units in the backbone of the polymer were involved in the hydrolysis as well as grafting the hydrolyzed zirconium butoxide. In addition, use of acetic acid as a catalyst resulted in further hydrolysis and condensation in the sol, which led to the growth of -Zr-O-Zr- networks among the polymer chains. These networks gradually transformed into a crystalline zirconia structure upon heating. The as-spun fiber was smooth but partially wrinkled on the surface. The average fiber diameter was $690{\pm}110\;nm$. The fiber exhibited a strong but broad blue photoluminescence with its maximum intensity at a wavelength of ~410 nm at room temperature. When the fiber was heat-treated at $400^{\circ}C$, the fiber diameter shrunk to $250{\pm}60\;nm$. Nanocrystals which belonged to a tetragonal zirconia phase and were ~5 nm in size appeared. A strong white photoluminescence was observed in this fiber. This suggests that oxygen or carbon defects associated with the formation of the nanocrystals play a role in generating the photoluminescence. Further heating to $800^{\circ}C$ resulted in a monoclinic phase beginning to form In the heat-treated fibers, coloring occurred but varied depending on the heating temperature. Crystallization, coloring, and phase transition to the monoclinic structure influenced the photoluminescence. At $600^{\circ}C$, the fiber appeared to be fully crystallized to a tetragonal zirconia phase.

• 대한화학회지
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• 제61권1호
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• pp.29-33
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• 2017

Formation of Au particles in nonstoichiometric $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$) oxide from aniline + hydrochloric acid mixtures and chloroauric acid in the ratios 30 : 1; 60 : 1; 90 : 1 (S1-S3) by volume and 0.01 mol of copper acetate, $Cu(OCOCH_3)_2.H_2O$, in each case is performed by sol-gel growth. Powder x-ray diffraction (XRD) results show Au particles are dispersed in tetragonal nonstoichiometric dicopper (I) dicopper (II) oxides, $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$). Average crystallite sizes of Au particles determined using Scherrer equation are found to be in the approximate ranges ${\sim}85-140{\AA}$, ${\sim}85-150{\AA}$ and ${\sim}80-150{\AA}$ in S1-S3, respectively which indicate the formation of Au nano-micro size particles in $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$) oxides. Hysteresis behaviour at 300 K having low loop areas and magnetic susceptibility values ${\sim}5.835{\times}10^{-6}-9.889{\times}10^{-6}emu/gG$ in S1-S3 show weakly ferromagnetic nature of the samples. Broad and isotropic electron paramagnetic resonance (EPR) lineshapes of S1-S4 at 300, 77 and 8 K having $g_{iso}$-values ${\sim}2.053{\pm}0.008-2.304{\pm}0.008$ show rapid spin-lattice relaxation process in magnetic $Cu^{2+}$ ($3d^9$) sites as well as delocalized electrons in Au ($6s^1$) nano-micro size particles in the $Cu_{2-x}{^I}Cu{_2}^{II}O_{3-{\delta}}$ ($x{\approx}0.20$; ${\delta}{\approx}0.10$) oxides. Broad and weak UV-Vis diffuse reflectance optical absorption band ~725 nm is assigned to $^2B_{1g}{\rightarrow}^2A_{1g}$ transitions, and the weak band ~470 nm is due to $^2B_{1g}{\rightarrow}^2E_g$ transitions from the ground state $^2B_{1g}$(${\mid}d_{x^2-y^2}$>) of $Cu^{2+}$ ($3d^9$) ions in octahedral coordination having tetragonal distortion.