• Journal of the Korean Ceramic Society
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• v.33 no.1
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• pp.1-6
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• 1996

A single phase Ba2(Ti8,472Zr0.528)O20 was prepared by the oxalate method from aqueous solution of BaCl2 TiCl4 and ZrOCl2. The structure ananlysis has been carried out by Rietveld analysis method at room temperature. Powder X-ray data of Ba2(Ti8,472Zr0.528)O20 was indexed with the triclinic lattice(a=7.4587 $\AA$ b=14.0672 $\AA$, c=13.3327 $\AA$, $\alpha$=89.87, $\beta$=79.45 ${\gamma}$=84.46) The R (Residual) values of structure refinement were in a range between 10.00 and 8.00 This analysis proved that the added Zr occupied Ti sites in th structure of Ba2Ti9O20. Ba2(Ti8,472Zr0.528)O20 has excellent dielectric properties(dielectric constant K=40.49 at 5.42 GHz Q=4621) so that it can be used as good microwave dielectric materials.

• Journal of the Korean Ceramic Society
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• v.22 no.1
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• pp.11-18
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• 1985

The effect of stress induced phase transformation on $Al_2 O_3$ matrix dispersed with $ZrO_2-Y_2O_3$ has been studied. In order to determinate the mechanical properties three $Al_2O_3-ZrO_2$ composite series containing 1, 3 and 5 mole% $Y_2O_3$ were prepared. The starting materials were $Al_2O_3$ and $ZrO_2-Y_2O_3$ which was prepared from the aqueous solution of high purity $YCl_3$.$6H_2O$ and $ZrOCl_2$.$8H_2O$. Powder mixtures of $Al_2O_3-ZrO_2$ containing $Y_2O_3$ have been prepared by ball-milling with methanol and the samples were formed by isostatic press and sintered at 150$0^{\circ}C$ for 2hrs. After sintering. the specimens were polished for mechanical determination. The relative density of sintered specimens were also measured. It was found that the addition of 1, 3mole% to {{{{ { ZrO}_{2 } }} allowed full retention of the tetragonal phase in $Al_2O_3-ZrO_2$ but partially stabilized zirconia (PSZ) was produced by additions of 5 mole% $Y_2O_3$.The critical stress-intensity factor KIc of $A_2O_3-ZrO_2$ (containing 1 mole% $Y_2O_3$) composite materials increased with increasing $ZrO_2$ content, The maximum value of KIC=7Mn/$m^3$/2 at 20 mole% $ZrO_2$ exhibited about twice that of the $Al_2 O_3$ The modulus of rupture exhibited a trend similiar to KIC The maximum value of MOR was 580MN/m2. As the amount of Y2O3 increase it was observed that the maximum of KIC and MOR decreased : Additions of 3 mole% $Al_2O_3$ $Y_2O_3$ allowed the maximum of KIC 6MN/$m^3$/2 MOR 540MN/$m^2$ at 15 mole% $ZrO_2$ additions of 5 mole% $Y_2O_3$ allowed the maximum of KIC 5MN/$m^3$/2 MOR 410MN/$m^2$ at 10 mole% $ZrO_2$.

• Journal of the Korean Ceramic Society
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• v.49 no.5
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• pp.454-460
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• 2012

The nano-sized zirconia powders were synthesized in an impregnation method using pulp and $ZrOCl_2{\cdot}8H_2O$ as an initial material. The synthesized powders were characterized by XRD and FE-SEM. The particle size of the powder was controlled by preparation conditions, such as drying temperature and time. As a result of the various drying and calcination conditions, 30~50 nm sized homogeneous zirconia particles were obtained at $800^{\circ}C$ for 1 h. Crystallization and the rapid growth of particles were accelerated with increasing calcination temperature and time. Tetragonal phase generated below $800^{\circ}C$ were transferred to monoclinic phase with increasing calcination temperature and time. Moreover, above $800^{\circ}C$, heat treatment time had very large influence on the particle growth, and the change of drying condition also had large influence on the growth of a crystal.

• Journal of the Korean Ceramic Society
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• v.23 no.4
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• pp.78-84
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• 1986

Zirconium acetate solution which was obtained from $ZrOCl_2$.$8H_2O$ was condensed polymerized and drawn to fibers by pulling method. Drawn gel fibers fired at 130$0^{\circ}C$ were short porous and mechanically weak. But addition of CaO about 13m/o caused the fibers to have the cubic structure and relatively dense microstructure. In order to clarify the condition for the synthesis of zirconia fibers viscosity measurement DTA-TG analysis X-ray diffraction infrared spectroscopy, SEM and specific surface area were studied.

• Journal of the Korean Ceramic Society
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• v.28 no.5
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• pp.399-405
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• 1991

Mullite-PSZ powders were synthesized by the sol-gel process using Al(sec-OC4H9)3, Si(OC2H5)4, ZrOCl2$.$8H2O and YCl3 solution and the characteristics of synthesized powders were studied. The sinterability and mechanical properties of powder compacts sintered at 1670$^{\circ}C$ for 4hr were also studied for various PSZ contents. ${\gamma}$-Al2O3(Al-Si spinel) formed at 980$^{\circ}C$ from amorphous dried gel, and mullite as well as ZrO2 formed above 1200$^{\circ}C$. At the room temperature, ZrO2 was a mixture of tetragonal and monoclinic phases. The specimens were densified to 97∼98% except the specimen containing 25 vol% PSZ which showed the relative density of 94%. The K1c value increased with the PSZ content and showed a maximum value of 4.1 MN/m3/2 at 25 vol% PSZ; this value was about 50% higher than that of the mullite without PSZ. Flexural strength had a maximum value of 280 Mn/㎡ at 20 vol% PSZ. In contrast, at 25 vol%, the flexural strength was even lower than that of the mullite possibly due to higher porosity of 6%.

• Proceedings of the Materials Research Society of Korea Conference
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• 2003.03a
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• pp.224-224
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• 2003

광통신을 위한 구성 요소는 빛을 발생시키는 발광소자, 빛을 검출하는 수광소자 그리고 광신호를 처리하는 광신호처리 소자로 구성된다. 이때 각 소자간 광전송과 광소자에 의한 광 신호 처리 과정에서 광전송 손실이 심각하게 일어나 광정보를 상실하게 되므로 각 요소별로 광신호 증폭이 반드시 필요하다. 뿐만 아니라 완전 광화에 의한 초고속/대용량 광통신망의 구축에는 저가이며, 광집적화가 가능한 광도파로형 광증폭기가 요구되고 있다. 짧은 거리에 높은 증폭 효율을 얻기 위한 광도파로형 광증폭기를 구현하기 위해서는 광통신 파장대인 1.55$\mu\textrm{m}$ 대역의 증폭이 가능한 Er 이온을 고농도로 도핑 할 필요가 있다. 그러나 Er 이온을 단순히 고농도로 첨가하면 Er-Er 간 뭉침 현상에 의해 더 이상의 증폭이 어렵게 된다. 본 연구에서는 이러한 문제를 해결하면서 스핀 코팅이 가능하여 저가 공정이 가능한 유/무기 졸-겔 재료 내에 Er 이온을 제어된 방법으로 첨가하고 그 결합 환경을 FT-IR 및 $^{17}$ O-NMR로 분석하였다. 유/무기 졸겔 재료 제조를 위하여 먼저 MPTS(MethAcryoxyPropylTrimethoxySilane)를 부분 가수분해한 후 ZrOCl$_2$.8$_2$O (Zirconyl Chloride Octahydrate) 와 ErCl$_3$. 6$H_2O$ (Erbium(III) Chloride Hexahydrate)를 순차적으로 결합시키고, Zr/MPTS 및 Zr/Er의 첨가비에 따른 발광 특성을 PL(photoluminescence) 스팩트럼으로 분석하여 Er 이온의 주위 결합 환경이 PL에 미치는 영향을 조사하였다. 또한 Si 기판에 코팅한 Er이 도핑된 유/무기 하이브리드 졸-겔 코팅막의 굴절율 등 광도파로 재료로서의 특성도 프리즘 커플러 등을 이용하여 조사하였다.

• Proceedings of the Korea Association of Crystal Growth Conference
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• 1996.06b
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• pp.55-85
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• 1996

지르코니아 분말은 ZrO2 결정상이 온도변화에 따라 부피변화를 수반하는 상전이변태를 나타낸다. 단사정 ZrO2가 110$0^{\circ}C$에서는 정방정으로, 2$700^{\circ}C$ 내외에서는 입방정으로 결정구조가 가역적으로 변한다. 이 ZrO2에 금속산화물을 고용시키면 형석 (CaF2:Florite)형의 입방정 결정구조가 실온에서도 안정하게 존재하게 된다. 안정화제 산화물은 caO, MgO등 2가 산화물외에 3가 또는 4가의 금속산화물로서 Sc2O3, Y2O3, Sm2O3, Nd2O3, Gd2O3, Y2O3, CeO2 등이며 이들은 금속이온의 원자가가 변하기 쉬운 희토류 산화물이다. 안정화 지르코니아는 형석형 결정구조이며 결정화학적으로 보면 금속양이온이 산소이온에 대해서 정육면체형의 8배위를 하고 있다. 이때 이온반경비(양이온/음이온)에 따라 Zr+4자리와 O-2자리의 격자위치와 모양이 형성되므로 비틀어진 정육면체구조이건 이상적인 정육면체 형석구조를 이룬다. 이는 지르코니아의 결정상의 2상-3상인 부분안정화 지르코니아다결정체(PSZ : partially stabilized zirconia)이거나 단일상-2상인 정방정 지르코니아다결정체(TZP : tetragonal zirconia polycrystal)의 결정구조를 가지는데 기인한다. PSZ는 주로 MgO, CaO를 안정화제로 고용시켜 입방정 영역에서 소결하고 이를 다시 입방정과 정방정의 상 영역에서 열처리하여 입방정 입자내부에 정방정을 석출 형성시킨 것이며 TZP는 Y2O3 및 CeO2를 고용시켜 PSZ와 다르게 일반적인 상압소결한 정방정 결정상의 미립자이다. 산화지르코늄 분말은 지르콘사에서 열분해시킨 지르코늄소결.융해괴(caustic fusion clinker)를 산처리하여얻어진 지르코늄산용액(zirconyl acid solution : cloride, sulfide, nitride 등)으로부터 제조된다. 고순도 산화지르코늄은 용액 결정석출법에 의해 ZrOCl2.8H2O, 5ZrO2.3SO3.15H2O, ZrO(NO3)2.xH2O 등의 지르코늄 수화물만을 재결정화시킨 것으로부터 얻을 수 있으며 이 지르코늄염 수용액으로부터 입자미세구조를 효과적으로 제어하여 산화지르코늄 및 안정화 지르코니아 분말제조가 가능하다. 안정화 지르코니아 분말은 ZrO2와 안정화산화물의 고용을위하여 가열처리를 필요로 하며 일정온도에서 최적상태로 숙성하므로서 2가지 상(phase) 이상의 고용체를 가지게 된다. 안정화 지르코니아 분말은 고용처리온도를 낮추고 효과적으로 생성시키기 위해서는 지르코늄 및 안정화제염을 혼합하고 습식 직접합성하여 저온에서 고용체의 합해진상 영역을 생성시키는 것이다. 이는 지르코니아 원료분말의 미세구조를 제어하므로서 가능하며 이때 화학성분조성과 크기형태가 균일하게 분포된 입자분말을 얻을 수 있다.

• Journal of Powder Materials
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• v.14 no.5
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• pp.309-314
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• 2007

Zirconia powders with nano size pores and high specific surface areas were synthesized via aqueous precipitation and hydrothermal synthetic method using $ZrOCl_28H_2O$ and $NH_4OH$ under pH=11 and ambient condition. By this reaction. zirconia hydrate $(ZrO_x(OH)_{4-2x})$ was primarily synthesized and the obtained zirconia hydrate was heat treated hydrothermally using an autoclave at various temperatures under pH=11. X-ray diffraction, Scanning electron microscopy, Energy dispersive X-ray spectroscopy, FT-IR, Raman, Particle size analysis, DTA-TG, and BET techniques were used for the characterization of the powder. The synthesized zirconia showed an amorphous phase, however, the phase was transformed to the crystalline state during the hydrothermal process. The observed crystalline phase above $160^{\circ}C$ was a mixed phase of monoclinic and tetragonal zirconia. By the BET analysis, it was found that the specific surface area was ranged in $126{\sim}276m^2/g$ and the zirconia had the cylindrical shaped pores with average diameter of $2{\sim}7nm$.

• Proceedings of the KIEE Conference
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• 1989.11a
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• pp.101-101
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• 1989

Multilayer films of inorganic analogues of Langmuir-Blodgett films have been prepared on silicon and gold substrates and characterized by ellipsometry, XPS, FT-IRRS, and electrochemical measurements. The deposition technique requires first covalent attachment or adsorption of a phosphonic acid anchoring agent; $HO(CH_3)(CH_2)_2Si(CH_2)_3PO_3H_2$ and $[-S(CH_2)_4PO_3H_2]_2$ were used with Si and Au, respectively. The functionalized substrates are exposed alternately to aqueous $ZrOCl_2$ and l,l0-decanediylbis(phosphonic acid) solutions to yield multilayer films. Surface-sensitive probes show that the films are compact and grow in an oriented fashion suggestive of good structural order.

• Journal of the Korean Chemical Society
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• v.58 no.1
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• pp.44-48
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• 2014

Catalytic performance of Lewis acids have been investigated in the synthesis of 1,2,3,4-tetrahydroquinolines via cyclocondensation reaction of aniline derivatives with cyclic enol ethers such as 3,4-dihydro-2H-pyran and 2,3-dihydrofuran. The catalytic activity of various of these catalysts in different solvents was compared with other classical catalysts such as KSF clay (1.5 g), $InCl_3$ (10-20 mol%), $ZrOCl_2$ (10 mol%), $Sc(OTf)_3$ (3 mol%), PANI-$InCl_3$ (10 mol%), $I_2$ (20 mol%), $InCl_3$ (5 mol%), 4-npa (25 mol%) and Cellulose-$SO_3H$ (0.03 g).