• 한국세라믹학회지
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• 제27권8호
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• pp.991-1003
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• 1990

A precipitation method, one of the most effective liquid phase reaction methods, was adopted in order to prepare high-tech Al2O3/ZrO2 composite ceramics. Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent, various types of metal hydroxides were obtained by single precipitation(series A) and co-precipitation(series B) method at the pH condition between 7 and 11. Fine Al2O3-ZrO2 powders were prepared at optimum calcination condition and the effects of ZrO2 on microstructures and mechanical properties of Al2O3 were investigated. The composition of Al2O3/ZrO2 composites wax fixed as Al2O3-15 v/o ZrO2(＋3m/o Y2O3). ZrO2 limited the grain growth of Al2O3 and increased grain size homogeneity of Al2O3 more effectively than MgO.Flexural strength values in Al2O3 and Al2O3/ZrO2 composites were 340-430 MPa and 540-820 MPa, respectively, and the effect of strength improvement showed 20-50% by adding ZrO2 to Al2O3. Fracture toughness of Al2O3/ZrO2 composites was improved by stress-induced phase transformation of tetragonal ZrO2 and toughening effect by microcrack was not observed. Also, ZrO2 particles located at Al2O3 grain junction contributed to toughening, while spherical ZrO2 particles located within Al2O3 grain did not contribute to toughening. Weibull moduli of Al2O3 ceramics and Al2O3/ZrO2 composites of series A and series B were 4.34, 5.17 and 9.06, respectively. Above 0.5 of failure probability, strength values in Al2O3 ceramics and Al2O3/ZrO3 composites of series A and series B were above 400 MPa, 700 MPa and 650 MPa, respectively.

• Advances in nano research
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• 제13권4호
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• pp.313-323
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• 2022

The microstructure and mechanical properties of Cr-Ni steel and Cr-Ni steel-matrix nanocomposites reinforced with nano-ZrO₂ particles were investigated in this study. Cr-Ni steel and Cr-Ni/ZrO₂ nanocomposites were produced using a combination of high-energy ball milling, pressing, and sintering processes. The microstructures of the specimens were analyzed using EDX and XRD. Compression and hardness tests were performed to determine the mechanical properties of the specimens. Nano-ZrO₂ particles were effective in preventing chrome carbide precipitate at the grain boundaries. While t-ZrO₂ was detected in Cr-Ni/ZrO₂ nanocomposites, m-ZrO₂ could not be found. Few α'-martensite and deformation bands were formed in the microstructures of Cr-Ni/ZrO₂ nanocomposites. Although nano-ZrO₂ particles had a negligible impact on the strength improvement provided by deformation-induced plasticity mechanisms in Cr-Ni/ZrO₂ nanocomposites, the mechanical properties of Cr-Ni steel were significantly improved by using nano-ZrO₂ particles. The hardness and compressive strength of Cr-Ni/ZrO₂ nanocomposite were higher than those of Cr-Ni steel and enhanced as the weight fraction of nano-ZrO₂ particles increased. Cr-Ni/ZrO₂ nanocomposite with 5wt.% nano-ZrO₂ particles had almost twofold the hardness and compressive strength of Cr-Ni steel. The nano-ZrO₂ particles were considerably more effective on particle-strengthening mechanisms than deformation-induced strengthening mechanisms in Cr-Ni/ZrO₂ nanocomposites.

• 한국세라믹학회지
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• 제28권5호
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• pp.422-428
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• 1991

The reaction sintering of Al2O3-ZrO2-Nb composite has been investigated using Al2O3, and ZrAl2 powders. Two kinds of specimens, 78.3Al2O3-14.0Nb2O5-7.7ZrAl2 in wt.% (AZN-5) and 72.3Al2O3-13.8Nb2O5-7.5ZrAl2-6.4ZrO2(AZN-10), were prepared. Powder compacts were sintered at various temperatures between 1$600^{\circ}C$ and 1$700^{\circ}C$ for 30 min in Ar. DTA and X-ray analysis have showen that a reaction between Nb2O5 and ZrAl2 started at 149$0^{\circ}C$ to form Al2O3, ZrO2, and Nb. The sintered density increased with the sintering temperature. AZN-10 specimen showed higher density than AZN-5 specimen for almost all the experimental conditions. Al2O3-ZrO2-Nb composite hot pressed after reaction sintering showed higher toughness and lower hardness than hot pressed Al2O3-ZrO2. The crack propagated through many metallic Nb particles which showed plastic deformation, and this is the cause of the increase in toughness of Al2O3-ZrO2-Nb composite over Al2O3-ZrO2.

• 한국세라믹학회지
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• 제36권7호
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• pp.734-741
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• 1999

Al2O3와 t-ZrO2 분말의 압분체를 공기중 150$0^{\circ}C$ 및 1$600^{\circ}C$에서 2시간 소결하여 제조된 입자복합체의 미세구조와 기계적 성질을 조사하였다. 소수의 미세한 구상의 ZrO2입자는 Al2O3의 입내에 존재하였으나 대분분은 입계에 존재하여 Al2O3의 입계를 고정시키는 것이 가능하였고, 따라서 Al2O3의 입성장을 둔화시켰다. 소결할 동안 입계 ZrO2 입자의 조대회는 응집된 ZrO2 입자내에서의 입계의 소멸과 Al2P3 입계의 이동에 의해서 끌어 당겨진 ZrO2 입자의 합체(coalescence)에 의해서 일어날 수 있었다. ZrO2의 첨가에 의한 Al2O3의 기계적 성질의 변화는 기지상인 Al2O3의 미세구조와 분산된 ZrO2 입자의 크기와 구조에 의존하였다.

• 한국세라믹학회지
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• 제29권10호
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• pp.797-805
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• 1992

Al2O3-20 wt% ZrO2 composite powders to be used as the starting materials of the Al2O3/ZrO2-Spinel composite system were prepared by the use of the emulsion-hot kerosene drying method. The crystalline phase of ZrO2 in the synthesized Al2O3-ZrO2 composite powders was 100% tetragonal but the small amount of t-ZrO2 was transformed into m-ZrO2 after crushing. The hardness, fracture toughness, and flexural strength of the composite, which was sintered at 1650$^{\circ}C$ for 4 hrs after calcining at 1100$^{\circ}C$ for 2 hrs and had the relative density of 99%, were 15.7 GPa, 4.97 MN/m3/2, and 390 MPa, respectively. The fracture form in the sintered composites was found to be the intergranular fracture.

• E2M - 전기 전자와 첨단 소재
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• 제16권9호
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• pp.64.2-65
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• 2003

A 4 nm layer of ZrOx (targeted x-2) was deposited on an interfacial layer(IL) of native oxide (SiO, t∼1.2 nm) surface on 200 mm Si wafers by a manufacturable atomic layer chemical vapor deposition technique at 30$0^{\circ}C$. Some as-deposited layers were subjected to a post-deposition, rapid thermal annealing at $700^{\circ}C$ for 5 min in flowing oxygen at atmospheric pressure. The experimental x-ray diffraction, x-ray photoelectron spectroscopy, high-resolution transmission electron microscopy, and high-resolution parallel electron energy loss spectroscopy results showed that a multiphase and heterogeneous structure evolved, which we call the Zr-O/IL/Si stack. The as-deposited Zr-O layer was amorphous $ZrO_2$-rich Zr silicate containing about 15% by volume of embedded $ZrO_2$ nanocrystals, which transformed to a glass nanoceramic (with over 90% by volume of predominantly tetragonal-$ZrO_2$(t-$ZrO_2$) and monoclinic-$ZrO_2$(m-$ZrO_2$) nanocrystals) upon annealing. The formation of disordered amorphous regions within some of the nanocrystals, as well as crystalline regions with defects, probably gave rise to lattice strains and deformations. The interfacial layer (IL) was partitioned into an upper Si $o_2$-rich Zr silicate and the lower $SiO_{x}$. The latter was sub-toichiometric and the average oxidation state increased from Si0.86$^{＋}$ in $SiO_{0.43}$ (as-deposited) to Si1.32$^{＋}$ in $SiO_{0.66}$ (annealed). This high oxygen deficiency in $SiO_{x}$ indicative of the low mobility of oxidizing specie in the Zr-O layer. The stacks were characterized for their dielectric properties in the Pt/{Zr-O/IL}/Si metal oxide-semiconductor capacitor(MOSCAP) configuration. The measured equivalent oxide thickness (EOT) was not consistent with the calculated EOT using a bilayer model of $ZrO_2$ and $SiO_2$, and the capacitance in accumulation (and therefore, EOT and kZr-O) was frequency dispersive, trends well documented in literature. This behavior is qualitatively explained in terms of the multi-layer nanostructure and nanochemistry that evolves.ves.ves.

• 한국세라믹학회지
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• 제37권1호
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• pp.50-56
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• 2000

Precursor gels with the composition of xZrO2·(100-x)SiO2 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 of tetragonal to monoclinic transformation of ZrO2 was investigated using XRD, in relation to the fracture toughness. The crystallization of tetragonal ZrO2 occurred through 3-dimensional diffusiion controlled growth(n=m=2) and the activation energy for crystallization was calculated using Kissinger and Matusita equations, as about 310∼325±10kJ/mol. The growth of t-ZrO2, in proportion to the cube of radius, increased with increasing heating temperature and hteat-treatment time. It was suggested that the diffusion of Zr4+ ions by Ostwald ripening was rate-limiting process for thegrowth of t-ZrO2 crystallite size. The fracture toughness of xZrO2·(100-x)SiO2 systems glass ceramics increased with increasing crystallite size of t-ZrO2. The fracture toughness of 30ZrO2·70SiO2 system glass ceramics heated at 1,100℃ for 5h was 4.84 MPam1/2 at a critical crystaliite size of 40 nm.

• 한국세라믹학회지
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• 제41권4호
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• pp.284-288
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• 2004

Al$_2$O$_3$/ZrO$_2$복합체의 기계적 성질 향상을 위하여 분산되는 ZrO$_2$상을 Zr-Y-polyester의 고분자화(polyesterization) 공정(Pechin법)을 이용하여 알루미나 기지 중에 초미립으로 균질하게 분산시키기 위한 방안을 고찰하여 보았다. 일반적으로 공침법에 의해 제조되는 $Al_2$O$_3$/ZrO$_2$ 복합체의 경우 초기 ZrO$_2$입자의 크기가 매우 작아도 알루미나 내에 분산되는 ZrO$_2$입자가 소결시에 비교적 빠르게 성장 및 입자간의 응집이 발생하게 되며 이로 인해 분산의 불균일을 유발하여 미세하고 균질한 복합체를 얻기가 힘들다. 따라서 상용 이소결성 $\alpha$-Al$_2$O$_3$분말(Sumitomo.AES-11(0.5$mu extrm{m}$))에 ZrO(NO$_3$)$_2$와 Y(NO$_3$)$_3$를 citric acid/ethylene glycol과 혼합한 polyesterization시켜 $\alpha$-Al$_2$O$_3$입자 표면에 미세하고 균질하게 코팅 형태로 부착되도록 하였다. 이를 90$0^{\circ}C$에서 하소한 후 1450∼1$600^{\circ}C$의 온도에서 소결하여 미세한 ZrO$_2$입자가 매우 균질하게 분산된 $Al_2$O$_3$/ZrO$_2$ 복합체를 제조하였으며 이의 기계적 성질을 관찰하였다.

• 한국세라믹학회지
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• 제27권3호
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• pp.361-368
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• 1990

The properties of the powder of ZrO2＋3m/o Y2O3 system prepared by co-precipitation method at the pH values of 7, 9, 10 and 11 were investigated. ZrOCl2.8H2O and YCl3.6H2O were used as starting materials and NH4OH as a precipitation agent. Zirconium hydroxide near by Zr(OH)4 structure showed more excellent crystallinity and lower formation temperature of tetragonal ZrO2. In the range of this study, cubic ZrO2 was not formed and stability of tetragonal ZrO2 prepared in the conditiion of pH 7 was most excellent. Average particle sizes and specific surface areas of tetragonal ZrO2 powders, prepared as calcining amorphous zirconium hydroxides at $600^{\circ}C$ for 1h, were 0.6-0.8${\mu}{\textrm}{m}$ and 45-70$m^2$/g, respectively.

• 한국세라믹학회지
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• 제26권3호
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• pp.423-437
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• 1989

Al2O3/ZrO2 composites were prepared by precipitation method using Al2(SO4)3.18H2O, ZrOCl2.8H2O and YCl3.6H2O as starting materials and NH4OH as a precipitation agent. Al2O3/ZrO2 composites(series A) were prepared by mixing Al2O3 powder obtained by single precipitation method with ZrO2(＋3m/o Y2O3) powder obtained by co-predipitation method. Al2O3/ZrO2 composites (series B) were prepared by co-precipitation method using the three starting materials. In all cases, the composition was controlled as Al2O3-15v/o ZrO2(＋3m/o Y2O3). The composites of series A showed higher final relative densities than those of series B and tetagonal ZrO2 in all cases was retained to about 95% at room temperature. ZrO2 particles were coalesced more rapidly in grain boundary of Al2O3 than within Al2O3 grain. ZrO2 particles were located at 3-and 4-grain junction of Al2O3 and limited the grain growth of Al2O3. It was observed that MgO contributed to densification of Al2O3 but limited grain growth of Al2O3 by MgO was not remarkable. In all Al2O3/ZrO2 composites, exaggerated grain growth of Al2O3 was not observed and Al2O3/ZrO2 composites were found to have homogeneous microstructures.