There is increasing interest in zirconia as a dental material due to its aesthetics, as well as the exceptionally high fracture toughness and high strength that are on offer when it is alloyed with certain oxides like yttria. In recent years, many solution based chemical synthesis methods have been reported for synthesis of zirconia, of which the sol-gel method is considered to be best. Here, we synthesize zirconia by a sol gel assisted precipitation method using either PEG or PVA as a stabilizing agent. Zirconia sol is first synthesized using the hydrothermal method. We used NaOH as the precipitating agent in this method because it is easy to remove from the final solution. Zirconium and yttrium salts are used as precursors and PEG or PVA are used as stabilizers to separate the metal ions. The resulting amorphous zirconia powder is calcined at 900˚C for 2 h to get crystallized zirconia. XRD analysis confirmed the partially stabilized zirconia synthesis in all the synthesized powders. SEM was taken to check the morphology of the powder synthesized using either PEG or PVA as a stabilizing agent and finally the transparency was calculated. The results confirmed that the powder synthesized with 10 % PVA as the stabilizing agent had highest percentage of transparency among all the synthesized powder.

The goal of this investigation was to produce a zirconia-family black ceramics that has enhanced functionality andreliability. Color zirconia ceramics have been produced by adding pigments. Pigments cause structural defects within zirconiaand result in a drop in physical properties. Using environmentally friendly rice husk, we produced a black zirconia that is freeof structural defects. In optimal firing conditions for black zirconia the calcining temperatures of the molding product arechanged from 400oC to 1200oC, and the firing temperatures are changed from 1400oC to 1600oC. Color of testing the specimenswas analyzed using Ultraviolet (UV) spectroscopy. Scanning Electron Microscope (SEM), EDAX (EDX), and Fourier transforminfrared spectroscopy (FT-IR) analyses were carried out in order to examine impregnation properties and crystal phases.Universial Test Machine (UTM) was used to measure the flexual strength as well as the compressive strength. Fromexperimental results, it was found that in optimal firing conditions the sample was calcined from 1000oC to 1500oC. Commissioninternationalde I’Edairage (CIE) values of manufactured black zirconia color were L*=29.73, a*=0.23, b*=−2.68. Thebending strength was 918 MPa and the compressive strength was 2676 MPa. These strength values are similar to typicalstrength values of zirconia, which confirms that carbon impregnation did not influence physical properties.

In this study, a novel-processing route for fabricating microcellular zirconia ceramics has been developed. The proposed strategy for making the microcellula zirconia ceramics involved hollow microspheres as pore former. Compared to conventional dense microspheres pore former, well-defined pore structured zirconia ceramics were successfully fabricated. Effects of hollow microsphere content and sintering temperature on microstructure, porosity, pore distribution, and strength were investigated in the processing of microcellular zirconia ceramics.

A diamond-like carbon (DLC) film deposited on a WC disk was investigated to improve disk wear resistance for injection molding of zirconia optical ferrule. The deposition of DLC films was performed using the filtered vacuum arc ion plating (FV-AIP) system with a graphite target. The coating processing was controlled with different deposition times and the other conditions for coating, such as input power, working pressure, substrate temperature, gas flow, and bias voltage, were fixed. The coating layers of DLC were characterized using FE-SEM, AFM, and Raman spectrometry; the mechanical properties were investigated with a scratch tester and a nano-indenter. The friction coefficient of the DLC coated on the WC was obtained using a pin-on-disk, according to the ASTM G163-99. The thickness of DLC films coated for 20 min. and 60 min. was about 750 nm and 300 nm, respectively. The surface roughness of DLC films coated for 60 min. was 5.9 nm. The Raman spectrum revealed that the G peak of DLC film was composed of sp3 amorphous carbon bonds. The critical load (Lc) of DLC film obtained with the scratch tester was 14.6 N. The hardness and elastic modulus of DLC measured with the nano-indenter were 36.9 GPa and 585.5 GPa, respectively. The friction coefficient of DLC coated on WC decreased from 0.2 to 0.01. The wear property of DLC coated on WC was enhanced by a factor of 20.

IS (요오드-황)프로세스의 HI 분해반응 공정에서의 적용을 목적으로 지르코니아 코팅 지지체를 이용하여 CVD법에 의해 수소분리막을 제작하였으며, 분리막으로서의 가능성을 평가하였다. 제작한 막의 형상 및 Si의 분포를 파악하기 위해 SEM 및 EPMA를 이용하여 분석하였다. 지르코니아를 코팅한 지지체를 이용하여 제작한 막에 Zr-Si-O층이 존재한다는 것을 알 수 있었다. 제작한 막의 수소와 질소가스의 단일 성분 투과속도를 300~600℃에서 측정하였다. 600℃에서 Z-1막에서의 수소투과속도는 1 × 10 -7 mol·Pa -1·m -2·s -1를 나타냈다. 질소에 대한 수소의 선택성은 Z-1 막에서 5.0, Z-2막에서 5.75를 나타냈다.

The usual ceramic process of mixing and milling in state of oxides ZrO2 and CeO2 was adopted in this study in a wet process to manufacture Ce-TZP. CeO2-ZrO2 ceramics containing 8~20 mol% CeO2 were made by heat treatment at 1250~1500˚C for 5hr. The maximum dispersion point of every slurry manufactured with a mixture of ZrO2 and CeO2 was neat at pH10. A stable slurry with average particle size of 90 nm can be manufactured when it is dispersed with the use of ammonia water and polycarboxylic acid ammonium. The sintered Ce-TZP ceramics manufactured with the addition of CeO2 in a concentration of less than 10 mol% progressed to the fracture of the specimen due to the existence of a monoclinic phase of more than 30% at room temperature. More than 99% of the tetragonal phase was created for the sintered body with the addition of CeO2 beyond 18 mol%, but the degradation of the mechanical properties on the entire specimen was brought about due to the CeO2 existing in a percentage above 3%. Consequently, the optimal Ce-TZP level combined in the oxide state was identified to be 16 mol% of CeO2 contents.

Yttria stabilized zirconia single crystals show plastic deformation at high temperatures by activating dislocations. The plastic deformation is highly dependent on crystallographic orientation. When the samples were deformed at different orientations, stress-strain curves changed by operating different slip systems. The strength of samples was also highly dependent on crystallographic orientation, i.e., samples without yield drop showed higher strength than that of samples exhibiting yield drop. The slip systems in the sample deformed along<112>,<111> and<001> agreed with the theoretical values of the plastic deformation, following Schmid's Law. Dislocations play a major role in the plastic deformation of this crystal. At the early stages of plastic deformation, all samples exhibited dislocation dipoles and, in the later stages, dislocation interactions occurred by forming nodes, tangles and networks. In this study, three different orientations, [11-2], [111] and [001] were employed to explain the plastic deformation behavior. A microstructural analysis was performed to elucidate the mechanism of the plastic behavior of this crystal.

Nano-crystalline hydroxyapatite (HAp) films were formed at the Ti surface by a single-step microarc oxidation (MAO), and HAp-zirconia composite (HZC) films were obtained by subsequent chemical vapor deposition (CVD) of zirconia onto the HAp. Through the CVD process, zero- and one-dimensional zirconia nanostructures having tetragonal crystallinity (t-ZrO2) were uniformly distributed and well incorporated into the HAp crystal matrix to form nanoscale composites. In particular, (t-ZrO2) was synthesized at a very low temperature. The HZC films did not show secondary phases such as tricalcium phosphate (TCP) and tetracalcium phosphate (TTCP) at relatively high temperatures. The most likely mechanism for the formation of the t-ZrO2 and the pure HAp at the low processing temperature was proposed to be the diffusion of Ca2+ ions. The HZC films showed increasing micro-Vickers hardness values with increases in the t-ZrO2 content. The morphological features and phase compositions of the HZC films showed strong dependence on the time and temperature of the CVD process. Furthermore, they showed enhanced cell proliferation compared to the TiO2 and HAp films most likely due to the surface structure change.

Zirconia powders with nano size pores and high specific surface areas were synthesized via aqueous precipitation and hydrothermal synthetic method using and under pH=11 and ambient condition. By this reaction. zirconia hydrate 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 was a mixed phase of monoclinic and tetragonal zirconia. By the BET analysis, it was found that the specific surface area was ranged in and the zirconia had the cylindrical shaped pores with average diameter of .

Zirconium nitride powders were synthesized at a relatively lower temperature using methane as a reducing agent in the nitridation of zircoia. ZrO2 powder was prepared by a sol-gel technique. The resulting sol-gel was centrifuged, and the gel was washed with deionized water. Anhydrous ammonia was used as the nitrogen source and methane was used as the reducing agent. Conversion diagrams show the equilibrium solid phase as a function of reagent concentrations for a specific temperature and gas pressure for the reagent system NH3-ZrO2-CH4. The reagent concentration ranges within which pure ZrN is formed increase with increasing reaction temperature. Low pressure with an excess of hydrogen decreases the reaction temperature at which pure ZrN is formed. Low pressure together with the introduction of excess hydrogen into the reaction system increases Zr and N conversion efficiency and retards C deposition.

Two-component ceramic (alumina-zirconia) composites were fabricated by a soft-solution process in which polyethylene glycol (PEG) was used as a polymeric carrier. Metal salts and PEG were dissolved in ethyl alcohol without any precipitation in 1:1 volume ratio of alumina and zirconia. In the non-aqueous system, the flammable solvent made explosive, exothermic reaction during drying process. The reaction resulted in formation of volume expanded, porous precursor powders by a vigorous decomposition of organic components in the precursor sol. The PEG content affected the grain size of sintered composites as well as the morphology of precursor powders. The difference of microstructure in sintered composite was attribute to the solubility and homogeneity of metal cations in precursor sol. At the optimum amount of the PEG polymer, the metal ions were dispersed effectively in solution and a homogeneous polymeric network was formed. It made less agglomerated particles in the precursor sol and affected on uniform grain size in sintered composite.

Al2O3/ZrO2 비수성 현탁액의 분산과 레올로지에 미치는 methyl isobutyl ketone (MIBK) /ethanol (EtOH) 용매혼합의 영향을 침전밀도, 점도를 측정함으로써 조사하였다. 분산제 'Hypermer' KD-1이 첨가된 다량의 MIBK를 함유하는 용매 (≥60vol%)에서 Al2O3와 ZrO2 입자의 침전밀도는 증가하였다. 80MIBK/20EtOH(vol%)에서 ball milling한 현탁액이 좁고 unimodal한 입자크기분포를 나타내었다. 모든 현탁액은 의가소성유동을 나타내었으나 shear thinning은 Al2O3/ZrO2의 혼합비, MIBK/EtOH의 혼합비에 따라서 다소 다르게 거동하였다. 순수한 MIBK를 사용한 Al2O3(<300 s-1 ) 및 ZrO2(<3000 s-1 ) 현탁액은 주어진 전단속도범위내에서 가장 강한 shear thinning을 나타내었다. 동일한 용매 (80MIBK/20EtOH, vol%)를 사용한 경우의 shear thinning은 Al2O3/ZrO2의 혼합비에 거의 의존하지 않았다.

Pechini방법으로 제조한 La0.8Ca0.2CrO3CLC소결체와 La0.8Ca0.2CrO3CLC-Green체를 YSZ에 적층한 후 온도의 함수로 계면에서의 미세구조와 성분이동 등의 거동을 고찰하였다. CLC-G/CLC와 CLC/YSZ계면에서의 CLC면은 반응온도에 상관없이 XRD 관찰에서 주상은 La1-x CaxCrO3그리고 CLC와 반응하지 않은 YSZ면의 결정 상은 cubic-ZrO2으로 각각 나타났다. CLC/YSZ반응 계면의 성분이동은 Zr > La>>Cr>>>Ca 순이었으며, 온도에 따른 개개 성분의 이동도 차이는 크지 않았다. CLC/YSZ계면간의 결합은 계면성분간의 과다한 성분이동 없이 현 연구의 온도전체에 걸쳐 가능한 것으로 나타났다. CLC-G/CLC간의 SEM미세구조는 결합 면을 경계로 저온에서는 결정의 입자크기 차이를 보이다가 온도가 증가할수록 균일화되는 경향을 보였다.였다. 보였다.였다.

세리아 안정화 지르코니아 성형체내에 이트리아를 침적법으로 도핑시켜 미세구조를 관철하였다. 도핑된 이트리아의 양과 열처리 조건을 제어하여 입계가 변형된 불규칙 입자형상의 미세구조를 형성시켰으며, 이때 입자형상의 불규칙 정도는 첨가된 이트리아의 양에 비례하였다. 0.2M 농도의 Y(NO3)3.6H2O의 수용액에 재침적하여 1650˚C에서 2시간 열처리한 시편의 미세구조는 표면부와 내부 모두에서 불규칙 입자형상을 나타내었으며, 입자의 불규칙도도 가장 큰 것으로 나타났다. 가압소결을 행한 결과 입계가 불규칙하게 변화된 미세구조가 창출됨과 동시에 평균입자 크기가 0.3μm 가량인 미세한 소결체를 제조할 수 있었으며, 상분석 결과 대부분 정방정상을 유지하고 있었다. 불규칙 입자형상의 미세구조를 가진 시편의 파괴인성값은, 정상적인 입자형상을 갖는 시편에서의 압흔 균열 크기로부터 비교 유추한 결과 17.6MPa.m(sup)1/2 이상인 것으로 나타났다.

PECVD(Plasma enhanced chemical vapor deposition)을 이용하여 yttria-stabilized zirconia(YSZ) 박막을 제조하였다. 반응물질로 금속유기화합물을 Zr[TMHD]4와 Y[TMHD]3그리고 산소를 사용하였으며, 증착온도는 425˚C, rf power는 0~100W까지 적용하였다. YSZ 박막은 (200)면이 기판에 평행한 입벙정상 구조를 가졌으며, 1시간 내에 1μm 두께를 형성하였다. EDX에 의한 막의 성분분석 결과로부터 환산된 박막내의 Y2O3의 함량은 0-36%의 범위였다. 버블러의 온도 및 운반기체의 유량이 증가함에 따라 박막의 두께 역시 비례하여 증가하였는데, 이는 precursor의 flux 증가로 인한 박막내의 Y2O3의 함량증가에 의한 것이었다. Zr 및 Y, O는 박막의 두께에 따라 일정한 조성비를 나타내었다. 운반기체를 Ar로 하였을 때 1000Å이하의 크기를 갖는 YSZ 입자들이 column 모양으로 기판에 수직하게 성장하였으며, 운반기체가 He인 경우에도 column 모양으로 성장하였으며 입도가 1000~2000Å으로 Ar의 경우보다 조대해졌다. XRD 분석결과 Y2O3의 함량이 증가함에 따라 YSZ의 격자상수 값이 약간씩 증가하였다. 이는 박막 전반에 걸쳐 형성된 균열에 의해 격자변형으로 인해 발생한 응력을 완화시켰지 때문이다.

등축정계의 결정구조를 지니는 무색 투명한 저코니아(Zr0.73Y0.27O1.87) 결정을 Y2O3를 안정제로 사용하여 Bridgman-Stockbager법(또는 Skull 용융법)으로 합성하였다. 육성된 결정은 유리광택을 나타내며 동시에 약간의 지방 광택도 띤다. 저코니아 결정은 편광현미경하에서 등방성을 나타내며 이방성의 징후는 발견되지 않는다. 모스 경도는 8∼8½이고 비중은 5.85이다. 자외선하에서는 약한 백색 형광을 낸다. 단결정법으로 결정한 저코니아의 결정구조는 등축정계이며, 공간군은 Fm3m(O5h)이다. 단위포 상수(a)는 5.1552(5)A이며, V=136.99(5)A, Z=4, R=0.0488이다. 저코니움 원자는 각 모서리에 산소 원자가 자리잡고 있는 육면체의 중심에 위치하고 있으며, 각 산소 원자는 저코니움 원자로 되어 있는 사면체의 중심에 위치하고 있다. 결국 8:4의 배위수가 성립하는 구조를 하고 있다.

수소 및 산소분위기 하에서 2Y-TZP 및 3Y-PZP 세라믹스를 소결하여 각각 제조한 다음, 각 시편의 미세구조 및 250˚C에서의 등온상전이 거동을 비교하여 고찰하였다. 그 결과 수소분위기에서 소결한 모든 시편의 표면에서는 Zr4+ 이온의 환원에 의해 산화분위기에서 소결한 시편에 비하여 색이 검게 변하였으며, 장시간 소결시 시편 표면에 조대 입자의 생성 및 입계 이완이 관찰되었다. 이에따라 수소분위기 하에서 장시간 소결된 시편의 경우 냉각 시 상전이가 일어나 다량의 단사정상이 상온에서 존재하였다. 저온 aging동안 등온상전이 속도는 산소분위기에서 소결한 시편보다 수소분위기에서 소결한 시편에서 낮게 나타났으며, 이러한 경향은 Y2O3의 고용량이 크고, 입자크기가 적은 시편일수록 증가하였다. 또한 2Y-TZP 시편에서는 입자크기에 상관없이 대부분의 정방정상이 단사정상으로 빨리 등온상전이를 일으켰으나, 3Y-TZP 시편의 경우, 등온상전이는 입자크기가 증가함에 따라 상전이 속도도 증가하였다.