3Y-TZP (3 mol% yttria-stabilized tetragonal zirconia polycrystals) ceramics have excellent mechanical properties including high fracture toughness, good abrasion resistance as well as chemical and biological stability. As a result, they are widely used in mechanical and medical components such as bearings, grinding balls, and hip implants. In addition, they provide excellent light transmittance, biocompatibility, and can match tooth color when used as a dental implant. Recently, given the materials’ resemblance to human teeth, these ceramics have emerged as an alternative to titanium implants. Since the introduction of CAD/CAM in the manufacture of ceramic implants, they’ve been increasingly used for prosthetic restoration where aesthetics and strength are required. In this study, to improve the surface roughness of zirconia implants, we modified the 3YTZP surface with a biocomposite of hydroxyapatite and forsterite using room temperature spray coating methods, and investigated the mixed effect of the two powders on the evolution of surface microstructure, i.e., coating thickness and roughness, and biological interaction during the in vitro test in SBF solution. We compared improvement in bioactivity by observing dissolution and re-precipitation on the specimen surface. From the results of in vitro testing in SBF solution, we confirmed improvement in the bioactivity of the 3Y-TZP substrate after surface modification with a biocomposite of hydroxyapatite and forsterite. Surface dissolution of the coating layer and the precipitation of new hydroxyapatite particles was observed on the modified surface, indicating the improvement in bioactivity of the zirconia substrate.

3Y-TZP ceramics obtained by doping 3 mol.% of Y2O3 to ZrO2 to stabilize the phase transition are widely used in the engineering ceramic industry due to their excellent mechanical properties such as high strength, fracture toughness, and wear resistance. An additional increase in mechanical properties is possible by manufacturing a composite in which a high-hardness material such as oxide or carbide is added to the 3Y-TZP matrix. In this study, composite powder was prepared by dispersing a designated percentage of WC in the 3Y-TZP matrix, and the results were compared after manufacturing the composite using the different processes of spark plasma sintering and HP. The difference between the densification behavior and porosity with the process mechanism was investigated. The correlation between the process conditions and phase formation was examined based on the crystalline phase formation behavior. Changes to the microstructure according to the process conditions were compared using field-emission scanning electron microscopy. The toughness-strengthening mechanism of the composite with densification and phase formation was also investigated.

As a case study on aspect ratio behavior, Kaolin, zeolite, TiO2, pozzolan and diatomaceous earth minerals are investigated using wet milling with 0.3 pai media. The grinding process using small media of 0.3 pai is suitable for current work processing applications. Primary particles with average particle size distribution D50, ~6 μm are shifted to submicron size, D50 ~0.6 μm, after grinding. Grinding of particles is characterized by various size parameters such as sphericity as geometric shape, equivalent diameter, and average particle size distribution. Herein, we systematically provide an overview of factors affecting the primary particle size reduction. Energy consumption for grinding is determined using classical grinding laws, including Rittinger's and Kick's laws. Submicron size is obtained at maximum frictional shear stress. Alterations in properties of wettability, heat resistance, thermal conductivity, and adhesion increase with increasing particle surface area. In the comparison of the aspect ratio of the submicron powder, the air heat conductivity and the total heat release amount increase 68 % and 2 times, respectively.

Zircon, having excellent thermal, chemical, and mechanical properties, is utilized in refractory materials, electronic materials, chemical machines, structural materials, etc. However, zircon generally shows thermal dissociation to zirconia(ZrO2) and silica(SiO2) around the sintering temperature of 1540 oC, and when zircon particles are small and impurities are present, thermal dissociation is known to occur at around 1100 oC. This reduces the mechanical properties of ZrSiO4. In this research, the effect of adding SiO2 and 3Y-TZP to ZrSiO4 has been studied in order to suppress dissociation and improve the mechanical properties. Addition of SiO2 suppressed the dissociation of ZrSiO4 at lower temperatures. It also enabled optimum packing between the particles, resulting in a dense microstructure and good mechanical properties. When 3Y-TZP was added, recombination with the dissociated SiO2 resulted in good mechanical properties by suppressing the generation of pores and the densification of the microstructure.

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.

Low temperature degradation behavior in yttria stabilized tetragonal zirconia polycrystal (Y-TZP) ceramics was microscopically observed from the phase contrast between monoclinic surface and tetragonal matrix. The degradation behavior was dependent on the surface treatment of sintered Y-TZP, even if the sintering history is same. In the mirror polished specimen, the monoclinic layer appeared in a uniform thickness from the surface. On the contrary, for the specimen with coarse scratch, the thickness of degraded surface was more than double especially from the coarse scratch. Since the scratch results in local deformation, the residual stress should be induced around the scratch. With the transformation from tetragonal to monoclinic, the volume expansion exerts a stress on a neighboring grains and promotes a successive phase transformation. Such a autocatalytic effect can be triggered from the part of coarse scratch.

In this study, 3 mol% yttria-tetragonal zirconia polycrystal (3Y-TZP) nanoparticles were synthesized by the glycothermal method under various reaction temperatures and times. The co-precipitated precursor of 3Y-TZP was prepared by adding NH4OH to starting solutions, and then the mixtures were placed in an autoclave reactor. Tetragonal yttria-doped zirconia nanoparticles were afforded through a glycothermal reaction at a temperature as low as 220˚C, using co-precipitated gels of ZrCl4 and YCl3·6H2O as precursors and 1,4-butanediol as the solvent. The synthesized 3Y-TZP particles were characterized by X-ray diffraction (XRD), field emission scanning electron microscopy (FESEM), transmission electron microscopy (TEM), and Raman spectroscopy. The 3Y-TZP particles have a stable tetragonal phase only at glycothermal temperatures above 200˚C. To investigate phase transition, the 3Y-TZP particles were heat treated from 400 to 1400˚C for 2 h. Raman analysis indicated that, after heat treatment, the tetragonal phase of the 3Y-TZP particles remained stable. The results of this study, therefore, suggest that 3Y-TZP powders can be prepared by the glycothermal method.

The phase stability of tetragonal phase in Y-TZP was investigated in terms of the distribution of grain sizes and heat-treating atmosphere. Y-TZP with various grain sizes were prepared using duration time at 1600℃ as experimental parameter. Accumulated grain size distributions were built from the SEM micrographs and the amount of tetragonal phase were measured using XRD. Both results were compared to determine the critical grain size before and after heat-treatment in vacuum. The critical grain size drastically decreased compared with the small increase of average grain size due to the autocatalytic effect which critically affects the tetragonal to monoclinic phase transformation. After heat-treatment in reductive atmosphere critical grain size relatively increased due to the stabilization of tetragonal phase. The formation of oxygen vacancies during heat-treatment was ascribed to the increase of stability.

3Y-TZP, 12Ce-TZP 및 3Y-TZP, 12Ce-TZP 현탁액의 제타포텐셜과 겉보기점도의 측정으로부터 슬립주입공정에 의한 다층복합체의 제조조건을 조사하였다. 아울러 다층복합체의 소결밀도, 미세구조, 결정상에 미치는 열처리의 영향을 검토하였다. 3Y-TZP와 12Ce-TZP 현탁액의 등전점을 pH 8부근이었으나 3Y-TZP/12Ce-TZP의 등전점은 pH8.6이었다. 현탁액은 전단속도의 증가와 더불어 점도가 감소하는 의가소성유동을 나타내었다. 15 및 20vol% 고체함량을 갖는 3Y-TZP와 3Y-TZP/12Ce-TZP 현탁액은 소량(0.3wt%)의 유기해교제의 첨가만으로 슬립주입에 적당한 유동성을 보유하였으나, 12Ce-TZP의 경우는 점도를 감소시키기 위하여 부가적인 전해질이 필요하였다. 이론밀도의 98% 이상을 보유하고 0.3~2.2μm의 입경을 갖는 치밀한 다층복합체가 1500˚C 소결로 얻어졌다.

다공성 알루미나 소결체내부로 3Y-TZP 및 12Ce-TZP 전구체를 각각 액상침투시킴으로써 2종류의 Al2O3/TZP복합체를 제조하였다. 소량의 (~11.0 wt%) TZP의 첨가는 Al2O3소결체 (1600˚C, 2시간)의 강도 (19~59%)와 파괴인성(14~157%)을 증가시켰다. 3Y-TZP의 첨가는 복합체의 강도의 향상에 12Ce-TZP의 첨가는 인성의 향상에 보다 효과적이었다. 침투도니 TZP는 복합체의 내부보다 표면에 집중되었으며, 그 결과 이곳에서의 입성장에 빨랐고 Al2O3의입성장 억제효과도 상대적으로 뛰어났다. 입계 및 입내균열전파가 일어났으나 Al2O3/12Ce-TZP의 경우가 Al2O3/3Y-TZP에 비하여 입계파괴가 우세하였다

2mol%의 이트리아로 안정화된 정방정상 지르코니아 분말을 800˚C부터 1500˚C 까지 온도별로 열처리하여 분말내 입자크기 및 입자간에 존재하는 구속력을 변화시킨 다음, 정방정상의 전이도 및 안정화효과가 무열상전이, 응력유기상전이, 등온상전이 에 미치는 영향을 고찰하였다. 그 결과 Y-TZP 분말내 정 방정상의 전이도는 고용체의 양이 일정할 경우 열처리온도의 변화에 따른 입자크기와 입자간에 존재하는 구속력의 크기에 의존하였는데 열처리온도가 증가함에 따라 전이도가 점차 증가하여 1300˚C로 열처리한 분말에서 최대값을 보였다. 그러나 1300˚C 이상으로 열처리한 분말에서는 열처리온도가 증가함에 따라 구속효과의 증가에 따라 전이도가 정차로 감소하였다. 전이도가 큰 분말에서는 정방정상이 무열상전이, 응력유기상전이, 등온상전이를 쉽게 일으켜 단사정상으로 전이하였다.