Formation and Sintering of Yttria-Doped Tetragonal Zirconia with 50 mol% Alumina Prepared by the Hydrazine Method

Al₂O₃/Y₂O₃-doped ZrO₂ composite powders with 50 mol% Al₂O₃ are prepared by the hydrazine method. As-prepared powders are mixtures of AlO(OH) gel and amorphous ZrO₂ solid solutions containing Y₂O₃ and Al₂O₃. The formation process leading to α-Al₂O₃- t -ZrO₂ composite powders is examined. Hot isostatic pressing is performed for 2 h at 1400°C under 196 MPa using θ-Al₂O₃- t -ZrO₂ composite powders. The resulting dense, sintered α-Al₂O₃- t -ZrO₂ composites show excellent mechanical strength.     

Crystal Structure of Zirconia Prepared with Alumina by Coprecipitation

Zirconia was prepared by firing the coprecipitate from ZrOCl₂and AlCl₃mixed aqueous solution with ammonia. When fired above 600°C, the products were fine crystalline tetragonal zirconia of crystallite size <10 nm. In previous studies, the tetragonal phase had been assumed to be a (Zr_{1− x} ⁴⁺Al _x ³⁺)O_{2− x /2}solid solution, where x ≤ 0.25. However, X-ray diffraction pattern simulation and Al K -edge XANES spectroscopy confirmed the present product to be a mixture of t -ZrO₂fine powder with a small amount of δ-Al₂O₃of very low crystallinity, even below the expected compositional range of x ≤ 0.25 in the (Zr_{1− x} ⁴⁺Al _x ³⁺)O_{2− x /2}solid solution.     

Hydrothermal Crystallization of Zirconia and Zirconia Solid Solutions

Zirconia as well as yttria-zirconia and calcia-zirconia solid-solution powders were crystallized under hydrothermal conditions from (co)precipitated hydroxides. The morphology of the powder particles is strongly dependent on the crystallization conditions. The powders crystallized in a water solution of Na, K, and Li hydroxides show elongated particles of much larger sizes than those which result from the process carried out in pure water or a water solution of Na, K, or Li chlorides. The shapes of the latter particles are isometric. The growth mechanism of the elongated particles is suggested.     

Formation of Alumina/Zirconia (3 mol% Yttria) Composite Powders Prepared by the Hydrazine Methods

Alumina/3 mol% yttria-doped zirconia composite powders have been prepared by the hydrazine method. As-prepared powders are AlO(OH) gel solid solutions and the mixtures of this and amorphous ZrO₂ below and above 10 mol% ZrO₂, respectively. The formation process leading to α–Al₂O₃– t -ZrO₂ composite powders is examined.     

Characteristics and Catalytic Properties of Alumina–Zirconia Mixed Oxides Prepared by a Modified Pechini Method

A modified Pechini method was used to prepare alumina–zirconia mixed oxides at three different molar ratios. For comparison, pure alumina and pure zirconia were prepared using the same method. The mixed oxides were characterised by the BET method for surface area, X-ray diffraction, CO₂ and NH₃ temperature-programmed desorption. Elimination of 2-propanol was used as a probe reaction to characterise the surface of the mixed oxides. The modified Pechini preparation resulted in a poor acid–base strength of alumina surface resulting in high acetone selectivity where imperfect crystal structure of the tetragonal zirconia favoured high propylene production in 2-propanol elimination at 200 °C.     

Sintering Behavior of Nanocrystalline Zirconia Doped with Alumina Prepared by Chemical Vapor Synthesis

Powders of nanocrystalline zirconia doped with 3–30 mol% alumina have been synthesized using chemical vapor synthesis (CVS). Dense or mesoporous ceramics of small and narrowly distributed grain and pore sizes in the nanometer range are obtained via pressureless vacuum sintering. The microstructural development of the doped samples is strongly dependent on the alumina content. Sintering of zirconia samples with 3 and 5 mol% alumina at temperatures of 1000°C for 1 h results in fully dense, transparent ceramics with grain sizes of 40–45 nm and homogeneous microstructures.     

Raman Spectroscopy of Tetragonal Zirconia Solid Solutions

Raman spectra of tetragonal zirconia were studied for the systems ZrO₂-Y₂O₃, ZrO₂-CeO₂, ZrO₂-Y₂O₃-Nb₂O₅, and ZrO₂-Y₂O₃-Ta₂O₅ There was no change in the Raman bands for tetragonal ziraconia in the ZrO₂-Y₂O₃ system as a function of Y₂O₃ content . On the other hand, in the ternary systems, the Raman lines corresponding to the stretching modes of two sets of cation-oxygen bonds shifted to greater wave numbers as either Nb₂O₅ Contents increased in Y₂O₃-stabilized tetragonal zirconia. This difference was interpreted by local bonding environments of the pentavalent cations, which were supposed to occupy tetrahedral sites in teteragonal zirconia solid solutions.     

Advanced Alumina and Zirconia Ceramics Produced by the Electroconsolidation Method

The possibility to produce advanced alumina and zirconia ceramics by the electroconsolidation method is studied.The technological parameters of Al_2O_3 and ZrO_2( 3 mass% Y_2O_3) production were developed and optimized.Electroconsolidated alumina and zirconia ceramics have higher values of properties in comparison with ordinary sintered samples in air.Advanced properties of electroconsolidated ceramics are defined by homogeneous,ultradense and fine-crystalline structure that was formed due to the effect to consolidate the materials to high density for a shortest time.     

Formation of Zirconia Titanate Solid Solution from Alkoxides

In the system ZrO₂–TiO₂, ZrTiO₄ solid solutions prepared by the simultaneous hydrolysis of zirconium and titanium alkoxides crystallize at low temperatures from amorphous materials between 30 and 70 mol% TiO₂. As zirconium is substituted for titanium, the solid solutions can be indexed in an orthorhombic unit cell with a and c decreasing linearly from 0.4832 to 0.4778 nm and from 0.5063 to 0.5002 nm, respectively, and b increasing linearly from 0.5401 to 0.5478 nm. The volume of the unit cell decreases continuously with increasing TiO₂ content. At higher temperatures the solid solutions decompose into ZrTiO₄ and either ZrO₂ (monoclinic) or TiO₂ (rutile), depeanding on the starting composition.     

Processing of Tape–Cast Laminates Prepared from Fine Alumina/Zirconia Powders

This paper addresses the effect of thermocompression pressure, shear deformation of green laminates, and postsinter HIPing on the microstructural homogeneity of cast tapes and laminates prepared from fine Al₂O₃, and Al₂O₃/ ZrO₂, powders. Green density increases with increasing thermo–compression pressure. Sintered densities, however, depend more on the macroscopic uniformity in the green tapes. When density gradients develop within the individual green tapes (because of improper drying), sintering is constrained in two dimensions and densities remain low. Postsinter HIPing does not significantly increase the sintered densities because of the retention of open porosity within the individual tape–cast layers. The use of a revised thermocompression process involving shear deformation results in higher sintered densities and complete densification after HIPing. Sintered densities increase with the degree of shear strain during green–state deformation processing. Thus, green-state deformation can improve homogeneity in laminates. A further variation of the shear deformation process has also been developed that allows the formation of complex shapes from tape–cast laminates in the green state, while retaining layer integrity.     

Preparation of Zirconia Base Solid Solution Nanopowder by Exothermal Solid-State Synthesis

A new method is put forward to prepare nanometer zirconia base solid solution by exothermal solid-state synthesis. This method is realized by agitating solid mixture of sodium hydroxide, zirconium oxychloride, and yttrium/calcium nitride. Fresh and final powders are studied by X-ray fluorescence, X-ray photoemission spectroscopy, X-ray diffraction, and transmission electron microscopy. The results show the obtained tetragonal/cubic zirconia solid solution nanopowders are highly pure and distribute around 5 nm. It is suggested that the coordinated water of zirconium oxychloride acts as micro medium and the nuclei of solid solution are formed under the superalkaline environment and grow during heat treatment. This method may be useful to prepare other metal oxide nanopowders.     

Alumina and Alumina/Zirconia Multilayer Composites Obtained by Slip Casting

The slip casting technique has been revealed as a powerful method to obtain multilayer composites close to theoretical density. From zeta potential and viscosity measurements of Al₂O₃ and Al₂O₃/ZrO₂ (4 vol% ZrO₂) suspensions, the corditions for the preparation of multilayer composites by slip casting have been determined. A microstructural analysis of the different layers by scanning electron microscopy is also reported.     

正交法优化均匀沉淀法制备超细氧化锆粉体工艺

研究以氧氯化锆、尿素为原料,采用均匀沉淀法制备超细氧化锆粉体,考察反应温度、尿素溶液浓度、反应物投料比、干燥方式、煅烧温度等对氧化锫粉体粒径的影响.确定最佳工艺条件:反应温度为100℃,尿素溶液浓度为13％,反应物投料摩尔比为2.1∶1,抽滤后的湿凝胶采用喷雾干燥,煅烧温度为550℃.在此条件下,可获得平均粒径为113.5 nm的单斜晶超细氧化锫粉体.     

沉淀法制备的固体聚羧酸减水剂性能研究

采用沉淀法制备了固体聚羧酸减水剂,依据国标方法对该聚羧酸减水剂的宏观性能进行测试,采用IR、GPC分析技术对其结构进行表征,并将其性能与传统方法制备的液体聚羧酸减水剂和外购固体聚羧酸减水剂进行比较研究.结果表明:采用沉淀法制备的固体聚羧酸减水剂减水率可达28%,初始坍落度为160 mm,经时坍损小;固化过程对聚羧酸减水剂官能团、分子量及多分散系数、水泥的吸附性均无明显影响;宏观性能方面虽然对水泥的分散作用、坍落度、硬化水泥砂浆抗压强度虽略低于液体聚羧酸减水剂,但各项指标均能达到国标要求,说明沉淀法制备固体聚羧酸减水剂是一条可行的途径.     

Preparation of Monodisperse Zirconia Particles by Thermal Hydrolysis in Highly Concentrated Solutions

Monodisperse zirconia particles were prepared by the thermal hydrolysis of mixtures of zirconyl chloride, zirconium hydroxide, and water at high concentrations corresponding to about 5 mol/L Zr. The particles, as first prepared, were temporarily agglomerated spheres composed of primary ultrafine zirconia crystals. The agglomerated particles collapsed and dispersed in water to form a translucent sol. When vacuum dried and followed by heat treatment, they were not dispersible. The size of the agglomerated particles increased with increasing molar ratio of the zirconium chloride in the starting mixture, varying from about 0.2 to 0.6 μm. Using the sample thus obtained, monodisperse tetragonal zirconia particles of about 0.35 μm containing 3 mol% Y₂O₃ with a relatively uniform composition were obtained by homogeneous precipitation of YOHCO₃ by heating with urea and calcination at 800°C.     

Structure of Zirconia Prepared by Homogeneous Precipitation

The structure of pure zirconia powders prepared by homogeneous precipitation was examined by electron microscopy. Some of these powders consisted of metastable tetragonal zirconia in the form of spherical aggregates up to 1 μm in diameter. The size of single crystals within these particles exceeded 100 nm, which is much larger than usually reported for metastable zirconia. We conclude that the existence of these large teragonal monocrystals is due principally to the very fine internal porosity within the domains, which gave rise to a surface area/volume ratio sufficient to stabilize tetragonal zirconia by the same mechanism as in nanocrystalline powders.     

固相法制备有机黏土改性聚丙烯

采用固相法对黏土进行有机化插层改性,制备出有机黏土;通过熔融插层法制备聚丙烯/有机黏土纳米复合材料。X射线衍射分析表明,固相法改性黏土可以与聚丙烯形成纳米复合材料。利用DSC研究了纳米复合材料的结晶和熔融过程,结果表明:聚丙烯/有机黏土纳米复合材料的结晶温度提高,熔融过程、熔点及结晶度没有明显变化。力学性能测试结果表明:有机黏土含量在3%～5%范围内,纳米复合材料的力学性能最佳。     

含Ce_xZr_(1-x)O_2固溶体三效催化剂的制备及性能研究

用共沉淀技术在室温、pH =10 0的条件下制备出了CexZr1-xO2 固溶体 ,将其用于Pd基三效催化剂的制备 ,对催化剂的性能进行了评价 ,结果表明 :和纯的CeO2 相比 ,含CexZr1-xO2 固溶体的催化剂具有较高的催化性能 ,其中Pd/Ce0 6Zr0 .4 O2 催化剂性能最佳 ,HC、CO、NO的转化率在A/F =14 6时分别为 97 33%、89 5 2 %、10 0 %;新鲜催化剂的起燃温度分别为 186、180、185℃ ,高温处理后起燃温度分别为 2 49、2 41、2 46℃。     

Biomimetic Preparation and Characterization of Bioactive Coatings on Alumina and Zirconia Ceramics

For the preparation of bioactive coatings on alumina and zirconia ceramic surfaces a fast biomimetic method using a supersaturated solution containing Na⁺, Ca²⁺, Cl⁻, HCO₃⁻, and PO₄³⁻ ions was used. The coatings were analysed with the use of an X-ray diffraction spectrometer and a transmission electron microscope equipped with an energy-dispersive spectroscopy detector. After the precipitation both coatings were composed of poorly crystallized, nanosized, plate-like particles with the octacalcium phosphate (OCP) crystal structure. The adhesion of the coatings was improved by a heat treatment at 1050°C for 1 h. During this heat treatment the calcium phosphate layer, deposited from a supersaturated solution onto the surface of the substrates, was sintered to form a dense coating. At the same time the OCP crystal structure was transformed into that of hydroxyl apatite, the coating's crystallinity was increased, and the particles grew isotropically up to 300 nm in size. The bioactivity of the coated ceramic was confirmed before and after the heat treatment using a simple simulated body fluid test.