超高温还原气氛下几种掺杂物对氧化铝晶体形貌的影响

用自行设计并安装的氢气气氛保护钼丝炉在超高温的条件下（〉１８５０℃）烧结ＨＮ－Ａｌ２Ｏ３的各种掺合试样，用光学显微镜，电子扫描显微镜，能谱及Ｘ射线衍射分析，比较详细地观察了各种掺杂物和温度对氧化铝晶形貌的影响，确定了板状氧化铝晶粒的尺寸，结果表明：在此烧结条件下，各试样中都含有板状氧化铝晶粒，各晶粒的发育情况与原料的纯度，掺杂物的种类和数量及烧结温度有关。     

自分散法低温烧成镁铝尖晶石制品的研究

采用金属铝粉氧化大量放热的自分散法与MgO合成镁铝尖晶石和在低温下直接制成高纯镁铝尖晶石制品进行了研究。结果表明：在1400℃温度下可制成镁铝尖晶石制品。     

Investigating the effect of SPS‎ parameters on densification ‎and fracture toughness of ZrB2-SiC nanocomposite‎

In this study, the effect of sintering parameters on densification and fracture toughness of spark plasma sintering ZrB₂-SiC nanocomposites was evaluated. For this purpose, ZrB₂-??30?vol% SiC nanocomposites in the conditions of ?1600?°C-4?min, 1700?°C-4?min, 1800?°C-4?min, 1800?°C-8?min, 1800?°C-12?min? were sintered.? Scanning Electron Microscopy (SEM) was used in order to investigate the ?microstructural variations. The bulk density was measured accoring to ASTM C 373–88. Single edge notch beam (SENB) method was used to ?determine the fracture toughness of samples. Microstructural observations showed that ?an increase in sintering temperature led to slight ?increase in SiC grains size but no sensitive variation in ZrB₂. However, increasing the sintering time resulted to increase both ZrB₂ and SiC grain size. Also, it was found, temperature and time ascent always increases the relative density. In addition, it was concluded that optimal temperature and time to reach the highest fracture toughness are 1800?°C and 8?min, respectively. Investigation of SEM images of the Vickers indent and their path propagation showed that the deviation and branching of crack are the most important toughening ?mechanisms in ZrB₂-SiC nanocomposites.?     

Grain growth kinetics and growth mechanism of columnar Al2O3 crystals in xNb2O5–7.5La2O3-Al2O3 ceramic composites

xNb₂O₅–7.5La₂O₃-Al₂O₃ ceramic composites with in-situ-grown columnar Al₂O₃ crystals were successfully prepared by microwave sintering at 1450–1525?°C using α-Al₂O₃, Nb₂O₅, and La₂O₃ powders as raw materials. X-ray diffraction results indicated that the main phases were Al₂O₃, LaNbO₄, and Nb₂O₅ in the prepared samples. A field emission scanning electron microscope (FESEM) showed that the Al₂O₃ crystals appeared as columnar in the structure. Moreover, the grain size of the columnar Al₂O₃ crystals increased with the Nb₂O₅ content. The ratio of the major axis to the minor axis of the crystals was largest when the Nb₂O₅ content was 15?vol%. Furthermore, the grain-growth kinetics index (n), growth activation energy (Q), and growth mechanism of the columnar Al₂O₃ crystals were studied. The results indicated that the Nb₂O₅ addition could promote formation and growth of columnar Al₂O₃ crystals, and the grain-growth activation energy indicated that the dissolution process controls the crystal growth. The growth mechanism of the columnar Al₂O₃ crystals was also studied. The present work demonstrated that Nb₂O₅ is a good additive for the preparation of Nb₂O₅–7.5La₂O₃-Al₂O₃ composite ceramics with columnar Al₂O₃ crystals.     

Improved shear strength of SiC-coated 3D C/SiC composite joints with a tailored Ti-Si-C interlayer

SiC-coated 3D C/SiC composites were successfully joined using SPS technology with a Ti-Si-C interlayer. The interface morphologies, phase composition, and mechanical properties of the joints were investigated in detail. By adjusting the joining temperature, the interlayer transitioned, in situ, from Ti-Si-C compounds to Ti₃SiC₂ grains without decomposition. Because of the plastic deformation behavior of Ti₃SiC₂ grains, the ability of the interlayer to inhibit crack propagation increased. For joints with different interlayer thickness, the distribution of thermal residual stress was calculated using finite element analysis, and the distribution was associated with the evolution of interlayer morphologies, which was eventually used to establish fracture models. Optimized bonding was achieved without erosion of carbon fibers and also without interfacial defects. Finally, a reliable joint with shear strength of 51 ± 3.0 MPa was obtained by precisely controlling the interlayer reaction and optimizing thermal residual stress.     

Transparent tetragonal-cubic zirconia composite ceramics densified by spark plasma sintering and hot isostatic pressing

Targeting higher toughness transparent ceramics, tetragonal (3 mol % yttria) and cubic (8 mol % yttria) ZrO₂ starting powder mixtures were densified by spark plasma sintering (SPS) in vacuum at 1100 °C and post hot isostatic pressing (HIP) in argon at 1100 °C. The influence of the ultra-fine microstructure and phase composition on the fracture resistance and light transmission in the visible and infra-red range was assessed. Of special interest was the influence of a thermal annealing step in air on the transparency of the SPS and SPS-HIP ceramics.     

Investigations of TaB2 on oxidation-inhibition property and mechanism of Si-based coatings in aerobic environment with broad temperature region for carbon materials

To investigate the formation mechanism of the dendrites glass-ceramics and the effect of TaB₂ modifier on the oxidation-inhibition ability of Si-based coatings in aerobic environment with broad temperature region for carbon materials, the Si-based coatings modified with different TaB₂ content were fabricated by the liquid phase sintering method. The fabricated coatings and its corresponding composite powders were investigated in dynamic TG aerobic environments up to 1500 ℃. The initial oxidation temperatures of Si-based coatings modified with TaB₂ powders are almost completely suppressed to 800 ℃. With the increase of TaB₂ phase content, the relative oxygen permeability of the Si-based coatings is significantly reduced, which can be interpreted as the generation of liquid boride, silicide and Ta-Si-B-O compound glass ceramics those can improve the stability of the coating. The formation mechanism of the dendrites glass-ceramics was illustrated.     

Optical and mechanical characterization of transparent α-alumina fabricated by spark plasma sintering

The aim of this work was the analysis of the experimental results of a transparent alumina (BMA15) ceramic which was fabricated by Spark Plasma Sintering (SPS) from nanopowder (BMA15, Baikowski Chimie, France), at different temperatures (1200°C, 1250°C, 1300°C). With the application of a maximum uniaxial pressure of 73 MPa during all the fabrication-cycle (more than 3 hours). We sought an optimal sintering temperature combining better optical and mechanical properties of our pellets. The sintered alumina (BMA15) has a crystalline and dense microstructure. The samples sintered at 1200°C exhibit the best optical properties, in particular: good real inline transmission (RIT) and an optical gap greater than those of the samples sintered at 1250°C and 1300°C. Due to their low density, the Young modulus of alumina sintered at 1200 °C, deduced by ultrasound, has a low value which is about 385 GPa. Similarly, its small grain size gives it a better Vickers hardness ~ 21 GPa. Therefore, the value of the coefficient of friction μ stabilizes around the mean value of 0.21.     

Sintering kinetics of ZrO2 nanopowders modified by group IV elements

The sintering behavior of tetragonal zirconia nanopowders modified by the group IV elements at the initial sintering stage was investigated. It was found that different additives SiO₂, SnO₂, and GeO₂ have a significant influence on the densification kinetics of 3Y-TZP nanopowders obtained by coprecipitation during sintering as it depends on the amount of additives (0-5 wt%). The shrinkage of zirconia-based specimens during the nonisothermal sintering was analyzed using the dilatometric data. The constant rate of heating technique was applied in order to determine the dominant mass transfer mechanism at the initial stage of sintering in modified zirconia nanopowders. It was found that there was a change in the mass transfer mechanism and diffusion activation energy in 3Y-TZP as a result of the additives. The dominant sintering mechanism in 3Y-TZP changed from the volume diffusion to the grain boundary diffusion due to the addition of SiO₂ and SnO₂ and the sintering activation energy increased in these cases. However, GeO₂ additive activated the viscous flow mechanism in sintering process of 3Y-TZP nanopowders which led to acceleration of the densification due to the decrease in the diffusion activation energy.     

Comparison of a laboratorial scale synthesized and a commercial yttria-tetragonal zirconia polycrystals ceramics submitted to microwave sintering

Conventional sintering techniques of yttria-tetragonal zirconia polycrystals (Y-TZP) ceramics have presented limitations regarding the sintering time and temperature, increasing the cost of the final dental and biomedical products. Herein, microwave sintering comes to be an interesting alternative by providing fast heating, high densification, and grain-size control. The aim of this study was to compare the effect of microwave sintering of Y-TZP dental ceramics prepared from a pre-sintered commercial block and produced from powders synthesized in a laboratorial scale by the precipitation route. The synthetized and commercial discs were submitted to microwave sintering at 1450°C and 1350°C for 15, 30, and 60 minutes. Densification, fracture toughness, grain size, and crystalline phase quantification of the sintered groups were evaluated. Both synthetized and commercial groups sintered at 1450°C for 15 and 30 minutes showed the higher densification results (98% TD). XRD quantitative phase analysis indicates that samples present 89% tetragonal and 11% cubic phases, except for the group prepared from coprecipitated powders sintered at 1450°C for 30 minutes, that presented 79% and 21% of tetragonal and cubic phases. The microwave sintering at 1450°C allows hardness and fracture toughness values comparable to conventional sintering.