Densification and mechanical properties of fine-grained Al2O3-ZrO2 composites consolidated by spark plasma sintering

Alumina matrix composites containing 5 and 10 wt% of ZrO₂ were sintered under 100 MPa pressure by spark plasma sintering process. Alumina powder with an average particle size of 600 nm and yttria-stabilized zirconia with 16 at% of Y₂O₃ and with a particle size of 40 nm were used as starting materials. The influence of ZrO₂ content and sintering temperature on microstructures and mechanical properties of the composites were investigated. All samples could be fully densified at a temperature lower than 1400 °C. The microstructure analysis indicated that the alumina grains had no significant growth (alumina size controlled in submicron level 0.66-0.79 μm), indicating that the zirconia particles provided a hindering effect on the grain growth of alumina. Vickers hardness and fracture toughness of composites increased with increasing ZrO₂ content, and the samples containing 10 wt% of ZrO₂ had the highest Vickers hardness of 18 GPa (5 kg load) and fracture toughness of 5.1 MPa m^1/2.     

Comparison of ZrB2-SiC ceramics with Yb2O3 additive prepared by hot pressing and spark plasma sintering

This work compared phase composition, microstructures and mechanical properties of ZrB₂—20 vol.% SiC—5 vol.%Yb₂O₃ prepared by hot pressing (HP) and spark plasma sintering (SPS) in vacuum. Despite the same raw material composition, the two densification techniques led to the appearance of different secondary phases. The HP ceramics had coarsened microstructure, predominantly intergranular fracture characteristic and high fracture toughness. The SPS ceramics exhibited refined microstructure, transgranular fracture model and high bending strength.     

Microstructure and mechanical properties of Al2O3-Cr2O3 composite coatings produced by atmospheric plasma spraying

Al₂O₃, Al₂O₃-Cr₂O₃ and Cr₂O₃ coatings were deposited by atmospheric plasma spraying. Phase composition of powders and as-sprayed coatings was determined by X-ray diffraction. Electron probe microanalyzer was employed to investigate the polished and fractured surface morphologies of the coatings. Mechanical properties including microhardness, fracture toughness and bending strength were evaluated. The results indicate that the addition of Cr₂O₃ is conducive to the stabilization of α-Al₂O₃. Compared with the pure Al₂O₃ and Cr₂O₃ coatings, Al₂O₃-Cr₂O₃ composite coatings show lower porosities and denser structures. Heterogeneous nucleation of α-Al₂O₃ occurs over the isostructural Cr₂O₃ lamellae and partial solid solution of Al₂O₃ and Cr₂O₃ might be occurring as well. Furthermore, grain refining and solid solution strengthening facilitate the mechanical property enhancement of Al₂O₃-Cr₂O₃ composite coatings.     

Rapid fabrication of the Ti3SiC2 bonded diamond composite by spark plasma sintering

A mixture of Ti/Si/TiC/diamond powders was employed to fabricate the Ti₃SiC₂ bonded diamond composite using the spark plasma sintering-reactive synthesis method. The addition of diamond does not inhibit the synthesis of Ti₃SiC₂ in the sintered product. In the matrix Ti₃SiC₂ grains developed lamellar morphology with an average length size of 5-10 μm. Ti₃SiC₂ matrix displays good pullout strength with diamond, and the Ti₃SiC₂ bonded diamond material exhibits good wear resistance.     

国外多孔基体氧化铝/氧化铝复合材料工程应用进展

氧化铝/氧化铝复合材料(Al2O3/Al2O3)是20世纪90年代兴起的一类连续陶瓷纤维增强陶瓷基复合材料,已经发展为与SiC/SiC、C/SiC等非氧化物陶瓷基复合材料并列的一类陶瓷基复合材料。与非氧化物陶瓷基复合材料相比,Al2O3/Al2O3具有长时抗氧化、高温耐腐蚀、低成本等独特优势,已经在航空发动机、地面燃气轮机等军民两用热结构材料领域展现出广阔的应用前景。本文从材料应用的角度出发,系统分析阐述了目前在Al2O3/Al2O3占主导地位的多孔基体Al2O3/Al2O3(P-Al2O3/Al2O3)的增韧机制、成型工艺和性能特点,重点归纳了国外近年来P-Al2O3/Al2O3的工程化应用进展及前景,最后指出了P-Al2O3/Al2O3存在的局限性并展望了未来发展方向,旨在为国内Al2O3/Al2O3体系发展提供借鉴和参考。     

An evaluation of Al2O3-ZrO2 composites produced by coprecipitation method

The objective of this work is to produce Al₂O₃-ZrO₂ composite from nano-sized powders processed by coprecipitation method. Al₂O₃ and mixture of Al₂O₃ + 10 wt.% ZrO₂ precipitated successfully by chemical route from aluminum sulfate and zirconium sulfate were pressed under uniaxial compression of 170 MPa and sintered at 1600 °C for 1 h. SEM investigations revealed that, pure alumina sample has a microstructure with coarse grains which anisotropically grown up to 30-40 μm in size. In alumina-zirconia composite, the structure consists of very fine equiaxed grains of typically 2 μm in which zirconia precipitates were uniformly dispersed. By adding zirconia to alumina, hardness and indentation fracture toughness were increased from 11.6 GPa to 16.8 GPa and from 3.2 MPa m^1/2 to 4.9 MPa m^1/2, respectively. Improvement in fracture toughness was attributed to bridging effects of zirconia particles as well as transformation toughening.     

In-situ TiB2 and Al2O3 formation by DC plasma spraying

In-situ plasma spraying (IPS) is a promising process to fabricate composite coatings with in-situ formed thermodynamically stable phases. In the present study, mechanically alloyed Al-12Si, B₂O₃ and TiO₂ powder was deposited onto an aluminum substrate using atmospheric plasma spraying (APS). It has been observed that, during the coating process, TiB₂ and Al₂O₃ are in-situ formed through the reaction between starting powders and finely dispersed in hypereutectic Al-Si matrix alloy. Also, obtained results demonstrate that in-situ reaction intensity strongly depends on spray conditions.     

Mechanical and tribological performance of Al2O3-TiO2 coatings elaborated by flame and plasma spraying

Mechanical properties and wear rates of Al₂O₃-13 wt.% TiO₂ (AT-13) and Al₂O₃-43 wt.% TiO₂ (AT-43) coatings obtained by flame and atmospheric plasma spraying were studied. The feed stock was either ceramic cords or powders. Results show that the wear resistance of AT-13 coatings is higher than that of AT-43 and it seems that the effect of hardness on wear resistance is more important than that of toughness. Additionally, it was established that, according to conditions used to elaborate coatings and the sliding tribological test chosen, spray processes do not seem to have an important effect on the wear resistance of these coatings.     

Al2O3/TiB2/Al复合材料的微观结构和高温力学性能

以细雾化铝粉和TiB₂颗粒为原料,通过粉末冶金和热轧制制备微米TiB₂和纳米Al₂O₃颗粒增强铝基复合材料。室温时,由于TiB₂和Al₂O₃的综合强化作用,Al₂O₃/TiB₂/Al复合材料的屈服强度和抗拉强度分别为258.7 MPa和279.3 MPa,测试温度升至350℃时,TiB₂颗粒的增强效果显著减弱,原位纳米Al₂O₃颗粒与位错的交互作用使得复合材料的屈服强度和抗拉强度达到98.2MPa和122.5 MPa。经350℃退火1000 h后,由于纳米Al₂O₃对晶界的钉扎作用抑制晶粒长大,强度和硬度未发生显著的降低。     

La2O3含量对Al2O3/Cu基复合材料组织与性能的影响

以La₂O₃粉、Al粉、CuO粉为反应物原料、纯铜为基体,采用原位合成技术和近熔点铸造法制备颗粒增强Cu基复合材料,研究La₂O₃对Al-CuO体系制备的Cu基复合材料组织及性能的影响。结果表明：添加La₂O₃可获得纳米Al₂O₃颗粒,且弥散分布于Cu基体中,制备的材料组织更加细小、均匀,其材料的电导率及摩擦磨损性能明显提高。当添加0.6%wtLa₂O₃,复合材料的电导率达到90.2%IACS,磨损量达到最小,相比未添加La₂O₃,其导电率提高10.1%,磨损量减小36.6%。     

Enhanced thermoelectric properties of n-type Bi2Te3-based nanocomposite fabricated by spark plasma sintering

Highly dense n-type Bi₂Te₃-based thermoelectric materials dispersed with x vol.% γ-Al₂O₃ nanoparticles (x = 0, 0.4, 1.0, 1.5) were fabricated by spark plasma sintering method. The effects of γ-Al₂O₃ addition on microstructure and the thermoelectric properties were studied. It was found that γ-Al₂O₃ nanoparticles locate both at grain boundaries and inside Bi₂Se_0.3Te_2.7 grains. The nanoparticles induce both potential barrier scattering effect and additional phonon scattering effect, which simultaneously enhance the Seebeck coefficient and reduce the lattice thermal conductivity of the nanocomposites in the measured temperature range of 300-500 K, respectively. The maximum dimensionless figure of merit (ZT_max) reaches up to 0.99 for the sample with x = 1.0 at 400 K, which is 35% improvement over the Bi₂Te₃-based matrix. More importantly, the average ZT value of the sample increases from 0.65 to 0.91 in the temperature range 300-500 K, making the nanocomposites much more applicable in cooling and power generation.     

过渡材料对等离子喷涂Al2O3梯度陶瓷涂层性能影响

针对Al2O3陶瓷涂层结合强度低、孔隙率高的实际,选择NiAl金属间化合物和金属铜粉作为过渡材料,利用等离子喷涂制备Al2O3梯度陶瓷涂层,并对梯度涂层进行组织形貌观察,测试结合强度和孔隙率.结果表明,梯度涂层的组织表现出宏观的不均匀性和微观连续性的分布特征,NiAl和Cu是金属基体与Al2O3涂层之间过渡层的理想材料,可以有效地提高涂层的结合强度,而Cu-Al2O3梯度涂层又比NiAl-Al2O3梯度涂层结合强度高;梯度涂层的孔隙率远低于双涂层的孔隙率,在Cu-Al2O3梯度涂层中随Al2O3含量的增加,涂层的孔隙率降低,而且孔隙率低于NiAl-Al2O3梯度涂层.     

Synthesis and characterization of Al2O3-Ce0.5Zr0.5O2 powders prepared by chemical coprecipitation method

Al₂O₃-Ce_0.5Zr_0.5O₂ catalytic powders were synthesized by the coprecipitation (ACZ-C) and mechanical mixing (ACZ-M) methods, respectively. As-synthesized powders were characterized by XRD, Raman spectroscopy, surface area and thermogravimetric analyses. It was found that the mixing extent of Al³⁺ ions affected the phase development, texture and oxygen storage capacity (OSC) of the Ce_0.5Zr_0.5O₂ powder. Single phase of ACZ-C could be maintained without phase separation and inhibit α-Al₂O₃ formation up to 1200 °C. The specific surface area value of ACZ-C (81.5 m²/g) was larger than that of ACZ-M (62.1 m²/g) and Ce_0.5Zr_0.5O₂ (17.1 m²/g) powders, which were calcined at 1000 °C. In comparison with ACZ-C and Al₂O₃, which were calcined at high temperature (900–1200 °C), it was found that the degradation rate of specific surface area of ACZ-C was lower than that of Al₂O₃. ACZ-C sample showed a higher thermal stability to resist phase separation and crystallite growth, which enhanced the oxygen storage capacity property for Ce_0.5Zr_0.5O₂ powders.     

Effect of Bi2O3 on structure and wetting studies of Bi2O3-ZnO-B2O3 glasses

Glasses with different Bi₂O₃ contents (37-42 mol%) have been prepared by conventional melt quench technique. The IR and Raman studies indicate that these glasses are made up of [BiO₆], [BiO₃], [BO₃] and [BO₄] basic structural units. The vibrations of [BiO₃] and [BO₃] become stronger as the content of Bi₂O₃ increases, which makes glass structure loosened. Viscosity of the glasses was measured by using a Rheotronic III paralleled plate rheometry, which shows that the viscosity of glass samples decreased when the content of Bi₂O₃ increased at the same temperature (400-460 °C). The temperature range which suits for glasses sealing was calculated by using the approximation of Arrhenian behaviour. The wetting performance of Bi₂O₃-ZnO-B₂O₃ glasses was described by using high-temperature microscope, which also proves that the structure of investigated Bi₂O₃-ZnO-B₂O₃ glasses become loosened due to the increasing of the content of Bi₂O₃.     

Effects of K2O-Li2O doping on surface and catalytic properties of Fe2O3/Cr2O3 system

The effects of K₂O and Li₂O-doping (0.5, 0.75 and 1.5 mol%) of Fe₂O₃/Cr₂O₃ system on its surface and the catalytic properties were investigated. Pure and differently doped solids were calcined in air at 400-600 °C. The formula of the un-doped calcined solid was 0.85Fe₂O₃:0.15Cr₂O₃. The techniques employed were TGA, DTA, XRD, N₂ adsorption at −196 °C and catalytic oxidation of CO oxidation by O₂ at 200-300 °C. The results revealed that DTA curves of pure mixed solids consisted of one endothermic peak and two exothermic peaks. Pure and doped mixed solids calcined at 400 °C are amorphous in nature and turned to α-Fe₂O₃ upon heating at 500 and 600 °C. K₂O and Li₂O doping conducted at 500 or 600 °C modified the degree of crystallinity and crystallite size of all phases present which consisted of a mixture of nanocrystalline α- and γ-Fe₂O₃ together with K₂FeO₄ and LiFe₅O₈ phases. However, the heavily Li₂O-doped sample consisted only of LiFe₅O₈ phase. The specific surface area of the system investigated decreased to an extent proportional to the amount of K₂O and Li₂O added. On the other hand, the catalytic activity was found to increase by increasing the amount of K₂O and Li₂O added. The maximum increase in the catalytic activity, expressed as the reaction rate constant (k) measured at 200 °C, attained 30.8% and 26.5% for K₂O and Li₂O doping, respectively. The doping process did not modify the activation energy of the catalyzed reaction but rather increased the concentration of the active sites without changing their energetic nature.     

Influences of annealing temperature on microstructure and mechanical properties of Mo-La2O3

Influences of annealing temperature on the microstructure and mechanical properties of Mo-La₂O₃ were investigated. Effects of annealing temperature on tensile properties, fracture toughness, and microhardness are discussed. Microstructure and fracture morphology of Mo alloys are observed by optical microscope, SEM, and TEM. The results indicate that grain size increased while tensile strength, fracture toughness, and microhardness decreased with increasing annealing temperature. Larger La₂O₃ particles are located at grain boundaries or sub-boundaries, while the majority of smaller La₂O₃ particles are located within the grain. The strengthening effect is quantitatively assessed, which yielded a predicted yield strength in good agreement with measurements.     

Photocatalytic performance of nano-photocatalyst from TiO2 and Fe2O3 by mechanochemical synthesis

Nano-particles of homogeneous solid solution between TiO₂ and Fe₂O₃ (up to 10 mol%) have been prepared by mechanochemical milling of TiO₂ and yellow Fe₂O₃/red Fe₂O₃/precipitated Fe (OH)₃ using a planetary ball mill. Such novel solid solution cannot be prepared by conventional co-precipitation technique. A preliminary investigation of photocatalytic activity of mixed oxide (TiO₂/Fe₂O₃) on photo-oxidation of different organic dyes like Rhodamine B (RB), Methyl orange (MO), Thymol blue (TB) and Bromocresol green (BG) under visible light (300-W Xe lamp; λ > 420 nm) showed that TiO₂ having 5 mol% of Fe₂O₃ (YFT1) is 3-5 times higher photoactive than that of P25 TiO₂. The XRD result did not show the peaks assigned to the Fe components (for example Fe₂O₃, Fe₃O₄, FeO₃, and Fe metal) on the external surface of the anatase structure in the Fe₂O₃/TiO₂ attained through mechanochemical treatment. This meant that Fe components were well incorporated into the TiO₂ anatase structure. The average crystallite size and particle size of YFT1 were found to be 12 nm and 30 ± 5 nm respectively measured from XRD and TEM conforming to nanodimensions. Together with the Fe component, they absorbed wavelength of above 387 nm. The band slightly shifted to the right without tail broadness, which was the UV absorption of Fe oxide in the Fe₂O₃/TiO₂ particle attained through mechanochemical method. This meant that Fe components were well inserted into the framework of the TiO₂ anatase structure. EPR and magnetic susceptibility show that Fe³⁺ is in low spin state corresponding to μ_B = 1.8 BM. The temperature variation of μ_B shows that Fe³⁺ is well separated from each other and does not have any antiferromagnetic or ferromagnetic interaction. The evidence of Fe³⁺ in TiO₂/Fe₂O₃ alloy is also proved by a new method that is redox titration which is again support by the XPS spectrum.     

三元共晶成分Al2O3/YAG/ZrO2粉体及陶瓷的制备与组织性能研究

本文采用醇水共沉淀法制备了三元共晶成分Al₂O₃/YAG/ZrO₂粉体,在600-1350_oC温度范围煅烧后研究其物相转变过程。经1300_oC煅烧后Al₂O₃/YAG/ZrO₂共晶成分粉体的物相由α-Al₂O₃、c-ZrO₂和YAG构成,且具有α-Al₂O₃相包裹c-ZrO₂相的特殊结构。将煅烧粉体在1550_oC下热压烧结,制备具有内晶型结构的共晶成分Al₂O₃/YAG/ZrO₂复相陶瓷,其致密度、室温抗弯强度、断裂韧性和高温(1000_oC)抗弯强度分别为98.8%、420 MPa、3.69 MPa.m_1/2和464 MPa,并对复相陶瓷组织结构的形成机理进行了探讨。     

Thermal conductivity and thermal cycle life of La2O3 and HfO2 doped ZrO2-Y2O3 coatings produced by EB-PVD

The effects of La₂O₃ and HfO₂ addition on thermal conductivity and thermal cycle life of EB-PVD YSZ coatings were investigated. La₂O₃ and HfO₂ were selected as additives, because they significantly suppress the sintering of YSZ. The developed coating showed low thermal conductivity as well as high resistance to sintering. Burner rig tests confirmed that the developed coating have a superior thermal insulating effect and have a longer life than that of a coating with conventional composition.     

CaO-Bi2O3-MoO3-xNb2O5复合掺杂对高磁导率Mn-Zn铁氧体的微观结构和电磁性能的影响

采用高温固相反应制备了CaO-Bi_2O_3-MoO_3-XNb_2O_5(X=0.000%~0.075%,质量分数,步长:0.015%)复合掺杂的高磁导率Mn-Zn铁氧体材料,利用XRD、SEM、四探针电阻测试仪、阻抗分析仪、和软磁测试仪等分析测试手段对材料结构和性能进行表征,研究了复合掺杂剂中Nb_2O_5掺杂量对高磁导率Mn-Zn铁氧体材料的结构和电磁性能的影响。结果表明:当Nb_2O_5少量掺杂时,Nb_2O_5可以改善材料的微观结构,提高其密度、频率稳定性和品质因数,提高其电阻率,降低其体积功耗;当Nb_2O_5过量掺杂时,Nb_2O_5将恶化材料的微观结构,导致材料的电磁性能变差。当Nb2O5掺杂量为0.030%时材料的综合电磁性能最佳。