ZrB2-ZrSi2-SiC composites prepared by reactive spark plasma sintering

ZrSi₂ and SiC are good candidates to improve both sinterability and mechanical properties of ZrB₂ ceramics, which were synthesized simultaneously by an in-situ reaction of ZrC and Si additives during the sintering processing in this work. The ZrB₂ ceramic composites with different amount of ZrSi₂ and SiC were fabricated by reactive spark plasma sintering (RSPS) method. X-ray diffraction, scanning microscopy and Archimedes's method are used to characterize the phase, microstructure and density of the composites. Meanwhile, fracture toughness and flexural strength of the obtained composites were investigated too. It's found that a fully dense composite can be achieved at 1500 °C by SPS. Both fracture toughness and flexural strength of ZrB₂ ceramics increased with increasing the concentration of ZrSi₂ and SiC additives and reached a maximum of 7.33 ± 0.24 MPa·m^1/2 and 471 ± 15 MPa, respectively, with the ZrSi₂ + SiC content of 30 wt%.     

MoSi_2/ZrB_2基超高温陶瓷SPS制备研究

ZrB2具有良好的抗氧化、抗热震和抗烧蚀性能。采用放电等离子体烧结(SPS)工艺,添加体积分数为10%~20%的MoSi2烧结助剂,选取不同的烧结参数,制备出超高温陶瓷成品。经测试,ZrB2-15%MoSi2(体积分数)体系的陶瓷致密度可达99.88%,维氏硬度可达1 612,通过SEM分析,该陶瓷具有典型的核(ZrB2)-壳(MoSi2、MoB)结构,可以作为高超声速飞行器热防护用陶瓷材料的候选方案。     

Effect of SiC nano-whisker addition on TiCN-based cermets prepared by spark plasma sintering

TiCN-based cermets with different amounts of SiC nano-whisker were prepared by spark plasma sintering at 1350 °C with an initial pressure of 30 MPa and a holding time of 8 min. The microstructural and mechanical properties of the as-prepared samples were investigated. The addition of SiC nano-whisker has a significant effect on the cermets, resulting in 6% increase in Vickers hardness and 63% increase in flexural strength, respectively, when 2.5 wt.% of SiC nano-whisker was added, as compared with its counterpart without whisker. X-ray diffraction analysis revealed that no SiC peaks were detected but some peaks of new hard phases due to the reactions of SiC with the cermet matrix. The resultant hard phases were present normally in the grain boundary in the cermets on the basis of observation by transmission electron microscopy, and they are responsible for the hardness increase of the as-obtained cermets. The observation by scanning electron microscopy on the microstructure indicated that the fracture mechanism of the as-obtained cermets was mainly inter-granular of TiCN grains.     

Spark plasma sintering of ZrB2-based composites co-reinforced with SiC whiskers and pulverized carbon fibers

Spark plasma sintering (SPS) process was used to preparation of ZrB₂-based composites co-reinforced with SiC whiskers as well as various amounts of pulverized carbon fibers. The effects of C_F content on microstructure and mechanical characteristics of ZrB₂–SiC_w–C_F composites were scrutinized. Although all composites approached high densification, a fully-dense sample was fabricated by the addition of 2.5 wt% C_F. The growth of ZrB₂ grains was remarkably inhibited in C_F-reinforced composites. No in-situ formed phase was detected by XRD; however, trace of nano-ZrC clusters was observed in SEM fractographs of ZrB₂–SiC_w–C_F samples. The formation of such nano-sized ZrC refractory phase was also proved by thermodynamics. The hardness of composites slightly decreased from 21.9 to 19 GPa with increasing the C_F content. Reversely, the fracture toughness values enhanced from 4.7 to 6 MPa.m^½ with increasing the amount of pulverized carbon fibers.     

Corrosion of MCrAlY: Pt composites prepared by spark plasma sintering

Cyclic oxidation tests of sintered MCrAlY:Pt composites were carried out at temperatures of 1223 and 1273?K. Composite tablets were previously produced by spark plasma sintering. To assess an effect of platinum dispersed, microstructural characterisation was performed on the tablets before and after the cyclic oxidation treatment. Scanning electron microscopy analysis of the oxide layer showed that the presence of typical α-Al₂O₃ and NiAl₂O₄ spinel had structure columnar and equiaxial in both samples. Fine sintered microstructure and addition of Pt into the MCrAlY matrix enhanced the resistance of the material to cyclic oxidation.     

Hydrogen storage performance of Mg-based composites prepared by spark plasma sintering

The hydrogen storage capacities, hydrogen absorption mechanism and hydride stability of Mg-based composites prepared by spark plasma sintering (SPS) were investigated in this paper. The results showed that the composites had a double-phase microstructure of Mg phase and V-based solid solution, with nanocrystalline magnesium existing at their sintering interface. With the addition of the V-based solid solution in 20% volume fraction, the composite exhibited a maximum reversible hydrogen storage capacity of 4.2 wt.% at 573 K, compared with that of pure Mg of almost zero. DSC results indicated that the hydride decomposition temperature of MgH₂ decreased sharply from 708 K in pure Mg to 636 K and to 591 K as the volume of V-based solid solution increased from 20 vol.% to 50 vol.%. With the addition of V-based solid solution, the hydrogen absorption kinetics of pure Mg was greatly improved at 573 K, and its hydrogen absorption mechanism changed from surface reaction control to diffusion control in the composite. Based on these experimental results, a model was put forward to describe the hydrogen absorption/desorption mechanism in these composites.     

Si含量对放电等离子烧结制备(1-x)Ti3SiC2+xSiC复合材料的影响

以钛粉、硅粉和石墨粉为原料,制备出(1-x)Ti3SiC2+xSiC(x=0.1～0.8)复合材料,并利用X射线衍射仪对样品进行相组成分析.结果表明经1300℃放电等离子烧结15min后,可以得到纯净的0.9Ti3SiC2-0.1SiC和含有 微量石墨的0.2Ti3SiC2-0.8SiC复合材料,0.9Ti3SiC2-0.1SiC和0.2Ti3SiC2-0.8SiC复合材料的显微硬度分别为8.8和10.5GPa,均明显高于Ti3SiC2的(4GPa).随着SiC含量的增加,复合材料的硬度也增加,但杂质(石墨)和孔洞的含量也增多,成分为0.5Ti3SiC2-0.5SiC的复合材料在烧结过程中有少量Si流出;而当SiC含量增加到0.2Ti3SiC2-0.8SiC时,烧结过程中大量的Si流出使得复合材料无法成功烧结.     

Effect of sintering process on the microstructures and properties of in situ TiB2–TiC reinforced steel matrix composites produced by spark plasma sintering

Spark plasma sintering (SPS) is a new technique to rapidly produce metal matrix composites (MMCs), but there is little work on the production of TiB₂–TiC reinforced steel matrix composites by SPS. In this work, in situ TiB₂–TiC particulates reinforced steel matrix composites have been successfully produced using cheap ferrotitanium and boron carbide powders by SPS technique. The effect of sintering process on the densification, hardness and phase evolution of the composite is investigated. The results show that when the composite is sintered at 1050 °C for 5 min, the maximum densification and hardness are 99.2% and 83.8 HRA, respectively. The phase evolution of the composite during sintering indicates that the in situ TiB₂–TiC reinforcements are formed by a hybrid formation mechanism containing solid–solid diffusion reaction and solid–liquid solution-precipitation reaction. The microstructure investigation reveals that fine TiB₂–TiC particulates with a size of ～2 μm are homogeneously distributed in the steel matrix. The TiB₂–TiC/Fe composites possess excellent wear resistance under the condition of dry sliding with heavy loads.     

Microstructure and mechanical properties of magnesium composites prepared by spark plasma sintering technology

Spark plasma sintering (SPS) technology was used to determine the appropriate conditions for SPS sintering of commercially pure magnesium as well as the magnesium alloy AZ31. It was found that the sintering temperatures of 585 °C and 552 °C were the most suitable sintering temperatures for the magnesium and the AZ31 alloy, respectively. Magnesium matrix and AZ31 alloy matrix composites reinforced with SiC particles were then successfully fabricated by the SPS method at sintering temperatures of 585 °C and 552 °C, respectively. A uniform distribution of SiC particles was observed along the boundary between matrix particles. The mechanical properties, i.e. hardness and tensile strength increased with increasing SiC content up to 10 wt%. However, when the SiC content was larger than 10 wt%, the tensile strength decreased due to the agglomeration of SiC particles. The agglomeration of SiC particles was found to lead to the degradation of the interfacial bonding strength between matrix and reinforcement.     

Microstructure,sintering behavior and mechanical properties of SiC/MoSi2 composites by spark plasma sintering

SiC/MoSi₂ composites were synthesized at different temperatures by spark plasma sintering using Mo, Si and SiC powders as raw materials. The phase composition, microstructure and mechanical properties of the as-prepared composites were investigated and the sintering behavior was also discussed. Results show that SiC/MoSi₂ composites are composed of MoSi₂, SiC and trace amount of Mo_4.8Si₃C_0.6 phase and exhibit a fine-grain texture. During the synthesis process, there was an evolution from solid phase sintering to liquid phase sintering. When sintered at 1600 °C, the SiC/MoSi₂ composites present the most favorable mechanical properties, the Vickers hardness, bending strength and fracture toughness are 13.4 GPa, 674 MPa and 5.1 MPa·m^1/2, respectively, higher 44%, 171%, 82% than those of monolithic MoSi₂. SiC can withstand the applied stress as hard phase and retard the rapid propagation of cracks as second phase, which are beneficial to the improved mechanical properties of SiC/MoSi₂ composites.     

不同结合剂原料放电等离子烧结制备TiC/Ti3SiC2复合结合剂金刚石复合材料

分别以Ti/Si/2TiC混合粉体和Ti₃SiC₂单相粉体作为结合剂原料,采用放电等离子体烧结技术合成了TiC/Ti₃SiC₂结合剂金刚石复合材料,探讨不同的结合剂原料和保温时间对TiC/Ti₃SiC₂结合剂金刚石复合材料的物相构成、微观形貌以及磨削性能的影响。结果表明:采用Ti/Si/2TiC为结合剂原料,保温1 min时,会形成较多量的Ti₃SiC₂,Ti₃SiC₂基体与金刚石结合良好,二者之间没有孔隙;当保温5 min时,Ti₃SiC₂发生分解,基体主相转变为TiC,同时有一定量的Si,金刚石表面被侵蚀,形成凹凸不平的表面。采用Ti₃SiC₂为结合剂原料时,Ti₃SiC₂基体发生严重的分解,生成TiC和Si;金刚石与基体间存在一个过渡层,厚度约15 μm。Ti/Si/2TiC为结合剂原料保温1 min时试样的磨耗比值最大,为1 128。单相Ti₃SiC₂为结合剂的2个试样的磨耗比值约为100左右。      

Electrochemical corrosion and bioactivity of titanium–hydroxyapatite composites prepared by spark plasma sintering

The corrosion resistance and bioactivity of titanium–hydroxyapatite (Ti–HA) composites prepared by mechanical alloying (MA) followed by spark plasma sintering were investigated. Potentiodynamic polarization tests showed that Ti composites containing 0–10% HA exhibited higher corrosion resistance than commercially pure Ti. An increase in HA concentration (20–30%) decreased corrosion resistance owing to the craterlike defects induced by ceramic particle detachment. Increasing MA time significantly reduced defect density and improved corrosion resistance. Bioactivity test on Ti HA composites in simulated body fluid revealed the growth of a nano-HA layer, which indicates the high potential of Ti–HA composites for application in biomedical implants.     

放电等离子烧结法制备Cu/金刚石复合材料的性能与显微组织

由于具备较高的热导率,铜/金刚石复合材料已成为应用于电子封装领域的新一代热管理材料。采用放电等离子烧结工艺（SPS）成功制备含不同金刚石体积分数的Cu/金刚石复合材料,研究复合材料的相对密度、微观结构均匀性和热导率（TC）随金刚石体积分数（50%、60%和70%）和烧结温度的变化规律。结果表明：随着金刚石体积分数的降低,复合材料的相对密度、微观结构均匀性和热导率均升高;随着烧结温度的提高,复合材料的相对密度和热导率不断提高。复合材料的热导率受到金刚石体积分数、微观结构均匀性和复合材料相对密度的综合影响。     

Bulk WC-Al2O3 composites prepared by spark plasma sintering

WC and WC-Al₂O₃ materials without metallic binder addition were densified by spark plasma sintering in the range of 1800-1900 °C. The densification behavior, phase constitution, microstructure and mechanical properties of pure WC and WC-Al₂O₃ composite were investigated. The addition of Al₂O₃ facilitates sintering and increases the fracture toughness of the composites to a certain extent. An interesting phenomenon is found that a proper content of Al₂O₃ additive helps to limit the formation of W₂C phase in sintered WC materials. The pure WC specimen possesses a hardness (HV₁₀) of 25.71 GPa, fracture toughness of 4.54 MPa·m^1/2, and transverse fracture strength of 862 MPa, while those of WC-6.8 vol.% Al₂O₃ composites are 24.48 GPa, 6.01 MPa·m^1/2, and 1245 MPa respectively. The higher fracture toughness and transverse fracture strength of WC-6.8 vol.% Al₂O₃ are thought to result from the reduction of W₂C phase, the crack-bridging by Al₂O₃ particles and the local change in fracture mode from intergranular to transgranular.