ZrB_2-SiC复相陶瓷的注浆成形与无压烧结

研究了ZrB2-SiC复相陶瓷的注浆成形技术,着重讨论了pH值和固相体积含量对料浆粘度的影响;分析了注浆成形后,生坯断面的显微结构以及相对应的烧结体的显微结构。结果表明:ZrB2原始粉料的研磨处理有利于复相陶瓷制品的烧结致密化。当pH值为11时,可制得固相体积含量为50%,粘度为660mPa.s的ZrB2-SiC浆料。     

ZrB_2-SiC复相陶瓷制备方法研究现状

综述了ZrB2-SiC复相陶瓷近年来的研究现状。总结了无压烧结、反应热压烧结、热压烧结、放电等离子烧结和一些其他方法制备ZrB2-SiC复相陶瓷的研究成果,并提出了ZrB2-SiC复相陶瓷目前研究中存在的问题和今后潜在的发展方向。     

硼化锆基碳化硅复相陶瓷

以钇铝石榴石(yttrium aluminum garnet,YAG)为烧结助剂,通过无压烧结工艺制备了ZrB2-SiC复相陶瓷.研究了复相陶瓷的相组成、抗烧蚀性能以及烧结助剂含量、烧结温度对复相陶瓷力学性能和显微结构的影响.结果表明:复相陶瓷的物相组成主要为ZrB2,SiC和少量玻璃相;添加YAG或提高烧结温度能使材料的晶粒显著长大,并显著提高材料的相对密度和力学性能.当YAG含量为9%(质量分数),烧结温度为1 800℃时陶瓷的相对密度为97.1%、Rockwell硬度HRa为88、弯曲强度为296MPa、断裂韧性为5.6MPa·m1/2.复相陶瓷具有优异的超高温抗烧蚀性能,在2800℃烧蚀30min,烧蚀率仅为0.001 mm/s,烧蚀后的显微结构呈现复杂的多层结构.     

ZrB2-SiC复相陶瓷的制备及其性能的研究

以ZrB2和SiC粉为原料,采用Si3N4球为球磨介质,通过等静压成型及无压烧结制备了ZrB2-SiC复相陶瓷。实验确定了ZrB2-SiC复相陶瓷的烧结制度,并研究了SiC含量与球磨时间对ZrB2-SiC复相陶瓷体积密度的影响。结果表明:随着ZrB2球磨时间的增加,ZrB2颗粒粒径逐渐减小,复相陶瓷的体积密度逐渐增加;随着SiC含量的增加,复相陶瓷体积密度降低。ZrB2最佳球磨时间为6h,SiC最佳含量为20%,ZrB2-SiC20%(体积分数)复相陶瓷体积密度达到4.98g/cm3。     

ZrB2-SiC复相陶瓷的制备及其力学性能研究

以ZrB2和SiC粉为原料,采用Si3N4球为球磨介质,通过热压烧结制备了ZrB2-SiC复相陶瓷.并对ZrB2-SiC复相陶瓷进行了相对密度、力学性能检测和微观结构分析.结果表明:随着ZrB2球磨时间和SiC含量的增加,该复相陶瓷相对密度先增加后略有降低,ZrB2最佳球磨时间为8小时,SiC最佳含量为20vol.%.ZrB2+20vol.%SiC复相陶瓷的相对密度达到98.3%,抗弯强度达到631±4MPa,断裂韧性达到5.4±0.2 MPa·m1/2.随着球磨时间的增加,ZrB2+20vol.%SiC复相陶瓷的断裂方式由穿晶断裂向沿晶断裂转变.     

液相烧结SiC陶瓷

采用Al2O3、Y2O3为助烧剂,热压烧结获得了致密的α-SiC和β-SiC陶瓷,研究了起始粉末的性能对烧结体的物相组成和显微结构的影响。实验结果表明,Al2O3、Y2O3原位形成了YAG,材料以液相烧结机制致密化,并通过溶解和再析出机制,促进晶体生长。物相分析表明,β-SiC陶瓷粉末在烧结过程中发生了β→α的相变。显微结构观察显示,β-SiC陶瓷中生成了长柱状晶粒。     

ZrB2-SiC/C层状复合陶瓷的高温氧化行为

利用流延法成膜和热压烧结工艺制备出了ZrB2-SiC层和石墨层交替排列、层厚均匀、界面清晰的ZrB2-SiC/C层状复合陶瓷.采用循环氧化法对ZrB2-SiC和ZrB2-SiC/C层状复合陶瓷在1000℃及1300℃空气中的氧化动力学曲线进行了研究.结果表明:在1000℃氧化增重时,ZrB2-SiC/C层状复合陶瓷在氧化反应初期表现为氧化增重,随着时间的增加,表现为氧化减重.在1300℃时,ZrB2-SiC/C层状复合陶瓷由于基体层ZrB2-SiC和弱夹层石墨相的氧化规律的相互叠加,使得其氧化增重曲线表现为抛物线规律.由XRD分析及扫描电镜观察发现,1300℃氧化15 h后,试样中不存在弱夹层石墨相,由于石墨相的挥发,材料残留孔隙.     

热压烧结制备AlN-Al2O3复相陶瓷及其性能

以AlN和Al2O3为原料,Y2O3为烧结助剂,在N2气氛下热压烧结制备出AlN-30%(质量分数)Al2O,复相陶瓷:运用X射线衍射、扫描电子显微镜和透射电子显微镜表征复相陶瓷的相组成及显微结构.研究了烧结温度对AlN-Al2O3复相陶瓷的相组成、显微结构、烧结性能、力学性能、热导率和介电性能的影响.结果表明:在1 ...     

ZrB2-SiC复合材料凝胶注模成型初探

研究了ZrB2-SiC复合材料的凝胶注模成型技术。着重讨论了分散剂、pH值、固相体积含量、有机单体等对ZrB2-SiC复合材料料浆的影响;分析了凝胶注模成型后,排胶前复合材料素坯断面的显微结构以及相对应的烧结体的显微结构。结果表明:当分散剂用量为8.74‰(质量分数),pH为10.8,有机单体含量为3.1%时,可制得固相体积含量为40%,粘度为610mPa.s的ZrB2-SiC复合浆料,此时烧结体的断面主要以穿晶断裂为主;凝胶注模成型的坯体内部的有机聚合物网络因高温而完全分解,使素坯的气孔分布较均匀,利于烧结体致密度的提高。     

ZrB2对Al2O3-ZrB2-SiC复相陶瓷室温力学性能影响

Al2O3陶瓷具有优异的室温和高温性能,但其脆性大,断裂韧性较低,限制了其应用.采用热压烧结工艺制备了应用于不同环境的Al2O3-ZrB2-SiC复相陶瓷(简称AZS),主要研究不同含量的ZrB2对Al2O3-SiC基陶瓷性能的影响.力学性能研究发现,当Al2O3陶瓷中ZrB2和SiC的体积百分比分别为20％和5％时,AZS3陶瓷具有最高的强度和韧性,分别为508.5MPa和6.65MPa· m1/2,相比纯氧化铝陶瓷的468.6MPa和5.56 MPa· m1/22提高了8.5％和19.6％.     

Different microstructure BaO–B2O3–SiO2 glass/ceramic composites depending on high-temperature wetting affinity

In this work, we propose a simple but effective method to fabricate BaO–B₂O₃–SiO₂ glass/ceramic composites with different microstructures that depend on the high-temperature wetting affinity. The experimental results showed that the wetting affinity between oxide ceramic and the BaO–B₂O₃–SiO₂ glass matrix could strongly affect the driving force of densification and crystallization and finally the microstructure of the glass/ceramic composites. It was found that suitable amounts of alumina powders could obviously increase the driving force for sintering of glass by increasing the capillary pressure. In this case, the contact angle between alumina and glass matrix is about 24° at high temperature and a densified and homogeneous microstructure of glass/alumina composite was obtained. On the contrary, rutile powders additive was found to result in higher phase separation and crystallization during the sintering of glass/rutile composites. In this case, the contact angle between rutile and glass matrix is about 124° at high temperature, and the sintered body has a lower dielectric loss than the sample with alumina additive. Therefore, the microstructure and dielectric property of glass/ceramic composites could be controlled by adjusting the ceramic composition and wetting affinity between ceramic additive and glass matrix in our study.     

Thermal conductivity of spark plasma sintered SiC ceramics with Alumina and Yttria

In this study, dense SiC ceramics were fabricated at 1650?1750 °C for 10?60 min by spark plasma sintering (SPS) using 3?10 wt.% Al₂O₃-Y₂O₃ as sintering additives. Effects of sintering temperature, sintering additive content and holding time on microstructure as well as correlations between microstructure and thermal conductivity were investigated. An increase in the sintering temperature promotes grain growth. Extending holding time has little influence on grain size but results in formation of continuous network of sintering additive, which increases interfacial thermal resistance and thus decreases thermal conductivity. For SiC ceramics composed of continuous SiC matrix and discrete secondary phase (yttrium aluminum garnet, YAG), an increase in the sintering additive content results in smaller grain size and lower thermal conductivity. The lower thermal conductivity of the SiC ceramic with higher sintering additive content is mainly due to the smaller grain size rather than the low intrinsic thermal conductivity of YAG.     

液相烧结氧化铝和氧化钇稳定四方氧化锆复相材料的显微结构与力学性能

以TiO2，MnO2及CaO—Al2O3-SiO2玻璃为烧结助剂，利用液相烧结法制备了氧化铝和3％氧化钇稳定四方氧化锆复相材料。研究了烧结助荆对材料致密化、显微结构及力学性能的影响。结果表明：除TiO2可与ZrO2晶粒形成部分固溶外，烧结助剂主要以晶间玻璃相的形式存在，并影响了Y2P3在ZrO2晶粒中的分布。烧结助荆的引入显著促进材料的致密化，降低了烧结温度，使材料具有细晶结构，因而具有良好的力学性能。     

Anomalous enhancement of photoluminescence intensity of sintered YAG:Ce particles‐embedded glasses

For high‐power white LED applications, YAG:Ce‐based yellow phosphors were embedded in a low‐T_g Bi₂O₃–B₂O₅–ZnO–Sb₂O₅ glass by sintering route. Effects of sintering temperature (325‐390°C) on the microstructure and photoluminescence properties were investigated. X‐ray diffraction was used to measure the retained fraction of YAG:Ce phase after sintering. Scanning electron microscope and transmission electron microscope, equipped with energy‐dispersive X‐ray spectrometry, were used to examine the microstructure, including the element distribution across the phosphor–glass interface. Photoluminescence properties of the samples before and after sintering were compared. With the increasing sintering temperature, the retained fraction of YAG:Ce decreased from 83.3% to 82%. This effect tends to reduce the luminescence intensity of the samples after sintering. The increasing sintering temperature also enhances the diffusion of cations (esp. Bi) from glass matrix to YAG:Ce. This effect tends to increase the luminescence intensity of the YAG:Ce particles after sintering. When the sintering temperature was lower (325°C), the effect of YAG:Ce loss was dominant, thus the luminescence intensity was reduced after sintering. When the sintering temperature was higher (350‐390°C), the effect of solute dissolution was dominant, resulting in luminescence intensity anomalously higher than that before sintering. Similar result has not been reported in literatures. The maximum luminescence intensity of the sintered samples is 1.57 times as high as that of the samples before sintering.     

Rapid Reactive Synthesis and Sintering of Submicron TiC/SiC Composites through Spark Plasma Sintering

Submicrometer TiC/SiC composites were fabricated by a rapid reactive sintering process through spark plasma sintering (SPS) technique using the carbon, titanium, and nanosized-SiC powders without any additive. It was found that the composite could be sintered in a relatively short time (8 min at 1480°C) to 97.9% of theoretical density. After sintering, the phase constituents and microstructures of the samples were analyzed by X-ray diffraction techniques and observed by scanning electron microscopy. The effect of nanosized and microsized SiC additives on the microstructure of TiC/SiC composites was investigated.     

Suppression of phosphor‐glass reactions in YAG:Ce phosphor‐embedded glasses

For high‐power white LED applications, YAG:Ce‐based yellow phosphors were embedded in a low‐T_g Bi₂O₃–B₂O₅–ZnO–Sb₂O₅ glass (BiG) by sintering route. A high‐T_g silicate glass (SiG) was also used for comparison. Dense (porosity<2%) phosphor‐glass composites were obtained after sintered at 800°C (for SiG) and 325°C (for BiG). XRD quantitative analysis indicates that the loss of phosphor content is in the range of 2.5%‐22%, caused by partial dissolution of phosphor particles into the glass matrix during sintering. The element distribution across the interface and within the reaction zone between phosphor and glass was analyzed by TEM/SEM‐EDS. The intrinsic emission characteristic of YAG:Ce is nearly not altered, possibly resulted from the slight modification of the YAG phase during sintering. Thus the final emission intensity of the sintered body is mainly determined by the residual amount of the YAG:Ce phase. Replace the high‐T_g SiG glass by the low‐T_g BiG glass, prenitridize the YAG:Ce phosphor, and change the sintering atmosphere from air to N₂ suppress the loss of phosphor during sintering. Therefore, the resulting loss of emission intensity of the phosphor‐embedded glass material can be reduced to only about 1.8%.     

Microstructure and Mechanical Properties of ZrB2-Based Composites Reinforced and Toughened by Zirconia

The present work reported the effect of addition of ZrO₂ on the microstructure and mechanical properties of ZrB₂-based ceramic composites by means of hot-pressed sintering. Observation of microstructure and systematic testing results of mechanical properties were carried out. Through X-ray diffraction analysis and calculation of the volume fraction of ZrO₂ phase transformability, the toughening mechanism of the present composites was explored. The phase transformation toughening by ZrO₂ additive played an important role in improving the fracture toughness of ZrB₂-based composites.     

Pressureless reaction sintering of yttrium aluminium garnet (YAG) from powder precursor in the hydroxyhydrogel form

Pressureless reaction sintering of YAG was carried out by using a precursor powder in the hydroxyhydrogel form synthesized by flash polycondensation technique. Reactive silica additive was used to modify Al-O-Y network where Si⁴⁺ was incorporated in the solvated form. The sintering experiments were carried out with the processed powder up to 1650 °C under ambient ambience. Densification indicated effective sintering with well-formed microstructure. Phase identification by XRD indicated only YAG in the sintered specimen.     

SPS烧结制备新型荧光玻璃材料

以实验室自制SiO2粉体和商用Ce∶YAG荧光粉为玻璃原料,采用放电等离子体烧结（SPS）技术,在1 200℃保温2 min烧结得到有望用于白光LED封装的Ce∶YAG荧光玻璃。用X射线衍射仪（XRD）、荧光光谱（PL）等方法对制备获得的荧光玻璃样品进行表征。结果显示,烧结并没有破坏Ce∶YAG荧光粉的晶体结构,且荧光玻璃主体相仍为玻璃体,该荧光玻璃在460nm具有强吸收峰,在此波长激发下发射出530 nm左右的黄光。研究结果表明,本实验制备的Ce∶YAG荧光玻璃是一种具有重要应用前景的LED封装用新型荧光材料。