纳米氧化钛陶瓷的烧结

将醇盐水解制备的纳米氧化钛粉体（～13nm）在500～800℃下煅烧,用XRD研究氧化钛相变过程中粉体的热稳定性,发现在加入0．4wt％的金红石相作为晶种后;晶粒生长受到较好的控制,同时分别在30、57和200MPa下对纳米氧化钛样品进行热压烧结,用密度仪、压汞仪和SEM对烧结前后的样品进行表征后表明,700℃的热压烧结样品已开始致密化,200MPa、800℃热压烧结样品的相对密度为97．2％,此时3～15nm的小气孔仍难以消除,这些小气孔的存在是纳米氧化钛陶瓷在较高的压力下难以完全致密的主要原因．     

溶胶-凝胶法制备CaCu_3Ti_4O_(12)粉体及其电性能

利用溶胶-凝胶法制备CaCu3Ti4O12粉体,采用差热分析、X射线衍射、扫描电子显微镜等技术进行表征,并探讨CaCu3Ti4O12粉体的烧结特性及电性能。结果表明,干凝胶经750℃低温煅烧可获得粒径分布较窄、平均粒径为80～100 nm的CaCu3Ti4O12粉体。CaCu3Ti4O12陶瓷在1 000℃时实现致密烧结,比固相反应法制备的粉体烧结温度降低100～200℃,具有较宽的烧结温区。溶胶-凝胶法制备的陶瓷经1 050℃烧结2 h,获得优良的电性能,相对介电常数为20 190,介电损耗为0.022,非线性系数为4.530。     

燃烧法合成铪酸钇粉体及其透明陶瓷的制备

以硝酸钇(Y(NO₃)₃)和氯化铪(HfCl₄)为原料, 乙二胺四乙酸(EDTA)作为燃剂, 采用燃烧法制备了粒径为50nm左右的纯相铪酸钇粉体. 粉体经1200℃煅烧后高能球磨15h, 然后在200MPa条件下进行冷等静压成型, 素坯尺寸为20mm×2.5mm, 最后采用真空烧结(1850℃保温6h), 制备出可见光波段直线透过率为50%的铪酸钇透明陶瓷. 研究了真空烧结温度对样品透过率和显微结构的影响, 当烧结温度高于1850℃时, 温度对于透过率影响不是很明显; 随着烧结温度的升高, 样品的晶粒尺寸增大.     

SPS烧结制备TiB2/TiC复合材料

采用金属钛粉和碳化硼为初始粉料,利用SPS放电等离子烧结技术制备了致密的纳米结构TiB2/TiC复合材料.并借助XRD、SEM考察了复合材料的相组成和显微结构,利用压痕法和小样品力学性能测试方法(MSP)测定了室温显微硬度、断裂韧性和MSP强度.研究结果表明:利用一步法直接升温至1550℃并保温6 min制备的复合材料,其晶粒尺寸大于1μm,MSP强度为833 MPa.而采用两步法升温至1550℃,然后迅速降低保温温度至1450℃,并保温6 min条件下使金属钛粉和碳化硼同步完成反应、烧结、致密化,生成晶粒细小的TiB2/TiC复合材料,晶粒尺寸大约为200 nm,并且所制备的复合材料力学性能更好,MSP强度达到1095 MPa.     

低温制备高致密度细晶W-10％TiC复合材料

采用高能球磨结合真空热压的手段制备了W-10％（质量分数）TiC复合材料。采用扫描电镜、透射电镜和x射线衍射等对复合粉体及复合材料进行表征。结果表明，通过高能球磨得到了粒径均匀，平均粒径约为100nm的纳米复合粉体，粉体经过1700℃真空热压烧结后致密度达到99．1％，并且保持细晶结构（平均晶粒尺寸为0．8gm）。热压和高能球磨导致的机械活化以及引入的Fe、Ni等杂质是复合材料低温烧结达到高致密度的重要原因。     

固相反应法合成碳化硼纳米粉体

以六方氮化硼和炭黑(或石墨)为原料, 采用固相反应法合成了碳化硼粉体. 碳源、反应气氛和温度对粉体合成产生重要影响. 以炭黑为碳源, 在1900℃真空下保温5 h, 得到了平均粒径约为100 nm的碳化硼纳米粉体. 与商业粉体相比, 合成的粉体具有较好的烧结活性. 在2000℃/30 MPa/1 h条件下烧结, 样品的相对密度达到97.9%(商业粉体样品为93.1%), 这可归结于合成的粉体具有细小的粒径、低的氧含量和一定程度的孪晶结构.     

AlN粉末特性对AlN-BN复合陶瓷致密化的影响

以比表面积分别为4.26和17.4 m2/g两种AlN粉末为原料,添加5%Y2O3作为烧结助剂制备AlN-15BN陶瓷(质量分数,%),研究了AlN粉末特性对复合陶瓷致密化过程的影响。结果表明,AlN粉末比表面积对复合陶瓷致密化有重要影响,比表面积高的AlN粉末所制备的复合陶瓷致密化过程主要发生在1500~1650℃,1650℃烧结3 h后,复合材料的相对密度达95.6%,继续升高温度,对材料的密度影响不大;而低比表面积的AlN粉末所制备的复合陶瓷的致密化过程主要发生在1650~1850℃,1850℃烧结3 h,复合陶瓷的相对密度为86.4%。即高比表面积的AlN粉末有利于获得相对密度高的AlN-BN复合材料。     

氧化锆纳米粉体烧结性能研究

为了研究纳米氧化锆粉体的烧结性能,以4种不同粒度的氧化锆粉体为原料,在热分析仪上测试了室温～1000℃范围内坯体的形变量和热膨胀性能.采用1450℃恒温1～6 h的烧结工艺,制备了氧化锆陶瓷,并进行了性能表征.结果表明:粉料1次粒子粒径越小,其初始烧结温度越低;粉料的团聚粒径越小,分布越窄,坯体的烧结致密化越容易.     

聚合物前驱体法制备(Ce,Cu)-SnO2纳米粉体及其烧结行为

采用聚合物前驱体法制备了CeO2-CuO-doped SnO2纳米粉体,并研究了掺杂SnO2纳米粉体的无压烧结行为.结果表明乙二醇、柠檬酸与金属离子的摩尔比为631时制得的掺杂SnO2粉体为分散良好的球形颗粒,大小为～15nm,粒度分布范围窄;CuO掺杂可显著提高SnO2的烧结性能,CeO2-CuO复合掺杂可进一步降低SnO2陶瓷的致密化温度;1.0%CeO2-1.5%CuO-doped SnO2可在1050℃烧结致密,相对密度达96%以上;两步法(先升温到1050℃保温15min,然后降到980℃烧结5h)烧结的1.0%CeO2-1.5%CuO-doped SnO2陶瓷相对密度为96.1%,其晶粒＜800nm.     

纳米钛酸钡粉体的制备和烧结动力学研究

以四氯化钛、八水合氢氧化钡和氨水为原料,首先制备出氢氧化钛凝胶,然后以乙醇为溶剂,采用两步沉淀法在低温常压下合成了立方相纳米钛酸钡粉体.研究了反应温度、反应物浓度和反应时间对粉体物相和粒径的影响,利用XRD和TEM对粉体进行了表征.实验结果表明,在低于80℃的反应温度下可以制备出粒径＜20nm、结晶性能良好且形貌规则的纳米钛酸钡粉体.此外,以合成的粉体为原料,以热膨胀仪为测试手段,对钛酸钡陶瓷的烧结动力学进行了研究.结果表明,陶瓷的烧结温度为1150～1250℃,在1250℃的烧结温度下保温2h,陶瓷坯体的相对密度约93%,室温介电常数约4020.     

Al_2O_3/B_4C的致密化机制

初始晶粒尺寸为0.33μm和7.0μm的Al2O3/14%B4C粉末在不同温度烧结,并模拟计算陶瓷粉末烧结过程。通过对比实验结果和计算结果,找出影响材料致密化的机制,讨论晶粒尺寸对扩散机制的影响,并估算出致密化激活能。在实验烧结温度范围内,界面反应被认为是影响Al2O3/B4C粉末致密化过程的主要因素。Al2O3/14%B4C陶瓷的致密化激活能是1820±60KJ.mol-1,这结果很大程度上支持界面反应致密化机制。     

Constitutive modeling of alumina sintering: grain-size effect on dominant densification mechanism

In the present work, alumina powders with the initial grain sizes of 0.9 and 7.0 μm, respectively, were sintered at different temperatures. Constitutive laws for densification were employed to model the sintering process of alumina ceramics. Based on the constitutive laws employed and the experimental results obtained, the dominant densification mechanism was identified and the effect of grain size on dominant densification mechanism was discussed. The activation energy for densification was also evaluated. In the investigated sintering temperature range, interface reaction was identified as the controlling process in sintering of alumina powders with the initial grain size of 0.9 μm, while grain-boundary diffusion was identified as the dominant process in sintering of alumina powders with the initial grain size of 7.0 μm. The activation energies for densification of the finer and coarser grain size alumina ceramics were determined as 342 and 384 kJ mol⁻¹, respectively, which provided a strong support on the densification mechanism investigation.     

无压烧结制备高致密度AlN-BN复合陶瓷

以低温燃烧合成前驱物制备的比表面积为17.4m²/g的AlN粉末和市售BN粉末为原料, 利用无压烧结工艺制备AlN-15BN复合陶瓷, 研究了复合陶瓷的烧结行为以及制备材料的性能, 结果表明: 由于AlN粉末的烧结活性好, 复合材料的烧结致密化温度主要集中在1500～1650℃之间, 在1650℃烧结后, AlN-15BN复合陶瓷的相对密度可达95.6%. 继续升高烧结温度, 材料的致密度变化不大, 热导率继续增加. 在1850℃烧结3h后, 可以制备出相对密度为96.1%, 热导率为132.6W·m^-1·K^-1, 硬度为HRA64.2的AlN-15BN复合陶瓷. 提出了高比表面积的AlN粉末促进复合陶瓷烧结的机理, 利用XRD, SEM等手段对烧结体进行了表征.     

球磨转速对Nd:YAG透明陶瓷的显微结构及光学性能的影响

以高纯商业Y₂O₃、α-Al₂O₃和Nd₂O₃粉体为原料, 以TEOS(正硅酸乙酯)和MgO为烧结助剂, 采用固相反应和真空烧结技术制备了1.0at%Nd:YAG透明陶瓷。系统研究了球磨转速(球磨时间10 h)对混合粉体的尺寸以及对陶瓷样品致密化行为、显微结构和光学性能的影响。结果表明: 通过球磨过程可以充分细化原料粉体的颗粒; 随着球磨转速的提高, 陶瓷烧结时样品中的气孔能更好地排除。但是球磨转速过高时, 陶瓷烧结体中存在少量的富铝第二相会降低样品的光学透过率。当球磨转速为130 r/min时, 真空烧结(1760℃×50 h)所得Nd:YAG透明陶瓷的微结构均匀致密, 几乎没有晶界和晶内气孔存在, 样品在1064 nm处的直线透过率高达83%。     

热等静压烧结制备细晶粒Ce,Y:SrHfO3闪烁陶瓷

Ce:SrHfO₃陶瓷因具有高密度和高有效原子序数, 对高能射线具有很强的阻止能力。同时, Ce:SrHfO₃陶瓷还具有快衰减和高能量分辨率等优异的闪烁性能, 引起了研究人员的广泛关注。由于传统的烧结方法难以实现非立方结构Ce:SrHfO₃陶瓷的透明化, 本研究采用真空长时烧结和短时真空预烧结合热等静压烧结(Hot Isostatic Pressing, HIP)方法制备Ce,Y:SrHfO₃陶瓷。以金属氧化物和碳酸盐为原料, 1200 ℃下煅烧8 h可以获得平均粒径为152 nm的纯相Ce,Y:SrHfO₃粉体。1800 ℃真空烧结20 h获得平均晶粒尺寸为28.6 μm的不透明的Ce,Y:SrHfO₃陶瓷, 而两步烧结法可以制备光学透过率良好的Ce,Y:SrHfO₃陶瓷。本研究详细分析了陶瓷致密化过程中微结构的演变, 探究了预烧结温度对Ce,Y:SrHfO₃陶瓷密度、显微结构和光学透过率的影响。真空预烧(1500 ℃×2 h)结合HIP后处理(1800 ℃×3 h, 200 MPa Ar)所获得的Ce,Y:SrHfO₃陶瓷在800 nm处的最高直线透过率为21.6%, 平均晶粒尺寸仅为3.4 μm。在X射线激发下, Ce,Y:SrHfO₃陶瓷在400 nm处产生Ce³⁺ 5d-4f发射峰, 其XEL积分强度比商用锗酸铋(BGO)晶体高3.3倍, Ce,Y:SrHfO₃陶瓷在1 μs门宽下的光产额约为3700 ph/MeV。良好的光学和闪烁性能可以拓宽Ce,Y:SrHfO₃陶瓷在闪烁探测领域的应用。     

Liquid-phase sintering in the glass-cordierite system: particle size effect

The effect of particle sizes of glass and ceramic filler on the densification kinetics of glassfilled ceramics has been studied using borosilicate glass-cordierite as the model system. Within the particle size range investigated, the densification is found to be significantly enhanced by increasing the cordierite size, reducing the glass size and increasing the green density. These results are attributed to both the increased driving force of densification by reducing the glass particle size and the decreased glass redistribution distance by either increasing the green density of compacts or increasing the particle size ratio between the cordierite and glass powders. In addition, a large cordierite-to-glass size ratio gives a dense, uniform microstructure of sintered body as a result of forming a homogeneous close packing of the low-melting glass phase around the refractory cordierite particles.     

掺Sr铬酸镧粉体的合成及低温烧结行为研究

通过溶胶-凝胶法制备了La_1-xSr_xCrO₃纳米粉体并实现了低温致密烧结, 用X射线衍射仪、透射电镜、差示扫描量热分析仪和扫描电镜对粉体和烧结体进行分析. 结果表明: 粉体的平均直径<50nm, 当x=0, 0.1时, 粉体为单一的La_1-xSr_xCrO₃, x=0.3时存在第二相SrCrO₄. Sr掺杂使铬酸镧晶格产生畸变, 随Sr含量的增加, 晶格常数逐渐变小. 铬酸镧纳米粉体的烧结分为两个阶段, 1200℃以前的缓慢放热和1350℃左右的较快放热, 分别对应烧结的初期和中期. 依据DSC分析结果制订了烧结工艺, 并在1380℃烧结得到相对密度91％的铬酸镧烧结体.     

Densification,microstructure, and properties of W-Mo-Cu alloys prepared with nano-sized Cu powders via large electric current sintering

This study rapidly fabricated a novel W-Mo-Cu alloy by large current electric field sintering at a relatively low temperature, and the effects of the powder size of Cu on the densification, microstructure, and properties were comprehensively investigated. The particle size of Cu did not influence the phase type but significantly affected the densification, microstructure, and properties. XRD and TEM results showed that the alloy contained three new phases aside from W, Mo, and Cu phases, i.e., Mo-W ordered phase, Mo-Cu solid solution, and Cu_0.4W_0.6 intermetallic compound. Copper powders with smaller sizes were beneficial to improving the distributional homogeneity of elements and the sintering densification. Therefore, the alloy prepared with 100 nm Cu powders had a denser and more homogeneous microstructure and better comprehensive properties than that prepared with 5 μm Cu powders. Overall, the W-Mo-Cu alloy prepared with 100 nm Cu powders at 980 °C proposed the best comprehensive properties, and its relative density can reach 98% approximately.     

Microstructure evolution and densification behavior of TiC/316L composite powders during cold/warm die compaction and solid-state sintering: 3D particulate scale numerical modelling and experimental validation

To identify the microstructure evolution and densification behavior of TiC/316L composites in powder metallurgy (PM) process, 3D particulate scale numerical simulations were conducted to reproduce the cold/warm compaction and solid-state sintering of TiC/316L composite powders with corresponding physical experiments being carried out for model validation. The effects of compaction parameters and sintering temperature on the densification behavior of TiC/316L composite powders were systemically investigated. The particle deformation and morphology, stress/strain and microstructure evolutions, and grain size distribution in the whole process were characterized and compared to further illustrate the densification behavior and the underlying dynamics/mechanisms. The results show that compared with the cold compaction, the warm compaction can not only achieve higher relative density, smaller and more uniform equivalent stress, and weaker spring back effect, but also improve the friction condition among powder particles. The plastic deformation of 316L particles is the main densification mechanism during compaction. In the solid-state sintering of TiC/316L compacts, the densification is mainly indicated by shrinkage and vanishing of large residual pores along with the growth of the sintering necks, accompanied by the particle movement and growth along the boundary regions. Meanwhile, the particle displacement and grain size distribution are more uniform in the warm compacted TiC/316L component. Moreover, the equivalent (von Mises) stress in 316L particles is smaller than that in TiC particles.