微米级α-Al2O3恒速无压烧结显微结构演变的预测

通过高温热膨胀仪对微米级α—Al2O3坯体进行两种升温速率（2℃／min和5℃／min）的恒速无压烧结,利用阿基米德法测量烧结体的相对密度,利用扫描电镜观察样品经不同烧结路径烧结后的显微结构;以Hansen全期烧结模型为基础,根据两种升温速率下得到的烧结曲线,建立了微米级α-Al2O3（平均粒径为2．5μm）主烧结曲线;利用主烧结曲线得到的相对密度和阿基米德法测得的烧结体（经过不同烧结制度）相对密度一致,说明主烧结曲线对烧结路径不敏感,烧结体的相对密度仅是时间和温度的函数,从而证明了所建主烧结曲线的有效性。烧结体的显微结构与烧结体密度密切相关,因此主烧结曲线可以用来预测和控制烧结体的显微结构,进而实现对氧化铝陶瓷性能的预测和控制。     

钛酸钡陶瓷烧结动力学曲线的研究

以超重力反应沉淀法(HGRP)制备的纳米钛酸钡粉体为原料,以热膨胀仪为测试手段,对钛酸钡陶瓷的烧结动力学曲线特征进行了研究.结果表明,烧结温度和成型坯片密度都会对钛酸钡陶瓷的烧结过程产生影响,所表现出的烧结动力学曲线特征也不相同,而升温速率几乎不对坯片的烧结动力学曲线特征产生影响.随着烧结温度的升高,坯片收缩率增大,当烧结温度由1150℃升到1300℃时,收缩率由6.7%增大到23.2%;坯片的密度增大,收缩率减小,当成型坯片相对密度由61.08%增大到64.42%时,收缩率由17.5%减少到14.4%;升温速率增大,坯片开始收缩的温度及收缩率几乎不变.     

亚微米级α-Al2O3陶瓷恒速无压主烧结曲线的建立

主烧结曲线对于预测陶瓷的烧结行为非常有用,以主烧结曲线理论为基础,对亚微米级a-Al5 O3(平均粒径为350nm)的恒速无压烧结行为进行了研究.根据Hansen提出的全期烧结模型,结合低升温速率条件下热膨胀仪记录的烧结数据建立了α-Al2O3的主烧结曲线,并由此得到其烧结过程中的表观激活能为1035kJ/mol.为验证所建立主烧结曲线的有效性,对同批次坯体样品进行不同路径的烧结,用Archimedes法实测烧结体密度,所测结果与主烧结曲线预测的结果相一致,从而证明了所建立主烧结曲线的有效性.因此亚微米级α-Al2O3主烧结曲线对烧结路径不敏感,可以对样品收缩率和最终相对密度进行预测,反之,根据目标相对密度可以制定相应的烧结制度.     

钇稳定氧化锆纳米粉体烧结工艺的研究

实验研究了钇全稳定氧化锆(8YSZ)纳米粉体的烧结工艺,根据阿基米德原理测瓷体密度,通过测定烧结前后瓷片尺寸获得烧结线收缩率,使用扫描电子显微镜观测样品微观形貌,并探讨了纳米粉体烧结的致密化过程,分析了烧结工艺对致密度和晶粒大小的影响,得到了8YSZ纳米粉体合理的烧结工艺为:采用两步烧结,首先升温到1500℃,升温速率为3℃/min,然后降低温度到1450℃,烧结时间为4h.结果显示,采用该工艺,可以得到相对密度98%,晶粒尺寸小于3μm的性能优异的8YSZ瓷体.研究发现,粉体粒度对烧结性能影响较大,纳米粉体比普通粉体具有较低的开始烧结温度,双粒度混合粉体可以进一步提高其烧结性能.     

热压烧结——理解烧结机理的新途径

通常采用热压烧结的方法可以把诸如 SiC、Si_3N_4、AlN、Sialon 等多数共价键材料烧结到理论密度。由于热压烧结的温度较低,时间较短,所以材料的显微结构主要是晶粒尺寸能够得以控制。当压力作为辅助参数时,也可把热压设备看作膨胀(收缩)计;而且人们能够对某种选定的材料的热压烧结曲线(当压力恒定,温度不同时,密度随时间的变化关系)和等温烧结曲线(当温度恒定,压力不同时,密度随时间的变化关系)进行试验。在过去的廿年里,加热烧结的动力学定律已经由致密材料蠕变的能力定律予以导出。运用等温曲线(在相对密度恒定的条件下),人们能推导出烧结速率与压力间的关系,而且从理论公式可以判断出烧结步骤究竟是扩散,界面反应,还是(?)性变形等,当各个步骤对整个烧结过程都作出贡献时,只要考虑烧结速率和压力间的关系图,就足以准确地判定这些步骤是如何作用的:是同时起作用,还是分别起作用。另外在不同的压力下,所得到的温度和晶粒尺寸的影响等其它信息,同样是有用的。这些分析不是单纯几何式的依赖关系,因为它们是基于动力学的研究。这样一来,它们比那些基于研究相对收缩率随时间变化关系的积分形式就更加可靠。     

亚微米级α-Al2O3坯体的恒速升温烧结行为

研究了平均粒径为300nm的α-Al2O3坯体的恒速烧结曲线,观察了升温速率对烧结密度的影响,得到了两种升温速率条件下,烧结体相对密度之差与温度的关系.通过对两种升温速率条件下样品致密化速率与相对密度关系曲线的比较可知,样品最大致密化速率均出现在相对密度73%左右,与升温速率无关.     

低温烧结细晶Y-TZP

通过在Ｙ－ＴＺＰ中加入适量的硅酸盐玻璃添加剂,使其烧结温度明显降低,并且制备出具有细晶粒、高强度的四方相氧化锆增韧陶瓷材料．分析了添加剂含量及烧结温度与材料致密度、显微结构及力学性能的关系,发现在Ｙ－ＴＺＰ材料中加入１ｗｔ％的添加剂,可以使材料在１４００℃下烧结,氧化锆晶粒尺寸约为１００～２００ｎｍ;其抗折强度可达９５０ＭＰａ．     

液相烧结碳化硅陶瓷的原位研究（英文）

采用原位分析设备与传统方法相结合的方式研究了以Al2O3和Y2O3为烧结助剂的Si C陶瓷的液相烧结过程。通过高温实时观测炉对样品在测试过程中的收缩曲线以及形貌变化进行了表征,以及对液相形成过程的模拟进行了观测。采用传统分析方法研究了样品的相对密度、抗弯强度、物相组成以及微结构演变从1640℃到1920℃以40℃为间隔的变化情况。研究发现,液相明显开始起作用的温度在1640℃到1680℃之间。经典的液相烧结三阶段理论可以通过微结构以及相对密度等的分析来得到验证。该烧结体系的最佳烧结温度确认为1880℃,最高密度为(99.46±0.37)%,最大强度为(650±26)MPa。     

利用主烧结曲线和Arrhenius曲线确定TiO_2陶瓷表观激活能

表观烧结激活能是研究陶瓷烧结机理的一个非常重要参量。采用纳米金红石相TiO2陶瓷坯体在空气中进行无压烧结,加热速率分别为1,2,5℃/min,用热膨胀仪记录试样收缩率,阿基米德法测量烧结体相对密度,分别用主烧结曲线法和Arrhenius法计算表观烧结激活能。结果表明:用主烧结曲线得到的激活能是一个定值,而用Arrhenius法得到的激活能是一个变化的值,激活能是相对密度的函数,随相对密度的增加而减小,且激活能和相对密度的变化趋势分成两段,当相对密度大于85%时,激活能随相对密度的增加而减小比小于85%时要快,这意味着在烧结过程中,控制烧结的扩散机制可能发生了变化。     

铝粉固相烧结过程中的微结构演化

在铝粉末样品的固相烧结过程中使用同步辐射CT(SR-CT)技术对其进行实时投影成像,用滤波反投影算法重建得到了铝粉末在烧结过程中不同时刻的内部微结构的二维断层重建图像,并用数字图像处理技术得到了三维重建图像;通过重建图像清晰地观测到样品在3个烧结阶段中颗粒的接触、烧结颈的形成、晶粒和气孔的长大以及气孔球化并收缩等现象,从而实现了对铝粉末烧结过程的实时和无损观测.统计了样品在不同烧结时刻的孔隙率、孔隙率随着烧结时间和烧结时间对数的变化曲线,并根据曲线分析了样品在不同烧结时刻致密化速率的变化,得到了烧结中期孔隙率与时间对数的线性关系,结果与现有烧结理论吻合.     

脉冲电流烧结机理的研究进展

脉冲电流烧结（Ｐｕｌｓｅ ｅｌｅｃｔｒｉｃ ｃｕｒｒｅｎｔ ｓｉｎｔｅｒｉｎｇ,ＰＥＣＳ）是材料科学领域开发出的一种新型快速烧结技术,已广泛应用于金属与合金、结构陶瓷、氧化物超导体、复合材料、热电材料、高分子材料以及功能梯度材料的制备．本文简介脉冲电流烧结特征,结合ＰＥＣＳ烧结条件对铜粉末和氧化铝粉体致密化及显微结构影响的实验证据,就脉冲电流烧结过程和机理进行探讨．     

Master sintering curve applied to the Field-Assisted Sintering Technique

The master sintering curve approach was extended theoretically to the Field-Assisted Sintering Technique (or SPS). Experimental data from constant heating rate testing confirm the general applicability of this framework. An apparent activation energy of ~290 kJ/mol was found for ultrafine alumina below 1200 °C. As alumina densifies by grain boundary diffusion in the present conditions, this low value of the apparent activation energy might be due to thermal gradients in the specimens induced by rapid heating.     

Electric Current-Assisted Sintering of 8YSZ: A Comparative Study of Ultrafast High-Temperature Sintering and Flash Sintering

Electric current-assisted sintering (ECAS) is a promising powder consolidation technique that can achieve short-term sintering with high heating rates. Currently, main methods of performing ECAS are indirect heating of the powder compact in a conductive tool or direct heating with current flowing through the powder compact. Various influencing factors have been identified to explain the rapid densification during ECAS, such as ultrahigh heating rates, extra-high temperatures, and electric field. However, the key consolidation-enhancing factor is still under debate. This study aims at understanding the role of heating rate on the enhanced densification during ECAS of 8 mol% Y₂O₃-stabilized ZrO₂ (8YSZ) by experimental and numerical methods. Two different heating modes, ultrafast high-temperature sintering (UHS, indirect heating) and flash sintering (FS, direct heating), are studied. The novel UHS technique is successfully applied to consolidate the 8YSZ samples. Additionally, finite element methods (FEM) combined with a constitutive model is adopted to predict the densification and grain growth. Furthermore, a comparison of UHS and FS is performed to investigate the thermal effect (heating rate) and athermal effect (electric field) individually. The results indicate that the high heating rate is the key factor of the rapid densification during UHS and FS of 8YSZ.     

Sintering mechanisms of blended Ti6Al4V powder from diffusion path analysis

The sintering of master alloy-blended Ti6Al4V powder has been investigated to elucidate the mechanisms of sintering. Both blended powder compacts and diffusion couple samples were investigated using backscattered imaging and energy dispersive analysis to determine the phases present, and the diffusion path for sintering which has not been previously reported for this system. Transient liquid-phase sintering does not occur, and it is shown for the first time that the reason for the rapid sintering of this material in the temperature range of 1000–1150 °C is due to enhanced diffusion kinetics resulting from a combination of the concentration gradient and stress induced by a phase transformation in the ternary system. The results of this study have implications for the development of blended master alloy combinations in other powder metallurgy systems.     

Sintering characteristics of microfine zirconia powder

In this paper the sintering characteristics of yttria-doped zirconia microfine powder are investigated by measuring shrinkage and shrinkage rate curves of powder compacts. The experimental results show that there is a transition point in the shrinkage-temperature curves and two peaks appear in the shrinkage rate-temperature curves. These results provide further support for the idea that the sintering of microfine zirconia powders is a two-stage process. In the first stage, sintering of the powder compact is mainly dominated by inner-sintering in agglomerates and in the second stage, sintering will occur among densified agglomerates. The microstructure of agglomerates during sintering is also studied by TEM and provides evidence that the transition point in the shrinkage-temperature curve is the end of the first sintering stage. Furthermore, the relationships between sintering characteristics and powder parameters are investigated. It is found that the shrinkage rate in the first stage is related to the primary grain size of the powder, and in the second stage it is related to agglomerate size. The effect of agglomerates on the sinterability of microfine Zr0₂ powder can be directly evaluated by the difference of shrinkage rate between the two sintering stages. Experiments also show that the shrinkage rate can be influenced by heating rate. A rapid heating rate would result in difficulties in the second sintering stage.     

SiCxOy相分解方式对SiCO(Al)纤维烧结致密化的影响

研究了SiCO(Al)纤维向SiC(Al)纤维的高温转化过程, 并研究了纤维中SiC_xO_y相的分解特征及不同高温处理方式对纤维结构和烧结致密化的影响。结果表明: 纤维中SiC_xO_y相分解的温度范围为1430~1850℃, 当采用连续处理方式处理, 即使在1800℃下, 纤维芯部SiC_xO_y相未能彻底分解, 且快速分解速率导致纤维中形成粗大结晶颗粒和气孔, 无法得到致密的高结晶结构。而在静态条件下处理, 可以提高SiC_xO_y相分解程度。1650℃下保温处理1 h后可以完全脱除SiC_xO_y相, 同时保持晶粒均匀。再经过1900℃烧结, 即可制得呈致密高结晶结构SiC(Al)纤维。     

升温速率对氧化铝粉末烧结行为的影响

采用不同的升温速率,在膨胀计中对脱脂后的氧化铝粉末射成形坯件进行一系列的烧结试验.结果表明,烧结致密化过程主要发生在升温阶段,快速升温有利于致密化的进行和抑止晶粒长大,但由于烧结时间较短和烧结炉最高温度的限制,产品的最终致密化程度不高.在低温时快速升温,高温时缓慢加热,可以获得较好的致密化效果和微观结构.试验和分析结果将为建立非等温烧结模型和烧结工艺参数的优化方法提供依据.     

Sintering and microstructural development of ceria-gadolinia dispersed powders

Well-dispersed ceria-gadolinia oxide powders were obtained from thoroughly isopropanol-washed coprecipitated oxalates, followed by calcination at 800 °C. The characteristics of the calcined powders and the microstructure of the green compacts were found to be of great importance in the sintering behaviour. Those green bodies in which some agglomerate survived after compaction reached a lower final density, while those having soft agglomerates were almost fully densified at a sintering temperature as low as 1400 °C. The densification process was studied by isothermal and constant heating rate dilatometry, and microstructural development at each stage in the processing was followed by SEM. By controlling the processing variables it was possible to obtain low-temperature near fully dense (better than 99%) and tough CeO₂-Gd₂O₃ bodies with homogeneous microstructure.     

Sintering enhancement in dynamically compacted commercial iron powders

Powder metallurgy compacts of near theoretical density have been made from commercial sponge iron and atomized iron powders, the latter with and without admixed lubricant. Equivalent compacts were made by conventional quasi-static die pressing and by the dynamic powder compaction method to allow for comparative testing of mechanical properties. The compacts were sintered over a range of temperatures from 700 to 1120°C. Test specimens were cut from the compacts and tested to produce data on tensile strength, ductility (area reduction) and cantilever beam (Izod) impact strength.

Compacts made dynamically from both the sponge iron and atomized iron powders exhibited higher tensile strengths and ductilities than those made quasi-statically and sintered to the same temperature. However, there were marked differences in the impact strength. With the sponge iron powder, dynamic compacts had lower impact strength than equivalent quasi-static compacts, but the reverse result was obtained with the atomized powder. The atomized powder was of much higher purity than the sponge iron and the microstructural evidence indicated that the inferior impact strength of the dynamically compacted sponge iron was due to interaction between the shock waves used for compaction and the numerous brittle inclusions present in this material.

The results with the lubricated powder showed no sintering enhancement attributable to dynamic powder compaction. This suggests that the mechanism for the sintering enhancement that can be achieved with this consolidation technique is related to the friction processes at the particle boundaries, possibly coupled with the elevated temperatures present at these boundaries during dynamic compaction.     

The pressure-assisted master sintering surface

It has been reported that the master sintering curve (MSC), in which the sintered density is a unique function of the integral of a temperature function over time, is insensitive to the heating path. The present research was undertaken to determine whether the MSC concept is applicable to hot pressing, and to develop the pressure-assisted master sintering surface for alumina. Densification of Sumitomo AKP30 alumina was continuously recorded during heating at 10°C/min at fixed pressures from 7 to 34.5 MPa. Final densities computed from the dilatometer traces were in excellent agreement with values determined by the Archimedes method. The thermocouple was calibrated using the melting point of the Ni/C eutectic. An accuracy of ±2°C was established. The pressure-assisted master sintering surface was successfully constructed. Using this surface, the final density can be predicted to about 1% accuracy for a fixed pressure and an arbitrary temperature-time path.