EFFECT OF GRINDING ON CRACKS AND THE STRENGTH OF CERAMICS

Abstract— Five kinds of silicon nitride samples with different microstructure were prepared in order to examine the effect of sintering condition on grain size and mechanical properties. The degradation in strength of ceramics caused by grinding is investigated in detail. It is shown that the critical process zone size is closely related to the grinding process. Futhermore, the crack size caused by grinding is estimated by the process zone size failure criterion and the Newman-Raju formula. It can be concluded that the process zone size failure criterion is useful when evaluating the sensitivity of ceramics to grinding.     

碳化硅泡沫陶瓷浆料成分与烧结性能

将用于制备碳化硅泡沫陶瓷的浆料烘干、制粉、干压、烧结,从而探讨浆料的成分与 烧结性能的关系.样品的抗弯强度与烧结助剂的含量之间存在最佳搭配关系,烧结对强度的贡 献主要来自于新相莫来石的生成和玻璃相对碳化硅颗粒的包覆、连接作用.同种成分的样品开 气孔率随着烧结温度的升高表现出单调下降的趋势,而抗弯强度与开气孔率的变化并没有表现 出完全相反趋势;不同成分样品的耐火度均保持在1730℃没有变化.采用最佳配方的浆料和 最佳烧结温度制备的碳化硅泡沫陶瓷抗弯强度可达到0.72MPa.     

Effects of sintering process on preparing iron-based friction material directly from vanadium-bearing titanomagnetite concentrates

In order to optimize an innovative two-stage process for preparing an iron-based friction material directly from vanadium-bearing titanomagnetite concentrates, this paper focuses on the effects of sintering process on the microstructures and properties of an iron-based friction material. On one hand, the samples were sintered at 900 °C, 950 °C, and 1000 °C for 3 h respectively; On the other hand, the samples were sintered at 1000 °C for 1 h, 2 h, 3 h, and 4 h respectively. As a result, after the samples were sintered at above 950 °C for more than 3 h, a lot of laminated microstructures appear in these samples owing to the formation of a large number of pearlites. Besides, the density, the hardness, and the friction coefficient of this material are positively correlated to the sintering temperature or the sintering time, and the wear rate of this material is negatively related to the sintering temperature or the sintering time. This study can contribute to the attainment of much clearer insight into the effects of sintering process and lay the foundation of practical application of this innovative two-stage process.     

Effect of process parameters on surface oxides on chromium-alloyed steel powder during sintering

The use of chromium in the PM steel industry today puts high demands on the choice and control of the atmosphere during the sintering process due to its high affinity to oxygen. Particular attention is required in order to control the surface chemistry of the powder which in turn is the key factor for the successful sintering and production of PM parts. Different atmosphere compositions, heating rates and green densities were employed while performing sintering trials on water atomized steel powder pre-alloyed with 3 wt.% Cr in order to evaluate the effect on surface chemical reactions. Fracture surfaces of sintered samples were examined using high resolution scanning electron microscopy combined with X-ray microanalysis. The investigation was complemented with thermogravimetric (TG) studies. Reaction products in particulate form containing strong-oxide forming elements such as Cr, Si and Mn were formed during sintering for all conditions. Processing in vacuum results in intensive inter-particle neck development during the heating stage and consequently in the excessive enclosure of surface oxide which is reflected in less good final mechanical properties. Enhanced oxide reduction was observed in samples processed in hydrogen-containing atmospheres independent of the actual content in the range of 3–10 vol.%. An optimum heating rate was required for balancing reduction/oxidation processes. A simple model for the enclosure and growth of oxide inclusions during the sinter-neck development is proposed. The obtained results show that significant reduction of the oxygen content can be achieved by adjusting the atmosphere purity/composition.     

热固性硅树脂压注法制备多孔硅基陶瓷型芯研究

以石英玻璃粉为基体, 热固性硅树脂为增塑剂, 利用压注方法制备了多孔硅基陶瓷型芯, 研究了烧结温度和保温时间对样品性能的影响。研究结果表明: 随着烧结温度的升高, 反玻璃化进程加快, 在烧结温度1250℃, 随着保温时间的延长, 玻璃相发生了转变, 逐渐析出方石英, 且含量不断增加; 样品的线收缩率和失重随烧结温度的升高略微增加, 但烧结时间的影响较小。样品的失重主要是由于硅树脂的分解引起的。在1250℃烧结10 h后, 得到样品的收缩率为0.93%, 显气孔率为32.8%, 抗弯强度为9.08 MPa。     

Investigation of Sintering Technology for Composite of Stainless Steel and Partially Stabilized Zirconia

The sintering technology for mixed powedered extrusion rods of different proportions of stainless steel to magnesia partially stabilized zirconia(PSZ) was investigated..The effects of some sintering parameters including holding time ,atmosphere and protective gas pressure on shrinkage,relative density,micostructure,micro-Vickers hardness and compression strength of sintered samples were mainly researched.The experimental results are as follows(1)The shrinkage and the relative density of the sintered samples decrease as increasing stainless steel content in the composite,except for the xase containing 90 percent of stainless steel;(2)The porosity in PSZ matrix rises as increasing the stainless steel content in the composite;(3)Longer sintering holding time ,higher sintering vacuum and gas-pressure sintering process not only enhance the relative density ,but also improve microstructure of composite;(4)Micre-Vickers hardness of PSZ matrix decreases as increasing stainless steel content,while that of stainless steel particles in sintered samples varies unnoticeably.     

放电等离子快速烧结纳米3Y-TZP材

本文采用放电等离子烧结技术（ＳＰＳ）快速烧结结纳米３Ｙ－ＴＺＰ材料,利用ＳＰＳ技术快速烧结,可制备出完整、致密的３Ｙ－ＴＺＰ材料,在烧结温度为１３００℃,保温３ｍｉｎ条件下,相对密度达９８．２％,晶粒仅１００￣１３０ｎｍ,研究发现,材料的密度随烧结温度的变化趋势与一般快速烧结有明显区别;材料的晶粒随烧结温度的提高而长大,但长大幅度小于其他一些烧结方法所得的３Ｙ－ＴＺＰ材料,本研究对这些现象进行了理     

Direct laser sintering of a silica sand

As an application study of rapid prototyping, commercially available silica sand was successfully direct-laser-sintered in a self-developed high-temperature laser sintering equipment. The mechanism of powder-state sand becoming a solid state block during the laser sintering process was disclosed by scanning electron microscope (SEM) and energy dispersive X-ray (EDX) analysis on sand particles and sintered samples. The effect of process parameters to the accuracy, strength and surface finish of sintered parts was investigated and thus a set of optimal parameters has been obtained for the sand sintering process. The feasibility of using this material and process to build casting moulds for metal casting was also investigated and discussed.     

Mechanisms Governing Microstructural Evolution During Consolidation of Nanoparticles

In micron-scale, powder consolidation process is driven by diffusion phenomenon, while in nano-scale the higher surface energy of particles leads to some anomalous behaviors within the process. In order to investigate the nano-sintering occurrence, an atomistic approach is employed via molecular dynamics simulations. Within this approach, the effect of particle size and temperature is examined. The study of particle structure emphasizes on a transition on the governing mechanism of process depending on the material energy levels. The results show that in a specific particle size at low temperatures, the main sintering mechanism is the plastic deformation, while at elevated temperatures it switches to the surface diffusion. Calculating the sintering activation energy, an anomalous trend is observed with the variations in the particle size. This trend can be described by annihilation of the grain boundary. The identified governing sintering mechanisms are presented in the sintering governing mechanism diagram. The diagram shows that the temperature, at which the main mechanism switches, depends on the particle size. The importance of this finding is that below the switching temperature, increasing time or temperature does not increase the efficiency of the process, significantly.     

Study on microstructure and thermal conductivity of Spark Plasma Sintering AlN ceramics

Dense aluminum nitride (AlN) ceramics were prepared by Spark Plasma Sintering with rare-earth oxide and CaF₂ as sintering additives. The effect of sintering additives on the density, phase composition, microstructure and thermal conductivity of AlN ceramics was investigated. The results showed that those sintering additives not only promoted densification through liquid-phase sintering but also improved thermal conductivity by decreasing oxygen impurities. Thermal conductivities of samples sintered with optimum proportion of rare-earth oxide and CaF₂ were higher than those of other samples. During the Spark Plasma Sintering process, the microstructures, especially the content and distribution of secondary phases, played important roles on the thermal conductivity of AlN ceramics.     

基于选择性激光烧结C-Al_2O_3复合粉体微观形貌和成型机理的研究

用正交试验设计来安排试验,对高温烧结前后样品的宏观和微观结构进行表征。结果表明,样品的结构特征与激光烧结工艺参数密切相关,并且激光烧结样品的致密度、升温和降温速率、保温时间以及烧结助剂的选择,对最终样品的致密度和力学性能的提高有着重大影响。同时分析了选择性激光烧结的机理,发现激光束与粉末的作用是一个动态瞬间的熔化-凝固的平衡过程。     

LAS系统微晶玻璃的制备及析晶研究

采用烧结法和溶胶-凝胶法制备了LAS系统微晶玻璃,并研究了其析晶性能。结果表明,烧结法制备的样品中晶粒尺寸为100～150nm,分布均匀,主晶相为β-锂辉石相,另外含有少量的Moganite石英相,溶胶-凝胶法制备的样品中晶粒尺寸为10～60nm,分布均匀,样品中存在Al2O3和LiAlO2相,而SiO2没有结晶,形成玻璃体。核化温度为600℃、晶化温度为680℃时,微晶玻璃的结晶效果比较好。     

模板转化法制备苎麻纤维织物SiC陶瓷

以苎麻纤维织物为生物模板,通过浸渍含有硅粉的酚醛树脂溶液,后经压制成型、碳化和1500℃烧结等工艺,制备了具有生物纤维形态的SiC陶瓷。利用XRD、SEM等测试技术,研究了不同烧结助剂对样品的各项性能和微观形貌的影响。结果表明:烧结助剂对苎麻纤维织物SiC陶瓷的失重率、显气孔率、体积收缩率等性能均产生了影响;添加Al_2O_3-Y_2O_3-SiO_2三元烧结助剂的SiC陶瓷具有最大的显气孔率和最小的体积收缩率;陶瓷中的SiC主要以β-SiC的形式存在;微观形貌分析显示,样品很好地保留了苎麻织物的纤维状微观结构。     

Effect of powder reactivity on microwave sintering of alumina

Effect of the reactivity of starting alumina powder of varying crystallinity on the sintering behavior in microwave process was studied. From X-ray amorphous to highly crystalline alumina, powders were obtained by conventional heating of compacts made of the precursor amorphous powder by heating it at different temperatures from 800 to 1500 °C. These samples were then sintered in a multimode microwave field of 2.45 GHz for 10 min at 1500 °C. The microwave effect on densification of the various alumina powders was evaluated by comparing the microwave and conventional sintering data. The results show significant microwave enhancement in the densification of the samples without any pretreatment. This enhancement became less significant as the temperature of the pretreatment increased and finally diminished. Since the pretreatment at elevated temperatures made the powder more stable thermodynamically, this study indicates that the sintering enhancement of a ceramic material in microwave is a metastability-related phenomenon.     

响应曲面法优化硫脲浸出烧结灰中银的工艺研究

以炼铁烧结机头除尘灰(烧结灰)为实验原料,通过XRF、XRD、SEM-EDS手段对原料进行表征,采用酸性硫脲法浸出烧结灰提取银。在单因素实验的基础上,使用响应曲面法(RSM)对烧结灰中提取银的工艺条件进行优化,以炼铁烧结灰中银的浸出率为响应值,选取对硫脲浸出烧结灰提银过程有显著影响的变量(反应温度、硫脲浓度、浸出时间)作为考察因素,采用Central Composite Design(CCD)中心设计方案以三因素五水平设计实验,得到最优的提银工艺条件,并获得拟合度高的二阶多项式模型。结果表明:硫脲浸出烧结灰中银的最佳工艺为反应温度50℃、硫脲浓度22g/L、浸出时间90min;在最佳提取条件下,银浸出率的模型预测值为89.38%,实验真实银的浸出率为89.9%,其相对误差为0.52%,表明实际值与模型预测值接近,可用于预测烧结灰提取银的浸出过程。     

Effects of sintering conditions on the microstructure and mechanical properties of SiC prepared using powders recovered from kerf loss sludge

The effects of sintering conditions on the microstructure and mechanical properties of the sintered SiC prepared using the SiC powder recovered from the kerf loss sludge were investigated. The recovered SiC powders were consolidated by spark plasma sintering (SPS) and conventional sintering methods. The effects of sintering temperature, time and methods (SPS and conventional sintering) on the phase, grain size and density of SiC were systematically studied. The Vickers hardness of spark plasma-sintered (SPSed) samples was higher than that of conventional sintered samples due to small grain size. When holding time was increased from 10 to 30 min, the grain size and relative density of SPSed samples were also increased, which lead to the almost constant Vickers hardness by competing effects of grain size and relative density. When holding time was over 30 min, no appreciable change of the relative density and grain size were observed, which can lead to similar values of Vickers hardness. SPS process can be used to make SiC with high density and hardness at relatively low temperature compared with the conventional sintering process.     

Herstellung neuer Hartmetalle mit Gradientenmikrostruktur durch Mikrowellensintern

Fabrication of New Cemented Carbides with Graded Microstructure by Microwave Sintering State of the art technologies for producing coated cermets and cemented carbides are in‐situ processes based on application of a reactive sintering atmosphere as well as ex‐situ processes, e. g., thermal CVD. Within the frame of the project summarised in the present paper, application of microwave radiation as heating source within both processing routes has been shown to be a viable and powerful new technology to accelerate processing rates as well as to integrate different processing steps into one process of sinter‐coating. Upon microwave sintering in reactive, e. g. nitrogen containing atmosphere, functionally graded materials are obtained from all Ti‐containing materials, with extended compositional gradients and dense Ti(C,N)‐coatings even in grades, which do not develop such coatings upon conventional vacuum sintering followed by reactive atmosphere heating. Microwave sintering offers therefore a much higher degree of variation in composition and gradient extension as compared to conventional processing routes. The acceleration of mass transport is impressive, yielding in some materials undesirably thick coatings at processing times of less than 1 h at temperature. Therefore further investigations are necessary in order to gain insight into the metallurgical processes occurring under the action of a microwave field. The thermal CVD‐process is not accelerated by the presence of the microwave field in such a significant way as the reactive atmosphere sintering is. However, using microwave heating a new reactor principle is developed, the so called “warm wall” reactor, in which only the samples are coated due to selective microwave heating, not the reactor. The coating process is performed at ambient pressure of an inert gas, immediatly after the sintering step, using precursors well known from conventional CVD. Due to microwave sintering no Co is enriched at the surface of the tool bits. Microwave sintering was expected to significantly increase the variability of processes which yield functionally graded cemented carbides and cermets and at the same time to improve the quality of the products or enable the synthesis of new materials. Based on preliminary results of cutting performance as well as process reproducibility and due the development of graded structures in materials which do not develop such microstructures under conventional processing conditions, these expectations were more than fulfilled.     

Establishment of process parameters for producing Al-foam by dissolution and powder sintering method

Al-foams have been manufactured by a dissolution and powder sintering process using crystalline raw cane sugar, as a novel leachable pattern. The method involves mixing and compaction, leaching and sintering processes. The influence of the process parameters on the microstructure of the produced foam is investigated in order to optimize the process conditions and produce high quality Al-foams. The differences between the actual and calculated porosity of the produced foam is ascribed to the joint effect of the retained porosity of the green product and the shrinkage during sintering. The optimum ranges of compaction pressure and sintering temperature are 250–300 MPa and 680–750 °C respectively.     

Thermal and mechanical properties of uranium nitride prepared by SPS technique

Nitride fuel is a promising nuclear fuel in fast breeder reactor (FBR) or accelerator-driven subcritical reactor (ADSR) system. In this study, high-density UN pellets were prepared by Spark plasma sintering (SPS) technique. The sample density strongly depended on the sintering temperature and pressure, and the pellets with 90% of theoretical density were easily obtained with low sintering temperature and short sintering time without any milling process. The grain size and pore size were much smaller compared with those for samples prepared by conventional sintering process. Despite of the small grain size, the thermal conductivity remains the high value. The SPS process permits easy densification of nitrides without any deterioration of thermal and mechanical properties, considered to be suitable as a preparation method of nitride fuels.     

Effects of Sintering Process Conditions on Size Shrinkages of Low-Temperature Co-Fired Ceramic Substrate

The effects of sintering process conditions on the size shrinkages of low-temperature co-fired ceramic (LTCC) substrate were investigated. The process variables investigated were thickness of the stacked raw tapes, lamination pressure, lamination-pressure holding time, pre-heating time, debinding time, sintering dwell time, and sintering temperature ramp. Results revealed that the size shrinkage percentage of the LTCC samples in the lateral directions was always smaller than that in the thickness direction. The lateral shrinkage deviations were less than 2.1% for all the experiments conducted in this study. Pre-heating time, lamination-pressure holding time, debinding time, sintering dwell time and sintering temperature ramp had almost no effects on the lateral size shrinkage of the LTCC samples, and the average of the lateral shrinkage values was 15.3%, with a standard deviation of 0.17%. Lamination pressure and stacked raw-tape thickness had effects on the lateral size shrinkage of the LTCC samples, and empirical equations for calculation of the size shrinkage values were obtained by curve fitting.