Fabrication of β-Sialon/ZrN/ZrON composites using fly ash and zircon

β-Sialon/ZrN/ZrON composites were successfully fabricated by an in-situ carbothermal reduction？nitridation process with fly ash, zircon and active carbon as raw materials. The effects of raw materials composition and holding time on synthesis process were investigated, and the formation process of the composites was also discussed. The phase composition and microstructure of the composites were characterized by means of XRD and SEM. It was found that increasing carbon content in a sample and holding time could promote the formation of β-Sialon, ZrN and ZrON. The proper processing parameters to synthesize β-Sialon/ZrN/ZrON composites were mass ratio of zircon to fly ash to active carbon of 49：100：100, synthesis temperature of 1550 °C and holding time of 15 h. The average grain size ofβ-Sialon and ZrN（ZrON） synthesized at 1550 °C for 15 h reached about 2 and 1μm, respectively. The fabrication process ofβ-Sialon/ZrN/ZrON composites included the formation ofβ-Sialon and ZrO2 as well as the conversion of ZrO2 to ZrN and ZrON.

常压烧结制备ZrN(ZrON)-SiAlON复合陶瓷

以粉煤灰(≤74μm)、锆英石(≤44μm)和活性炭为原料,采用碳热还原氮化法在1 550℃保温6 h合成了ZrN-SiAlON复合材料。以加工成的ZrN-SiAlON复合微粉为主原料,加入聚乙烯醇结合剂,分别在1 450、1 500和1 550℃下埋炭粉常压烧结1 h制备ZrN(ZrON)-SiAlON复合陶瓷,研究了烧成温度对复合陶瓷相组成、显微结构和烧结性能的影响。结果表明:1)控制烧成温度可以制备出不同组成的β-SiAlON基复合陶瓷;在1 550℃保温1 h制备的复合陶瓷的主晶相为ZrN、ZrON和β-SiAlON(z=2,Si4Al2O2N6);2)从不同温度烧后试样的微观结构中均能观察到ZrN(ZrON)、β-SiAlON和一种铁硅系化合物存在,且ZrN(ZrON)颗粒均匀地分布于β-SiAlON基质中;3)提高烧成温度会使复合陶瓷的收缩率增大,当烧成温度由1 450℃升至1 550℃时,试样的体积收缩率由19.4%增加至40.3%。

添加Y2O3对ZrN(ZrON)-SiAlON性能的影响

为了以较低成本制备较高性能的ZrN(ZrON)-SiAlON复合陶瓷材料,先以粉煤灰、锆英石和活性炭为主要原料,经碳热还原氮化法合成ZrN-SiAlON复合粉;然后在ZrN-SiAlON复合粉中添加不同量(质量分数分别为0、5%、10%)的Y2O3,在1500℃保温1 h埋碳烧结制备了ZrN(ZrON)-SiAlON复合陶瓷材料,并研究了ZrN(ZrON)-SiAlON复合陶瓷材料的相组成、烧结性能和力学性能等。结果表明:Y2O3可促进ZrN和β-SiAlON等主晶相的形成,同时促进材料的烧结致密化。添加5%(w)的Y2O3制得的ZrN(ZrON)-SiAlON复合陶瓷材料的显气孔率为5.3%,体积密度为3.47 g·cm-3,常温耐压强度为29.4 MPa,性能较优。

Preparation of ZrN(ZrON)-SiAION Composite Ceramics via a Pressureless Sintering Process

ZrN-SiAlON composite materials were synthesized at 1 550 ℃ for 6 h via a carbothermal reduction nitridation route using fly ash （≤74 μm）,zircon （≤ 44 μm） and active carbon as starting materials.The processed ZrN-SiAlON composite micropowders were mixed with polyvinyl alcohol as binder to prepare ZrN （ZrON）-SiAlON composite ceramics by carbon-embedded pressureless firing at 1 450,1 500 and 1 550 ℃ for 1 h,respectively.Influences of firing temperature on the phase compositions,microstructure and sintering properties of the ceramics were investigated.The results show that：（1） β-SiAlON based composite ceramics with different compositions can be prepared by controlling firing temperature,and the main crystalline phases of the specimen fired at 1 550 ℃ for 1 h involve ZrN,ZrON and β-SiAlON （z =2,Si4Al2O2N6）; （2） ZrN （ZrON）,β-SiAlON and a Fe-Si based compound can be observed in the microstructures of the specimens fired at different temperatures.ZrN （ZrON） particles distribute homogeneously in the β-SiAlON matrix; （3） raising firing temperature can increase the shrinkage ratio of the ceramics,and the volume shrinkage ratio increases from 19.4％ to 40.3％ when the firing temperature rises from 1 450 to 1 550 ℃.

Preparation of β-Sialon/ZrN bonded corundum composites from zircon by nitridation reaction sintering process

β-Sialon/ZrN bonded corundum composites were synthesized using fused white corundum,alumina micro powder,zircon and carbon black by nitridation reaction sintering process. Phase composition and microstructure of the synthesized composites were investigated by X-ray powder diffraction and scanning electronic microscope,and the formation process of the composites was discussed. The results show that the composites with different compositions can be obtained by controlling the heating temperature and contents of zircon and carbon black. The proper temperature to synthesize the composites is 1773 K.