Investigation of the effect of LiCl and LiF additives on the kinetics of Spark Plasma Sintering of fine-grained alumina

M. Boldin, A. Popov, G. Shcherbak, K. Smetanina, D. Permin, V. A. Koshkin, A. Nokhrin, V. Chuvil’deev, А. А. Moskvichev, A. Murashov
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Abstract

The effect of the lithium chloride and lithium fluoride additives (2 wt. %) on the kinetics of Spark Plasma Sintering of industrial fine alumina powder was investigated. The Al2O3 + 2 % LiF powder was obtained by mixing the α-Al2O3 fine powders with the aqueous solution of LiF. The Al2O3 + 2 % LiCl fine powder was obtained by joint grinding of the components in a planetary mill. The sintering of the powders was performed with the heating rates of 10 and 50 °C/min up to the temperature corresponding to the end of the shrinkage. The ceramics sintered with the heating rate of 10 °C/min had the relative density of 97.4 – 98.7 %. The addition of lithium fluoride into the alumina powder was found to allow reducing the temperature of the beginning of the intensive powder shrinkage from 1400 – 1500 °C down to 1255 – 1335 °C. LiCl was shown to evaporate at low heating temperatures and not to affect the compaction intensity of the Al2O3 powder. The presence of the overheated LiF melt (not having enough time to evaporate from the specimen volume completely) in the ceramics leads to the appearance of the residual porosity and to the reduction of the hardness of the ceramics. Using the Young – Cutler equation, the powder compaction mechanisms were determined for pure alumina α-Al2O3 and for the powder compositions with the LiCl and LiF additives in the rapid heating conditions. The sintering activation energy was shown to be close to the one of the grain boundary diffusion. The LiF melt was found to promote the sliding of the Al2O3 fine particles during the low-temperature compaction stage.
LiCl和LiF添加剂对细晶氧化铝放电等离子烧结动力学影响的研究
研究了氯化锂和氟化锂添加剂(2 wt. %)对工业细铝粉火花等离子烧结动力学的影响。将α-Al2O3细粉与LiF水溶液混合,得到Al2O3 + 2% LiF粉体。在行星磨机上对各组分进行联合研磨,得到了Al2O3 + 2% LiCl细粉。将粉末以10和50℃/min的升温速率烧结至相应的收缩结束温度。升温速率为10℃/min时,烧结陶瓷的相对密度为97.4% ~ 98.7%。在氧化铝粉末中加入氟化锂可以将粉末开始剧烈收缩的温度从1400 - 1500℃降低到1255 - 1335℃。LiCl在低温下蒸发,不影响Al2O3粉末的压实强度。在陶瓷中存在过热的liff熔体(没有足够的时间从试样体积中完全蒸发),导致残余孔隙的出现和陶瓷硬度的降低。利用Young - Cutler方程,确定了在快速加热条件下纯氧化铝α-Al2O3和添加LiCl和LiF的粉末组分的粉末压实机理。烧结活化能与晶界扩散活化能相近。在低温压实阶段,LiF熔体促进了Al2O3细颗粒的滑动。
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