单晶生长用AlN粉料的烧结提纯工艺实验研究

Experimental Research on AlN Powder Source Purification by Sintering Process for AlN Crystal Growth

摘要:

使用自主研发的钨系统中频感应加热炉对AlN粉料进行了烧结提纯处理实验,并用XRD、SEM、IGA和GDMS等表征方法分析了烧结后的样品。实验发现,高温(2 250℃)长时间(50h)烧结提纯工艺效果显著,但AlN粉料损耗高达47.37%;而低温(小于2 000℃)分段式短时间(每段10h)烧结提纯工艺粉料损耗低于2%,但是提纯效果一般。通过对实验结果的综合分析,提出了一种AlN粉料烧结提纯的改进工艺,最终得到了氧含量仅238ppm、碳含量135ppm的高质量AlN单晶生长原料,并且显著增加了原料的利用率。

Abstract:

In this paper, two sintering experiments were conducted on a proprietary medium radio-frequency induction reactor with a tungsten setup. XRD, SEM, IGA and GDMS were used to analyze the obtained sintered samples. Experiments show that oxygen and carbon impurities can be effectively removed for the process sintering at 2 250 ℃ with 50 h holding time, but with AlN powder source loss of 47.37%. On the other hand, for the sintering temperature below 2 000 ℃, the process is not sufficient enough to reduce oxygen and carbon impurities, although the AlN powder source loss is below 2%. Based on the experimental results, a sintering process is proposed, which can produce high-quality AlN powder source with oxygen and carbon concentrations at 238 ppm and 135 ppm respectively, and maintain low loss of AlN powder as well.