以ＡＩＮＨ＿４（ＳＯ＿４）＿２·１２Ｈ＿２Ｏ和ＭｇＳＯ＿４·７Ｈ＿２Ｏ为原料，用焙烧法制得ＭｇＡｌ＿２Ｏ＿４尖晶石微粉。用ＸＲＤ，ＳＥＭ，ＴＧ／ＤＴＡ等手段分析了实验结果，表明该粉纯度高，分散性好，颗粒细小均匀。用该超微粉制得了光学质量完好的尖晶石单晶体。同时研究了反应过程中的相变情况及保温过程工艺参数与相成份、晶形变化的相互关系。 AINH_4 (SO_4) _2 · 12H_2O and MgSO_4 · 7H_2O were used as raw materials to prepare MgAl_2O_4 spinel powder by roasting method. The experimental results were analyzed by XRD, SEM, TG / DTA and other means, indicating that the powder has high purity, good dispersibility and fine particle uniformity. A fine optical quality spinel single crystal was obtained by using the superfine powder. At the same time, the phase change in the reaction process and the relationship between the process parameters and the phase composition and crystal form change during the heat preservation process were studied.