Low-Temperature Synthesis of α-Al2O3 Powder via Calcining Aluminum Ammonium Sulfate Double Salt Process: Effects of Glucose and Pre-pressing
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摘要: 以NH4Al(SO4)2·12H2O为原料，通过加入不同含量的葡萄糖来合成α-Al2O3，并研究了葡萄糖含量和预压处理对α-Al2O3粉体合成工艺和温度的影响。结果表明，葡萄糖的存在可以明显改变相变过程，降低合成温度。添加30%（质量分数，下同）葡萄糖时，可在950 ℃合成单相α-Al2O3粉体，比不添加葡萄糖时低200 ℃左右。添加75%葡萄糖后，α-Al2O3的合成温度可进一步降低至900 ℃。葡萄糖降低α-Al2O3合成温度的主要原因分为两个：一是葡萄糖氧化分解热加速NH4Al(SO4)2·12H2O的热分解，二是使NH4Al(SO4)2·12H2O分散均匀并无定形化。结果还表明，预压可使α-Al2O3的合成温度进一步降低25~50 ℃，这可能是由于团聚体的破坏和粉末分散体的进一步均质化所致。Abstract: The α-Al2O3 powder was synthesized by calcining NH4Al(SO4)2·12H2O with different content glucose added. The effects of glucose content and sample pre-pressing on the synthesis process and temperature of α-Al2O3 powder were investigated. The results showed that the existing of glucose could change the phase transition process and decrease the synthesizing temperature obviously. With 30wt% glucose added, α-Al2O3 powder could be synthesized at 950 ℃, which was about 200 ℃ lower than that of no glucose added. With 75wt% glucose added, the synthesizing temperature of α-Al2O3 could be further decreased to 900 ℃. Two effects of glucose are believed to be the main reasons for the decrease of α-Al2O3 synthesizing temperature. One is accelerating the thermal decomposition of NH4Al(SO4)2·12H2O, the other is to make NH4Al(SO4)2·12H2O disperse evenly and amorphous. The results also showed that pre-pressing could further decrease the synthesizing temperature of α-Al2O3 by 25-50 ℃, which might cause by the destruction of agglomeration and the further homogenization of powder dispersion.
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Key words:
- Low temperature synthesis /
- α-Al2O3 /
- Glucose /
- Pre-pressing
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图 1 A0样品在不同温度煅烧4 h后的XRD图谱
Figure 1. XRD pattern of sample A0 after calcination at different temperatures for 4 h
图 2 A2(a)和A4(b)样品在不同温度煅烧4 h后的XRD图谱
Figure 2. XRD patterns of samples A2(a) and A4(b) after calcination at different temperatures for 4 h
图 3 A0(a)、A2(b)和A4(c)样品在不同温度下煅烧4 h后的质量损失曲线
Figure 3. Thermogravimetric curves of samples A0 (a), A2(b) and A4(c) after calcination at different temperatures for 4 h
图 4 A0和A2样品在800℃煅烧4 h后的XRD慢扫描图谱
Figure 4. Slow scanning XRD patterns of samples A0 and A2 after calcination at 800℃ for 4 h
图 5 A1(a)、A3(b)和A5(c)样品在不同温度煅烧4 h后的XRD图谱
Figure 5. XRD patterns of A1(a), A3(b) and A5(c)samples after calcination at different temperatures for 4 h
表 1 不同样品的配方组成
Table 1. Proportion of different samples
Sample number w(Glucose)/% pressure/25 MPa A0 0 - A1 0 √ A2 30 - A3 30 √ A4 75 - A5 75 √ 
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表 2 不同配方样品制备得到的α-Al2O3的SBET
Table 2. SBET of α-Al2O3 prepared by samples of different formulations
Formula Temperature/℃ SBET/m2·g−1 A0 1150 8.1265 A3 900 10.0056 A5 850 24.5134
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