形核密度对AlON粉体合成及其透明陶瓷制备的影响

doi:10.15541/jim20170206

摘要/Abstract

摘要：

以α-Al₂O₃为原料, 采用碳热还原氮化法合成AlON粉体, 利用活性炭和亚微米碳粉改变球磨后一次粉体(α-Al₂O₃和C混合粉体)的形核密度, 并研究形核密度对AlON粉体相组成、形貌及其透明陶瓷透光性的影响。结果表明, 形核密度不同的一次粉体在1750℃保温60 min均能合成纯相AlON粉体, 但是所合成的两种AlON粉体形貌和性能差异较大。高形核密度下(添加活性炭)合成的AlON粉体形貌不规则、结构疏松且晶粒较小, 并易于球磨获得细颗粒粉体(~0.93 μm); 而低形核密度下(添加亚微米碳粉)合成的AlON粉体整体形貌呈近球形, 晶粒发育较完整, 且尺寸较大, 该粉体球磨后颗粒尺寸较大(~2.13 μm)。因此, 形核密度是影响AlON粉体形貌、结构特征和破碎性的主要因素。研究结果表明, 高形核密度粉体合成的AlON粉体具有更好的烧结活性, 它在1880℃保温150 min获得的透明陶瓷最大红外透过率达76.5% (3 mm厚), 比低形核密度粉体制备的透明陶瓷提高48.3%。因此, 以α-Al₂O₃为原料时, 提高形核密度有利于制备颗粒较小的高活性AlON粉体, 该粉体适合制备高透过率AlON透明陶瓷。

关键词: AlON, α-Al₂O₃;, 形核密度, 活性炭, 亚微米碳粉

Abstract:

Aluminum oxynitride (AlON) powders were synthesized by carbothermal reduction and nitridation process using α-Al₂O₃ powder as starting material. Activated charcoal powder and submicron carbon powder were mixed with α-Al₂O₃ respectively to vary nucleation density of AlON. Influence of nucleation density on phase assemblages, morphology of AlON powders and transparence of AlON ceramics were studied. Single phase AlON powders were synthesized after holding at 1750℃ for 60 min with for both mixture powders of different nucleation density. The results show that the synthesized powders exhibit different morphology and milling property. The AlON powder synthesized by α-Al₂O₃ and activated charcoal mixture show irregular shape, loose structure and small particle size, due to its high nucleation density. Moreover, it is easier to mill the obtained AlON powder into small particle (0.93 μm). However, for the AlON powder synthesized by mixture of α-Al₂O₃ and submicron carbon powder, their grain grow obviously during the synthesis of the AlON powder, due to its low nucleation density with large near sphere particles close to 2.13 μm in diameter. Therefore, nucleation density plays a key role in controlling morphology, structure characteristics and milling performance of the AlON powders. Using the AlON powder synthesized by high nucleation density powders, high transparent AlON ceramics was fabricated by pressureless sintering at 1880℃ for 150 min, the maximum transmittance was ~76.5% (3 mm in thickness). It is 48.3% higher than that using AlON powder synthesized by low nucleation density powders. Therefore, for using α-Al₂O₃ as starting material to prepare AlON powder, high nucleation density is beneficial to AlON powder with small particle size and high sintering ability, which contributes to the high transmittance of AlON ceramics.

Key words: AlON, α-Al₂O₃;, nucleation density, activated charcoal powder, submicron carbon

中图分类号:

TB321
TB332

许建鑫, 单英春, 王光, 徐久军, 王亮, 李江涛. 形核密度对AlON粉体合成及其透明陶瓷制备的影响[J]. 无机材料学报, 2018, 33(4): 373-379.

XU Jian-Xin, SHAN Ying-Chun, WANG Guang, XU Jiu-Jun, WANG Liang, LI Jiang-Tao. Nucleation Density on the Synthesis of AlON Powder and Preparation of Transparent Ceramics[J]. Journal of Inorganic Materials, 2018, 33(4): 373-379.

图/表 13

图1 α-Al2O3粉体的SEM照片

Fig. 1 SEM image of α-Al2O3 powder

图2 活性炭(a, b)和亚微米碳粉(c)的SEM照片

Fig. 2 SEM images of activated charcoal powder (a, b) and submicron carbon (c)

图3 亚微米碳粉粒度分布图

Fig. 3 Particle size distribution curve of submicron carbon powder

图4 α-Al2O3与碳粉混合球磨后粉体的粒度分布

Fig. 4 Particle size distribution curves of milled powders (α-Al2O3 and carbon)

图5 α-Al2O3和C混合粉体的SEM照片

Fig. 5 SEM images of the mixtures of α-Al2O3 and C(a) AA powder; (b) SA powder

图6 一次粉体AA(a)和SA(b)在不同处理工艺的XRD图谱

Fig. 6 XRD patterns of powders synthesized by activated charcoal powder (a) and submicron carbon (b)

图7 用AA(a)~(b)和SA(c)~(d)粉体合成AlON粉体的SEM照片

Fig. 7 SEM images of AlON powders synthesized by activated charcoal powder (a)-(b) and submicron carbon (c)-(d)

图8 用AA(a)和SA(b)粉体合成AlON粉体球磨后的SEM照片

Fig. 8 SEM images of milled AlON powders synthesized by activated charcoal powder (a) and submicron carbon (b)

图9 球磨后AlON粉体的粒度分布图

Fig. 9 Particle size distribution of milled AlON powders synthesized by activated charcoal powder (a) and submicron carbon (b)

图10 碳热还原氮化法合成AlON粉体的形成过程示意图

Fig. 10 Formation process of AlON powder synthesized by carbothermal reduction and nitridation(a) Mixture of Al2O3 and C; (b) Heated to 1550℃; (c) Held at 1550℃ for 60 min; (d) ≥1700℃; (e) After holding at 1750℃ for a period of time (<60 min); (f) Held at 1750℃ for 60 min

图11 AlON陶瓷的XRD图谱

Fig. 11 XRD patterns of AlON ceramics

图12 AlON陶瓷的断口形貌

Fig. 12 Fracture surfaces of AlON ceramics(a) Activated charcoal powder; (b) Submicron carbon

图13 AlON透明陶瓷的透过率曲线

Fig. 13 Transmittance curves of the transparent ceramics (a) Visible light; (b) Infrared band

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