采用XRD、SEM和XRF等表征方法研究In2O3、SnO2及其混合粉(In2O3与SnO2质量比为9:1)在N2、空气及O2气氛下于1300~1600℃烧结过程中的粉末分解质量损失、反应固溶、新相生成及孔洞形成等行为,以期为高密度铟锡氧化物(ITO)靶材制备奠定基础。结果表明:在1300~1600℃高温烧结中,In2O3和SnO2均分解升华, SnO2较In2O3更易于分解,增大烧结气氛的氧分压,有利于抑制分解反应的发生;在O2气氛下,ITO粉在1500℃开始显著分解产生质量损失;ITO粉在N2、空气和O2气氛中于1300℃下烧结4 h,样品中均存在SnO2相;于1400℃下烧结4 h,SnO2相消失,In4Sn3O12相出现;随着烧结温度的进一步升高,In4Sn3O12分解消失,其分解温度随烧结气氛氧分压增大而提高;在O2气氛下烧结,所得ITO粉晶格常数最低,且较为稳定,颗粒收缩较均匀,有利于高密度ITO靶材制备。
The sintering behaviors, such as the decomposition and mass loss, reactive solid solution, generation of new phases and holes of In2O3 and SnO2 as well as their mixed (mass ratio of In2O3 to SnO2 9:1) powders, were studied in the temperature range of 1 300~1 600℃under the atmospheres of N2, air and O2 by means of characterization methods of XRD, SEM, XRF, and so on, in order to lay the foundation for preparing high density ITO targets. The results show that, during the sintering processes in the temperature range of 1 300~1 600℃, both In2O3 and SnO2 may decompose and sublime. Compared to In2O3, SnO2 powders are easier to decompose, increasing oxygen partial pressure of the sintering atmosphere is beneficial to inhibiting their decompositions, and under O2 atmosphere, ITO powders begin to decompose and lose mass until as high as 1 500℃. After sintering under atmospheres of N2, air and O2 for 4 h, SnO2 still exists in ITO powders at 1 300℃, and at 1 400℃, phase SnO2 will disappear with the formation of a new phase, In4Sn3O12. With the further increase of sintering temperature, phase In4Sn3O12 will disappear, and the higher the oxygen partial pressure of the sintering atmosphere is, the higher the temperature is, in which phase In4Sn3O12 disappears. In case of sintering under O2 atmosphere, the lattice parameters of ITO powders obtained are the lowest and more stable, and moreover, the particle shrinkage during sintering is also more uniform, which are beneficial to preparing high density ITO targets.
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