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納米級(jí)ITO粉體對(duì)燒結(jié)法制備靶材的影響
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國家高技術(shù)研究發(fā)展計(jì)劃(“863”計(jì)劃)基金資助項(xiàng)目(2004AA303542)


Effect of Nanosized ITO Powders on Preparation of ITO Targets by Sintering Method
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    摘要:

    采用化學(xué)共沉淀法制備ITO前驅(qū)物,分別于600及1000 ℃下熱處理前驅(qū)物,得到兩種ITO粉體。粉體模壓成型得到素坯,在400~1550 ℃內(nèi)采用燒結(jié)法、氧氣氛下燒結(jié)素坯制備出ITO靶材。對(duì)粉體及靶材進(jìn)行表征和分析,研究了燒結(jié)過程中晶粒生長情況、靶材微結(jié)構(gòu)與溫度之間關(guān)系及靶材的失氧現(xiàn)象。得出600 ℃粉體為單相ITO固溶體、粒徑為15 nm,1000℃粉體有少量SnO2析出、粒徑為28 nm且其分散性和晶化程度優(yōu)于600 ℃的粉體。兩種粉體燒結(jié)制備靶材過程符合Coble固相燒結(jié)理論,1550 ℃時(shí)晶體出現(xiàn)類似二維成核生長方式的生長臺(tái)階。靶材密度隨溫度升高而增加,1550 ℃時(shí)隨保溫時(shí)間延長而增加。靶材致密化過程由團(tuán)聚程度及團(tuán)聚體大小決定,1000 ℃粉體制備的靶材密度高于600 ℃粉體所制靶材。兩類靶材含氧量均低于理論值,1000 ℃粉體所制靶材含氧量高于600 ℃的含氧量。

    Abstract:

    Two kinds of nanosized indium-tin-oxide (ITO) powders were prepared by heating the ITO precursors at 600 and 1000 oC respectively. The compacts were obtained by press molding of the powders. Then ITO targets were prepared by sintering the compacts at 400-1550 oC in oxygen atmosphere. The powders and the targets were characterized. The grain growth during sintering, the relationship between the targets’ microstructure and the sintering temperature, and the oxygen content of the targets were investigated. The results show that powders prepared by heating the ITO precursors at 600 oC (600 oC ITO powder) are single phase, and their grain size is 15 nm. Powders prepared by heating the ITO precursors at 1000 oC (1000 oC ITO powder) contain a little SnO2, and the grain size is 28 nm. 1000 oC ITO powders exhibit better dispersivity and keep higher crystallization degree. The sintering process of these two kinds of ITO powders corresponds with Coble Solid Phase Sintering process. When the sintering temperature is 1550 oC, crystal growth steps similar to the steps appearing in the two-dimensional nucleation growth can be observed. ITO targets’ density increases as the temperature rises and holding time extends. The density of ITO targets made from 1000 oC ITO powders is higher than that of the targets made from 600 oC ITO powders. This phenomenon indicates that targets’ densification is determined by the degree of agglomeration and the size of agglomerates. Both types of targets contain less oxygen than the theoretical value. And the oxygen content of targets made from 1000 oC ITO powders are higher than that of targets made from 600 oC ITO powders.

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王 玥,劉家祥,劉 宸.納米級(jí)ITO粉體對(duì)燒結(jié)法制備靶材的影響[J].稀有金屬材料與工程,2011,40(12):2179~2183.[Wang Yue, Liu Jiaxiang, Liu Cheng. Effect of Nanosized ITO Powders on Preparation of ITO Targets by Sintering Method[J]. Rare Metal Materials and Engineering,2011,40(12):2179~2183.]
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  • 收稿日期:2010-12-21
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