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首页> 外文会议>International Conference on Proceeding amp; Manufacturing of Advanced Materials; 20060704-08; Vancouver(CA) >Production of titanium nitride by carbothermic reduction of the anatase and rutile forms of titanium dioxide
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Production of titanium nitride by carbothermic reduction of the anatase and rutile forms of titanium dioxide

机译：通过碳热还原锐钛矿和金红石形式的二氧化钛生产氮化钛

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Two types of titanium oxide were used, rutile ( > 99.9% TiO_2) and anatase ( > 99% TiO_2). Both samples were mixed with graphite in accordance with the required stoichiometry, and then milled in a tumbling mill for 50 hours in an argon atmosphere to ensure thorough mixing. The mill vial was loaded with five 25.4 mm diameter stainless steel balls giving a powder to ball mass ratio of 1:43. After milling, samples were heated to 1400℃ in an alumina crucible at 20℃ min~(-1) under a flowing nitrogen (100 mL min~(-1)) atmosphere in a thermogravimetric analyser (TGA). Srilankite was detected in the as-milled anatase sample but the anatase to rutile transformation was not completed during milling. After heating to 800℃ most of the anatase had transformed to rutile. Reduction of anatase started just below 900℃ whilst rutile underwent reduction below 800℃. TGA results showed that the anatase reduction was more complex than the rutile reduction with several stages evident between 880 and 1000℃ in the anatase sample whilst only two steps were observed for rutile. The initial identified products were Ti_5O_9 and Ti_4O_7 prior to TiN in anatase sample but in rutile sample only Ti_4O_7 was detected. Reduction was completed in rutile sample before 1180℃ whilst in anatase completed at 1230℃. TiN was the final product in both systems after heating to 1400℃. These results are discussed in light of recent work demonstrating the different reductions paths of rutile and anatase.
机译：使用两种类型的二氧化钛，金红石型（> 99.9％TiO_2）和锐钛矿型（> 99％TiO_2）。根据所需的化学计量，将两种样品与石墨混合，然后在氩气气氛下在滚筒式磨机中研磨50小时，以确保充分混合。研磨瓶中装有五个直径为25.4 mm的不锈钢球，粉末与球的质量比为1:43。研磨后，在热重分析仪（TGA）中，在流动的氮气（100 mL min〜（-1））气氛下，在氧化铝坩埚中于20℃min〜（-1）下将样品加热至1400℃。在研磨后的锐钛矿样品中检测到斯里兰卡绢矿，但是在研磨过程中锐钛矿向金红石的转化没有完成。加热到800℃后，大多数锐钛矿转化为金红石型。刚好在900℃以下还原锐钛矿，而金红石在800℃以下还原。 TGA结果表明，锐钛矿还原过程比金红石还原过程更为复杂，在880到1000℃之间，锐钛矿样品有多个阶段，而金红石只有两个步骤。最初鉴定的产物是锐钛矿样品中TiN之前的Ti_5O_9和Ti_4O_7，但在金红石样品中仅检测到Ti_4O_7。在1180℃之前，金红石样品中的还原完成，而在1230℃时，锐钛矿中的还原完成。加热到1400℃后，TiN是两个系统中的最终产品。根据最近的工作讨论了这些结果，这些工作表明了金红石和锐钛矿的不同还原途径。

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