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內(nèi)凝膠工藝結(jié)合碳熱氮化法制備ZrN納米粉體
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新型陶瓷與精細(xì)工藝國家重點實驗室

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國家自然科學(xué)基金資助(項目號No. 51420105006)


Preparation of ZrN Nanopowders by Internal Gelation and Carbothermic Nitridation
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State Key Laboratory of New Ceramics and Fine Processing,Collaborative Innovation Center of Advanced Nuclear Energy Technology,Institute of Nuclear and New Energy Technology,Tsinghua University

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    摘要:

    采用內(nèi)凝膠工藝制得無定形的氧化鋯凝膠與炭黑均勻混合的前驅(qū)體粉末,獲得的前驅(qū)體在氮氣條件下進(jìn)行碳熱氮化處理后得到氮化鋯(ZrN)納米粉體。結(jié)合熱重/差式掃描量熱分析(TGA/DSC)、X射線衍射(XRD)、掃描電子顯微鏡(SEM)和透射電子顯微鏡(TEM)等手段,對內(nèi)凝膠前驅(qū)體的熱處理行為、所得產(chǎn)物的物相組成、微觀形貌及顯微結(jié)構(gòu)等進(jìn)行了表征。研究結(jié)果表明,氮化溫度的升高有利于氮化程度的提高,1400℃氮化溫度下可得到純相納米ZrN粉體;此外,碳的引入在熱處理過程中起到了必要的還原作用,且碳的加入量需要適當(dāng),C/Zr摩爾比接近2是獲得純相ZrN粉體產(chǎn)物較為合適的條件。

    Abstract:

    Zirconium nitride (ZrN) nanopowders were prepared by carbothermic nitriding of precursor in flowing nitrogen. The precursor was mixture of zirconia gel and carbon black which was obtained by using internal gelation process. The heat treatment behavior of the precursor material, phase composition, morphology and microstructure of powder products were characterized by simultaneous thermogravimetric analysis and differential scanning calorimetric analysis (TGA/DSC), X-ray diffraction (XRD), scanning electron microscope (SEM) and transmission electron microscope (TEM). With increase in temperature, nitriding level increased. Pure ZrN phase was achieved at 1400°C and the particle size of the powder product was in nanometers. Carbon plays an important role of reductant in nitridation process and the carbon to zirconium mole ratio should be properly controlled to ~2 such that desired ZrN products could be prepared.

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趙世嬌,馬景陶,趙興宇,郝少昌,李自強,鄧長生,劉兵.內(nèi)凝膠工藝結(jié)合碳熱氮化法制備ZrN納米粉體[J].稀有金屬材料與工程,2020,49(2):732~736.[Zhao Shijiao, Ma Jingtao, Zhao Xingyu, Hao Shaochang, Li Ziqiang, Deng Changsheng, Liu Bing. Preparation of ZrN Nanopowders by Internal Gelation and Carbothermic Nitridation[J]. Rare Metal Materials and Engineering,2020,49(2):732~736.]
DOI:10.12442/j. issn.1002-185X. QH20190020

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  • 收稿日期:2019-03-12
  • 最后修改日期:2019-04-22
  • 錄用日期:2019-10-23
  • 在線發(fā)布日期: 2020-03-12
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