碳化铌高温磷化制备MAX相Nb_(2)PC  

Preparation of MAX phase Nb_(2)PC by phosphating of niobium carbide at high-temperature

作　　者：丛良伟 庞昇 王志[2] 李来时 吴玉胜[1] CONG Liangwei;PANG Sheng;WANG Zhi;LI Laishi;WU Yusheng(College of Materials Science and Engineering,Shenyang University of Technology,Shenyang 110870,Liaoning,China;Key Laboratory of Green Process and Engineering,Chinese Academy of Sciences,National Engineering Research Center for Green Recycling of Strategic Metal Resources,Institute of Process Engineering,Chinese Academy of Sciences,Beijing 100190,China)

机构地区：[1]沈阳工业大学材料科学与工程学院,沈阳110870 [2]中国科学院过程工程研究所,中国科学院绿色过程与工程重点实验室,战略金属资源绿色循环利用国家工程研究中心,北京100190

出　　处：《矿冶》2025年第1期104-111,168,共9页Mining And Metallurgy

基　　金：国家自然科学基金资助项目(52374418,52404328);中国博士后面上基金资助项目(2024M753248)。

摘　　要：理论计算结果已经证实MAX相Nb_(2)PC机械性能优于其它MAX相,是极具发展潜力的结构材料。但受限于现有含磷MAX相制备过程存在的原料成本高(原料需使用高纯金属、红磷、石墨粉体)、反应器设计复杂(反应需在密闭石英反应器中进行)以及反应时间长(由于磷沸点低,需进行长时间的低温磷化—高温反应制备MAX相)等瓶颈问题,含磷MAX相的深入研究一直被忽视。基于此,提出基于气固反应机理的含磷MAX相高温磷化制备新思路,利用磷铁渣中的FeP高温释放磷蒸汽特征,使其在高温下对Nb_(2)O_(5)碳热还原产物NbC进行磷化,成功实现了MAX相Nb_(2)PC的高效制备。同时,探究了原料配比、烧结温度及保温时间对产物纯度的影响。结果表明,当NbC与磷铁渣摩尔比为1∶5时,在1200℃下保温1 h可得到纯度大于99%的Nb_(2)PC。该方法有望为含磷MAX相的低成本、规模化制备提供技术基础。Theoretical calculations have unequivocally demonstrated that within the MAX phase,Nb_(2)PC exhibts superior mechanical properties in comparison to its counterparts,making it a highly promising material for structural applications.However,extensive exploration into phosphorus-containing MAX phases has been overlooked due to significant challenges,including exorbitant raw material expenses(necessitating high-purity metals,red phosphorus,and graphite powders),intricate reactor designs(mandating reactions within sealed quartz reactors),and protracted reaction durations(owing to phosphorus's low boiling point,necessitating a prolonged low-temperature phosphating/high-temperature reaction process for MAX phase synthesis).To address these challenges,this paper introduced an innovative strategy for the high-temperature phosphating synthesis of phosphorus-containing MAX phases,rooted in gas-solid reaction mechanisms.By utilizing the increased release of phosphorus vapor from FeP in the by-product ferrophosphorus slag during yellow phosphorus production,this method facilitated the phosphating of NbC—a carbon thermal reduction product of Nb_(2)O_(5)—at elevated temperatures,culminating in the successful and efficient production of the Nb_(2)PC MAX phase.Furthermore,the study delved into the influence of raw material ratios,sintering temperature,and thermal retention time on product purity.The results indicate that a molar ratio of 1∶5 between NbC and ferrophosphorus slag,combined with a holding temperature of 1200℃for 1 hour,yields Nb_(2)PC with a purity exceeding 99%.This pioneering approach holds great promise in establishing a technical foundation for the cost-effective and large-scale production of phosphorus-containing MAX phases.

关 键 词：磷铁渣 NBC 高温磷化 气固反应 Nb_(2)PC 

分 类 号：TF83[冶金工程—有色金属冶金] TF84