碳源对先驱体转化法制备TaC陶瓷粉体微观结构及性能影响  

Effects of Carbon Sources on Structure and Properties of TaC Ceramic Powder Prepared by Polymer Derived Ceramics

作　　者：孙敬伟 王洪磊 孙楚函 周新贵[1] 纪小宇 SUN Jingwei;WANG Honglei;SUN Chuhan;ZHOU Xingui;JI Xiaoyu(Science and Technology on Advanced Ceramic Fibers and Composites Laboratory,College of Aerospace Science and Engineering,National University of Defense Technology,Changsha 410073,China;National Key Laboratory of Science and Technology on Vessel Integrated Power System,Naval University of Engineering,Wuhan 430033,China)

机构地区：[1]国防科技大学空天科学学院,新型陶瓷纤维及其复合材料重点实验室,长沙410073 [2]海军工程大学舰船综合电力技术国防科技重点实验室,武汉430033

出　　处：《无机材料学报》2023年第2期184-192,共9页Journal of Inorganic Materials

基　　金：湖南省自然科学基金(2020JJ4667)。

摘　　要：先驱体转化法是制备耐超高温陶瓷和粉体的有效方法之一,但原料种类对先驱体交联固化程度和陶瓷产率的影响鲜有报道。本研究分别采用两种碳源与聚钽氧烷(PTO)合成了TaC先驱体,研究了碳源种类、裂解温度和钽碳比例等因素对先驱体转化法制备TaC陶瓷粉体微观结构及性能的影响。结果表明,含C=C的PF-3树脂可以有效促进PTO的交联固化,提高先驱体的陶瓷产率。当钽碳质量比分别为PTO:PF-3树脂=1:0.25和PTO:2402树脂=1:0.4时,在1400℃下裂解获得的TaC陶瓷粉体不含残余Ta2O5,陶瓷产率分别为54.02%和49.64%,晶粒尺寸分别为47.2和60.9 nm。PF-3树脂在提高陶瓷产率的同时能够减小晶粒尺寸,但对粉体纯度与粒度影响较小。不同碳源制备的TaC陶瓷粉体纯度分别为96.50%和97.36%,中位径分别为131和129 nm。Polymer derived ceramic is one of the effective methods for producing ultra-high temperature ceramics and powders,but effect of source material type on precursor cross-linking degree and ceramic yield has rarely been reported.Here,TaC precursors were synthesized using two carbon sources and poly-tantalumoxane(PTO).Phase composition and microstructure of TaC ceramic powders from different carbon sources,tantalum/carbon mass ratios,and pyrolysis temperatures were characterized.It was found that PF-3 resin with C=C was effective in promoting the cross-linking of PTO and increasing the ceramic yield.When the mass ratio of PTO to PF-3 Resin was 1:0.25 and PTO to 2402 Resin was 1:0.4,TaC ceramic powders could be obtained at 1400℃without residue Ta2O5.Ceramic yields of ceramic powders were 54.02%and 49.64%,and the crystal sizes were 47.2 and 60.9 nm,respectively.Therefore,PF-3 resin is able to reduce crystal size while increasing ceramic yield,but has less impact on the powder purity and particle size.The purity of TaC ceramic powders derived from different carbon sources are 96.50%and 97.36%,respectively,meanwhile the median diameters are 131 and 129 nm,respectively.

关 键 词：聚钽氧烷(PTO) 先驱体转化法 TAC 交联 固化 陶瓷产率 

分 类 号：TH145[一般工业技术—材料科学与工程]