粉末冶金材料科学与工程
粉末冶金材料科學與工程
분말야금재료과학여공정
POWDER METALLURGY MATERIALS SCIENCE AND ENGINEERING
2014年
6期
955-961
,共7页
肖海波%李詠侠%邹丹%刘艳军%姚锐%阳东方%郑峰
肖海波%李詠俠%鄒丹%劉豔軍%姚銳%暘東方%鄭峰
초해파%리영협%추단%류염군%요예%양동방%정봉
草酸盐共沉淀%Co-V-Cr合金粉末%煅烧
草痠鹽共沉澱%Co-V-Cr閤金粉末%煅燒
초산염공침정%Co-V-Cr합금분말%단소
oxalate co-precipitation%Co-V-Cr alloy powder%calcination
以Co、V、Cr的可溶性氯盐和草酸铵为原料,采用草酸盐共沉淀法制备Co、V、Cr的复合粉末的前驱体,热分解后获得Co-V-Cr复合粉末。通过DSC/TG分析对该前驱体在不同气氛(真空、氩气与氮气)中的热分解过程进行研究,通过扫描电镜观察与比表面积测试,对Co-V-Cr复合粉末的性质进行分析与表征。结果表明,不论在什么气氛下锻炼,所得Co-V-Cr复合粉末的粒径都达到纳米级,分散较均匀,V和Cr完全固溶在Co相中。前驱体合理的煅烧温度为450℃。在氩气气氛下前驱体粉末在421℃时直接分解成Co-V-Cr复合粉末;而在空气中的DSC-TG曲线在366℃出现放热峰,原因是此温度下发生氧化反应,前驱体先分解成Co-V-Cr然后被氧化。在氩气气氛下煅烧得到的Co-V-Cr复合粉末比表面积最大,为41.50 m2/g,粒径最小,平均晶粒尺寸为11~12 nm。
以Co、V、Cr的可溶性氯鹽和草痠銨為原料,採用草痠鹽共沉澱法製備Co、V、Cr的複閤粉末的前驅體,熱分解後穫得Co-V-Cr複閤粉末。通過DSC/TG分析對該前驅體在不同氣氛(真空、氬氣與氮氣)中的熱分解過程進行研究,通過掃描電鏡觀察與比錶麵積測試,對Co-V-Cr複閤粉末的性質進行分析與錶徵。結果錶明,不論在什麽氣氛下鍛煉,所得Co-V-Cr複閤粉末的粒徑都達到納米級,分散較均勻,V和Cr完全固溶在Co相中。前驅體閤理的煅燒溫度為450℃。在氬氣氣氛下前驅體粉末在421℃時直接分解成Co-V-Cr複閤粉末;而在空氣中的DSC-TG麯線在366℃齣現放熱峰,原因是此溫度下髮生氧化反應,前驅體先分解成Co-V-Cr然後被氧化。在氬氣氣氛下煅燒得到的Co-V-Cr複閤粉末比錶麵積最大,為41.50 m2/g,粒徑最小,平均晶粒呎吋為11~12 nm。
이Co、V、Cr적가용성록염화초산안위원료,채용초산염공침정법제비Co、V、Cr적복합분말적전구체,열분해후획득Co-V-Cr복합분말。통과DSC/TG분석대해전구체재불동기분(진공、아기여담기)중적열분해과정진행연구,통과소묘전경관찰여비표면적측시,대Co-V-Cr복합분말적성질진행분석여표정。결과표명,불론재십요기분하단련,소득Co-V-Cr복합분말적립경도체도납미급,분산교균균,V화Cr완전고용재Co상중。전구체합리적단소온도위450℃。재아기기분하전구체분말재421℃시직접분해성Co-V-Cr복합분말;이재공기중적DSC-TG곡선재366℃출현방열봉,원인시차온도하발생양화반응,전구체선분해성Co-V-Cr연후피양화。재아기기분하단소득도적Co-V-Cr복합분말비표면적최대,위41.50 m2/g,립경최소,평균정립척촌위11~12 nm。
Co-V-Cr composite powder was obtained after thermal decomposing oxalic acid salt precursor of Co-V-Cr powder prepared through oxalate co-precipitation method using Co, V, Cr soluble chloride and ammonium oxalate as raw materials. The decomposition process of precursor was studied by DSC and TG. The properties of composite were analyzed and characterized by SEM and BET. The results show that the particle size of Co-V-Cr composite powder is nanometer grade, well dispersing and V, Cr soluting in Co completely. The appropriate calcination temperature is 450℃. Precursor powder decompose into Co-V-Cr composite powder directly in argon atmosphere at 421℃; Whereas in air, DSC and TG curves present an exothermic peak at 366℃ indicating an oxidation reaction at this temperature, which suggests that the precursor powders first decompose into composite powder, then followed by a process of oxidation. Co-V-Cr composite powders with maximum specific area of 41.50 (m2/g) and the smallest grain size of 11~12 nm are obtained in argon atmosphere calcination.