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作 者:湛菁[1] 邬建辉[1] 张传福[1] 岳建峰[1]
机构地区:[1]中南大学冶金科学与工程学院,湖南长沙410083
出 处:《矿冶工程》2010年第2期64-69,共6页Mining and Metallurgical Engineering
基 金:中国博士学科点新教师基金(20090162120080);湖南省自然科学基金资助项目(09JJ4028);中国博士后基金资助项目(20070410989);中南大学科学基金(748310000)
摘 要:以可溶性镍盐和草酸或草酸铵为原料,利用氨为配位剂,通过配位沉淀法制备了纤维状氧化亚镍粉新型前驱体,并采用XRD、红外光谱(IR)和扫描电镜(SEM)研究了前驱体粉末的物相、成分与形貌,系统考察配位沉淀条件包括溶液pH值、反应温度、反应物浓度和表面活性剂对前驱体粉末形貌、粒度和成分的影响。结果表明:Ni(Ⅱ)-C2O4^2--NH3-NH4^+H2O反应体系中,在溶液pH值为8.2~8.8,温度为60-70℃,Ni^2+浓度为0.5—0.8mol/L,表面活性剂聚乙烯吡咯烷酮(PVP)用量为0.1%~0.5%条件下得到的新型前驱体为草酸镍氨复盐,其形貌为纤维状;氨与镍离子配合并生成草酸镍氨复盐是纤维状形貌形成的内在机制。通过在空气中热分解该种前驱体即可得到比表面积为5.944m^2/g、轴径比大于50的纤维状氧化亚镍粉末。A novel precursor for fiber-like nickel oxide powders has been synthesized by coordination-precipitation process using NiCl2 · 6H2O and oxalate or ammonia oxalate as starting materials and ammonia as complexing agent. The phase, composition and morphology of the novel precursor were analyzed by XRD, IR and SEM. The influences of various coordination-precipitation conditions including pH value, precipitation temperature, reactant concentration and surfactant addition on the morphology, composition and size of the precursor particles were investigated in detail. The resuits showed that the precursors obtained in the reaction system of Ni( Ⅱ )-C2O4^2--NH3-NH4^+-H2O under the conditions such as pH value of 8.2 - 8.8, Ni^2+ concentration of 0. 60 - 75 ℃ and surfactant PVP dosage of 0.1% - 0.5% was 5 - 0. 8 mol/L, coordination-precipitation temperature of nickel oxalate-ammonia complex salt, which has a fiber- like morphology. The coordination of ammonia with nickel ions resulted in nickel oxalate-ammonia complex salt, which tells the intrinsic mechanism of the formation of fiber-like morphology. The fiber-like NiO powders with axis/diameter ratio more than 50 and specific surface area of 5. 944 m^2/g can be produced by thermal decomposition of the novel precursor in air.
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