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纳米铜锰复合氧化物固相反应法的制备与表征
Preparation and characterization of nano-sized Cu-Mn composite oxide by solid-state reaction method

作  者: ;

机构地区: 海南医学院药学院药学系

出  处: 《无机盐工业》 2007年第11期30-33,共4页

摘  要: 以乙酸铜、乙酸锰与草酸为原料,采用固相化学反应法制备了纳米铜锰复合氧化物前驱物,利用均匀设计考察了微波功率与加热时间、热分解温度及时间对产物粒径的影响。研究表明热分解温度对产品粒径的影响最大。最小粒径产物的制备条件是:微波功率540 W,微波加热时间15 min;热分解温度370℃,热分解时间2 h。XRD和TEM分析结果表明,此产品主要物相为Cu1.5Mn1.5O4,结构属立方晶系,空间群为Fd3m,平均粒径16.9-19.0 nm。应用TG-DTG和DSC技术研究了纳米铜锰复合氧化物的热分解过程以及热分解动力学,采用Ozawa积分法和Coats-Redfern积分法得前驱体的热分解机理函数均为G(α)=[-ln(1-α)]^2/3。 Precursor of nano - sized Cu - Mn composite oxide was synthesized by solid - state chemical reaction method with cupric acetate [ Cu ( CH3 COO ) 2 · H2O ], manganese acetate [ Mn ( CH3 COO ) 2 · 4 H2O ] and oxalic acid [ H2 C2 O4 · 2H2 O] as the raw materials. The influences of microwave power, heating time, thermal decomposition temperature and time on the particle size of the product were investigated by homogeneous design. Experimental results showed that thermal decomposition temperature had the greatest influence on the particle size. The optimum conditions for preparing the product with the smallest particle size were:microwave power = 540 W,microwave heating time =15.0 min,thermal decomposition temperature-370℃ and thermal decomposition time = 2 h. The results of XRD and TEM showed that the product's main phase was Cu1.5 Mn1 5 O4,which belonged to isometric system;the space group was Fd3m; and the average particle size was 16.9 - 19.0 nm. Besides, the thermal decomposition process and thermal decomposition dynamics of nano - sized Cu - Mn composite oxide were studied with the application of TG - DTG and DSC techniques. The obtained thermal decomposition mechanism functions of the precursor were all G(α) = [ - ln( 1 - α) ]^ 2/3 either with Ozawa integral method or Coats - Redfern integral method.

关 键 词: 均匀设计 固相化学反应法 纳米铜锰复合氧化物 热分解机理

领  域: [化学工程]

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