草酸-硝酸盐低热固相反应法制备(Ni_(0.58)Cu_(0.2)Zn_(0.22))Fe_(1.96)O_4铁氧体

Synthesis of Nanocrystalline(Ni_(0.58)Cu_(0.2)Zn_(0.22))Fe_(1.96)O_4 by Low-heating Solid-state Reaction

以草酸和金属硝酸盐为原料,用低热固相反应法合成了纳米(Ni0.58Cu0.2Zn0.22)Fe1.96O4尖晶石型铁氧体,借助FT-IR、DSC-TG、XRD、TEM以及SEM等技术对固相反应过程和样品进行了研究及表征。FT-IR研究表明,草酸和金属硝酸盐在研磨过程中发生低热固相反应,生成金属草酸盐前驱体;FT-IR和XRD分析表明,前驱体经不同温度焙烧后得到单一尖晶石相的NiCuZn铁氧体粉末;依据TEM和SEM表征证明,前驱体在450℃分解1h后铁氧体粒径约为30～40nm,铁氧体于900℃烧结为陶瓷体后,晶粒约为2～4μm,烧结致密,磁谱测量表明,900℃烧结样品的磁导率为210,截止频率为28MHz。

Nanocrystalline （Ni0.58Cu0.2Zn0.22）Fe1.96O4 with spinel structure is prepared by low-heating solidstate reaction method. The reaction process and thermal decomposition of oxalate precursors are investigated using FT-IR spectra, DSC-TG and XRD techniques. The results show that the metal ions can react with the oxalic acid by grinding for 30 minutes. The particle sizes of NiCuZn ferritenano-powders are about 30-40nm using TEM analysis. The results of X-ray diffraction technique reveal that NiCuZn ferrite powders prepared are the single spinel phase and the spinel crystal structure integrates gradually with the increase of the calcinations temperature. The NiCuZn ferrites sample can be sintered at 900℃ with properties of μi =210 and cutoff frequency being 28MHz.