微波水热法合成纳米BaTiO3粉体的掺杂改性与性能研究

Study on doping modification and properties of nano-BaTiO3 powders synthesized by microwave hydrothermal method

以正钛酸四正丁酯(C16H36O4Ti)、Ba(OH)2·8H2O、NbCl5和NaOH试剂为原料,利用微波水热法,制备了不同含量Nb掺杂的纳米BaTi1-xNbxO3(x=0,0.01,0.02,0.03,0.04,0.05,0.06)粉体。然后,将纳米BaTi1-xNbxO3粉体压制成形并进行烧结处理,获得了不同含量Nb掺杂的BaTi1-xNbxO3压电陶瓷。采用X射线衍射(XRD)、拉曼光谱、扫描电子显微镜(SEM)等对纳米BaTi1-xNbxO3粉体的物相结构、表面形貌和晶粒尺寸进行分析,采用振动磁强计对BaTi1-xNbxO3压电陶瓷的烧结密度和磁性能进行分析。XRD和拉曼光谱分析表明,不同含量Nb掺杂的纳米BaTi1-xNbxO3(x=0,0.03,0.06)粉体具有四方特性;SEM形貌分析表明,纳米BaTi1-xNbxO3(x=0,0.03,0.06)粉体由粒径极细、分散性良好的球形颗粒组成,随着Nb含量的增加,粉体的颗粒尺寸也不断增加,其平均粒径分别约为60,90和120 nm;烧结密度研究表明,随着Nb含量的增加,BaTi1-xNbxO3压电陶瓷的烧结密度不断增大,当Nb含量为0.06时,BaTi1-xNbxO3压电陶瓷的烧结密度达到最大;磁性能分析表明,当Nb掺杂量为0.03时,BaTi1-xNbxO3压电陶瓷的剩余磁化强度最大(8.235 μC/cm2),且其矫顽力(5.762 kV/cm)与不掺杂Nb的BaTiO3陶瓷(5.556 kV/cm)相差不大。因此,Nb掺杂量为0.03时,BaTi1-xNbxO3压电陶瓷的压电性能最优。

Using tetrabutyl titanate (C16H36O4Ti), Ba(OH)2·8H2O, NbCl5 and NaOH reagents as raw materials, nano BaTi1-xNbxO3 (x=0, 0.01, 0.02, 0.03, 0.04, 0.05, 0.06) powders doped with different Nb contents were prepared by microwave hydrothermal method. Then, nano BaTi1-xNbxO3 powders were compacted and sintered to obtain BaTi1-xNbxO3 piezoelectric ceramics with different content of Nb doping. The phase structure, surface morphology and grain size of nano BaTi1-xNbxO3 powders were analyzed by X-ray diffraction (XRD), Raman spectroscopy and scanning electron microscopy (SEM). The sintering density and magnetic properties of BaTi1-xNbxO3 piezoelectric ceramics were analyzed by vibration magnetometer. XRD and Raman spectra showed that nano BaTi1-xNbxO3 (x=0, 0.03, 0.06) powders doped with different Nb content had tetragonal properties. SEM morphology analysis showed that nano BaTi1-xNbxO3 (x=0, 0.03, 0.06) powders were composed of spherical particles with fine particle size and good dispersibility. With the increase of Nb content, the particle size of nano BaTi1-xNbxO3 powders also increased. The average particle size of nano BaTi1-xNbxO3 powders was about 60, 90 and 120 nm, respectively. The sintering density of BaTi1-xNbxO3 piezoelectric ceramics increased with the increase of Nb content. When Nb content was 0.06, the sintering density of BaTi1-xNbxO3 piezoelectric ceramics reached the maximum. The analysis of magnetic properties showed that when Nb doping amount was 0.03, the residual magnetization of BaTi1-xNbxO3 piezoelectric ceramics was the highest (8.235 μC/cm2), and its coercivity (5.762 kV/cm) was similar to that of Nb-free BaTiO3 ceramics (5.556 kV/cm). Therefore, when Nb doping was 0.03, the piezoelectric properties of BaTi1-xNbxO3 piezoelectric ceramics were the best.