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通过熔盐合成法制备的球形和棒状PbTiO粉末的结构表征与介电性能

Structural Characterizations and Dielectric Properties of Sphere- and Rod-Like PbTiO Powders Synthesized via Molten Salt Synthesis.

作者信息

Ji Qing, Xue Piaojie, Wu Heng, Pei Zhipeng, Zhu Xinhua

机构信息

National Laboratory of Solid State Microstructures, School of Physics, Nanjing University, Nanjing, 210093, China.

出版信息

Nanoscale Res Lett. 2019 Feb 21;14(1):62. doi: 10.1186/s11671-019-2899-9.

Abstract

By reaction of PbCO and TiO in the eutectic NaCl-KCl salts, both sphere- and rod-like PbTiO (PTO) powders were synthesized via molten salt synthesis (MSS) and template MSS methods, respectively. X-ray diffraction patterns reveal that all the PTO powders crystallize in a tetragonal phase structure. Increasing the molar ratio of PbCO:TiO:NaCl:KCl from 1:1:10:10 to 1:1:60:60 in the MSS process has little effect on the sphere-like morphology of the PTO powders synthesized at 950 °C for 5 h. Large-scale polycrystalline rod-like PTO powders with diameters of 480 nm-1.50 μm and lengths up to 10 μm were synthesized at 800 °C for 5 h by template MSS method, where the rod-like anatase TiO precursors were used as templates and the molar ratio of PbCO:TiO:NaCl:KCl was equal to 1:1:60:60. X-ray energy dispersive spectroscopy spectra reveal that all the PTO powders are composed of Pb, Ti, and O elements, and the measured Pb:Ti atomic ratios are close to 1:1. In the template MSS process, the molten salt content plays an important role in forming the rod-like PTO powders. Under low molten salt content, the rod-like PTO powders cannot be synthesized even if the rod-like TiO templates are used. In addition, prolonging the reaction time suppressed the formation of rod-like PTO powders but promoted the formation of sphere-like PTO nanoparticles. The dielectric properties the sphere- and rod-like PTO powders were comparatively investigated. At room temperature, the dielectric constant and dielectric loss of the spherical PTO powders synthesized by MSS method with the molar ratio of PbCO:TiO:NaCl:KCl equal to 1:1:30:30 were ~ 340 and 0.06 (measured at 10 Hz), respectively. The corresponding values for the rod-like PTO powders synthesized by template MSS method with the molar ratio of PbCO:TiO:NaCl:KCl equal to 1:1:60:60 were 140 and 0.08, respectively. The present results demonstrate the sphere-like PTO powders have better dielectric properties, which have promising applications in the fields of multilayer capacitors and resonators.

摘要

通过在共晶NaCl-KCl盐中使碳酸铅(PbCO)与二氧化钛(TiO)反应,分别采用熔盐合成法(MSS)和模板MSS法合成了球状和棒状的钛酸铅(PTO)粉末。X射线衍射图谱表明,所有PTO粉末均结晶为四方相结构。在MSS过程中,将PbCO:TiO:NaCl:KCl的摩尔比从1:1:10:10增加到1:1:60:60,对在950℃下反应5小时合成的球状PTO粉末的形貌影响不大。通过模板MSS法,以棒状锐钛矿TiO前驱体为模板,在800℃下反应5小时,合成了直径为480nm-1.50μm、长度可达10μm的大规模多晶棒状PTO粉末,此时PbCO:TiO:NaCl:KCl的摩尔比为1:1:60:60。X射线能量色散光谱表明,所有PTO粉末均由Pb、Ti和O元素组成,测得的Pb:Ti原子比接近1:1。在模板MSS过程中,熔盐含量对棒状PTO粉末的形成起着重要作用。在低熔盐含量下,即使使用棒状TiO模板也无法合成棒状PTO粉末。此外,延长反应时间会抑制棒状PTO粉末的形成,但会促进球状PTO纳米颗粒的形成。对球状和棒状PTO粉末的介电性能进行了比较研究。在室温下,通过MSS法合成的PbCO:TiO:NaCl:KCl摩尔比为1:1:30:30的球状PTO粉末的介电常数和介电损耗(在10Hz下测量)分别约为340和0.06。通过模板MSS法合成的PbCO:TiO:NaCl:KCl摩尔比为1:1:60:60的棒状PTO粉末的相应值分别为140和0.08。目前的结果表明,球状PTO粉末具有更好的介电性能,在多层电容器和谐振器领域具有广阔的应用前景。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/3ca8/6384292/8363a6c2453f/11671_2019_2899_Fig1_HTML.jpg

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