Nakashima Kouichi, Hironaka Kouta, Oouchi Kazuma, Ajioka Mao, Kobayashi Yoshio, Yoneda Yasuhiro, Yin Shu, Kakihana Masato, Sekino Tohru
Department of Materials Science and Engineering, Graduate School of Science and Engineering, Ibaraki University, 4-12-1, Nakanarusawa, Hitachi, Ibaraki 316-8511, Japan.
Department of Biomolecular Functional Engineering, College of Engineering, Ibaraki University, 4-12-1, Nakanarusawa, Hitachi, Ibaraki 316-8511, Japan.
ACS Omega. 2021 Nov 24;6(48):32517-32527. doi: 10.1021/acsomega.1c04013. eCollection 2021 Dec 7.
Barium titanate (BaTiO) nanocubes with a narrow particle size distribution were synthesized using a three-step approach. First, a water-soluble Ti complex was synthesized using a hydrolysis method. Next, the titanium dioxide (TiO) raw material was synthesized via a hydrothermal method using various water-soluble titanium (Ti) complexes. The TiO exhibited various particle sizes and crystal structures (anatase, rutile, or brookite) depending on the water-soluble Ti complex and the hydrothermal conditions used in its synthesis. Finally, BaTiO nanocubes were subsequently created through a hydrothermal method using the synthesized TiO particles and barium hydroxide octahydrate [Ba(OH)·8HO] as raw materials. The present study clarifies that the particle size of the BaTiO nanocubes depends on the particle size of the TiO raw material. BaTiO particles with a narrow size distribution were obtained when the TiO particles exhibited a narrow size distribution. We found that the best conditions for the creation of BaTiO nanocubes using TiO involved using lactic acid as a complexing agent, which resulted in a particle size of 166 nm on average. This particle size is consistent with an average of the width of the cubes measured from corner to corner diagonally, which corresponds to a side length of 117 nm. In addition, surface reconstruction of the BaTiO was clarified via electron microscopy observations, identifying the outermost surface as a Ti layer. Electron tomography using high-angle annular dark-field (HAADF)-scanning transmission electron microscopy (STEM) confirmed the three-dimensional (3D) structure of the obtained BaTiO nanocubes.
采用三步法合成了粒径分布窄的钛酸钡(BaTiO₃)纳米立方体。首先,通过水解法合成了一种水溶性钛配合物。接下来,使用各种水溶性钛(Ti)配合物通过水热法合成二氧化钛(TiO₂)原料。根据合成中使用的水溶性钛配合物和水热条件,TiO₂呈现出各种粒径和晶体结构(锐钛矿、金红石或板钛矿)。最后,以合成的TiO₂颗粒和八水合氢氧化钡[Ba(OH)₂·8H₂O]为原料,通过水热法制备了BaTiO₃纳米立方体。本研究表明,BaTiO₃纳米立方体的粒径取决于TiO₂原料的粒径。当TiO₂颗粒呈现窄粒径分布时,可获得粒径分布窄的BaTiO₃颗粒。我们发现,使用TiO₂制备BaTiO₃纳米立方体的最佳条件是使用乳酸作为络合剂,平均粒径为166 nm。该粒径与从角对角测量的立方体宽度平均值一致,对应边长为117 nm。此外,通过电子显微镜观察阐明了BaTiO₃的表面重构,确定最外层表面为Ti层。使用高角度环形暗场(HAADF)扫描透射电子显微镜(STEM)的电子断层扫描证实了所得BaTiO₃纳米立方体的三维(3D)结构。