原位加热电镜技术研究WO3-BiVO4非晶复合薄膜退火相变过程

宋海利,黄 荣*

原位加热电镜技术研究WO3-BiVO4非晶复合薄膜退火相变过程

宋海利,黄 荣*

(1. 中山大学化学学院,生物无机与合成化学教育部重点实验室,广东广州510006;2.华东师范大学,极化材料与器件教育部重点实验室,上海 200062)

  本文利用原位加热电镜技术和高分辨透射电镜研究了WO3-BiVO4非晶复合薄膜原位退火相变过程。退火过程中,薄膜中的Bi元素逐渐挥发,由于电镜中的高真空缺氧环境,加热到600 ℃时,形成的结晶相大部分为立方W相,少量的WOx(0<x≤3)、VOx (0<x≤2.5)和BixVOy(0<x≤1, 0<y≤4)氧化物晶相,完全不同于利用脉冲激光沉积方法在充足氧气气氛和600 ℃条件下生长退火后形成的WO3纳米柱嵌入BiVO4基质中的垂直异质外延结晶复合薄膜。因此,退火气氛和样品的受热方式对薄膜的结晶相变过程有很大影响。

关键词  原位加热电镜技术;WO3-BiVO4复合薄膜;退火相变

中图分类号:TG115.21+5.3;O484.1;O76;TB34  文献标识码:A  doi:10.3969/j.issn.1000-6281.2023.03.002

 

Phase transition of WO3-BiVO4 amorphous composite film investigated by in-situ heating electron microscopy

SONG Hai-li1,HUANG Rong2*

(1. Key Laboratory of Bioinorganic and Synthetic Chemistry of Ministry of Education, School of Chemistry, Sun Yat-Sen University, Guangzhou 510275;2. Key Laboratory of Polar Materials and Devices (MOE) and Department of Electronics, East China Normal University, Shanghai 200062, China)

Abstract  The phase transition of WO3-BiVO4 amorphous composite film was investigated by in-situ heating electron microscopy. During the annealing process, Bi elements were easily evaporated. The main crystalline phase was a cubic W phase with a small amount of orthorhombic WOx, orthorhombic VOx and tetragonal BixVOy phases when the film was heated to550 oC. This is different from the vertical heteroepitaxial crystalline composite film with WO3 nanopillars embedded in the BiVO4 matrix grown in the sufficient oxygen at 600 oC by pulsed laser deposition. Thus, the atmosphere during the annealing process and the heating mode greatly influence the crystallization process of the composite film.

Keywords  in-situ heating electron microscopy;WO3-BiVO4 composite film;annealing and phase transition


 

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