pH对水热合成法制备铬渣源复合薄膜性能的影响

doi:10.3724/SP.J.1077.2013.12239

摘要/Abstract

摘要：

以铬渣为基本原料, 采用水热合成法制备了复合薄膜, 对样品进行了SEM、ICP、XRD、FT-IR及薄膜厚度表征分析, 以薄膜的折射率和反射率为对比参数, 研究了水热反应初始pH对薄膜的影响。研究结果表明, 当水热反应初始pH达11以上时, 薄膜表面呈现完美的空间三维立体网状结构; 当水热反应的pH为9、10时, 样品中形成了Al₂O₃、Fe₂O₃、Fe(OH)₃、Cr₂O₃、AlO(OH)和MgO晶体, 且其衍射峰较强; 样品内部纳米颗粒间存在毛细孔水和表面吸附水, 水热体系内的碱性基团促进膜物质与基底间形成化学键力的结合。薄膜越厚, 其折射率越小, 水热反应pH为11时, 薄膜最薄, 折射率最大; 水热反应的初始pH为12时制备的薄膜对紫外光反射率低于玻璃基底, 水热反应的初始pH为11时制备的薄膜对可见光的反射率小于玻璃基底。

关键词: 铬渣, 综合利用, 水热合成, 复合薄膜

Abstract:

With chromium residue as main raw materials, the composite films were prepared by hydrothermal method. The samples were characterized by SEM, ICP, XRD, FT-IR and film thickness, and the influences of hydrothermal pH value on the performance of composite films were investigated using the films’ refractive index and reflectivity as evaluation indexes. The results show that the perfect three dimension networks are appeared on the film surface when pH value is above 11. At pH value of 9 or 10, Al₂O₃, Fe₂O₃, Fe(OH)₃, Cr₂O₃, AlO(OH) and MgO crystals are formed in the sample, and the diffraction peak of them is strong. There are pores and surface absorbed water between internal nanoparticles in the samples. In the process of hydrothermal synthesis, the formation of chemical bonds force between the membrane material and basement are facilitated by the alkaline groups. Meanwhile, the thicker film is the smaller the refractive index of the film will be. At pH value of 11, the film is the thinnest and the refractive index is the biggest. At the initial pH value of 12, the refractive index of the film to ultraviolet light is weaker than glass substrate, and at the initial pH value of 11, the refractive index of the film to visible light is weaker than that of glass substrate.

Key words: chromium residue, comprehensive utilization, hydrothermal synthesis, composite film

中图分类号:

X753
TB332

孙彤, 刘连利, 徐姝颖, 彭晓琳, 杨海龙. pH对水热合成法制备铬渣源复合薄膜性能的影响[J]. 无机材料学报, 2013, 28(4): 387-392.

SUN Tong, LIU Lian-Li, XU Shu-Ying, PENG Xiao-Lin, YANG Hai-Long. Influence of pH Value on the Performance of Composite Films Prepared from Chromium Residue by Hydrothermal Method[J]. Journal of Inorganic Materials, 2013, 28(4): 387-392.

图/表 6

图1 水热反应不同pH下制备薄膜的SEM照片

Fig. 1 SEM microphotographs of the films prepared with different hydrothermal pH values (a) pH=7; (b) pH=8; (c) pH=9; (d) pH=10; (e) pH=11; (f) pH=12

Table 1 The percentage composition of metallics in the powders

Metallic element	Fe₂O₃	Al₂O₃	CaO	Cr₂O₃	MgO	Na₂O	K₂O
Mass percentage/%	30.46	12.26	5.27	5.83	13.71	2.98	0.97

图2 不同pH下水热反应制备粉体的XRD图谱

Fig. 2 XRD patterns of the powders prepared with different hydrothermal pH values (a) pH=7; (b) pH=8; (c) pH=9; (d) pH=10; (e) pH=11; (f) pH=12

图3 不同pH下水热反应制备粉体的FT-IR表征结果

Fig. 3 FT-IR spectra of the powders prepared with different hydrothermal pH values (a) pH=7; (b) pH=8; (c) pH=9; (d) pH=10; (e) pH=11; (f) pH=12

图4 不同pH下水热反应制备薄膜的膜厚及折射率

Fig. 4 Film thickness and refractive index of the films prepared with different hydrothermal pH values

图5 不同pH下水热反应制备薄膜的反射率

Fig. 5 Reflectivity of the films prepared with different hydrothermal pH values

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