二氧化硅粉体粒度对硅酸盐转化膜制备的影响<sup>*</sup>

doi:10.11901/1005.3093.2013.940

材料研究学报

2014, Vol. 28

Issue (6): 462-468 DOI: 10.11901/1005.3093.2013.940

本期目录 | 过刊浏览

二氧化硅粉体粒度对硅酸盐转化膜制备的影响^*

孔纲¹,张双红¹(

),孙子文²,车淳山¹,卢锦堂¹

1. 华南理工大学材料学院广州 510640
2. 广东省计量科学研究院广州 510405

Effect of Size of Silica Powder on Preparation of Silicate Conversion Coatings on Galvanized Steel

Gang KONG¹,Shuanghong ZHANG^1,^**(

),Ziwen SUN²,Chunshan CHE¹,Jintang LU¹

1. School of Materials Science and Engineering, South China University of Technology, Guangzhou 510640
2. Guangdong Institute of Metrology, Guangzhou 510405

引用本文:

孔纲,张双红,孙子文,车淳山,卢锦堂. 二氧化硅粉体粒度对硅酸盐转化膜制备的影响^*[J]. 材料研究学报, 2014, 28(6): 462-468.
Gang KONG, Shuanghong ZHANG, Ziwen SUN, Chunshan CHE, Jintang LU. Effect of Size of Silica Powder on Preparation of Silicate Conversion Coatings on Galvanized Steel[J]. Chinese Journal of Materials Research, 2014, 28(6): 462-468.

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摘要:

用微米和纳米粒度的SiO₂粉体分别配制SiO₂质量分数为5%、模数(SiO₂/Na₂O摩尔比)为3.50的硅酸钠溶液, 并用之浸泡热镀锌钢制备了硅酸盐钝化膜。用X射线衍射(XRD)、反射红外光谱(RA-IR)分析二氧化硅粉体, 用透射红外光谱(FT-IR)和核磁共振(NMR)分析硅酸钠溶液的结构, 用原子力显微镜(AFM)、电化学阻抗谱(EIS)分析转化膜的结构。结果表明: 与微米级二氧化硅相比, 纳米级二氧化硅含有Si-OH键较多, 用它配制的硅酸钠溶液中硅酸负离子的聚合程度较低, 成膜过程脱水量较多而生成微观孔隙较多的转化膜。

关键词 ：无机非金属材料, 硅酸盐转化膜, 热镀锌, 硅酸钠, 二氧化硅

Abstract：

Sodium silicate solutions of SiO₂: Na₂O molar ratio 3.50 were prepared with 5 mass fraction % of micro- and nano-SiO₂ respectively, and then silicate conversion coatings were obtained by immersing hot-dip galvanized (HDG) steel sheets in the solutions. The SiO₂ powders were characterized by X-ray diffraction (XRD) and reflectance absorption infrared spectroscopy (RA-IR), the sodium silicate solutions were characterized by Fourier transform infrared spectroscopy (FT-IR) and nuclear magnetic resonance spectroscopy (²⁹Si NMR), and the silicate conversion coatings were characterized by atomic force microscope (AFM) and electrochemical impedance spectroscopy (EIS). The results show that there exist more Si-OH bonds in nano-SiO₂ rather than that in micro-SiO₂; the degree of polymerization of the silicate ions in sodium silicate solution with nano-SiO₂ is lower, therefore, the amount of dehydration generated in the coating formation process is higher, as a consequence, the formed silicate conversion coating possesses higher porosity.

Key words： inorganic non-metallic materials silicate conversion coating hot-dip galvanizing sodium silicate silica

收稿日期: 2013-12-11

基金资助:* 国际铅锌研究组织ILZRO/IZA/CN201212, 广东省教育部产学研结合2012B091100312, 中央高校基本科研业务费2012ZM0011资助项目。

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https://www.cjmr.org/CN/10.11901/1005.3093.2013.940 或 https://www.cjmr.org/CN/Y2014/V28/I6/462

图1 MS和NS粉体的XRD谱

图2 MS和NS粉体的RA-IR图

图3 MS粉体的SEM图和NS粉体的TEM图

图4 MS硅酸钠溶液和NS硅酸钠溶液的FT-IR谱

图5 硅酸钠溶液中5种硅氧连接示意图

图6 MS硅酸钠溶液和NS硅酸钠溶液的29SiNMR谱

图7 硅酸钠溶液的Si-O连接类型的分布

图8 MS硅酸盐转化膜和NS硅酸盐转化膜的AFM图

图9 HDG和两种硅酸盐膜试样的Bode图和拟合结果和等效电路图

表1 根据图9c算得的HDG及两种硅酸盐膜试样的等效元件的拟合参数值

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