周雄,胡广洪.基于正交实验优化不锈钢表面纳米孔结构制备工艺[J].表面技术,2019,48(1):161-167.
ZHOU Xiong,HU Guang-hong.Preparation Process of Nanoporous Structure on Stainless Steel Surface by Orthogonal Experimental Methods[J].Surface Technology,2019,48(1):161-167
基于正交实验优化不锈钢表面纳米孔结构制备工艺
Preparation Process of Nanoporous Structure on Stainless Steel Surface by Orthogonal Experimental Methods
投稿时间:2018-07-28  修订日期:2019-01-20
DOI:10.16490/j.cnki.issn.1001-3660.2019.01.021
中文关键词:  正交优化  不锈钢  纳米孔  阳极氧化  硝酸电解质  田口实验
英文关键词:orthogonal optimization  stainless steel  nanoporous  anodizing  nitric acid electrolyte  Taguchi experiment
基金项目:
作者单位
周雄 上海交通大学,上海 200030 
胡广洪 上海交通大学,上海 200030 
AuthorInstitution
ZHOU Xiong Shanghai Jiao Tong University, Shanghai 200030, China 
HU Guang-hong Shanghai Jiao Tong University, Shanghai 200030, China 
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中文摘要:
      目的 通过正交实验优化不锈钢表面纳米孔制备工艺。方法 通过田口实验方法设计正交试验优化工艺。采用含有氯化钠和硫脲的硝酸溶液阳极氧化制备纳米孔,在含有氯化钠、盐酸和硫酸的水溶液中进行扩孔处理。通过扫描电子显微镜、能谱仪对表面处理后的试样表面形貌和元素进行分析,应用软件统计SEM图片孔隙率,并将孔隙率作为响应指标,利用极差分析和方差分析研究阳极氧化工艺和扩孔时间对表面形貌及孔隙率的影响,并优化工艺参数。结果 SEM照片和5个水平的均值表明,硝酸浓度的提高有利于提高孔隙率,较高的硫脲浓度有利于形成均匀有序的纳米孔结构,氯化钠浓度、氧化时间、氧化电压和扩孔时间对表面形貌和孔隙率影响不明显。元素分析表明,纳米孔的材料仍然是不锈钢,而不是金属氧化物。正交实验优化的工艺参数是:硝酸的体积浓度为90 mL/L,硫脲的质量浓度为3.5 g/L,氯化钠的质量浓度为20 g/L,氧化时间为120 s,氧化电压为5.0 V,扩孔时间为50 s。结论 通过实验验证,优化后的工艺能够制备出表面较平整、孔隙率较高的纳米孔结构。
英文摘要:
      The work aims to optimize the preparation process of nanopore on stainless steel surface by the orthogonal ex-periment. The orthogonal experiment was designed by Taguchi experimental method to optimize the process. Nanopores were prepared by anodization of nitric acid solution containing sodium chloride and thiourea and expanded in aqueous solution con-taining sodium chloride, hydrochloric acid and sulfuric acid. The surface morphology and elements of the treated samples were analyzed by scanning electron microscopy & energy spectrometry. The porosity of the SEM images was counted by software. Porosity was used as a response indicator and the influence level and significance of the anodizing process and the expanding time on the surface morphology and porosity were studied by the range analysis and variable analysis and the process parameters were optimized. The SEM photograph and the mean value of the five levels indicated that the increase in nitric acid concentration was beneficial to increase the porosity and the higher thiourea concentration was favorable for the formation of a uniform ordered nanoporous structure. The sodium chloride concentration, oxidation time, oxidation voltage and expanding time had no significant effect on surface morphology and porosity. Elemental analysis indicated that the material of the nanopores was still stainless steel rather than metal oxide. The process parameters optimized by orthogonal experiment are: nitric acid concentration of 90 mL/L, thiourea concentration of 3.5 g/L, sodium chloride concentration of 20 g/L, oxidation time of 120 s, oxidation voltage of 5.0 V, and expanding time of 50 s. Through experimental verification, a nanoporous structure with flat surface and high porosity can be prepared by optimized process.
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