CN108468044A - 一种在铝合金表面制备掺杂石墨烯自组装复合膜的方法 - Google Patents
一种在铝合金表面制备掺杂石墨烯自组装复合膜的方法 Download PDFInfo
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- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 8
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 8
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- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 9
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- 235000019441 ethanol Nutrition 0.000 claims description 6
- 229910000989 Alclad Inorganic materials 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 238000004458 analytical method Methods 0.000 claims description 3
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- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
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- 238000003756 stirring Methods 0.000 claims description 2
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
- C23C22/05—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions
- C23C22/06—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6
- C23C22/48—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals using aqueous solutions using aqueous acidic solutions with pH less than 6 not containing phosphates, hexavalent chromium compounds, fluorides or complex fluorides, molybdates, tungstates, vanadates or oxalates
- C23C22/56—Treatment of aluminium or alloys based thereon
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C22/00—Chemical surface treatment of metallic material by reaction of the surface with a reactive liquid, leaving reaction products of surface material in the coating, e.g. conversion coatings, passivation of metals
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Abstract
本发明公开了一种在铝合金表面制备掺杂石墨烯自组装复合膜的方法。对铝合金依次进行洗涤、打磨、超声波水洗等预处理；随后再采用氢氟酸溶液侵蚀，接着用盐酸溶液侵蚀，最后用去离子水清洗，干燥备用；配置自组装溶液，加入还原石墨烯，超声波分散，制得混合溶液，然后把前处理后的铝合金浸入混合溶液中浸泡后取出，放入去离子水中超声波清洗以去除铝合金表面未反应的小分子和溶剂，最后在真空干燥箱中固化，即实现在铝合金表面制备掺杂石墨烯自组装复合膜。本发明方法操作简单，在铝合金表面制备出的具有超疏水‑耐腐蚀功能的掺杂石墨烯自组装膜，与基体结合牢固，表面平整均匀致密，该膜层具有较高的电化学阻抗，较低的腐蚀电流密度。
Description
技术领域
本发明属于金属材料表面电化学腐蚀领域，特别涉及一种在铝合金表面制备掺杂石墨烯自组装复合膜的方法。
背景技术
铝及铝合金由于具有强度高、密度小、导电导热性强、力学性能优异、可加工性好等优点而广泛应用于化学工业、航空航天工业、汽车制造业、食品工业、电子、仪器仪表业以及海洋船舶工业等领域。但在实际应用过程中，铝合金就呈现出表面硬度较低、耐磨性及耐蚀性差等诸多问题，这在很大程度上限制了铝合金的应用范围。铝合金成分和热处理对铝合金性能的提高固然很大，但在许多场合还要求铝合金表面具有耐磨、耐腐蚀等特殊性能，而且大部分铝合金材料的失效大都是从表面开始的，因而提高材料的表面性能显得尤为重要。目前通过自组装技术和刻蚀技术相结合在基体表面形成由化学键连接的具有一定取向、紧密排列的二维有序的分子膜。该方法操作简单方便，无需复杂贵重的仪器，而且得到的自组装膜具有超疏水性、更强的稳定性和高耐蚀性。
发明内容
本发明的目的是提供一种在铝合金表面制备掺杂石墨烯自组装复合膜的方法。
具体步骤为：
（1）铝合金先用浓度为30~60 g/L的NaOH溶液除去表面包铝层；随后依次用600#、1000#和1200#砂纸打磨至光滑，用分析纯乙醇超声波清洗5~15 min，再在去离子水中超声波震动清洗5~30 min；随后再采用浓度为2~6 mol/L的氢氟酸溶液侵蚀5~30 min，在浓度为2~10mol/L的盐酸溶液中侵蚀10~30 min，最后用去离子水清洗2~3次，80~120 ℃下烘干备用，得到处理过的铝合金。
（2）配制总体积为23~100 mL的溶液：其中包含20~65 mL无水乙醇、1~5 mL 双（γ-三乙氧基硅基丙基）四硫化物、1~10 mL聚乙二醇200和1~20 mL浓度为100g/L的硫化钾水溶液，用醋酸将溶液的pH值调至2~6，所得溶液在20~50 ℃磁力搅拌器中搅拌1~5 h，然后加入1~80 mg的还原石墨烯（rGO），超声波分散处理20~120 min，制得混合溶液。
（3）将步骤（1）得到的处理过的铝合金浸入步骤（2）制得的混合溶液中浸泡30~120min后取出，放入去离子水中超声波清洗以去除铝合金表面未反应的小分子和溶剂，最后在80~120 ℃的真空干燥箱中固化1~3 h，即实现在铝合金表面制备掺杂石墨烯自组装复合膜。
本发明方法成本低，制备工艺简单，所制备的自组装膜具有超疏水性、高阻抗、低腐蚀电流密度，在铝合金基体上结合力好，能很好的提高铝合金表面防腐蚀能力，且对环境和设备不造成污染。
附图说明
图1为本发明实施例中在铝合金表面制备的掺杂石墨烯自组装复合膜的极化曲线图。
图2为本发明实施例中在铝合金表面制备的掺杂石墨烯自组装复合膜的SEM照片及接触角测试图。
具体实施方式
实施例：
铝合金的前处理：试验用6061铝合金试片先用浓度为45 g/L的NaOH溶液除去表面包铝层；随后依次用600#、1000#和1200#砂纸打磨至光滑，用分析纯乙醇超声波清洗10 min，再在去离子水中超声波震动清洗10 min；随后再采用浓度为3.75 mol/L的氢氟酸溶液侵蚀10min，在浓度为4 mol/L的盐酸溶液中侵蚀12 min，最后用去离子水清洗3次，100 ℃下烘干备用，得到处理过的铝合金。
配制总体积为50mL的溶液：包含37.5 mL无水乙醇，2.5 mL双（γ-三乙氧基硅基丙基）四硫化物，5 mL聚乙二醇200和5 mL（100g/L)硫化钾水溶液，用醋酸调pH值至4.0，在35℃磁力搅拌器中搅拌1 h，然后加入40 mg还原石墨烯（rGO），超声波分散处理60min，制得混合溶液。
将预处理过的铝合金置于制得的混合溶液中反应1 h后取出，放入去离子水中超声波清洗以去除未反应的小分子和溶剂，最后在100 ℃下固化1 h后，即实现在铝合金表面制备掺杂石墨烯自组装复合膜。
极化曲线是腐蚀科学中常用的电化学手段之一，是研究膜层、涂层、转化膜等覆盖金属电极腐蚀速率的有效工具。对本实施例制得的掺杂石墨烯自组装复合膜进行电化学耐蚀性能测试，采用三电极体系，3.5%的NaCl为腐蚀介质，对其进行塔菲尔曲线扫描得到结果如图1所示。
从图1得到，铝合金表面制备的掺杂石墨烯自组装复合膜的腐蚀电流密度为1.676×10-9 A·cm-2，要比空白铝合金表面的3.783×10-5 A/cm-2减小4个数量级，表现出明显的耐蚀性能。膜层的形貌及超疏水性能如图2所示。
Claims (1)
1.一种在铝合金表面制备掺杂石墨烯自组装复合膜的方法，其特征在于具体步骤为：
（1）铝合金先用浓度为30~60 g/L的NaOH溶液除去表面包铝层；随后依次用600#、1000#和1200#砂纸打磨至光滑，用分析纯乙醇超声波清洗5~15 min，再在去离子水中超声波震动清洗5~30 min；随后再采用浓度为2~6 mol/L的氢氟酸溶液侵蚀5~30 min，在浓度为2~10mol/L的盐酸溶液中侵蚀10~30 min，最后用去离子水清洗2~3次，80~120 ℃下烘干备用，得到处理过的铝合金；
（2）配制总体积为23~100 mL的溶液：其中包含20~65 mL无水乙醇、1~5 mL 双（γ-三乙氧基硅基丙基）四硫化物、1~10 mL聚乙二醇200和1~20 mL浓度为100g/L的硫化钾水溶液，用醋酸将溶液的pH值调至2~6，所得溶液在20~50 ℃磁力搅拌器中搅拌1~5 h，然后加入1~80 mg的还原石墨烯，超声波分散处理20~120 min，制得混合溶液；
（3）将步骤（1）得到的处理过的铝合金浸入步骤（2）制得的混合溶液中浸泡30~120 min后取出，放入去离子水中超声波清洗以去除铝合金表面未反应的小分子和溶剂，最后在80~120 ℃的真空干燥箱中固化1~3 h，即实现在铝合金表面制备掺杂石墨烯自组装复合膜。
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| CN103985552A (zh) * | 2014-05-21 | 2014-08-13 | 南开大学 | 过渡金属硫化物与石墨烯复合材料对电极及其制备和应用 |
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| CN105543823A (zh) * | 2016-03-16 | 2016-05-04 | 燕山大学 | 一种在铝合金表面制备钛/硒多彩复合转化膜的方法 |
| CN105925975A (zh) * | 2016-05-12 | 2016-09-07 | 上海渊泉集币收藏品有限公司 | 一种在银制品表面制备黄色系化学转化膜的方法 |
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| CN110644036A (zh) * | 2019-08-14 | 2020-01-03 | 桂林理工大学 | 一步电沉积法制备超疏水和自清洁复合功能膜层的方法 |
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