CN106544652A - 类水滑石‑二氧化硅复合薄膜的制备方法 - Google Patents

类水滑石‑二氧化硅复合薄膜的制备方法 Download PDF

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CN106544652A
CN106544652A CN201611052461.9A CN201611052461A CN106544652A CN 106544652 A CN106544652 A CN 106544652A CN 201611052461 A CN201611052461 A CN 201611052461A CN 106544652 A CN106544652 A CN 106544652A
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李长英
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Shaanxi Yipinda Petrochemical Co Ltd
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Abstract

本发明公开了一种类水滑石‑二氧化硅复合薄膜的制备方法，先对金属铝进行预处理，再制备SiO2溶胶，在预处理的金属铝表面通过浸涂法制得一层致密的SiO2涂层，再以此为基体采用原位生长法制备类水滑石薄膜，得到类水滑石‑二氧化硅复合薄膜。薄膜晶粒均匀致密、对金属铝表现出稳定的防腐蚀效果。

Description

类水滑石-二氧化硅复合薄膜的制备方法
技术领域
本发明属于复合材料的制备领域，具体涉及一种类水滑石-二氧化硅复合薄膜的制备方法。
背景技术
类水滑石（LDH）是一类阴离子型层状功能材料。LDH薄膜对金属基体具有很好的腐蚀保护作用，在金属防腐领域有着广阔的应用前景。LDH类化合物主体层板的元素种类及组成比例、层间阴离子的种类及数量、二维孔道结构均可以根据需要在宽范围内调变，从而获得具有特殊结构和性能的材料。该类化合物在金属基体表面形成一层致密且结合力强的膜层从而能有效阻止腐蚀性介质的渗入，起到保护金属基体的作用。
随着经济的发展，金属材料的使用激增。金属的腐蚀问题仍然是亟待解决的关键问题，尤其对于石油、化工和燃气等高危行业，控制金属管道的腐蚀尤为重要，否则会造成巨大的经济损失和人身安全问题。目前，常用的金属防腐蚀方法包括有机涂层和无机功能薄膜等，但单一的薄膜通常保护作用有限，很难对金属起到长久有效的保护。例如，有机涂层会因微生物的聚集酶化或起泡剥离而失效；而无机功能薄膜常因阻挡性较差而受限。另外，虽然铬酸盐转化膜技术的防腐效果显著，但由于其毒性、致癌性以及污染环境等因素而被限制使用。因此，研发新型防腐蚀效果显著且环境友好的薄膜材料具有重要的研究意义和应用价值。为了提高单一薄膜的耐蚀性，研究者考虑将两种或多种具有防腐蚀性能的材料进行复合。传统的复合薄膜大多是通过向有机涂层中添加具有缓蚀效果的粉体材料，然后再涂敷在金属基体上而制得。这种方法无法从根本上解决有机涂层因霉化、起泡、剥离等原因而失效的问题。
发明内容
本发明提供一种类水滑石-二氧化硅复合薄膜的制备方法，制备得到的薄膜对金属铝表现出稳定的防腐蚀效果。
本发明是通过以下技术方案实现的。
类水滑石-二氧化硅复合薄膜的制备方法，包含以下步骤：
（1）纯铝片的预处理：把纯铝片切成2.5 cm×5 cm大小的长方形，先用丙酮超声清洗10min，然后用去离子水超声清洗5 min，清洗完毕将其放至60 ℃烘箱干燥2h后，将其浸泡于0.1 mol/L的NaOH溶液15min，取出铝片，用去离子水清洗后干燥备用；
（2）SiO2溶胶的制备：将50g正硅酸乙酯与100mL乙醇混合，磁力搅拌使其混合均匀，得到溶液A；分别取乙醇、去离子水、4%的稀硝酸各20Ml、30mL、25mL，混合、搅拌，得到混合溶液B；将混合溶液B滴加入混合溶液A中，其中溶液A 始终保持磁力搅拌状态，滴加完成后继续在室温下搅拌30 min得到混合溶液C；将混合溶液C在60 ℃下回流搅拌90 min后，继续搅拌至冷却至室温；将得到的溶胶密封保存，静置48h后得到SiO2溶胶，备用；
（3）SiO2涂层的制备：将步骤（1）处理好的纯铝片浸入步骤（2）制备好的SiO2溶胶中进行浸涂，将纯铝片先在室温下放置4h，然后将其放入烘箱中进行干燥处理，即可得到SiO2涂层；
（4）类水滑石-二氧化硅复合薄膜的制备：分别称取Mg（NO3）2·6H2O、Al（NO3）3·9H2O和尿素各10.0g，加入1000mL去离子水中搅拌，超声处理，然后将步骤（3）得到的具有SiO2涂层的铝片浸入该混合溶液中，密封并放入120 ℃烘箱中进行反应，反应24h后，取出铝片、用去离子水冲洗5次、真空干燥，撕下形成的薄膜，得到类水滑石-二氧化硅复合薄膜。
优选地，上述步骤（3）中干燥的条件为105℃下干燥6h。
优选地，上述步骤（4）中真空干燥的条件为在65℃下干燥5h。
本发明的优点：
本发明先采用浸涂法将SiO2溶胶涂在铝片上，经热处理后得到SiO2涂层，然后在SiO2涂层修饰的铝基体上原位生长类水滑石薄膜，制得类水滑石-二氧化硅复合薄膜晶粒均匀致密、对金属铝表现出稳定的防腐蚀效果。
具体实施方式
实施例1
类水滑石-二氧化硅复合薄膜的制备方法，包含以下步骤：
（1）纯铝片的预处理：把纯铝片切成2.5 cm×5 cm大小的长方形，先用丙酮超声清洗10min，然后用去离子水超声清洗5 min，清洗完毕将其放至60 ℃烘箱干燥2h后，将其浸泡于0.1 mol/L的NaOH溶液15min，取出铝片，用去离子水清洗后干燥备用；
（2）SiO2溶胶的制备：将50g正硅酸乙酯与100mL乙醇混合，磁力搅拌使其混合均匀，得到溶液A；分别取乙醇、去离子水、4%的稀硝酸各20Ml、30mL、25mL，混合、搅拌，得到混合溶液B；将混合溶液B滴加入混合溶液A中，其中溶液A 始终保持磁力搅拌状态，滴加完成后继续在室温下搅拌30 min得到混合溶液C；将混合溶液C在60 ℃下回流搅拌90 min后，继续搅拌至冷却至室温；将得到的溶胶密封保存，静置48h后得到SiO2溶胶，备用；
（3）SiO2涂层的制备：将步骤（1）处理好的纯铝片浸入步骤（2）制备好的SiO2溶胶中进行浸涂，将纯铝片先在室温下放置4h，然后将其放入烘箱中进行干燥处理，即可得到SiO2涂层；
（4）类水滑石-二氧化硅复合薄膜的制备：分别称取Mg（NO3）2·6H2O、Al（NO3）3·9H2O和尿素各10.0g，加入1000mL去离子水中搅拌，超声处理，然后将步骤（3）得到的具有SiO2涂层的铝片浸入该混合溶液中，密封并放入120 ℃烘箱中进行反应，反应24h后，取出铝片、用去离子水冲洗5次、真空干燥，撕下形成的薄膜，得到类水滑石-二氧化硅复合薄膜。
实施例2
类水滑石-二氧化硅复合薄膜的制备方法，包含以下步骤：
（1）纯铝片的预处理：把纯铝片切成2.5 cm×5 cm大小的长方形，先用丙酮超声清洗10min，然后用去离子水超声清洗5 min，清洗完毕将其放至60 ℃烘箱干燥2h后，将其浸泡于0.1 mol/L的NaOH溶液15min，取出铝片，用去离子水清洗后干燥备用；
（2）SiO2溶胶的制备：将50g正硅酸乙酯与100mL乙醇混合，磁力搅拌使其混合均匀，得到溶液A；分别取乙醇、去离子水、4%的稀硝酸各20Ml、30mL、25mL，混合、搅拌，得到混合溶液B；将混合溶液B滴加入混合溶液A中，其中溶液A 始终保持磁力搅拌状态，滴加完成后继续在室温下搅拌30 min得到混合溶液C；将混合溶液C在60 ℃下回流搅拌90 min后，继续搅拌至冷却至室温；将得到的溶胶密封保存，静置48h后得到SiO2溶胶，备用；
（3）SiO2涂层的制备：将步骤（1）处理好的纯铝片浸入步骤（2）制备好的SiO2溶胶中进行浸涂，将纯铝片先在室温下放置4h，然后将其放入烘箱中进行干燥处理，干燥的条件为105℃下干燥6h，即可得到SiO2涂层；
（4）类水滑石-二氧化硅复合薄膜的制备：分别称取Mg（NO3）2·6H2O、Al（NO3）3·9H2O和尿素各10.0g，加入1000mL去离子水中搅拌，超声处理，然后将步骤（3）得到的具有SiO2涂层的铝片浸入该混合溶液中，密封并放入120 ℃烘箱中进行反应，反应24h后，取出铝片、用去离子水冲洗5次、真空干燥，真空干燥的条件为在65℃下干燥5h，撕下形成的薄膜，得到类水滑石-二氧化硅复合薄膜。

Claims (3)

1.类水滑石-二氧化硅复合薄膜的制备方法，其特征在于：包含以下步骤：
（1）纯铝片的预处理：把纯铝片切成2.5 cm×5 cm大小的长方形，先用丙酮超声清洗10min，然后用去离子水超声清洗5 min，清洗完毕将其放至60 ℃烘箱干燥2h后，将其浸泡于0.1 mol/L的NaOH溶液15min，取出铝片，用去离子水清洗后干燥备用；
（2）SiO2溶胶的制备：将50g正硅酸乙酯与100mL乙醇混合，磁力搅拌使其混合均匀，得到溶液A；分别取乙醇、去离子水、4%的稀硝酸各20Ml、30mL、25mL，混合、搅拌，得到混合溶液B；将混合溶液B滴加入混合溶液A中，其中溶液A 始终保持磁力搅拌状态，滴加完成后继续在室温下搅拌30 min得到混合溶液C；将混合溶液C在60 ℃下回流搅拌90 min后，继续搅拌至冷却至室温；将得到的溶胶密封保存，静置48h后得到SiO2溶胶，备用；
（3）SiO2涂层的制备：将步骤（1）处理好的纯铝片浸入步骤（2）制备好的SiO2溶胶中进行浸涂，将纯铝片先在室温下放置4h，然后将其放入烘箱中进行干燥处理，即可得到SiO2涂层；
（4）类水滑石-二氧化硅复合薄膜的制备：分别称取Mg（NO3）2·6H2O、Al（NO3）3·9H2O和尿素各10.0g，加入1000mL去离子水中搅拌，超声处理，然后将步骤（3）得到的具有SiO2涂层的铝片浸入该混合溶液中，密封并放入120 ℃烘箱中进行反应，反应24h后，取出铝片、用去离子水冲洗5次、真空干燥，撕下形成的薄膜，得到类水滑石-二氧化硅复合薄膜。
2.根据权利要求1所述的类水滑石-二氧化硅复合薄膜的制备方法，其特征在于：步骤（3）中干燥的条件为105℃下干燥6h。
3.根据权利要求1所述的类水滑石-二氧化硅复合薄膜的制备方法，其特征在于：步骤（4）中真空干燥的条件为在65℃下干燥5h。
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109023299A (zh) * 2018-07-31 2018-12-18 山东科技大学 一种镁/镁合金的水滑石-氧化铝复合涂层的制备方法
CN110396307A (zh) * 2019-06-20 2019-11-01 山东盈科新型材料科技有限公司 一种铝银浆颜料制备方法
CN112779534A (zh) * 2020-07-20 2021-05-11 绍兴科霆新材料有限公司 一种用于铝合金铸造模具的防腐涂层及其制备工艺

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109023299A (zh) * 2018-07-31 2018-12-18 山东科技大学 一种镁/镁合金的水滑石-氧化铝复合涂层的制备方法
CN110396307A (zh) * 2019-06-20 2019-11-01 山东盈科新型材料科技有限公司 一种铝银浆颜料制备方法
CN112779534A (zh) * 2020-07-20 2021-05-11 绍兴科霆新材料有限公司 一种用于铝合金铸造模具的防腐涂层及其制备工艺

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