CN112342590A - 一种铝合金表面超疏水着色膜的制备方法 - Google Patents

一种铝合金表面超疏水着色膜的制备方法 Download PDF

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CN112342590A
CN112342590A CN202011125024.1A CN202011125024A CN112342590A CN 112342590 A CN112342590 A CN 112342590A CN 202011125024 A CN202011125024 A CN 202011125024A CN 112342590 A CN112342590 A CN 112342590A
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温玉清
李姣姣
李家平
尚伟
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Guilin University of Technology
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/16Pretreatment, e.g. desmutting
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D5/00Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
    • B05D5/08Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface
    • B05D5/083Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures to obtain an anti-friction or anti-adhesive surface involving the use of fluoropolymers
    • CCHEMISTRY; METALLURGY
    • C23COATING 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
    • C23GCLEANING OR DE-GREASING OF METALLIC MATERIAL BY CHEMICAL METHODS OTHER THAN ELECTROLYSIS
    • C23G1/00Cleaning or pickling metallic material with solutions or molten salts
    • C23G1/24Cleaning or pickling metallic material with solutions or molten salts with neutral solutions
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/06Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
    • C25D11/08Anodisation of aluminium or alloys based thereon characterised by the electrolytes used containing inorganic acids
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/18After-treatment, e.g. pore-sealing
    • C25D11/24Chemical after-treatment
    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D11/00Electrolytic coating by surface reaction, i.e. forming conversion layers
    • C25D11/02Anodisation
    • C25D11/04Anodisation of aluminium or alloys based thereon
    • C25D11/18After-treatment, e.g. pore-sealing
    • C25D11/24Chemical after-treatment
    • C25D11/243Chemical after-treatment using organic dyestuffs

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Abstract

本发明公开了一种铝合金表面超疏水着色膜的制备方法。(1)先把铝合金打磨至光滑,水洗,再在70‑90℃除油液(30‑50g/L磷酸钠,5‑15g/L硅酸钠)中除油1‑4min,后在乙醇水溶液超声清洗10min,烘干;(2)配制体积比为5%‑20%的硫酸溶液,将步骤(1)处理后的样品在电压15‑30V,电流0.1‑0.5A,阳极氧化20‑50min,再烘干;(3)配制铬酸钾质量比为5‑15%的甲溶液、醋酸铅质量比为15‑25%的乙溶液;(4)将阳极氧化后的铝合金分别浸入甲、乙溶液液,2‑5分钟,水洗后沸水浴封孔5‑20min,干燥;(5)移取2‑6ml全氟辛基三乙氧基硅烷(POTS)加入到30‑50ml乙醇溶液中,30‑50℃磁力搅拌1‑3h。(6)将步骤(4)所得样品浸入30‑50℃自组装液中1‑3h,清洗烘干。本发明成本低,制备工艺环保,所制备自组装膜具有超疏水性能及表面装饰功能。

Description

一种铝合金表面超疏水着色膜的制备方法
技术领域
本发明涉及铝合金超疏水表面研究领域,特别涉及一种制备铝合金表面超疏水着色膜的方法。
背景技术
超疏水表面是指水静态接触角大于150°的表面,这一现象是受到荷叶的启发。固体表面的非润湿性在防腐,高端制造等领域有重大意义。铝及铝合金制品以其独特的优点使得它的应用十分的广泛,尤其是近年来在移动设备,飞机制造等方面。人工建立超疏水表面通常是先构建微观纳米结构,然后在材料表面上覆盖上一层低表面能的物质,其主要的方法有模板法,分子自组装法,刻蚀法,溶胶-凝胶法,沉积法等。本文中使用阳极氧化着色,再用沸水封孔后,在表面自组装低表面能物质,不仅具有优异的耐腐蚀性能和鲜艳的颜色,在复杂环境下也可以展现出超疏水膜层的高稳定性,在航空航天、新材料、电力、电子和新能源等领域具有良好的应用前景。
现有技术公开了多种超疏水表面的制备方法,但多数方法制备的超疏水膜层制备过程对环境不够友好,操作复杂,且稳定性不足,着色效果欠理想。为此,开发一种铝合金表面超疏水着色膜的制备方法尤为必要。
发明内容
本发明的目的是提供一种制备铝合金表面超疏水着色膜的方法。
步骤为:
(1)先将6061铝合金基板切割成30mm×40mm×2mm大小的试样,再对样品进行砂粒度为600#,800#,1200#,1500#的耐水SiC磨砂纸的打磨,后经蒸馏水冲洗,再在除油液(30-50g/L磷酸钠,5-15g/L硅酸钠,70-90℃)中除油1-4min,用乙醇和去离子水溶液进行超声波清洗10min烘干。
(2)配制浓硫酸与蒸馏水体积比为5%-20%的溶液,将步骤(1)处理后的样品在控制电压15-30V,电流0.1-0.5A,时间为20-50min,进行阳极氧化,再烘干。阳极氧化后的铝片用(0.5-3%)的氨水中和半分钟,再冲洗干净后即可着色。
(3)以水为溶剂,配制铬酸钾量质量比为5-15%的甲液、醋酸铅质量比为15-25%的乙液。
(4)将步骤(2)处理后的铝合金浸入步骤(3)制备的甲、乙液中着色,分别交替浸入2-5分钟,冲洗后沸水浴封孔5-20min,烘干待用。
(5)移取2-6ml全氟辛基三乙氧基硅烷(POTS)加入到30-50ml乙醇溶液中,30-50℃磁力加热搅拌1-3h。
(6)将步骤(4)所得样品浸入步骤(5)中的30-50℃全氟辛基三乙氧基硅烷(POTS)自组装溶液1-3h,取出后清洗烘干待测试。
本发明方法制备工艺绿色环保,操作方法简单,且所制备铝合金超疏水表面具有鲜艳的颜色。
附图说明
图1为本发明实施例中铝合金表面超疏水着色膜的不同倍率SEM图和接触角图。(其中a为膜层500倍率图,b为膜层5000倍率图,c为膜层20000倍率图,d为水滴在膜层的接触角图)
图2为本发明实施例中铝合金表面超疏水着色膜的元素分布EDS图。
具体实施方式
实施例:
(1)先将6061铝合金基板切割成30mm×40mm×2mm大小的试样,再对样品进行砂粒度为600#,800#,1200#,1500#的耐水SiC磨砂纸的打磨,后经蒸馏水冲洗,再在除油液(30-50g/L磷酸钠,5-15g/L硅酸钠,70-90℃)中除油1-4min,用乙醇和去离子水溶液进行超声波清洗10min烘干。
(2)配制浓硫酸与蒸馏水体积比为5%-20%的溶液,将步骤(1)处理后的样品在控制电压15-30V,电流0.1-0.5A,时间为20-50min,进行阳极氧化,再烘干。阳极氧化后的铝片用(0.5-3%)的氨水中和半分钟,再冲洗干净后即可着色。
(3)以水为溶剂,配制铬酸钾量质量比为5-15%的甲液、醋酸铅质量比为15-25%的乙液。
(4)将步骤(2)处理后的铝合金浸入步骤(3)制备的甲、乙液中着色,分别交替浸入2-5分钟,冲洗后沸水浴封孔5-20min,烘干待用。
(5)移取2-6ml全氟辛基三乙氧基硅烷(POTS)加入到30-50ml乙醇溶液中,30-50℃磁力加热搅拌1-3h。
(6)将步骤(4)所得样品浸入步骤(5)中的30-50℃全氟辛基三乙氧基硅烷(POTS)自组装溶液1-3h,取出后清洗烘干待测试。
从图1中可以看出复合膜层致密均匀,接触角达到超疏水标准。通过图2显示了膜层中各元素分布情况。

Claims (1)

1.一种在铝合金表面超疏水着色膜的制备方法,其特征在于具体步骤为:
(1)先将6061铝合金基板切割成30mm×40mm×2mm大小的试样,再对样品进行砂粒度为600#,800#,1200#,1500#的耐水SiC磨砂纸的打磨,后经蒸馏水冲洗,再在70-90℃的除油液中除油1-4min,用乙醇和去离子水溶液进行超声波清洗10min烘干备用;所述除油液的配方为:40g/L磷酸钠,10g/L硅酸钠;
(2)配制浓硫酸与蒸馏水体积比为5%-20%的溶液,将步骤(1)处理后的样品在控制电压15-30V,电流0.1-0.5A,时间为20-50min,进行阳极氧化,再烘干;阳极氧化后的铝片用0.5-3%的氨水中和半分钟,再冲洗干净后即可着色;
(3)以水为溶剂,配制铬酸钾量质量比为5-15%的甲液、醋酸铅质量比为15-25%的乙液;
(4)将步骤(2)处理后的铝合金浸入步骤(3)制备的甲、乙液中着色,分别交替浸入2-5分钟,冲洗后沸水浴封孔5-20min,烘干待用;
(5)移取2-6ml全氟辛基三乙氧基硅烷加入到30-50ml乙醇溶液中,30-50℃磁力加热搅拌1-3h;
(6)将步骤(4)所得样品浸入步骤(5)中的30-50℃全氟辛基三乙氧基硅烷自组装溶液1-3h,取出后清洗烘干待测试。
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Application publication date: 20210209