CN113604851B - 一种镁合金表面无需低表面能物质修饰的超疏水涂层及其制备方法 - Google Patents
一种镁合金表面无需低表面能物质修饰的超疏水涂层及其制备方法 Download PDFInfo
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- 229910000861 Mg alloy Inorganic materials 0.000 title claims abstract description 82
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- 238000006243 chemical reaction Methods 0.000 claims abstract description 23
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- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 10
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- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 10
- 239000011258 core-shell material Substances 0.000 claims abstract description 4
- 238000005498 polishing Methods 0.000 claims abstract description 4
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 claims abstract description 4
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical compound [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims abstract description 4
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- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 21
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 21
- 239000011734 sodium Substances 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- PUZPDOWCWNUUKD-UHFFFAOYSA-M sodium fluoride Chemical compound [F-].[Na+] PUZPDOWCWNUUKD-UHFFFAOYSA-M 0.000 claims description 12
- XIOUDVJTOYVRTB-UHFFFAOYSA-N 1-(1-adamantyl)-3-aminothiourea Chemical compound C1C(C2)CC3CC2CC1(NC(=S)NN)C3 XIOUDVJTOYVRTB-UHFFFAOYSA-N 0.000 claims description 9
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 6
- 239000011775 sodium fluoride Substances 0.000 claims description 6
- 235000013024 sodium fluoride Nutrition 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 239000002073 nanorod Substances 0.000 claims description 4
- 244000137852 Petrea volubilis Species 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 229910021538 borax Inorganic materials 0.000 claims description 3
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 3
- 239000001488 sodium phosphate Substances 0.000 claims description 3
- 229910000162 sodium phosphate Inorganic materials 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 239000004328 sodium tetraborate Substances 0.000 claims description 3
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 3
- XMVONEAAOPAGAO-UHFFFAOYSA-N sodium tungstate Chemical compound [Na+].[Na+].[O-][W]([O-])(=O)=O XMVONEAAOPAGAO-UHFFFAOYSA-N 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 claims description 3
- 239000012530 fluid Substances 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 claims 1
- 230000007797 corrosion Effects 0.000 abstract description 15
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- 239000011159 matrix material Substances 0.000 abstract description 4
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- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
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- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical compound Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 150000004673 fluoride salts Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000007769 metal material Substances 0.000 description 1
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- 230000009466 transformation Effects 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/026—Anodisation with spark discharge
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/14—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials to metal, e.g. car bodies
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- C09D187/00—Coating compositions based on unspecified macromolecular compounds, obtained otherwise than by polymerisation reactions only involving unsaturated carbon-to-carbon bonds
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D11/00—Electrolytic coating by surface reaction, i.e. forming conversion layers
- C25D11/02—Anodisation
- C25D11/30—Anodisation of magnesium or alloys based thereon
Abstract
本发明公开了一种在镁合金表面无需低表面能物质修饰的超疏水涂层及其制备方法。该镁合金表面ZnO@ZIF‑8超疏水涂层具体包括依次附着于镁合金表面的微弧氧化层、ZnO层和ZIF‑8层。对镁合金基体依次进行打磨抛光、除油、超声清洗,而后进行微弧氧化处理,在表面形成微弧氧化膜之后;将其多次置于装有不同溶液的聚四氟乙烯反应釜中高温高压反应,干燥后获得镁合金表面ZnO@ZIF‑8涂层。本发明制备方法所制备的ZnO@ZIF‑8涂层具有核壳结构,与镁合金基材有着良好的结合力,并能够均匀分布于镁合金表面,无需低表面能物质修饰,不仅具备超疏水性,也具有良好的耐腐蚀性能。
Description
技术领域
本发明属于金属材料耐腐蚀的超疏水涂层,具体而言是一种在镁合金表面制备无需低表面能物质修饰的超疏水涂层及其制备方法。
背景技术
镁及其合金被认为是21世纪绿色工程材料。由于具有密度低、良好的机械性能、优异的铸造性、生物降解性好以及储氢容量大等物理化学性能,在汽车工业、生物医学以及3C产品(计算机、通信和消费电子)等领域有着广阔的应用前景。而且得益于国内汽车工业和3C等行业的转型升级以及国内制造业的高速发展,镁合金行业令市场看好。然而,镁合金强度相对较低、塑性差和耐蚀性差等缺陷,阻碍了镁合金的实际应用,而在功能材料中镁合金快速降解等问题亟待解决,以拓宽镁合金的应用范围。针对这一现象,科研工作者们发展了许多处理技术,而超疏水涂层因具有众多的优异特性备受欢迎。目前,结合强度弱是超疏水涂层在实际应用中的一个致命缺点。因此,引入微弧氧化层作为过渡层,利用表面的微孔结构有利于提高超疏水涂层与基体的附着力。传统上,超疏水涂层的制备需要用低表面能物质(氟化物或硅化物)修饰,这些有毒材料会对环境造成负面影响。所以开发一种无需低表面能物质修饰的超疏水涂层是材料科学的一个长期探索。本申请旨在镁合金表面制备强附着力并且无需低表面能物质修饰的超疏水涂层,有效抑制镁合金的快速降解,延长其使用寿命。
发明内容
本发明的目的是提供一种在镁合金表面无需低表面能物质修饰的超疏水涂层及其制备方法。
制备该超疏水涂层的具体步骤为:
(1)镁合金预处理
为了将镁合金表面的污渍及其氧化物去除,选用了#180、#600、#1000、#1500的金相砂纸进行打磨抛光,之后,用大量的去离子水冲洗残留物;在60~80℃的条件下进行60s的除油处理;最后分别使用乙醇和水超声处理10~15min,干燥获得处理后的镁合金;所用除油液组成为:15~20g/L NaOH、30~40g/LNa2CO3、15~20g/L Na3PO4。
(2)微弧氧化处理
在室温下,将步骤(1)获得的处理后的镁合金作为阳极,采用不锈钢片为阴极,置于微弧氧化溶液中采用脉冲电压进行微弧氧化处理,获得微弧氧化处理的镁合金载体;设定电参数为:频率50~200Hz,占空比30~50%,终止电压180~220V,微弧氧化时间30~40min;所用微弧氧化溶液组成为:10~15g/LNaOH、5~10g/L Na2SiO3、5~10g/L NaF、4~6g/L Na2B4O7、1~5g/L Na2WO4、3~5mL/L C3H8O3和3~5mL/L C6H15NO3。
(3)超疏水涂层制备
①首先,按照六水合硝酸锌:水:氢氧化钠的摩尔比为1:220:6配制溶液,随后,将溶液转移到悬挂有经过步骤(2)微弧氧化处理的镁合金的聚四氟乙烯反应釜中,在120℃下恒温反应2h。反应结束后在空气中自然冷却至室温,将镁合金取出用去离子水清洗5~10次,50℃干燥。
②然后,将①获得的镁合金放入含有ZnO生长液的聚四氟乙烯反应釜中,在150℃下恒温反应4h。待反应釜自然冷却至室温后,取出覆盖有ZnO纳米棒的镁合金,用去离子水清洗5~10次,50℃干燥。所用ZnO生长液的组成为:0.25mol/L六水合硝酸锌、1.5mol/L氢氧化钠。
③最后,将1.23g的2-甲基咪唑溶解于30mL的甲醇中,倒入悬挂有②获得的镁合金的聚四氟乙烯反应釜中,150℃下恒温反应3h,反应结束后在空气中自然冷却至室温,取出镁合金用去离子水清洗5~10次,50℃干燥,从而获得ZnO@ZIF-8超疏水涂层。
所述氢氧化钠、碳酸钠、磷酸钠、硅酸钠、氟化钠、四硼酸钠、钨酸钠、三乙醇胺、丙三醇、六水合硝酸锌、2-甲基咪唑、甲醇和乙醇均为化学纯及以上纯度。
本发明制备方法所制备的ZnO@ZIF-8涂层具有核壳结构,与镁合金基材有着良好的结合力,并能够均匀分布于镁合金表面,无需低表面能物质修饰,具备超疏水性。通过电化学性能测试发现该涂层也具有良好的耐腐蚀性能。
附图说明
图1为实施例1制得的MAO涂层和ZnO@ZIF-8超疏水涂层的SEM图像。
图2为实施例1制得的ZnO@ZIF-8超疏水涂层的物相表征XRD图谱。
图3为实施例1制得的MAO涂层和ZnO@ZIF-8超疏水涂层的接触角测试图。
图4为实施例1制得的MAO涂层和ZnO@ZIF-8超疏水涂层的动电位极化曲线。
具体实施方式
实施例:
(1)镁合金预处理
为了将镁合金表面的污渍及其氧化物去除,选用了#180、#600、#1000、#1500的金相砂纸进行打磨抛光,之后,用大量的去离子水冲洗残留物;在70℃的条件下进行60s的除油处理(20g/L NaOH、30g/L Na2CO3、20g/L Na3PO4);最后分别使用乙醇和水超声处理10min,干燥待用;
(2)微弧氧化处理
微弧氧化是在硅酸盐体系中采用脉冲电压进行,在室温下,将步骤(1)处理后的镁合金作为阳极,采用不锈钢片为阴极,置于微弧氧化溶液中采用脉冲电压进行微弧氧化处理,设定电参数为:频率50Hz,占空比30%,终止电压220V,微弧氧化时间30min;过程所用的微弧氧化溶液组成:11g/L NaOH,5g/L Na2SiO3,8g/L NaF,4g/L Na2B4O7,1g/L Na2WO4,5mL/L C3H8O3,4mL/LC6H15NO3。
(3)超疏水涂层制备
首先,按照六水合硝酸锌:水:氢氧化钠的摩尔比为1:220:6配制溶液,随后,将溶液转移到悬挂有经过步骤(2)微弧氧化处理的镁合金的聚四氟乙烯反应釜中,在120℃下恒温反应2h。反应结束后在空气中自然冷却至室温,将镁合金取出用去离子水清洗6次,50℃干燥。然后,将上述镁合金和ZnO生长液置于聚四氟乙烯反应釜中,在150℃下恒温反应4h。待反应釜自然冷却至室温后,取出覆盖有ZnO纳米棒的镁合金,用去离子水清洗6次,50℃干燥。最后,将1.23g的2-甲基咪唑溶解于30mL的甲醇中,倒入悬挂有覆盖ZnO纳米棒的镁合金的聚四氟乙烯反应釜中,150℃下恒温反应3h,反应结束后在空气中自然冷却至室温,取出镁合金用去离子水清洗5次,50℃干燥,从而获得ZnO@ZIF-8超疏水涂层。所用ZnO生长液的组成为:0.25mol/L六水合硝酸锌、1.5mol/L氢氧化钠。
所述氢氧化钠、碳酸钠、磷酸钠、硅酸钠、氟化钠、四硼酸钠、钨酸钠、三乙醇胺、丙三醇、六水合硝酸锌、2-甲基咪唑、甲醇和乙醇均为化学纯及以上纯度。
本实施例制得的镁合金表面ZnO@ZIF-8涂层通过SEM和XRD表征表明,该涂层具有核壳结构,与镁合金基材有着良好的结合力,并能够均匀分布于镁合金表面。利用水滴静态接触角测试仪测试其水接触角,其水接触角为155.97°,在无需低表面能物质修饰的情况下具备了超疏水性。对本实施例所制备的ZnO@ZIF-8涂层进行耐腐蚀性能表征,利用CHI760电化学工作站,在三电极体系(甘汞电极为参比电极,铂电极为辅助电极,镁合金表面涂层为工作电极)下进行测试,3.5wt.%的氯化钠溶液为电解液。选用动电位极化曲线研究镁合金表面涂层的耐腐蚀性能,待开路电位稳定后,采用5mV/s的扫描速率进行测试。本实施例所获得的镁合金表面MAO/ZIF-8涂层的腐蚀电位为-1.479V,腐蚀电流密度为5.611×10-9A·cm-2,微弧氧化膜的腐蚀电位为-1.559V,腐蚀电流密度为1.131×10-6A·cm-2,AZ91镁合金基体的腐蚀电位为-1.605V,腐蚀电流密度为4.275×10-5A·cm-2,MAO/ZIF-8超疏水涂层的腐蚀电位发生了正移,腐蚀电流密度分别比微弧氧化膜的和镁合金基体的减小了三个和四个数量级,显著提高了镁合金的耐蚀性能。
Claims (2)
1.一种镁合金表面无需低表面能物质修饰的超疏水涂层的制备方法,其特征在于,该镁合金表面ZnO@ZIF-8超疏水涂层由依次附着于镁合金表面的微弧氧化层、ZnO层和ZIF-8层组成,ZnO@ZIF-8超疏水涂层具有核壳结构;具体步骤为:
(1)镁合金预处理
为了将镁合金表面的污渍及其氧化物去除,选用了#180、#600、#1000、#1500的金相砂纸进行打磨抛光,之后,用大量的去离子水冲洗残留物;在60~80 ℃的条件下进行60 s的除油处理;最后分别使用乙醇和水超声处理10~15 min,干燥获得处理后的镁合金;所用除油液组成为:15~20 g/L NaOH、30~40 g/L Na2CO3、15~20 g/L Na3PO4;
(2)微弧氧化处理
在室温下,将步骤(1)获得的处理后的镁合金作为阳极,采用不锈钢片为阴极,置于微弧氧化溶液中采用脉冲电压进行微弧氧化处理,获得微弧氧化处理的镁合金载体;设定电参数为:频率50~200 Hz,占空比30~50 %,终止电压180~220 V,微弧氧化时间30~40 min;所用微弧氧化溶液组成为:10~15 g/L NaOH、5~10 g/L Na2SiO3、5~10 g/L NaF、4~6 g/LNa2B4O7、1~5 g/L Na2WO4、3~5 mL/L C3H8O3和3~5 mL/L C6H15NO3;
(3)超疏水涂层制备
①首先,按照六水合硝酸锌:水:氢氧化钠的摩尔比为1: 220: 6配制溶液,随后,将溶液转移到悬挂有经过步骤(2)微弧氧化处理的镁合金的聚四氟乙烯反应釜中,在120 ℃下恒温反应2 h;反应结束后,在空气中自然冷却至室温,将镁合金取出用去离子水清洗5~10次,50 ℃干燥;
②然后,将①获得的镁合金放入含有ZnO生长液的聚四氟乙烯反应釜中,在150 ℃下恒温反应4 h;待反应釜自然冷却至室温后,取出覆盖有ZnO纳米棒的镁合金,用去离子水清洗5~10次,50 ℃干燥;所用ZnO生长液的组成为:0.25 mol/L 六水合硝酸锌、1.5 mol/L 氢氧化钠;
③最后,将1.23 g 的2-甲基咪唑溶解于30 mL的甲醇中,倒入悬挂有②获得的镁合金的聚四氟乙烯反应釜中,150 ℃下恒温反应3 h,反应结束后在空气中自然冷却至室温,取出镁合金用去离子水清洗5~10次,50 ℃干燥,从而获得ZnO@ZIF-8超疏水涂层。
2.根据权利要求1所述的镁合金表面无需低表面能物质修饰的超疏水涂层的制备方法,其特征在于,所述氢氧化钠、碳酸钠、磷酸钠、硅酸钠、氟化钠、四硼酸钠、钨酸钠、三乙醇胺、丙三醇、六水合硝酸锌、2-甲基咪唑、甲醇和乙醇均为化学纯及以上纯度。
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