WO2008151495A1 - Film mince d'hydroxydes bicouches, superhydrophobes, et son procédé de fabrication - Google Patents

Film mince d'hydroxydes bicouches, superhydrophobes, et son procédé de fabrication Download PDF

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Publication number
WO2008151495A1
WO2008151495A1 PCT/CN2007/070124 CN2007070124W WO2008151495A1 WO 2008151495 A1 WO2008151495 A1 WO 2008151495A1 CN 2007070124 W CN2007070124 W CN 2007070124W WO 2008151495 A1 WO2008151495 A1 WO 2008151495A1
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WO
WIPO (PCT)
Prior art keywords
layered
bishydroxy
metal oxide
superhydrophobic
oxide film
Prior art date
Application number
PCT/CN2007/070124
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English (en)
Chinese (zh)
Inventor
Fazhi Zhang
Hongyun Chen
Xue Duan
Shanshan Fu
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Beijing University Of Chemical Technology
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Filing date
Publication date
Application filed by Beijing University Of Chemical Technology filed Critical Beijing University Of Chemical Technology
Priority to PCT/CN2007/070124 priority Critical patent/WO2008151495A1/fr
Publication of WO2008151495A1 publication Critical patent/WO2008151495A1/fr

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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
    • C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
    • C09K3/00—Materials not provided for elsewhere
    • C09K3/18—Materials not provided for elsewhere for application to surfaces to minimize adherence of ice, mist or water thereto; Thawing or antifreeze materials for application to surfaces
    • 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
    • C23C28/00—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D
    • C23C28/04—Coating for obtaining at least two superposed coatings either by methods not provided for in a single one of groups C23C2/00 - C23C26/00 or by combinations of methods provided for in subclasses C23C and C25C or C25D only coatings of inorganic non-metallic material
    • 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
    • C25D11/04—Anodisation of aluminium or alloys based thereon

Definitions

  • the invention belongs to the technical field of thin film materials, and particularly relates to a superhydrophobic layered bishydroxy composite metal oxide film grown on an anodized aluminum substrate and a preparation method thereof.
  • Layered bishydroxy composite metal oxides are a class of anionic layered functional materials consisting of parallel and positively charged layers composed of balanced anions and water molecules. . Its chemical composition is: ⁇ m3 ⁇ 40, where M 2+ and M 3+ are respectively divalent and trivalent metal ions on the laminate, and A n _ represents an interlayer anion. Due to its unique crystal structure and physicochemical properties, these materials have shown great application prospects in many fields such as ion exchange, adsorption, catalysis, polymer modification, optical materials, magnetic materials, and electrical materials.
  • superhydrophobic surfaces have attracted widespread attention.
  • superhydrophobic surface is generally meant a surface having a contact angle with water droplets greater than 150°. It is generally believed that the composite structure in which micro and nano are combined is the root cause of superhydrophobic surface, and thus the superhydrophobic surface has a large contact angle.
  • the superhydrophobic surface is also water resistant, anti-pollution, anti-oxidant, biocompatible, lubricious and resistant to current conduction. In nature, superhydrophobicity is also widespread. For example, the lotus leaf has a superhydrophobic film on its surface, so that the water droplets are easy to roll on its surface, and the water droplets can roll off while still on the surface of the lotus leaf.
  • Superhydrophobic materials have extremely broad application prospects in industrial and agricultural production and people's daily life. For example: textiles, coatings, gene transfer, microfluidics, and lossless liquid transport.
  • superhydrophobic surfaces can be prepared by two methods.
  • One is in a hydrophobic material
  • the antennae are larger than 90°.
  • the other is to modify the rough surface with low surface energy materials such as fluorosilicone and long chain fatty acids.
  • Most of the literature reports currently use the former method to prepare superhydrophobic surfaces. For example: in the literature 1433 and Angew. Chem. Int. Ed, 2 03 (43): 4338, Jiang Lei et al. constructed a rough structure on the surface of a hydrophobic polymer material film to make the surface of the film exhibit excellent superhydrophobic properties.
  • An object of the present invention is to provide a superhydrophobic layered bishydroxy composite metal oxide film; another object is to provide a method for preparing the superhydrophobic layered bishydroxy composite metal oxide film.
  • the superhydrophobic layered bishydroxy composite metal oxide film provided by the invention is an LDHs film grown on an anodized aluminum substrate, and the chemical formula of the LDHs film is:
  • M 2+ represents a divalent metal ion, and may be, for example, Mg 2+ , Co 2+ , M 2+ , Ca 2+ , Cu 2+ , Any one of Fe 2+ and Mn 2+ , wherein Ni 2+ , Co 2+ or Mg 2+ is preferred; wherein Al 3+ is formed in situ from A1 on the aluminum substrate; 0.2 x 0.4, 0 ⁇ 2;
  • the LDHs film has a nano/micro composite structure and a surface roughness of 250 nm to 860 nm; the contact angle of the superhydrophobic LDHs film with water droplets is 150 to 170°.
  • the LDHs film has a nano/micro composite structure and is formed on the surface of the substrate.
  • the hydrotalcite hexagonal flaky crystal grains are vertically grown on the surface of the substrate, and the thickness of the hexagonal flaky crystal grains is in the nanometer scale range (60 to 80 nm), and the hexagonal flaky crystal grains are respectively The length of the sides is in the micron range (0.5 to 1.5 ⁇ ).
  • the aluminum substrate with a purity greater than 80% and a thickness of 0.01 ⁇ 1mm is first ultrasonically cleaned with ethanol for 5 ⁇ 10min, then ultrasonically cleaned with water for 5 ⁇ 10min to remove surface oil, then used as an anode on the anodizing device, with lead plate or The stainless steel plate is used as the cathode, the electrolyte is 0.5 ⁇ 3.0 mol/L sulfuric acid solution, the oxidation current is 1 ⁇ 5A, the aluminum piece is anodized for 30 ⁇ 100min, and then taken out, and the electrolyte is washed away with deionized water to obtain anodized aluminum base.
  • the surface anodized aluminum substrate is suspended in the reaction solution, and reacted at 25 to 180 ° C for 0.5 to 96 hours.
  • the aluminum substrate is taken out, rinsed with an ethanol solution, and dried at room temperature to obtain a layered layer.
  • M 2+ is any one of Mg 2+ , Co 2+ , Ni 2+ , Ca 2+ , Cu 2+ , Fe 2+ and Mn 2+ , preferably Ni 2+ , Co 2+ or Mg 2+ ;
  • Y is any one of C0 3 2 —, N0 3 _, S0 4 2 _, Cl_, F and Br—, preferably C0 3 2 —, N0 3 — or Cl—
  • the preferred pH range of the reaction solution is 5.5 to 8.5.
  • the concentration of the ammonia water in the step B may be 0.1 to 5% by weight, preferably 0.5 to 3 Torr.
  • the preferred reaction condition is to carry out the reaction at 50 to 150 ° C for 3 to 60 hours, and the preferred reaction conditions are 50 ⁇ : Reaction at 130 ° C for 5 to 20 hours.
  • Step D The preferred reaction conditions are a reaction at 25 to 80 ° C for 0.5 to 10 hours, and a more preferred reaction condition is a reaction at 30 to 50 ° C for 2 to 5 hours.
  • the invention has the beneficial effects that: the invention adopts an in-situ synthesis technique to prepare a layered bishydroxy composite metal oxide film on an aluminum sheet having anodized surface, and the layered bishydroxy composite metal oxide film obtained has the obtained layer.
  • Nano/micro composite structure with a surface roughness of 250 nm to 860 nm.
  • the surface of the film after surface hydrophobic treatment in a long-chain fatty acid surfactant solution still maintains this nano/micro composite structure, at nano/ A gas film is formed between the surface layer of the micro-composite structure and the water droplets, and the contact angle with the water droplets is as high as 170°, and the sewage splashes onto the surface to automatically roll off without leaving any traces, thereby achieving the purpose of self-cleaning.
  • the surfactant solution used is not fluorine-containing, and is not available to the human body. Any toxic effect and no pollution to the environment.
  • the method is simple, the raw materials are easy to obtain, the cost is low, and the repeatability is good.
  • the obtained film has excellent superhydrophobicity and self-cleaning performance, and the superhydrophobic layered bishydroxy composite metal oxide film is expected to be used as a metal in engineering materials. The surface is protected against dust and fog.
  • FIG. 1 is a SEM photograph of the surface of the surface anodized aluminum sheet obtained in Example A, Step A;
  • FIG. 2 is a surface SEM photograph of the LDHs film sample obtained in Example 1, Step C;
  • FIG. 3 is a first embodiment.
  • Fig. 4 is an optical photograph of the surface of the superhydrophobic LDHs film sample prepared by the water droplets in Example 1;
  • Fig. 5 is the object of the water droplet on the surface of the superhydrophobic LDHs film sample prepared in Example 1. photo.
  • the aluminum sheet with a thickness of 0.1mm (purity of 99.5 %) is first ultrasonically cleaned with ethanol for 5 minutes, then ultrasonically cleaned with water for 5mm to remove surface oil, then anodized on the anodizing device for 50mm, and the aluminum piece is taken out, using deionized water.
  • the electrolyte was rinsed off to obtain an anodized aluminum substrate for use.
  • the anodizing device uses a lead plate or a stainless steel plate as a cathode, and the electrolyte is a 1.0 mol/L sulfuric acid solution, and the oxidation current is 2 A.
  • the above LDHs film was suspended in 0.05 mol/L sodium laurate (Cui ⁇ COONa) aqueous solution at 25 °C for 5 hours, and the film was taken out, rinsed with ethanol, and dried at room temperature. A hydrophobic LDHs film.
  • Fig. 1 is a SEM photograph of the surface of an aluminum sheet after surface anodization obtained in Example 1
  • Figure 2 is a SEM photograph of a surface of a sample of LDHs prepared in Example 1 and Example C. It can be clearly seen from Fig.
  • a hexagonal sheet-like substance exists on the surface of the anodized aluminum that is, a thin film layer of LDHs is formed, and the hexagonal flaky crystal grains of the hydrotalcite are vertically grown on the surface of the substrate, and hexagonal plate crystals are formed.
  • the thickness of the particles is in the nanometer scale range (60 ⁇ 80 nm), and the length of each side of the hexagonal flake grains is in the micrometer range.
  • FIG. 3 is a SEM photograph of a superhydrophobic LDHs film sample prepared in Example 1, Step D. Comparing Fig. 2 and Fig. 3, it can be found that the morphology of the hydrophobized film is substantially unchanged from that before the treatment, and the bird's nest morphology is maintained.
  • FIG. 4 is an optical photograph of the surface of a superhydrophobic LDHs film sample prepared by water droplets in Example 1.
  • Fig. 5 is a physical photograph of a superhydrophobic LDHs film sample prepared by water droplets in Example 1.
  • the surface roughness of the LDHs film samples obtained by the step C was 477.34 nm using a Digital Nanoscope III atomic force microscope (AFM) from Veeco, USA.
  • AFM Digital Nanoscope III atomic force microscope
  • the aluminum sheet with a thickness of 0.1mm (purity of 99.5 wt%) is first ultrasonically cleaned with ethanol for 5mm, then ultrasonically cleaned with water for 5mm to remove surface oil, then anodized on the anodizing device for 50mm, and the aluminum piece is taken out and deionized.
  • the electrolyte is rinsed off with water to obtain an anodized aluminum substrate for use.
  • the anodizing device uses a lead plate or a stainless steel plate as a cathode, and the electrolyte is a 1.0 mol/L sulfuric acid solution, and the oxidation current is 2 A.
  • the aluminum sheet with a thickness of 0.1mm (purity of 99.5 wt%) is first ultrasonically cleaned with ethanol for 5mm, then ultrasonically cleaned with water for 5mm to remove surface oil, then anodized on the anodizing device for 50mm, and the aluminum piece is taken out and deionized.
  • the electrolyte is rinsed off with water to obtain an anodized aluminum substrate for use.
  • the anodizing device uses a lead plate or a stainless steel plate as a cathode, and the electrolyte is a 1.0 mol/L sulfuric acid solution, and the oxidation current is 2 A.
  • the aluminum sheet with a thickness of 0.5mm (purity of 80% by weight) was first ultrasonically cleaned with ethanol for 10 minutes, then ultrasonically cleaned with water for 5 mm to remove surface oil, then anodized on an anodizing device for 100 mm, and the aluminum piece was taken out and deionized.
  • the electrolyte is rinsed off with water to obtain an anodized aluminum substrate for use.
  • the anodizing device uses a lead plate or a stainless steel plate as a cathode, and the electrolyte is a 2.0 mol/L sulfuric acid solution with an oxidation current of 2 A.
  • the aluminum sheet with a thickness of 0.5mm (purity of 80% by weight) was first ultrasonically cleaned with ethanol for 10 minutes, then ultrasonically cleaned with water for 5 mm to remove surface oil, then anodized on an anodizing device for 100 mm, and the aluminum piece was taken out and deionized.
  • the electrolyte is rinsed off with water to obtain an anodized aluminum substrate for use.
  • the anodizing device uses a lead plate or a stainless steel plate as a cathode, and the electrolyte is a 1.5 mol/L sulfuric acid solution with an oxidation current of 2 A.
  • the aluminum sheet with a thickness of 0.5 mm (80% purity) was first ultrasonically cleaned with ethanol for 10 min, then ultrasonically cleaned 5 mm with water to remove surface oil, and then anodized on an anodizing device. Mm, remove the aluminum sheet, rinse off the electrolyte with deionized water, and obtain an anodized aluminum substrate for use.
  • the anodizing device uses a lead plate or a stainless steel plate as a cathode, and the electrolyte is a 1.5 mol/L sulfuric acid solution, and the oxidation current is 2 A.
  • the above LDHs film was suspended in O.lmol/L potassium oleate (C 15 H 31 COOK) aqueous solution at 60 ° C for 5 hours, then rinsed with ethanol and dried at room temperature.
  • the contact angle of the water droplets on the surface of the superhydrophobic LDHs film was measured to be 151 ° ⁇ 2 °.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Mechanical Engineering (AREA)
  • Metallurgy (AREA)
  • Combustion & Propulsion (AREA)
  • Chemical Treatment Of Metals (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)

Abstract

L'invention porte sur un film mince d'hydroxydes bicouches, superhydrophobes, formé sur un substrat d'Al anodisé et sur son procédé de fabrication. Le procédé de fabrication met en jeu une technologie in situ, dans laquelle le film mince d'hydroxydes bicouches formé sur une feuille d'Al anodisée a une structure composite nano/microscopique et sa rugosité de surface est de 250-860 nm. Après un traitement hydrophobe conduit dans une solution contenant un agent tensioactif qui est de façon substantielle un sel aliphatique à longue chaîne, le film a une propriété hydrophobe supérieure et l'angle de contact avec l'eau peut être de jusqu'à 150-170°. L'agent tensioactif utilisé est exempt de fluor et il n'empoisonne pas les êtres humains ni ne pollue l'environnement. Le présent procédé utilise un traitement simple et un matériau pouvant aisément être obtenu, et il a un coût inférieur et a une bonne reproductibilité. Le film obtenu a une performance superhydrophobe et d'auto-nettoyage. Le film mince d'hydroxydes bicouches, superhydrophobe, a la propriété d'être utilisé dans les matériaux industriels comme revêtement pour protéger la surface métallique vis-à-vis de poussières et de brouillard, etc.
PCT/CN2007/070124 2007-06-15 2007-06-15 Film mince d'hydroxydes bicouches, superhydrophobes, et son procédé de fabrication WO2008151495A1 (fr)

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Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101967673A (zh) * 2010-08-27 2011-02-09 中国科学院海洋研究所 利用电解刻蚀在金属铝表面制备超疏水膜的方法
CN102818118A (zh) * 2011-06-10 2012-12-12 中国石油天然气股份有限公司 一种天然气站场设备防冰堵的方法
CN110355075A (zh) * 2018-03-26 2019-10-22 青岛海尔智慧厨房电器有限公司 一种超双疏叶轮及其制备方法和应用
CN111926363A (zh) * 2020-08-05 2020-11-13 上海电力大学 一种环保的长效耐用铝合金表面处理工艺
CN112853258A (zh) * 2021-01-12 2021-05-28 国家能源集团宁夏煤业有限责任公司 超疏水碳钢及其制备方法
CN113445051A (zh) * 2021-07-13 2021-09-28 中国石油大学(华东) 一种在铝合金多孔氧化膜表面制备超疏水锂铝类水滑石涂层的方法
CN114082225A (zh) * 2021-11-12 2022-02-25 中国石油大学(华东) 一种具有自修复功能的无氟超疏水油水分离网材料及其制备方法
CN115029756A (zh) * 2022-06-16 2022-09-09 烟台大学 一种多功能Zr基非晶合金超疏水表面的制备方法

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US20040030013A1 (en) * 2001-02-28 2004-02-12 Hoy Edgar Franklin Novel rheology modified hydrophobic compositions, modification agents, and methods of making
CN1717368A (zh) * 2002-12-23 2006-01-04 科学与工业研究委员会 水滑石和水镁石型带正电层的制备
CN1792449A (zh) * 2005-12-06 2006-06-28 北京化工大学 以铝为基体的类水滑石结构化催化剂及其制备方法
CN1908244A (zh) * 2006-07-14 2007-02-07 北京化工大学 一种以类水滑石为前驱体制备复合金属氧化物薄膜的方法
CN101054194A (zh) * 2006-04-12 2007-10-17 北京化工大学 超疏水层状双羟基复合金属氧化物薄膜及其制备方法

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040030013A1 (en) * 2001-02-28 2004-02-12 Hoy Edgar Franklin Novel rheology modified hydrophobic compositions, modification agents, and methods of making
CN1717368A (zh) * 2002-12-23 2006-01-04 科学与工业研究委员会 水滑石和水镁石型带正电层的制备
CN1792449A (zh) * 2005-12-06 2006-06-28 北京化工大学 以铝为基体的类水滑石结构化催化剂及其制备方法
CN101054194A (zh) * 2006-04-12 2007-10-17 北京化工大学 超疏水层状双羟基复合金属氧化物薄膜及其制备方法
CN1908244A (zh) * 2006-07-14 2007-02-07 北京化工大学 一种以类水滑石为前驱体制备复合金属氧化物薄膜的方法

Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101967673A (zh) * 2010-08-27 2011-02-09 中国科学院海洋研究所 利用电解刻蚀在金属铝表面制备超疏水膜的方法
CN102818118A (zh) * 2011-06-10 2012-12-12 中国石油天然气股份有限公司 一种天然气站场设备防冰堵的方法
CN110355075A (zh) * 2018-03-26 2019-10-22 青岛海尔智慧厨房电器有限公司 一种超双疏叶轮及其制备方法和应用
CN111926363A (zh) * 2020-08-05 2020-11-13 上海电力大学 一种环保的长效耐用铝合金表面处理工艺
CN112853258A (zh) * 2021-01-12 2021-05-28 国家能源集团宁夏煤业有限责任公司 超疏水碳钢及其制备方法
CN112853258B (zh) * 2021-01-12 2022-08-16 国家能源集团宁夏煤业有限责任公司 超疏水碳钢及其制备方法
CN113445051A (zh) * 2021-07-13 2021-09-28 中国石油大学(华东) 一种在铝合金多孔氧化膜表面制备超疏水锂铝类水滑石涂层的方法
CN113445051B (zh) * 2021-07-13 2022-04-01 中国石油大学(华东) 一种在铝合金多孔氧化膜表面制备超疏水锂铝类水滑石涂层的方法
CN114082225A (zh) * 2021-11-12 2022-02-25 中国石油大学(华东) 一种具有自修复功能的无氟超疏水油水分离网材料及其制备方法
CN115029756A (zh) * 2022-06-16 2022-09-09 烟台大学 一种多功能Zr基非晶合金超疏水表面的制备方法
CN115029756B (zh) * 2022-06-16 2024-01-26 烟台大学 一种多功能Zr基非晶合金超疏水表面的制备方法

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