AU2021101783A4 - Method of preparing superhydrophobic surface on magnesium alloy substrate - Google Patents

Method of preparing superhydrophobic surface on magnesium alloy substrate Download PDF

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AU2021101783A4
AU2021101783A4 AU2021101783A AU2021101783A AU2021101783A4 AU 2021101783 A4 AU2021101783 A4 AU 2021101783A4 AU 2021101783 A AU2021101783 A AU 2021101783A AU 2021101783 A AU2021101783 A AU 2021101783A AU 2021101783 A4 AU2021101783 A4 AU 2021101783A4
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magnesium alloy
phosphonic acid
superhydrophobic
preparing
water
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AU2021101783A
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Jiaojiao DONG
Ting PAN
Xiaowei XUN
Dongmian ZANG
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East China Jiaotong University
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East China Jiaotong University
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    • 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
    • C23CCOATING 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
    • C23C22/00Chemical 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
    • C23C22/05Chemical 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
    • C23C22/06Chemical 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
    • C23C22/48Chemical 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
    • C23C22/57Treatment of magnesium or alloys based thereon
    • 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
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/16Antifouling paints; Underwater paints
    • C09D5/1681Antifouling coatings characterised by surface structure, e.g. for roughness effect giving superhydrophobic coatings or Lotus effect
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B05SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05DPROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
    • B05D1/00Processes for applying liquids or other fluent materials
    • B05D1/18Processes for applying liquids or other fluent materials performed by dipping
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B08CLEANING
    • B08BCLEANING IN GENERAL; PREVENTION OF FOULING IN GENERAL
    • B08B3/00Cleaning by methods involving the use or presence of liquid or steam
    • B08B3/04Cleaning involving contact with liquid

Abstract

The present invention belongs to the field of treatment of metallic material surfaces, and particularly disclosed is a method of preparing a superhydrophobic surface on a magnesium alloy substrate. The method includes the following steps: (1) mechanically polishing and cleaning a magnesium alloy; (2) dissolving a water-soluble organic phosphonic acid in deionized water, immersing the magnesium alloy material in the step (1) in 0.01-0.1 mol/L of aqueous solution of phosphonic acid, heating up to 95-100°C, and keeping the temperature constant for 16-24 h; and (3) taking the magnesium alloy material in the step (2) out from the phosphonic acid solution, washing the magnesium alloy with the deionized water, and drying to obtain a phosphonated superhydrophobic coating. The solution is mainly used for preparing a surface film on a magnesium alloy substrate, and solves the problem of limited application of preparation of superhydrophobic surfaces. Fig. 1 Photograph of spherical water droplets with different sizes on superhydrophobic surface. Fig. 2 Scanning electron micrograph of the superhydrophobic surface. 1/1

Description

Fig. 1 Photograph of spherical water droplets with different sizes on
superhydrophobic surface.
Fig. 2 Scanning electron micrograph of the superhydrophobic surface.
1/1
METHOD OF PREPARING SUPERHYDROPHOBIC SURFACE ON MAGNESIUM ALLOY SUBSTRATE TECHNICAL FIELD
The present invention belongs to the technical field of materials, and particularly
disclosed is a method of preparing a superhydrophobic surface on a magnesium alloy
substrate.
BACKGROUND OF THE PRESENT INVENTION
The superhydrophobicity is widely researched in the field of metallic material
surfaces because of its excellent self-cleaning, corrosion resistant, anti-fouling and
anti-icing characteristics. Traditionally, a superhydrophobic surface is usually
constructed by two strategies based on two-step method. Strategy (1) includes the
steps of manufacturing a rough structure, and then modifying the surface with
low-surface-energy materials (such as fluoroalkyl silane). Strategy (2) includes the
steps of modifying the surface of low-surface-energy materials, and then roughening
the surface.
At present, the methods for preparing the superhydrophobic surface include
etching, template-assisted fabrication, electrospinning, sol-gel, anodic oxidation,
micro-arc oxidation, ion exchange, dealloying, etc. All these methods have relatively
high requirements for experimental equipment, complicated operation and limitations
in production, so that the application is limited.
SUMMARY OF THE PRESENT INVENTION
The purpose of the present invention is to provide a method of preparing a
superhydrophobic surface on a magnesium alloy substrate to solve the problem of
limited application of preparation of superhydrophobic surfaces.
To achieve the above purpose, a technical solution adopted in the present
invention is as follows: a method of preparing a superhydrophobic surface on a
magnesium alloy substrate includes the following steps:
(1) mechanically polishing and cleaning an AZ31 magnesium alloy;
(2) dissolving a water-soluble organic phosphonic acid in deionized water,
immersing the magnesium alloy material in the step (1) in a water-soluble phosphonic
acid solution, and keeping the temperature constant for 16-24 h; and
(3) taking the magnesium alloy material in the step (2) out from the phosphonic
acid solution, washing the magnesium alloy with the deionized water, and drying to
obtain a phosphonated superhydrophobic coating.
The present invention has the following technical effects.
(1) The surface activity and the interface reaction characteristics of metallic
materials are utilized in the present invention; the inventors find that because a
phenylphosphonic acid has dual functions of constructing a rough structure and
reducing surface energy, a phosphonated superhydrophobic surface of a magnesium
alloy substrate can be prepared by a one-step method instead of a two-step method in
the process.
(2) The phenylphosphonic acid becomes negatively charged after deprotonation
in the solution, and produces stable chemical bonding to magnesium ions on the
surface of the magnesium alloy substrate, thereby providing excellent hydrophobic
properties for the coating, wherein a contact angle of the coating is greater than 150;
and the phenylphosphonic acid reacts with magnesium to construct the rough structure
and further reduce the surface energy of magnesium alloy.
(3) The preparing method provided by the present invention is simple, quick, low
in cost and universal; and the coating has corrosion resistant and anti-fouling
characteristics showing wide application prospects.
Further, the pretreatment of magnesium alloy material in the step (1) includes:
cutting the magnesium alloy material; mechanically polishing the magnesium alloy
material with SiC abrasive paper until the surface is smooth and flat; then
ultrasonically cleaning the metal surface with acetone, absolute ethyl alcohol and
deionized water for 5-10 min in sequence to remove impurities and oil stains on the
metal surface; and blow-drying. The magnesium alloy is treated by the above method
to facilitate the formation of the superhydrophobic coating on the surface of the magnesium alloy substrate.
Further, the SiC abrasive paper 400#, 800#, 1200# and 2000# are used for
sequentially polishing the magnesium alloy in the step (1). The surface of the
magnesium alloy substrate can become flat and smooth by being sequentially polished
with the SiC abrasive paper of the above models, thereby facilitating the formation of
the superhydrophobic coating on the surface of the magnesium alloy substrate.
Further, the water-soluble phosphonic acid in the step (2) is phenylphosphonic
acid. The phenylphosphoric acid can reduce the surface energy while constructing the
rough structure.
Further, the constant temperature of the water-soluble phosphonic acid solution
in the step (2) is 95-100°C. The phosphonation of the surface of the magnesium alloy
substrate can be accelerated by using the water-soluble phosphonic acid solution at
the above temperature.
Further, the concentration of the water-soluble phosphonic acid solution in the
step (2) is 0.01-0.1 mol/L. The coating with uniform thickness can be formed on the
surface of the magnesium alloy substrate by using water-soluble phosphonic acid
solution within the above concentration range.
BRIEF DESCRIPTION OF THE DRAWINGS
Fig. 1 is a photograph of spherical water droplets with different sizes on
superhydrophobic surface in the present invention; and
Fig. 2 is a scanning electron micrograph of the superhydrophobic surface in the
present invention.
DETAILED DESCRIPTION OF THE PRESENT INVENTION
The present invention will be further described in detail below through specific
embodiments.
In this context, "superhydrophobicity" refers to a superhydrophobic property or
the formation of the superhydrophobic property, i.e., being extremely difficult to wet.
It has always been well known in the industry that a stable contact angle formed by droplets on the surface of a solid substrate can quantitatively measure the wettability of a specific solid. Wetting is the ability of a liquid to maintain contact with a solid surface as a result of intermolecular interactions when the liquid is brought together with the solid surface. The degree of wetting (wettability) is determined by the force balance between adhesive force and cohesive force. If the stable contact angle between the water droplets and the surface of the substrate is greater than 90, it is generally considered to be hydrophobic. For example, a material on which the droplets have a high stable contact angle is present, such as water on paraffin wax, for which the stable contact angle is about 107°. Hydrophobic coatings with stable contact angles greater than 150° are needed in many applications. Such coatings are called superhydrophobic coatings. A method of preparing a superhydrophobic surface on a magnesium alloy substrate includes following steps: (1) pretreating a magnesium alloy; cutting the magnesium alloy material; mechanically polishing with SiC abrasive paper 400#, 800#, 1200# and 2000# in sequence until the surface becomes smooth and flat; then ultrasonically cleaning with acetone, absolute ethyl alcohol and deionized water in sequence for 5 min to remove impurities and oil stains on the metal surface; and blow-drying; (2) dissolving a water-soluble organic phosphonic acid, which is preferably phenylphosphonic acid in the present embodiment, in deionized water; immersing the magnesium alloy material in the step (1) in a water-soluble phosphonic acid solution with a concentration of 0.01-0.1 mol/L, preferably 0.1 mol/L in the present embodiment; heating up the water-soluble phosphonic acid solution to 95-100°C, preferably 100°C in the present embodiment; and keeping the temperature constant for 16-24 h, preferably for 24 h in the present embodiment; (3) taking the magnesium alloy material in the step (2) out from the phosphonic acid solution; washing the magnesium alloy with the deionized water; and drying to obtain a phosphonated superhydrophobic coating as shown in Fig. 1 and Fig. 2. Embodiment 1 The magnesium alloy material was cut and then was mechanically polished with
SiC abrasive paper 400#, 800#, 1200# and 2000# until the surface is smooth and flat.
The metal surface was ultrasonically cleaned with acetone, absolute ethyl alcohol and
deionized water in sequence for 5 min to remove impurities and oil stains on the metal
surface, and then was blow-dried. 0.5269 g of phenylphosphonic acid was weighed
and dissolved in 100 ml of deionized water. The pretreated metal material was
immersed in the prepared phenylphosphonic acid solution, was taken out after
hydrothermal reaction at 95°C for 16 h, and was blow-dried after being rinsed with the
deionized water. A static contact angle and a rolling angle of the coating were 151.4°
and 7.6, respectively, as measured by a contact angle meter.
Embodiment 2
The magnesium alloy material was cut and then was mechanically polished with
SiC abrasive paper 400#, 800#, 1200# and 2000# until the surface is smooth and flat.
The metal surface was ultrasonically cleaned with acetone, absolute ethyl alcohol and
deionized water in sequence for 8 min to remove impurities and oil stains on the metal
surface, and then was blow-dried. 0.7905 g of phenylphosphonic acid was weighed
and dissolved in 100 ml of deionized water. The pretreated metal material was
immersed in the prepared phenylphosphonic acid solution, was taken out after
hydrothermal reaction at 98°C for 20 h, and was blow-dried after being rinsed with the
deionized water. A static contact angle and a rolling angle of the coating were 154.5°
and 5.4°, respectively, as measured by a contact angle meter.
Embodiment 3
The magnesium alloy material was cut and then was mechanically polished with
SiC abrasive paper 400#, 800#, 1200# and 2000# until the surface is smooth and flat.
The metal surface was ultrasonically cleaned with acetone, absolute ethyl alcohol and
deionized water in sequence for 10 min to remove impurities and oil stains on the
metal surface, and then was blow-dried. 1.5809 g of phenylphosphonic acid was
weighed and dissolved in 100 ml of deionized water. The pretreated metal material
was immersed in the prepared phenylphosphonic acid solution, was taken out after
hydrothermal reaction at 100°C for 24 h, and was blow-dried after being rinsed with
the deionized water. A static contact angle and a rolling angle of the coating were
159.10and 2.3, respectively, as measured by a contact angle meter.
In the solution, a coating contact angle meter (German Dataphysics contact angle
meter OCA15EC) is used for detection.
The above only illustrates the embodiments of the present invention. The
common knowledge of the specific structure and characteristics well-known in the
solution is not described here. It should be noted that those skilled in the art can make
several modifications and improvements without departing from the structure of the
present invention; and the modifications and improvements shall also fall within the
protection scope of the present invention, and will not affect the implementation effect
of the present invention and the practicability of patent.

Claims (6)

  1. CLAIMS 1. A method of preparing a superhydrophobic surface on a magnesium alloy
    substrate, comprising the following steps:
    (1) mechanically polishing and cleaning an AZ31 magnesium alloy;
    (2) dissolving a water-soluble organic phosphonic acid in deionized water,
    immersing the magnesium alloy material in the step (1) in a water-soluble phosphonic
    acid solution, and keeping the temperature constant for 16-24 h; and
    (3) taking the magnesium alloy material in the step (2) out from the phosphonic
    acid solution, washing the magnesium alloy with the deionized water, and drying to
    obtain a phosphonated superhydrophobic coating.
  2. 2. The method of preparing the superhydrophobic surface on the magnesium
    alloy substrate according to claim 1, wherein the pretreatment of magnesium alloy
    material in the step (1) comprises: cutting the magnesium alloy material;
    mechanically polishing the magnesium alloy material with SiC abrasive paper until
    the surface is smooth and flat; then ultrasonically cleaning the metal surface with
    acetone, absolute alcohol and deionized water for 5-10 min in sequence to remove
    impurities and oil stains on the metal surface; and blow-drying.
  3. 3. The method of preparing the superhydrophobic surface on the magnesium
    alloy substrate according to claim 2, wherein the SiC abrasive paper 400#, 800#,
    1200# and 2000# are used for sequentially polishing the magnesium alloy in the step
    (1).
  4. 4. The method of preparing the superhydrophobic surface on the magnesium
    alloy substrate according to claim 1, wherein the water-soluble phosphonic acid in the
    step (2) is phenylphosphonic acid.
  5. 5. The method of preparing the superhydrophobic surface on the magnesium
    alloy substrate according to claim 1, wherein the constant temperature of the
    water-soluble phosphonic acid solution in the step (2) is 95-100°C.
  6. 6. The method of preparing the superhydrophobic surface on the magnesium
    alloy substrate according to claim 1, wherein the concentration of the water-soluble
    phosphonic acid solution in the step (2) is 0.01-0.1 mol/L.
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AU2021101783A 2021-04-07 2021-04-07 Method of preparing superhydrophobic surface on magnesium alloy substrate Active AU2021101783A4 (en)

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AU2021101783A4 true AU2021101783A4 (en) 2021-06-03

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