CN110552038A - super-hydrophobic material and preparation method thereof - Google Patents
super-hydrophobic material and preparation method thereof Download PDFInfo
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- CN110552038A CN110552038A CN201910926770.1A CN201910926770A CN110552038A CN 110552038 A CN110552038 A CN 110552038A CN 201910926770 A CN201910926770 A CN 201910926770A CN 110552038 A CN110552038 A CN 110552038A
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- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- 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
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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
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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
- C25D11/04—Anodisation of aluminium or alloys based thereon
- C25D11/06—Anodisation of aluminium or alloys based thereon characterised by the electrolytes used
Abstract
the invention discloses a super-hydrophobic material and a preparation method thereof. The super-hydrophobic material has a lotus leaf-shaped nano structure. The lotus leaf-shaped nano structure is similar to a T-shaped structure, and can directly realize super-hydrophobicity without using organic low-surface-energy substances for modification, and the material for realizing super-hydrophobicity only by structure regulation has better stability. The material with the lotus leaf-shaped nano structure can be aluminum oxide which is used as a wear-resistant corrosion-resistant coating of a common workpiece, so that the nano aluminum oxide with the special structure prepared by the micro-arc oxidation method also has excellent stability. In addition, the preparation method of the super-hydrophobic material provided by the invention is simple and easy to operate, has lower cost and has potential application value.
Description
Technical Field
The invention relates to the technical field of super-hydrophobic materials, in particular to a super-hydrophobic material and a preparation method thereof.
Background
the super-hydrophobic material has a wide application prospect in a plurality of interface scientific fields including scenes of cleaning, anti-icing, anti-fogging, flow resistance reduction, oil-water separation, metal corrosion prevention and the like due to the special wettability of the surface of the super-hydrophobic material.
In recent years, three strategies mainly exist for preparing a super-hydrophobic material, namely, a micro-nano structure is constructed on the surface of a hydrophobic low-surface-energy material; secondly, constructing a micro-nano structure on the surface of the material, and then modifying by using organic low-surface-energy substances; and thirdly, constructing a T-shaped micro-nano structure on the surface of the material. Wherein, organic low surface energy substances are used in the first two strategies, and the stability such as temperature resistance and the like is poor. And the third strategy can realize the super-hydrophobicity only by constructing a special T-shaped structure, organic low-surface-energy substances are not used for modification in the process, the material often shows better stability, and the method has obvious advantages in a plurality of methods for preparing the super-hydrophobic material.
At present, a T-shaped structure is constructed on the surface of a material so as to obtain super-hydrophobicity, and a laser etching method or a chemical etching method is mainly adopted to accurately regulate and control the surface structure. However, most laser etching methods or chemical etching methods have the problems of harsh experimental conditions, complex steps, high cost, incapability of batch preparation and the like.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to solve the problems of the existing preparation method which only depends on regulating and controlling the material structure to obtain the super-hydrophobic material, and provides a super-hydrophobic material with a lotus-shaped nano structure similar to a T-shaped structure and a method thereof, which are simple and low in cost.
The technical scheme of the invention is as follows:
A superhydrophobic material, wherein the superhydrophobic material has a lotus-leaf like nanostructure.
Further, the super-hydrophobic material is a metal oxide with a lotus-shaped nano structure.
Still further, the superhydrophobic material is alumina having a lotus-shaped nanostructure.
a preparation method of a super-hydrophobic material is provided, wherein the super-hydrophobic material with a lotus leaf-shaped nano structure is prepared by adopting a micro-arc oxidation technology.
Further, comprising the steps of:
Providing a metal substrate;
And forming a metal oxide with a lotus leaf-shaped nano structure on the metal base material by adopting a micro-arc oxidation technology to obtain the super-hydrophobic material.
Further, comprising the steps of:
Providing aluminum or aluminum alloy, and sequentially polishing and cleaning the aluminum or aluminum alloy;
Putting the treated aluminum or aluminum alloy into an alkaline electrolyte, connecting the aluminum or aluminum alloy with the anode of a power supply, connecting the cathode of the power supply with a working electrode, contacting the working electrode with the electrolyte, and starting the power supply to perform micro-arc oxidation treatment;
After micro-arc oxidation treatment, washing and drying are carried out, and aluminum oxide with a lotus leaf-shaped nano structure is obtained on the surface of aluminum or aluminum alloy, so that the super-hydrophobic material is obtained.
Still further, the alkaline electrolyte includes: 3-20g/L of phosphate, 1-5g/L of alkaline hydroxide and water as a solvent.
Still further, the phosphate is selected from one or more of sodium hexametaphosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium tripolyphosphate, trisodium phosphate, and sodium pyrophosphate.
Still further, the alkaline hydroxide is selected from one or more of sodium hydroxide and potassium hydroxide.
Further, the process conditions of the micro-arc oxidation treatment comprise:
The selected power supply is a pulse power supply, and the operating parameters of the pulse power supply are that the current density is 1-40A/dm 2, the frequency is 100-2000Hz, the duty ratio is 10-15%, and the micro-arc oxidation time is 1-10min in a constant current mode.
Has the advantages that: the invention provides a super-hydrophobic material with a lotus-shaped nano structure, wherein the lotus-shaped nano structure is similar to a T-shaped structure, and super-hydrophobicity can be directly realized without modification by using an organic low-surface-energy substance. In addition, the super-hydrophobic material with the lotus leaf-shaped nano structure has the advantages of simple preparation method, easiness in operation, lower cost and potential application value.
drawings
fig. 1 is a front SEM image of the nano-alumina lotus leaf super-hydrophobic material prepared in example 1.
FIG. 2 is a sectional SEM image of the lotus leaf-shaped nano alumina super-hydrophobic material prepared in example 1.
Fig. 3 is an XRD pattern of the lotus leaf-shaped nano alumina super-hydrophobic material prepared in example 1.
fig. 4 is a contact angle graph of the lotus-shaped nano alumina super-hydrophobic material prepared in example 1 to water.
Detailed Description
The invention provides a super-hydrophobic material and a preparation method thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and effect of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The embodiment of the invention provides a super-hydrophobic material, wherein the super-hydrophobic material has a lotus-leaf-shaped nano structure.
The T-shaped structure can directly endow the surface of the material with super-hydrophobicity, and the upward surface tension of water drops on the edge of the T-shaped structure is greater than the downward gravity, so that the water drops are difficult to wet the surface, and the super-hydrophobicity of the material can be directly realized without modifying by using organic low-surface-energy substances. In the embodiment, the lotus-shaped nanostructure is a special structure similar to a T shape, and the contact angle to water is 150 +/-3 degrees, so that the material with the lotus-shaped nanostructure shows super-hydrophobicity, does not need to be modified by organic low-surface-energy substances, and shows better stability.
Further, the super-hydrophobic material is a metal oxide with a lotus-shaped nano structure.
Still further, the superhydrophobic material is alumina having a lotus-shaped nanostructure. In the embodiment, the lotus leaf-shaped nano structure is similar to a T-shaped structure, and the super-hydrophobicity can be directly realized without using organic low-surface-energy substances for modification, so that the material for realizing the super-hydrophobicity only by regulating and controlling the structure has better stability; the material with the lotus leaf-shaped nano structure is alumina which is used as a common wear-resistant and corrosion-resistant coating of a workpiece, so the nano alumina with the special structure also has excellent stability.
the embodiment of the invention provides a preparation method of a super-hydrophobic material, wherein the super-hydrophobic material with a lotus-shaped nano structure is prepared by adopting a micro-arc oxidation technology.
The embodiment of the invention provides a preparation method of a super-hydrophobic material, which comprises the following steps:
Providing a metal substrate;
And forming a metal oxide with a lotus leaf-shaped nano structure on the metal base material by adopting a micro-arc oxidation technology to obtain the super-hydrophobic material.
The embodiment of the invention provides a preparation method of a super-hydrophobic material, which comprises the following steps:
S10, providing aluminum or aluminum alloy, and sequentially polishing and cleaning the aluminum or aluminum alloy;
S20, placing the processed aluminum or aluminum alloy into alkaline electrolyte, connecting the aluminum or aluminum alloy with the positive electrode of a power supply, connecting the negative electrode of the power supply with a working electrode, contacting the working electrode with the electrolyte, and starting the power supply to perform micro-arc oxidation treatment;
S30, washing and drying after micro-arc oxidation treatment, and obtaining the aluminum oxide with the lotus leaf-shaped nano structure on the surface of the aluminum or the aluminum alloy, namely obtaining the super-hydrophobic material.
In the embodiment, the aluminum oxide with the lotus leaf-shaped nano structure is synthesized in an alkaline electrolyte system by adopting a micro-arc oxidation method on aluminum or aluminum alloy, and the method has the advantages of one-step synthesis, simple experimental conditions and low cost; the obtained nano structure is a lotus leaf-shaped nano structure, is similar to a T-shaped structure, can directly realize super-hydrophobicity without using organic low-surface-energy substances for modification, and the material for realizing super-hydrophobicity only by structure regulation has better stability; the material with the lotus leaf-shaped nano structure is aluminum oxide which is used as a wear-resistant corrosion-resistant coating of a common workpiece, so that the nano aluminum oxide with the special structure prepared by the micro-arc oxidation method has excellent stability.
In step S10, in one embodiment, the step of sequentially polishing and cleaning the aluminum or aluminum alloy includes: and polishing the aluminum or the aluminum alloy by using high-mesh sand paper, and sequentially selecting deionized water, absolute ethyl alcohol or acetone for ultrasonic cleaning for 10-30 min.
In one embodiment, the aluminum or aluminum alloy may be pure aluminum, a 2-series, 5-series, 6-series, or 7-series aluminum alloy.
in step S20, in one embodiment, the alkaline electrolyte includes: 3-20g/L of phosphate, 1-5g/L of alkaline hydroxide and water (such as deionized water) as a solvent.
In a particular embodiment, the phosphate is selected from one or more of sodium hexametaphosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium tripolyphosphate, trisodium phosphate, and sodium pyrophosphate.
In a preferred embodiment, the phosphate in the alkaline electrolyte is 5g/L sodium tripolyphosphate. The alkaline electrolyte prepared from 5g/L sodium tripolyphosphate has a good dispersing effect, can enable liquid and solid particles to be better dissolved in the electrolyte, plays a role in solubilization in the micro-arc oxidation process, and is more beneficial to obtaining a stable alumina film layer.
In a specific embodiment, the alkaline hydroxide is selected from one or more of sodium hydroxide and potassium hydroxide.
In one embodiment, the process conditions of the micro-arc oxidation treatment include:
The selected power supply is a pulse power supply, and the operating parameters of the pulse power supply are that the current density is 1-40A/dm 2, the frequency is 100-2000Hz, the duty ratio is 10-15%, and the micro-arc oxidation time is 1-10min in a constant current mode.
In a preferred embodiment, the current density is 2A/dm 2, because a moderate current density balances the growth and corrosion processes of the alumina film, and when the current density is too high, the alumina film grows too fast, is easy to sinter, and is not easy to corrode the lotus-shaped nano-structure.
In a preferred embodiment, the frequency is 200Hz, and too high frequency causes the alumina film layer to grow too fast, whereas too low frequency is not favorable for obtaining a dense alumina film layer and corrosion.
In a preferred embodiment, the micro-arc oxidation time is 5min, so that an ideal lotus-shaped nano structure can be obtained, and the structure cannot be damaged due to excessive corrosion.
The invention is further illustrated by the following specific examples.
Example 1
The method comprises the following steps of cutting 2A12 aluminum alloy serving as an aluminum source into rectangular samples with the size of 50mm multiplied by 25mm multiplied by 2mm, polishing the samples by using common 1200-mesh metallographic abrasive paper, and then carrying out ultrasonic cleaning on the samples for 30min by using deionized water and absolute ethyl alcohol in sequence to obtain samples for later use. Preparing an alkaline electrolyte system for micro-arc oxidation, which comprises the following steps: 5g/L sodium tripolyphosphate, 1.5g/L sodium hydroxide and deionized water as a solvent are placed in a stainless steel electrolyte container for later use.
and (3) using a pulse power supply in the micro-arc oxidation process, adjusting power supply parameters to be that under a constant current mode, the current density is 2A/dm 2, the frequency is 200Hz, and the air-to-space ratio is 12 percent, after the power supply parameters are adjusted, taking the aluminum alloy to be used as an anode and the stainless steel electrolyte container as a cathode, starting the power supply, after micro-arc oxidation is carried out for 5min, obtaining the aluminum alloy with the oxide layer, finally washing with deionized water, and naturally drying to obtain the super-hydrophobic material with the lotus leaf-shaped nano aluminum oxide.
The SEM results of the front and cross-section of the material are shown in fig. 1 and 2, and it can be seen that the film layer is composed of irregular lotus leaf-like sheet structures randomly distributed, mostly in the shape of a disk, and has an average diameter of about 500 nm. The layers have a gap in the range of 200-1200 nm. Cross section of the material it can be seen that the total thickness of the obtained membrane layer with the lotus-like nanostructures is about 1 μm. The lotus-shaped structure on the top of the film is not as smooth as the real lotus leaf, but the surface has some folds and unevenness, because the sample and the electrolyte react rapidly and violently under the condition of arc discharge, and the surface of the growing film has certain roughness and shows an uneven state. The lotus leaf lamellar structure at the top is supported by the rods so that the structure cannot collapse, and the structural diameters of the rods are different and the shapes of the rods are irregular due to the corrosion effect of the electrolyte. The XRD result of the obtained material is shown in figure 3, and the characteristic peak of amorphous alumina appears on the aluminum sheet at the position of 15.1-35.6 degrees, which confirms that the surface of the 2A12 aluminum alloy generates alumina phase after micro-arc oxidation treatment. As shown in fig. 4, the contact angle value of the material with water was measured to be 150 ± 3 °, and superhydrophobicity was exhibited. The 20 microliter water droplet was able to maintain a spherical shape on the surface of the material, confirming that the material had uniform superhydrophobicity.
Example 2
Using 5005 aluminum alloy as an aluminum source, cutting the aluminum alloy into rectangular samples with the dimensions of 50mm multiplied by 25mm multiplied by 2mm, polishing the rectangular samples by using 1200-mesh metallographic abrasive paper, and then sequentially using deionized water and absolute ethyl alcohol to perform ultrasonic cleaning for 30min to obtain samples for later use. Preparing an alkaline electrolyte system for micro-arc oxidation, which comprises the following steps: 5g/L sodium tripolyphosphate, 1.5g/L sodium hydroxide and deionized water as a solvent are placed in a stainless steel electrolyte container for later use.
and (3) using a pulse power supply in the micro-arc oxidation process, adjusting power supply parameters to be that under a constant current mode, the current density is 2A/dm 2, the frequency is 200Hz, and the air-to-space ratio is 12 percent, after the power supply parameters are adjusted, taking the aluminum alloy to be used as an anode and the stainless steel electrolyte container as a cathode, starting the power supply, after micro-arc oxidation is carried out for 5min, obtaining the aluminum alloy with the oxide layer, finally washing with deionized water, and naturally drying to obtain the super-hydrophobic material with the lotus leaf-shaped nano aluminum oxide.
example 3
6061 aluminum alloy is used as an aluminum source, the aluminum alloy is cut into rectangular samples with the size of 50mm multiplied by 25mm multiplied by 2mm, 1200-mesh metallographic abrasive paper is used for polishing the rectangular samples, and deionized water and absolute ethyl alcohol are sequentially used for ultrasonic cleaning for 30min to obtain samples for later use. Preparing an alkaline electrolyte system for micro-arc oxidation, which comprises the following steps: 5g/L sodium tripolyphosphate, 1.5g/L sodium hydroxide and deionized water as a solvent are placed in a stainless steel electrolyte container for later use.
And (3) using a pulse power supply in the micro-arc oxidation process, adjusting power supply parameters to be 2.5A/dm 2 in a constant current mode, 250Hz in frequency and 12% in air ratio, after the power supply parameters are adjusted, taking the aluminum alloy to be used as an anode and a stainless steel electrolyte container as a cathode, starting the power supply, performing micro-arc oxidation for 5min to obtain the aluminum alloy with the oxide layer, finally washing with deionized water, and naturally drying to obtain the super-hydrophobic material with the lotus leaf-shaped nano aluminum oxide.
Example 4
Cutting 7075 aluminum alloy serving as an aluminum source into rectangular samples with the sizes of 50mm multiplied by 25mm multiplied by 2mm, polishing the rectangular samples by using 1200-mesh metallographic abrasive paper, and then ultrasonically cleaning the rectangular samples for 30min by sequentially using deionized water and absolute ethyl alcohol to obtain samples for later use. Preparing an alkaline electrolyte system for micro-arc oxidation, which comprises the following steps: 5g/L sodium tripolyphosphate, 1.5g/L sodium hydroxide and deionized water as a solvent are placed in a stainless steel electrolyte container for later use.
and (3) using a pulse power supply in the micro-arc oxidation process, adjusting power supply parameters to be that under a constant current mode, the current density is 2A/dm 2, the frequency is 200Hz, and the air-to-space ratio is 12 percent, after the power supply parameters are adjusted, taking the aluminum alloy to be used as an anode and the stainless steel electrolyte container as a cathode, starting the power supply, after micro-arc oxidation is carried out for 5min, obtaining the aluminum alloy with the oxide layer, finally washing with deionized water, and naturally drying to obtain the super-hydrophobic material with the lotus leaf-shaped nano aluminum oxide.
example 5
The method comprises the following steps of cutting 2A12 aluminum alloy serving as an aluminum source into rectangular samples with the size of 50mm multiplied by 25mm multiplied by 2mm, polishing the rectangular samples by using 1200-mesh metallographic abrasive paper, and then ultrasonically cleaning the rectangular samples for 30min by using deionized water and absolute ethyl alcohol in sequence to obtain samples for later use. Preparing an alkaline electrolyte system for micro-arc oxidation, which comprises the following steps: 5g/L sodium tripolyphosphate, 2.1g/L potassium hydroxide and deionized water as a solvent are placed in a stainless steel electrolyte container for later use.
and (3) using a pulse power supply in the micro-arc oxidation process, adjusting power supply parameters to be that under a constant current mode, the current density is 2A/dm 2, the frequency is 200Hz, and the air-to-space ratio is 12 percent, after the power supply parameters are adjusted, taking the aluminum alloy to be used as an anode and the stainless steel electrolyte container as a cathode, starting the power supply, after micro-arc oxidation is carried out for 5min, obtaining the aluminum alloy with the oxide layer, finally washing with deionized water, and naturally drying to obtain the super-hydrophobic material with the lotus leaf-shaped nano aluminum oxide.
In summary, the invention provides a super-hydrophobic material and a preparation method thereof, wherein aluminum or aluminum alloy is subjected to micro-arc oxidation technology, and aluminum oxide with a lotus-leaf-shaped nano structure is prepared in alkaline electrolyte in one step, so that the synthesis of the super-hydrophobic aluminum oxide material is realized. The super-hydrophobic alumina material realizes super-hydrophobicity only by depending on a special micro-nano structure, does not need to be modified by any organic low-surface-energy substance, and has the advantages of simple preparation method, easy operation, low cost and potential application value.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (10)
1. A superhydrophobic material, wherein the superhydrophobic material has a lotus-leaf-like nanostructure.
2. the superhydrophobic material of claim 1, wherein the superhydrophobic material is a metal oxide having a scalloped nanostructure.
3. The superhydrophobic material of claim 2, wherein the superhydrophobic material is alumina having a scalloped nanostructure.
4. The preparation method of the super-hydrophobic material is characterized in that the micro-arc oxidation technology is adopted to prepare the super-hydrophobic material with the lotus leaf-shaped nano structure.
5. The method for preparing the superhydrophobic material of claim 4, comprising the steps of:
Providing a metal substrate;
And forming a metal oxide with a lotus leaf-shaped nano structure on the metal base material by adopting a micro-arc oxidation technology to obtain the super-hydrophobic material.
6. The method for preparing the superhydrophobic material of claim 4, comprising the steps of:
Providing aluminum or aluminum alloy, and sequentially polishing and cleaning the aluminum or aluminum alloy;
Putting the treated aluminum or aluminum alloy into an alkaline electrolyte, connecting the aluminum or aluminum alloy with the anode of a power supply, connecting the cathode of the power supply with a working electrode, contacting the working electrode with the electrolyte, and starting the power supply to perform micro-arc oxidation treatment;
After micro-arc oxidation treatment, washing and drying are carried out, and aluminum oxide with a lotus leaf-shaped nano structure is obtained on the surface of aluminum or aluminum alloy, so that the super-hydrophobic material is obtained.
7. The method for preparing the superhydrophobic material of claim 6, wherein the alkaline electrolyte comprises: 3-20g/L of phosphate, 1-5g/L of alkaline hydroxide and water as a solvent.
8. The method of claim 7, wherein the phosphate is selected from one or more of sodium hexametaphosphate, sodium dihydrogen phosphate, disodium hydrogen phosphate, sodium tripolyphosphate, trisodium phosphate, and sodium pyrophosphate.
9. The method for preparing a superhydrophobic material of claim 7, wherein the alkaline hydroxide is selected from one or more of sodium hydroxide and potassium hydroxide.
10. The preparation method of the super-hydrophobic material as claimed in claim 6, wherein the process conditions of the micro-arc oxidation treatment comprise:
The selected power supply is a pulse power supply, and the operating parameters of the pulse power supply are that the current density is 1-40A/dm 2, the frequency is 100-2000Hz, the duty ratio is 10-15%, and the micro-arc oxidation time is 1-10min in a constant current mode.
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