CN109337105B - Method for preparing hydrophilic-hydrophobic interaction distribution microstructure surface - Google Patents
Method for preparing hydrophilic-hydrophobic interaction distribution microstructure surface Download PDFInfo
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- C08J2433/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
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Abstract
The invention belongs to the technical field of preparation of marine antifouling materials, and particularly relates to a method for preparing a hydrophilic-hydrophobic interaction distribution microstructure surface, which comprises the steps of covering a photomask of an electron beam etching set pattern on a monocrystalline silicon surface, etching a set pattern with a set depth, taking the etched monocrystalline silicon surface as a female die, obtaining a hydrophobic organic silicon microstructure surface with a set structure by utilizing etching and die turning, filling hydrogel in an organic silicon microstructure in order through the processes of plasma treatment, hydrogen peroxide activation, hydrophobic liquid hole sealing, cleaning and hydrogel perfusion to obtain a hydrophilic-hydrophobic interaction distribution microstructure surface with a regular structure, adjusting the projection area ratio and the space area ratio of a hydrophilic-hydrophobic region in the hydrophilic-hydrophobic interaction distribution microstructure surface by controlling the height of the hydrogel in the microstructure, and solving the problem of combination of hydrophilic-hydrophobic property and microstructure, the broad-spectrum antifouling performance of the microstructure material is improved, and the microstructure material is used for preventing and removing the biofouling on the surfaces of ships and marine structures.
Description
The technical field is as follows:
the invention belongs to the technical field of preparation of marine antifouling materials, and particularly relates to a method for preparing a hydrophilic-hydrophobic interaction distribution microstructure surface.
Background art:
marine biofouling is a phenomenon in which marine organisms living in the camps and the anchorings and living in the attachments grow on the bottom of ships or the surfaces of artificial facilities and cause adverse effects. Any structure immersed in seawater can be subjected to the problem of attachment of fouling organisms, the attachment of the fouling organisms on the surface of the structure can bring great harm to the structure, such as the problems of increased ship navigation resistance, pipeline blockage, reduced heat conductivity of a heat exchanger, reduced fishing yield of mariculture and the like, and the adoption of effective measures for preventing fouling of marine organisms is of great significance.
Marine fouling is most commonly prevented by applying an antifouling coating, such as an antifouling-type coating, to the submerged surface of a vessel or structure, whereby the coating releases chemicals to form a concentrated layer that inhibits fouling organisms from attaching. The antifouling paint for ships and marine facilities disclosed in the chinese patent 201010135154.3 can control the release rate of Cu + by adjusting the formula ratio of the flake glass composition, or adjusting the percentage content of the flake glass in the antifouling paint; chinese patent 200910030819.1 discloses a method for preparing low-toxicity marine antifouling paint by using Cu2Preparing a low-toxicity marine antifouling paint by using O hollow sub-microspheres alone or embedding a non-toxic organic antifouling agent as an antifouling agent; the products of the above patents have good antifouling effect, but the accumulation of antifouling agents containing tin or copper in marine environment affects ecological environment, so the use of the antifouling agents is gradually forbidden or limited, and the development of low-toxicity or non-toxic green antifouling technical means is urgently needed.
Fouling release type antifouling coatings achieve the goal of antifouling by designing specific surface characteristics so that marine fouling organisms do not easily attach to the surface of the coating, such as an antifouling coating composition disclosed in U.S. patent 4910252; U.S. patent 6265515 discloses an antifouling composition comprising a fluorinated silicone resin. In addition, the specially designed microstructure can reduce the attachment sites of specific fouling organisms and prevent the attachment of the fouling organisms, and is one of the important characteristics of such antifouling materials, for example, the scale-adjustable porous microstructure surface antifouling material disclosed in the Chinese patent 201110256062.5 is prepared by mixing organosilicon acrylic acid copolymer resin, amine nucleation promoter and curing agent according to the volume ratio; chinese patent 201110376218.3 discloses a method for preparing an antifouling material with a cross-shaped regular microstructure on the surface; chinese patent 200910018937.0 discloses a method for preparing a spherical protruding microstructure surface antifouling material, which is prepared by coating a film after proportionally mixing acrylate resin mixed solution hinged with organic silicon gel particles and resin with low surface energy characteristics. Since different fouling organisms differ in their structural characteristics for selective rejection (biofoulding, 2006,22:55-60), there is also a certain difficulty in achieving broad-spectrum antifouling using only microstructure design. In addition, the hydrophilicity and hydrophobicity are also important characteristics of fouling release type antifouling materials, the surface of the material with the hydrophilicity and hydrophobicity molecular structure has good antifouling performance (Langmuir,2006,22:5075-5086.), if the hydrophilicity and hydrophobicity is combined with a specially designed microstructure, the broad-spectrum antifouling performance of the material can be promoted, and how to prepare the material is the key for developing the material. Therefore, a method for preparing the hydrophilic-hydrophobic interaction distribution microstructure surface is researched and designed, the problem of combination of hydrophilicity and hydrophobicity and a microstructure is solved, the broad-spectrum antifouling performance of the microstructure material is improved, and the method has a very good application prospect.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and provides a method for preparing a hydrophilic-hydrophobic interaction distribution microstructure surface.
In order to achieve the purpose, the preparation method of the hydrophilic-hydrophobic interaction distribution microstructure surface comprises the following process steps: firstly, etching a photomask with a set pattern by using an electron beam, covering the photomask on the surface of monocrystalline silicon, etching the set pattern with a set depth on the surface of the monocrystalline silicon by using plasma, taking the etched monocrystalline silicon surface as a female die, and obtaining a hydrophobic organic silicon microstructure surface by die turnover; then, carrying out plasma activation treatment on the surface of the hydrophobic organic silicon microstructure for 5-10 minutes under a vacuum condition, then dropwise adding a hydrochloric acid hydrogen peroxide solution on the surface of the hydrophobic organic silicon microstructure, covering a layer of hydrophobic liquid, flushing the surface of the hydrophobic organic silicon microstructure with a solvent after 2-15 minutes, and drying by using nitrogen; and finally, dripping a hydrogel solution on the surface of the hydrophobic organic silicon microstructure, and curing the hydrogel solution to obtain the microstructure surface with hydrophilic and hydrophobic interaction distribution.
The plasma activation treatment conditions according to the present invention include: the voltage is 1.0-3.0V and the current is 0.4-2A.
The invention relates to a hydrochloric acid hydrogen peroxide solution which is prepared from 37 mass percent of hydrochloric acid, 30 mass percent of hydrogen peroxide and water according to the mass ratio of 1:1: 5.
The hydrophobic liquid is one or a combination of more of dimethyl silicone oil, methyl phenyl silicone oil, diesel oil, gasoline, liquid paraffin, chlorinated paraffin, vegetable oil and fluoroether oil.
The solvent is one or a combination of more of distilled water, acetone, toluene, ethanol, petroleum ether and diethyl ether.
The hydrogel solution is an aqueous solution of polyacrylamide, polyacrylic acid, agar, polyvinyl alcohol, alginic acid or sodium alginate before gelation.
The hydrophilic-hydrophobic interaction distribution microstructure surface prepared by the invention is a hydrophilic-hydrophobic interaction distribution micro-array with a regular structure, and the projection area ratio and the space area ratio of a hydrophilic-hydrophobic area in the hydrophilic-hydrophobic interaction distribution microstructure surface can be adjusted by controlling the height of hydrogel in the micro-array.
Compared with the prior art, the method has the advantages that the hydrophobic organic silicon microstructure surface with a set structure is obtained by etching and turning over the mold, the hydrogel is orderly filled in the organic silicon microstructure through the processes of plasma treatment, hydrogen peroxide activation, hydrophobic liquid hole sealing, cleaning and hydrogel perfusion, the hydrophilic-hydrophobic interaction distribution micro-array surface with a regular structure is obtained, the projection area ratio and the space area ratio of hydrophilic and hydrophobic areas are adjusted by controlling the height of the hydrogel in the micro-array, the problem of combination of the hydrophilic-hydrophobic property and the micro-structure is solved, and the broad-spectrum antifouling property of the micro-structure material is improved.
Description of the drawings:
FIG. 1 is a schematic view of the surface of a negative film of single crystal silicon prepared in example 1 of the present invention.
Fig. 2 is a schematic surface view of the hydrophilic-hydrophobic interaction distribution microstructure prepared in example 1 of the present invention.
FIG. 3 is a schematic view of the surface of the negative film of single crystal silicon prepared in example 2 of the present invention.
Fig. 4 is a schematic surface view of the hydrophilic-hydrophobic interaction distribution microstructure prepared in example 2 of the present invention.
The specific implementation mode is as follows:
the following is a further description by way of example and with reference to the accompanying drawings.
Example 1:
the method for preparing the hydrophilic-hydrophobic interaction distribution microstructure surface comprises the following process steps: firstly, etching a photomask with a set pattern by using an electron beam, covering the photomask on a monocrystalline silicon surface, etching the set pattern with the depth of 20 microns on the monocrystalline silicon surface by using plasma, taking the etched monocrystalline silicon surface as a female die, as shown in figure 1, obtaining a hydrophobic organic silicon microstructure surface by die turning, then carrying out plasma activation treatment on the hydrophobic organic silicon microstructure surface for 10 minutes under the vacuum condition by using the voltage of 1.0V and the current of 0.4A, secondly, dropwise adding a hydrogen peroxide solution on the hydrophobic organic silicon microstructure surface, covering a layer of dimethyl silicone oil, washing the hydrophobic organic silicon microstructure surface by using distilled water and drying the hydrophobic organic silicon microstructure surface by using nitrogen after 15 minutes, finally, dropwise adding a polyacrylamide hydrogel solution on the hydrophobic organic silicon microstructure surface, and obtaining a hydrophilic-hydrophobic interaction distribution microstructure surface as shown in figure 2 after the polyacrylamide hydrogel solution is solidified, wherein the cylinder is made of hydrophobic organic silicon material, the rest parts are made of hydrophilic polyacrylamide hydrogel material, and the height difference between the surface of the polyacrylamide hydrogel and the upper end face of the organic silicon cylinder is 5 micrometers.
Example 2:
the method for preparing the hydrophilic-hydrophobic interaction distribution microstructure surface comprises the following process steps: firstly, etching a photomask with a set pattern by using an electron beam, covering the photomask on the surface of monocrystalline silicon, etching a set pattern with the depth of 20 microns on the surface of the monocrystalline silicon by using plasma, taking the etched monocrystalline silicon surface as a female die, obtaining a hydrophobic organic silicon microstructure surface by turning over the die as shown in figure 3, then carrying out plasma activation treatment on the hydrophobic organic silicon microstructure surface for 5 minutes under the vacuum condition by using the voltage of 3.0V and the current of 2.0A, secondly, dropwise adding a hydrochloric acid hydrogen peroxide solution on the hydrophobic organic silicon microstructure surface, covering a layer of liquid paraffin, after 5 minutes, washing the hydrophobic organic silicon microstructure surface by using a mixed solution formed by mixing diethyl ether and petroleum ether with the volume ratio of 1:1, blowing the hydrophobic organic silicon microstructure surface by using nitrogen for drying, finally, dropwise adding a polyacrylic hydrogel solution on the hydrophobic organic silicon microstructure surface, and after the polyacrylic hydrogel solution is cured, and obtaining the hydrophilic-hydrophobic interaction distribution microstructure surface shown in fig. 4, wherein the cylinder is a hydrophobic organosilicon material, the rest parts are hydrophilic polyacrylic acid hydrogel materials, and the height difference between the polyacrylic acid hydrogel surface and the upper end surface of the organosilicon cylinder is 11 micrometers.
Example 3:
the method for preparing the hydrophilic-hydrophobic interaction distribution microstructure surface comprises the following process steps: firstly, etching a photomask with a set pattern by using an electron beam, covering the photomask on the surface of monocrystalline silicon, etching the set pattern with the depth of 10 microns on the surface of the monocrystalline silicon by using plasma, taking the etched monocrystalline silicon surface as a female die, obtaining a hydrophobic organic silicon microstructure surface by turning over the die, then carrying out plasma activation treatment on the hydrophobic organic silicon microstructure surface for 8 minutes under the vacuum condition by using the voltage of 2.0V and the current of 1.0A, secondly, dropwise adding a hydrogen peroxide solution hydrochloride on the hydrophobic organic silicon microstructure surface, covering a layer of mixed liquid formed by mixing dimethyl silicone oil and methyl phenyl silicone oil with the volume ratio of 1:1, flushing the hydrophobic organic silicon microstructure surface by using toluene and drying the hydrophobic organic silicon microstructure surface by using nitrogen after 2 minutes, finally, dropwise adding a polyvinyl alcohol hydrogel solution on the hydrophobic organic silicon microstructure surface, and after the polyvinyl alcohol hydrogel solution is cured, and (3) obtaining a hydrophilic-hydrophobic interaction distribution microstructure surface, wherein the surface of the polyvinyl alcohol hydrogel and the upper end surface of the organic silicon cylinder are in the same plane.
Claims (6)
1. A method for preparing a hydrophilic-hydrophobic interaction distribution microstructure surface is characterized by comprising the following technological processes: firstly, etching a photomask with a set pattern by using an electron beam, covering the photomask on the surface of monocrystalline silicon, etching a cylindrical pattern with the depth of 10 microns or 20 microns on the surface of the monocrystalline silicon by using plasma, taking the etched monocrystalline silicon surface as a female die, and obtaining a hydrophobic organic silicon microstructure surface by die turnover; then, carrying out plasma activation treatment on the surface of the hydrophobic organic silicon microstructure for 5-10 minutes under a vacuum condition, then dropwise adding a hydrochloric acid hydrogen peroxide solution on the surface of the hydrophobic organic silicon microstructure, covering a layer of hydrophobic liquid, flushing the surface of the hydrophobic organic silicon microstructure with a solvent after 2-15 minutes, and drying by using nitrogen; finally, dripping a hydrogel solution on the surface of the hydrophobic organic silicon microstructure, and obtaining a microstructure surface with hydrophilic and hydrophobic interaction distribution after the hydrogel solution is solidified; the hydrogel solution is an aqueous solution of polyacrylamide, polyacrylic acid, agar, polyvinyl alcohol, alginic acid or sodium alginate before gelation.
2. The method for preparing the hydrophilic-hydrophobic interactive distribution microstructure surface according to claim 1, wherein the plasma activation treatment conditions include: the voltage is 1.0-3.0V and the current is 0.4-2A.
3. The method for preparing the hydrophilic-hydrophobic interaction distribution microstructure surface according to claim 1, wherein the hydrochloric acid hydrogen peroxide solution is prepared from hydrochloric acid with a mass percentage concentration of 37%, hydrogen peroxide with a mass percentage concentration of 30% and water according to a mass ratio of 1:1: 5.
4. The method for preparing the surface of the hydrophilic-hydrophobic interaction distribution microstructure according to claim 1, wherein the hydrophobic liquid is one or a combination of several of simethicone, methyl phenyl silicone oil, diesel oil, gasoline, liquid paraffin, chlorinated paraffin, vegetable oil and fluoroether oil.
5. The method for preparing the hydrophilic-hydrophobic interaction distribution microstructure surface according to claim 1, wherein the solvent is one or more of distilled water, acetone, toluene, ethanol, petroleum ether and diethyl ether.
6. The method for preparing the hydrophilic-hydrophobic interaction distribution microstructure surface according to claim 1, wherein the prepared hydrophilic-hydrophobic interaction distribution microstructure surface is a hydrophilic-hydrophobic interaction distribution micro-array with a regular structure.
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| CN113985505A (en) * | 2021-10-21 | 2022-01-28 | 浙江大学 | Method for preparing micro-lens array based on hydrogel microstructure template |
| CN115044086B (en) * | 2022-07-12 | 2023-08-22 | 哈尔滨工程大学 | Polylysine-polyvinyl alcohol hydrogel bionic antifouling material and preparation method thereof |
| CN115287889A (en) * | 2022-07-15 | 2022-11-04 | 华电宁德电力开发有限公司 | UHMWPE antifouling material and preparation method thereof |
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