CN112793288A - Preparation method of shape memory micro-pattern with bidirectional reversible wetting - Google Patents
Preparation method of shape memory micro-pattern with bidirectional reversible wetting Download PDFInfo
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- CN112793288A CN112793288A CN202110048281.8A CN202110048281A CN112793288A CN 112793288 A CN112793288 A CN 112793288A CN 202110048281 A CN202110048281 A CN 202110048281A CN 112793288 A CN112793288 A CN 112793288A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/162—Cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/14—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers
- B32B37/24—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the properties of the layers with at least one layer not being coherent before laminating, e.g. made up from granular material sprinkled onto a substrate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/164—Drying
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B2038/0052—Other operations not otherwise provided for
- B32B2038/0076—Curing, vulcanising, cross-linking
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B38/00—Ancillary operations in connection with laminating processes
- B32B38/16—Drying; Softening; Cleaning
- B32B38/164—Drying
- B32B2038/168—Removing solvent
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- Exposure Of Semiconductors, Excluding Electron Or Ion Beam Exposure (AREA)
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Abstract
The invention discloses a preparation method of a shape memory micro-pattern with bidirectional reversible wetting, belonging to the technical field of polymer science. Mixing the shape memory polymer and the stimulus response substance, then adding toluene, and uniformly stirring; after drying, removing residual toluene, and cutting the obtained product for later use; fixing the cleaned silicon wafer on a hot-pressing die, uniformly spreading the dried matrix material on the silicon wafer, and curing for 1-3h at the temperature of 100-; and stripping the cured bidirectional reversible wetting microarray at 50-80 ℃ to obtain the shape memory micropattern with the bidirectional reversible wetting property. The micro pattern with reversible wettability prepared by the invention has a bidirectional reversible recovery function under no stress, can realize reversible transformation of an upright/toppling state of the micro array pattern through heating/cooling circulation, realizes controllability of a surface wetting state, and is a good method for preparing the micro pattern with reversible wettability.
Description
Technical Field
The invention relates to a preparation method of a shape memory micro-pattern with bidirectional reversible wetting, belonging to the technical field of polymer science.
Background
The shape memory polymer has wide application in the fields of aerospace, textile industry, optics, biomedicine, microelectronics and the like, and the shape memory micro-pattern combines a micro-patterning technology with the shape memory polymer, expands a macroscopic shape memory effect to the microscopic field, and changes surface properties (such as surface adhesion, surface wettability and the like) through adjustment of the microscopic field, so that the shape memory micro-pattern has great application potential in the directions of anti-icing surfaces, intelligent adhesives, micro-optical devices and the like. However, the shape recovery of the existing shape memory micro-patterns is mostly one-way recovery, so that the application of the materials has great limitation.
The preparation of the shape memory micro-pattern with the bidirectional reversible wettability is very meaningful, and the shape memory micro-pattern with the bidirectional reversible wettability has very wide application potential. Compared with the traditional one-way shape memory micro-pattern, the shape memory micro-pattern with two-way reversible wetting has excellent recovery controllability. This makes the micropattern applicable in the field of droplet storage and the like.
Disclosure of Invention
In order to solve the above problems, the present invention provides a method for preparing a shape memory micro pattern having bidirectional reversible wetting. The shape memory micro-pattern prepared by the invention has a bidirectional shape memory function, and the recovery of the micro-array pattern has the characteristic of controllability. The characteristics of the micro-array pattern which are recovered at different temperatures are different, and the method is a good method for preparing the shape memory micro-pattern with the bidirectional reversible wetting function.
The invention firstly provides a preparation method of a shape memory micro-pattern with bidirectional reversible wetting, which comprises the following steps:
step (1): cleaning the surface of the silicon wafer to remove impurities on the surface;
step (2): mixing the shape memory polymer and the stimulus response substance according to the ratio of 100: (1-5), then adding the mixture into toluene, and uniformly stirring to uniformly disperse the stimulus response substance in the shape memory polymer matrix;
and (3): drying the mixed solution prepared in the step (2) at 10-30 ℃, removing residual toluene, and cutting the obtained product for later use;
and (4): fixing the silicon wafer obtained in the step (1) on a hot-pressing die, uniformly paving the dried base material obtained in the step (3) on the silicon wafer, and curing for 1-3h at the temperature of 100-;
and (5): and taking out the cured bidirectional reversible wetting microarray from the hot-pressing mold at 50-80 ℃ and stripping to obtain the shape memory micropattern with the bidirectional reversible wetting property.
In one embodiment of the present invention, in step (1), the surface of the silicon wafer is preferably cleaned with alcohol and deionized water.
In one embodiment of the invention, the shape memory polymer is a thermotropic shape memory polymer.
In one embodiment of the present invention, the shape memory polymer is preferably Ethylene Vinyl Acetate (EVA).
In one embodiment of the invention, the stimuli-responsive substance comprises one or both of Benzoyl Peroxide (BPO), dicumyl peroxide (DCP).
In one embodiment of the present invention, in the step (4), the toluene is removed by heating in a vacuum drying oven.
The invention also provides the application of the method in the fields of aerospace, textile industry, liquid drop storage, optics, biomedicine and microelectronics.
The invention also provides the shape memory micropattern with bidirectional reversible wetting prepared by the method.
Has the advantages that:
the shape memory polymer is excellent in performance, the shape memory micro-pattern prepared by taking the shape memory polymer as a matrix has a bidirectional shape memory function, and the recovery of the micro-array pattern has the characteristic of controllability. The preparation method can obtain the inclined microarray pattern by pressing the surface micro-column array, the microarray can be reversibly switched between an upright state and an inclined state along with the change of temperature without external stress, the preparation process is simple, the operability is strong, and the preparation method is favorable for the application of the shape memory polymer material in various fields of aerospace, liquid drop storage, textile industry and the like.
Drawings
FIG. 1 is a schematic diagram of a method for preparing a shape memory micro-pattern with reversible wetting in two directions according to the present invention.
FIG. 2 is a microarray silicon wafer of three different patterns.
FIG. 3 is a schematic diagram of the two-way shape memory effect of a two-way reversible wetting microarray pattern.
FIG. 4 the resulting two-way reversible wetting microarray pattern prepared in example 1.
FIG. 5 the resulting two-way reversible wetting microarray pattern prepared in comparative example 1.
FIG. 6 deformation results at 70 ℃ of the bidirectional reversible wetting microarray pattern prepared in comparative example 1.
Detailed Description
The present invention is further described below with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
A preparation method of a shape memory micro-pattern with bidirectional reversible wetting is disclosed, FIG. 1 is a schematic diagram of the preparation method of the shape memory micro-pattern with bidirectional reversible wetting, and the preparation process comprises the following steps:
step (1): classifying the silicon wafers with three different patterns, and cleaning the surfaces of the silicon wafers by using alcohol and deionized water to remove impurities on the surfaces;
step (2): mixing a shape memory polymer ethylene-vinyl acetate copolymer (EVA) and a stimulus response substance dicumyl peroxide (DCP) according to the ratio of 100: 3, then adding a toluene solvent for dissolving, and uniformly stirring to uniformly disperse the stimulus response substance in the matrix;
and (3): drying the mixed solution at room temperature, placing the mixed solution in a vacuum drying oven to remove the residual toluene, and shearing the mixed solution for later use;
and (4): fixing a silicon wafer on a hot-pressing die, uniformly paving the dried matrix material on the silicon wafer, and curing for 3 hours at the temperature of 150 ℃;
and (5): and taking the cured bidirectional reversible wetting microarray out of the hot-pressing mold at 60 ℃ to obtain the shape memory micropattern with the bidirectional reversible wetting property.
FIG. 2 shows the prepared microarray silicon wafer with three different patterns. Fig. 3 is a schematic diagram of the two-way shape memory effect of the two-way reversible wetting microarray pattern, fig. 4 is a schematic diagram of a product of the two-way reversible wetting microarray pattern prepared by changing the temperature of the two-way shape memory polymer between 20 ℃ and 70 ℃, the surface of the two-way reversible wetting microarray pattern is transformed from a completely inclined state to an upright state, and the wettability of the surface is changed along with the change of the temperature, and the change from hydrophilicity (contact angle at 20 ℃ is 73 ℃) to hydrophobicity (contact angle at 70 ℃ is 125 ℃) is displayed.
Example 2
A preparation method of a shape memory micro-pattern with bidirectional reversible wetting is disclosed, FIG. 1 is a schematic diagram of the preparation method of the shape memory micro-pattern with bidirectional reversible wetting, and the preparation process comprises the following steps:
step (1): classifying the silicon wafers with three different patterns, and cleaning the surfaces of the silicon wafers by using alcohol and deionized water to remove impurities on the surfaces;
step (2): shape memory polymer Ethylene Vinyl Acetate (EVA) and stimulus responsive material Benzoyl Peroxide (BPO) were mixed according to a 100: 4, then adding a toluene solvent for dissolving, and uniformly stirring to uniformly disperse the stimulus response substance in the matrix;
and (3): drying the mixed solution at room temperature, placing the mixed solution in a vacuum drying oven to remove the residual toluene, and shearing the mixed solution for later use;
and (4): fixing the silicon wafer on a hot-pressing die, uniformly paving the dried matrix material on the silicon wafer, and curing for 1.25h at 125 ℃;
and (5): and taking the cured bidirectional reversible wetting microarray out of the hot-pressing mold at 80 ℃ to obtain the shape memory micropattern with the bidirectional reversible wetting property.
The prepared two-way shape memory polymer can be transformed from a completely inclined state to an upright state through the temperature change between 20 ℃ and 70 ℃, the surface wettability is changed along with the change of the temperature change, and the transition from hydrophilicity (the contact angle is 70 ℃ at 20 ℃) to hydrophobicity (the contact angle is 125 ℃ at 70 ℃) is displayed.
Comparative example 1
When the peeling temperature in step 5 was room temperature (25 ℃), the surface micro pattern prepared according to the remaining process steps was deformed, as shown in fig. 5, and the shape memory effect (see fig. 6) and the wettability of the pattern were deteriorated.
Although the present invention has been described with reference to the preferred embodiments, it should be understood that various changes and modifications can be made therein by those skilled in the art without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (9)
1. A method of making a shape memory micropattern with bi-directional reversible wetting, the method comprising the steps of:
step (1): cleaning the surface of the silicon wafer to remove impurities on the surface;
step (2): mixing the shape memory polymer and the stimulus response substance according to the ratio of 100: (1-5), then adding the mixture into toluene, and uniformly stirring to uniformly disperse the stimulus response substance in the shape memory polymer matrix;
and (3): drying the mixed solution prepared in the step (2) at 10-30 ℃, removing residual toluene, and cutting the obtained product for later use;
and (4): fixing the silicon wafer obtained in the step (1) on a hot-pressing die, uniformly paving the dried base material obtained in the step (3) on the silicon wafer, and curing for 1-3h at the temperature of 100-;
and (5): and taking out the cured bidirectional reversible wetting microarray from the hot-pressing mold at 50-80 ℃ and stripping to obtain the shape memory micropattern with the bidirectional reversible wetting property.
2. The production method according to claim 1, wherein in the step (1), the surface of the silicon wafer is cleaned with alcohol and water.
3. The method of claim 1 or 2, wherein the shape memory polymer is a thermotropic shape memory polymer.
4. The method according to any one of claims 1 to 3, wherein the shape memory polymer is an ethylene-vinyl acetate copolymer.
5. The method according to any one of claims 1 to 4, wherein the stimuli-responsive substance comprises one or both of benzoyl peroxide and dicumyl peroxide.
6. The production method according to any one of claims 1 to 5, wherein in the step (4), the toluene is removed by heating in a vacuum drying oven.
7. Use of the preparation process according to any one of claims 1 to 6 in the fields of aerospace, textile industry, droplet storage, optics, biomedicine, microelectronics.
8. The shape memory micropattern with bidirectional reversible wetting prepared by the preparation method according to any one of claims 1 to 6.
9. Micro-optics or smart adhesives comprising the shape memory micro-pattern with two-way reversible wetting of claim 8.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115195241A (en) * | 2022-07-27 | 2022-10-18 | 哈尔滨工程大学 | In-situ wettability conversion structure, preparation method thereof and liquid drop dynamic control platform prepared by same |
Citations (2)
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|---|---|---|---|---|
| CN104891426A (en) * | 2015-04-07 | 2015-09-09 | 哈尔滨工业大学 | Preparation method for micropattern film with selective stimulation recovery function |
| CN106082111A (en) * | 2016-06-16 | 2016-11-09 | 哈尔滨工业大学 | A kind of isotropism and the preparation method of the changeable super hydrophobic surface of anisotropic |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104891426A (en) * | 2015-04-07 | 2015-09-09 | 哈尔滨工业大学 | Preparation method for micropattern film with selective stimulation recovery function |
| CN106082111A (en) * | 2016-06-16 | 2016-11-09 | 哈尔滨工业大学 | A kind of isotropism and the preparation method of the changeable super hydrophobic surface of anisotropic |
Non-Patent Citations (2)
| Title |
|---|
| JUAN WANG,ET,AL.: "《Tunable shape memory polymer mold for multiple microarray replications》", 《JOURNAL OF MATERIAL CHEMISTRY A》 * |
| 李文兵: "《多刺激相应形状记忆聚合物复合材料的性能研究》", 《中国博士学位论文全文数据库工程科技Ⅰ辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115195241A (en) * | 2022-07-27 | 2022-10-18 | 哈尔滨工程大学 | In-situ wettability conversion structure, preparation method thereof and liquid drop dynamic control platform prepared by same |
| CN115195241B (en) * | 2022-07-27 | 2023-12-12 | 哈尔滨工程大学 | In-situ wettability conversion structure, preparation method thereof and liquid drop dynamic control platform prepared by same |
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