CN110628068A - Method for preparing surface pattern structure with magnetic response - Google Patents
Method for preparing surface pattern structure with magnetic response Download PDFInfo
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- CN110628068A CN110628068A CN201910944572.8A CN201910944572A CN110628068A CN 110628068 A CN110628068 A CN 110628068A CN 201910944572 A CN201910944572 A CN 201910944572A CN 110628068 A CN110628068 A CN 110628068A
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- pdms
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2425/00—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 at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2425/02—Homopolymers or copolymers of hydrocarbons
- C08J2425/04—Homopolymers or copolymers of styrene
- C08J2425/06—Polystyrene
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2275—Ferroso-ferric oxide (Fe3O4)
Abstract
The invention discloses a method for preparing a magnetic response surface pattern structure, which comprises the steps of firstly, mixing a prepolymer with magnetic Fe3O4Mixing and stirring, heating and curing to obtain a magnetic PDMS elastic substrate, dissolving PS in tetrahydrofuran solution, and spin-coating to form a film on the magnetic PDMS elastic substrate to obtain the polystyrene film/PDMS double-layer system. In the preparation process of the invention, the elastic modulus and Fe of PDMS are changed3O4The content of (3) controls the magnetic response degree, and the thickness of the film is controlled by the content of PS in the organic solvent, so that the period and the amplitude of the surface pattern are controlled. The invention avoids complex and fussy operation steps, longer preparation time and high equipment and experimental consumable loss, has the characteristics of simplicity, rapidness, good repeatability and the like, and can drain the water on the surface of the material and the structure of the microcircuitHas potential application prospect in the fields of construction and the like.
Description
Technical Field
The invention relates to the technical field of preparation of soft magnetic elastomers.
Background
The combination of polymers with nano-or fine solid materials shows new, often enhanced, properties compared to traditional materials. They open up possibilities for the application of new technologies. Materials whose physical properties change with the application of a magnetic field belong to a special class of smart materials. The magnetic field controllable soft material comprises ferrofluid, magnetorheological fluid, magnetic gel and magnetic elastomer. Magnetic gels and elastomers (magnetoelastomers) are a new class of composite materials consisting of small magnetic particles in the nanometer to micrometer range dispersed in a highly elastic polymer matrix. Thin film materials with surface patterning have attracted much attention and are also widely used in human life, such as superhydrophobic materials and flexible electronic devices. Patterning on soft magnetic elastomer materials is also a trend and hot spot for future technology development.
Disclosure of Invention
In view of the above prior art, the present invention provides a method for preparing a magnetic-responsive surface pattern structure. In the preparation process, the elastic modulus and Fe of PDMS are changed3O4The content of (3) controls the magnetic response degree, and the thickness of the film is controlled by the content of PS in the organic solvent, so that the period and the amplitude of the surface pattern are controlled. The method avoids complicated operation steps, long preparation time and high equipment and experimental consumable loss, and is simple and efficient.
In order to solve the technical problem, the invention provides a method for preparing a pattern structure with a magnetic response surface, which comprises the following steps:
step one, mixing a PDMS prepolymer and a cross-linking agent according to a mass ratio of 5-20: 1, pouring the mixture into a centrifugal tube, and adding Fe3O4Wherein, Fe3O4The mass fraction of the mixture is 30-50%, and a glass rod is used for stirring to form a uniform mixture;
step two, mixing PDMS prepolymer, cross-linking agent and Fe3O4The mixture is subjected to vacuum degassing treatment for 1h, poured into a culture dish and uniformly distributed in the culture dish;
step three, pouring the prepolymer, the cross-linking agent and Fe into a culture dish3O4The mixture is subjected to vacuum degassing treatment for 30min, and then is placed into an oven to be heated and cured for 2h at the temperature of 80 ℃; obtaining a magnetic PDMS elastomer;
step four, preparing a polystyrene tetrahydrofuran solution with the mass fraction of 2-5%, and ultrasonically mixing uniformly;
step five, spin-coating the polystyrene tetrahydrofuran solution prepared in the step four on the surface of the magnetic PDMS elastomer, wherein the spin-coating amount is per cm2Spin coating 3 μ L meter;
seventhly, thermally expanding and wrinkling for 2 hours at 80 ℃;
and step eight, air cooling to normal temperature to obtain the polystyrene film/PDMS double-layer system.
Further, the preparation method of the invention adjusts the mass ratio of PDMS to the cross-linking agent and Fe in the first step3O4And the mass fraction of the polystyrene tetrahydrofuran solution in the fourth step, thereby obtaining PS films with different surface morphologies.
In the first step, the mass ratio of the PDMS prepolymer to the cross-linking agent is 5:1, and Fe is contained in the mixture3O4The mass fraction of (A) is 50%; in the fourth step, the prepared mass fraction of the polystyrene tetrahydrofuran solution is 2%.
In the first step, the mass ratio of the PDMS prepolymer to the cross-linking agent is 5:1, and Fe is contained in the mixture3O4The mass fraction of (A) is 50%; in the fourth step, the prepared mass fraction of the polystyrene tetrahydrofuran solution is 5%.
In the first step, the mass ratio of the PDMS prepolymer to the cross-linking agent is 20:1, and Fe is contained in the mixture3O4The mass fraction of (A) is 30%; in the fourth step, the prepared mass fraction of the polystyrene tetrahydrofuran solution is 2%.
In the first step, the mass ratio of the PDMS prepolymer to the cross-linking agent is 20:1, and Fe is contained in the mixture3O4The mass fraction of (A) is 30%; in the fourth step, the prepared mass fraction of the polystyrene tetrahydrofuran solution is 5%.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a method for preparing a free polymer film material with a patterned surface on a soft magnetic elastomer in a short time, and the method can be used for preparing films with different surface morphologies by simply controlling the mass ratio and the content of magnetic particles, has the characteristics of simplicity, rapidness, good repeatability and the like, avoids the defects of complex preparation process, expensive equipment, low efficiency and the like, and has potential application prospects in the fields of surface hydrophobic materials, micro-circuit construction and the like.
Drawings
FIG. 1 is a stereomicroscope photograph of the product obtained in example 1 of the present invention;
FIG. 2 is a stereomicroscope photograph of the product obtained in example 2 of the present invention;
FIG. 3 is a stereomicroscope photograph of the product obtained in example 3 of the present invention;
FIG. 4 is a stereomicroscope photograph of the product obtained in example 4 of the present invention.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, which are not intended to limit the invention in any way.
Example 1:
a method of making a structure having a magnetically responsive surface pattern, comprising the steps of:
the method comprises the following steps: mixing the PDMS prepolymer with a cross-linking agent according to the weight ratio of 5:1, pouring the mixture into a centrifuge tube, and adding Fe3O4Wherein, Fe3O4The mass fraction of the mixture is 50 percent, and a glass rod is used for stirring to form a uniform mixture;
step two: PDMS prepolymer, cross-linking agent and Fe3O4The mixture is subjected to vacuum degassing treatment for 1h, poured into a square culture dish and uniformly distributed in the culture dish;
step three: pouring the prepolymer, the cross-linking agent and Fe into a culture dish3O4The mixture is subjected to vacuum degassing treatment for 30min, and then is placed into an oven, and is heated and cured for 2h at the temperature of 80 ℃ to obtain a magnetic PDMS elastomer, wherein the elastic modulus of the magnetic PDMS elastomer is 1.8 MPa;
step four: dissolving 0.04g of polystyrene monomer in 2g of tetrahydrofuran, and ultrasonically mixing uniformly to obtain a polystyrene tetrahydrofuran solution with the mass fraction of 2%;
step five: cutting a 1cm multiplied by 1cm magnetic PDMS system;
step six: spin coating the 2% polystyrene tetrahydrofuran solution prepared in the fourth step on the surface of the 1cm × 1cm magnetic PDMS elastomer;
step seven: thermally expanding and wrinkling for 2 hours at 80 ℃; air-cooling to normal temperature to obtain the polystyrene film/PDMS two-layer system shown in FIG. 1.
Example 2:
example 2 is different from example 1 only in that the amount of the polystyrene monomer in the fourth step is changed from 0.04g to 0.1g, the mass fraction of the obtained tetrahydrofuran solution is 5%, and the finally obtained polystyrene film/PDMS bilayer system is shown in FIG. 2.
Example 3:
a method for preparing a pattern structure having a magnetically responsive surface, example 2 differing from example 1 only by:
in the first step, the mass ratio of the PDMS prepolymer to the cross-linking agent is changed from 5:1 to 20:1, and Fe in the mixture3O4The mass fraction of (A) is changed from 50% to 30%; the elastic modulus of the intermediate product magnetic PDMS elastomer is 0.4 MPa; the final polystyrene film/PDMS bilayer system is shown in FIG. 3.
Example 4:
a method for preparing a pattern structure having a magnetically responsive surface, example 2 differing from example 1 only by:
in the first step, the mass ratio of the PDMS prepolymer to the cross-linking agent is changed from 5:1 to 20:1, and Fe in the mixture3O4The mass fraction of (A) is changed from 50% to 30%; the elastic modulus of the intermediate product magnetic PDMS elastomer is 0.4 MPa; in the fourth step, the amount of the polystyrene monomer is changed from 0.04g to 0.1g, and the mass fraction of the obtained tetrahydrofuran solution is 5 percent; the final polystyrene film/PDMS bilayer system is shown in FIG. 4.
In conclusion, the method mainly comprises the steps of spin-coating a PS solution on a magnetic PDMS substrate to form a PS film, and changing the modulus of a PDMS elastomer by using magnetic nanoparticles to finally obtain films with different appearances. And films with different morphologies are obtained by adjusting the mass ratio of the prepolymer to the cross-linking agent and the content of the magnetic particles. As can be seen from fig. 1 to 4, the patterned degree of the PDMS surfaces with different magnetism is observed under a stereomicroscope, the PDMS elastomer is soft, and the wrinkle period of the PS film is long; the PS solution has high mass fraction, thick PS film and long wrinkle period.
While the present invention has been described with reference to the accompanying drawings, the present invention is not limited to the above-described embodiments, which are illustrative only and not restrictive, and various modifications which do not depart from the spirit of the present invention and which are intended to be covered by the claims of the present invention may be made by those skilled in the art.
Claims (6)
1. A method of making a patterned structure having a magnetically responsive surface, comprising the steps of:
step one, mixing a PDMS prepolymer and a cross-linking agent according to a mass ratio of 5-20: 1, pouring the mixture into a centrifugal tube, and adding Fe3O4Wherein, Fe3O4The mass fraction of the mixture is 30-50%, and a glass rod is used for stirring to form a uniform mixture;
step two, mixing PDMS prepolymer, cross-linking agent and Fe3O4The mixture is subjected to vacuum degassing treatment for 1h, poured into a culture dish and uniformly distributed in the culture dish;
step three, pouring the prepolymer, the cross-linking agent and Fe into a culture dish3O4The mixture is subjected to vacuum degassing treatment for 30min, and then is placed into an oven to be heated and cured for 2h at the temperature of 80 ℃; obtaining a magnetic PDMS elastomer;
step four, preparing a polystyrene tetrahydrofuran solution with the mass fraction of 2-5%, and ultrasonically mixing uniformly;
step five, spin-coating the polystyrene tetrahydrofuran solution prepared in the step four on the surface of the magnetic PDMS elastomer, wherein the spin-coating amount is per cm2Spin coating 3 μ L meter;
seventhly, thermally expanding and wrinkling for 2 hours at 80 ℃;
and step eight, air cooling to normal temperature to obtain the polystyrene film/PDMS double-layer system.
2. The method for preparing a structure having a magnetically-responsive surface pattern according to claim 1, wherein the mass ratio of PDMS to the cross-linking agent and Fe in the first step are adjusted3O4And the mass fraction of the polystyrene tetrahydrofuran solution in the fourth step, thereby obtaining PS films with different surface morphologies.
3. The method for preparing a structure with a pattern on a magnetically responsive surface as claimed in claim 2, wherein in the step one, the mass ratio of the PDMS prepolymer to the cross-linking agent is 5:1, and Fe is contained in the mixture3O4The mass fraction of (A) is 50%; in the fourth step, the prepared mass fraction of the polystyrene tetrahydrofuran solution is 2%.
4. The method for preparing a structure with a pattern on a magnetically responsive surface as claimed in claim 2, wherein in the step one, the mass ratio of the PDMS prepolymer to the cross-linking agent is 5:1, and Fe is contained in the mixture3O4The mass fraction of (A) is 50%; in the fourth step, the prepared mass fraction of the polystyrene tetrahydrofuran solution is 5%.
5. The method for preparing a magnetic response surface pattern structure as claimed in claim 2, wherein in the step one, the mass ratio of the PDMS prepolymer to the cross-linking agent is 20:1, and Fe is contained in the mixture3O4The mass fraction of (A) is 30%; in the fourth step, the prepared mass fraction of the polystyrene tetrahydrofuran solution is 2%.
6. The method for preparing a magnetic response surface pattern structure as claimed in claim 2, wherein in the step one, the mass ratio of the PDMS prepolymer to the cross-linking agent is 20:1, and Fe is contained in the mixture3O4The mass fraction of (A) is 30%; in the fourth step, the prepared mass fraction of the polystyrene tetrahydrofuran solution is 5%.
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| CN201910944572.8A CN110628068A (en) | 2019-09-30 | 2019-09-30 | Method for preparing surface pattern structure with magnetic response |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112489853A (en) * | 2020-11-25 | 2021-03-12 | 北京石墨烯研究院 | Flexible conductive film, preparation method thereof and flexible electronic device |
| CN113817320A (en) * | 2021-08-13 | 2021-12-21 | 广东省科学院健康医学研究所 | Magnetic response elastomer and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212180A (en) * | 2014-09-19 | 2014-12-17 | 大连海事大学 | Polydimethylsiloxane with magnetism and preparation method thereof |
| US20170217082A1 (en) * | 2016-02-02 | 2017-08-03 | Sourabh Kumar Saha | Method to suppress period doubling during manufacture of micro and nano scale wrinkled structures |
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2019
- 2019-09-30 CN CN201910944572.8A patent/CN110628068A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104212180A (en) * | 2014-09-19 | 2014-12-17 | 大连海事大学 | Polydimethylsiloxane with magnetism and preparation method thereof |
| US20170217082A1 (en) * | 2016-02-02 | 2017-08-03 | Sourabh Kumar Saha | Method to suppress period doubling during manufacture of micro and nano scale wrinkled structures |
Non-Patent Citations (1)
| Title |
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| DONG CHOON HYUN等: ""Substrate Thickness: An Effective Control Parameter for Polymer Thin Film Buckling on PDMS Substrates"", 《JOURNAL OF APPLIED POLYMER SCIENCE》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112489853A (en) * | 2020-11-25 | 2021-03-12 | 北京石墨烯研究院 | Flexible conductive film, preparation method thereof and flexible electronic device |
| CN112489853B (en) * | 2020-11-25 | 2022-11-22 | 北京石墨烯研究院 | Flexible conductive film, preparation method thereof and flexible electronic device |
| CN113817320A (en) * | 2021-08-13 | 2021-12-21 | 广东省科学院健康医学研究所 | Magnetic response elastomer and preparation method and application thereof |
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Application publication date: 20191231 |