CN110734037B - Method for constructing surface fold structure of high polymer material - Google Patents
Method for constructing surface fold structure of high polymer material Download PDFInfo
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- CN110734037B CN110734037B CN201911024823.7A CN201911024823A CN110734037B CN 110734037 B CN110734037 B CN 110734037B CN 201911024823 A CN201911024823 A CN 201911024823A CN 110734037 B CN110734037 B CN 110734037B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00023—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems without movable or flexible elements
- B81C1/00126—Static structures not provided for in groups B81C1/00031 - B81C1/00119
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00015—Manufacture or treatment of devices or systems in or on a substrate for manufacturing microsystems
- B81C1/00206—Processes for functionalising a surface, e.g. provide the surface with specific mechanical, chemical or biological properties
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B81—MICROSTRUCTURAL TECHNOLOGY
- B81C—PROCESSES OR APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OR TREATMENT OF MICROSTRUCTURAL DEVICES OR SYSTEMS
- B81C1/00—Manufacture or treatment of devices or systems in or on a substrate
- B81C1/00436—Shaping materials, i.e. techniques for structuring the substrate or the layers on the substrate
- B81C1/00444—Surface micromachining, i.e. structuring layers on the substrate
Abstract
The invention discloses a method for constructing a high polymer material surface fold structure, and relates to a method for constructing a high polymer material surface fold structure. The invention aims to solve the problems of complex method and thin surface layer thickness of the existing method for constructing the folded structure, and the method comprises the following steps: 1. pre-cleaning the base material; 2. carrying out irradiation treatment on the matrix by using heavy ions, electrons or protons; 3. and (3) carrying out heat treatment on the irradiated matrix material, then placing the matrix material in air for cooling, and constructing a wrinkle structure on the surface of the matrix, thus completing the preparation. The invention realizes the precise regulation and control of the fold wavelength and the amplitude by controlling the irradiation energy, the flux, the fluence, the heat treatment temperature and the time, and the thickness of the surface layer can be adjusted from nano-scale to millimeter-scale. The invention is applied to the field of construction of surface micro-nano structures.
Description
Technical Field
The invention relates to a method for constructing a high polymer material surface fold structure.
Background
The method has the advantages that micro-nano-scale folds can be constructed on the surface of the material in a controllable manner, particularly, the biomimetic preparation of a polymer material surface microstructure is significant in the fields of optical regulation, intelligent sensors, surface-enhanced Raman scattering, fluorescence enhancement effect, micro-nano robots, surface wettability, fog prevention, ice removal and surface dust prevention, and is an important research direction in the field of nanotechnology.
At present, the scheme for constructing the wrinkled microstructure on the surface of the high polymer material mainly comprises the following steps: (1) Depositing a surface layer on the surface of a substrate to form the fold construction of a surface layer/substrate double-layer system: depositing gold, silver, graphene and silicon oxide on the surface of a substrate to form a bilayer system, and generatingThe stress mismatch builds a corrugated structure. The scheme forms a new surface layer on the surface of the substrate, and the surface layer is usually a hard layer, so that the functional use of the substrate is limited; (2) fold formation on a heterogeneous graded matrix: the proposal has higher requirements on the matrix and has great limitations in practical application; (3) wrinkle construction on a homogeneous matrix: the scheme can maintain the functional characteristics of the matrix to the maximum extent. At present, the surface wrinkle construction method based on homogeneous and uniform matrix mainly comprises reactive plasma etching (RIE) and ultraviolet/O 3 Irradiation and laser irradiation, which generally have the defects of complex preparation scheme, thin surface layer thickness, most micro-nano, difficulty in realizing large-area preparation and high cost. Therefore, the method has important significance in developing a surface fold construction scheme which is widely applicable to various matrixes, simple to operate, low in cost and capable of realizing large-scale preparation.
Disclosure of Invention
The invention aims to solve the problems of complex method and thin surface layer thickness of the existing method for constructing the wrinkled structure, and provides a method for constructing the wrinkled structure on the surface of a high polymer material.
The invention relates to a method for constructing a high polymer material surface fold structure, which comprises the following steps:
1. pre-cleaning of the base material: carrying out ultrasonic washing on a thermoplastic polymer matrix material, and then drying the thermoplastic polymer matrix material by using high-purity nitrogen to obtain a cleaned matrix material;
2. carrying out irradiation treatment on the matrix: carrying out irradiation treatment on the cleaned matrix material by using heavy ions, electrons or protons to obtain an irradiated matrix material;
3. heating the irradiated substrate material to a glass transition temperature T g And performing heat treatment, then placing in air for cooling, and constructing a wrinkle structure on the surface of the matrix to finish the preparation.
The invention makes the thermoplastic macromolecule matrix material surface generate cross-linking to form surface layer by heavy ion, electron and proton irradiation, when the temperature is higher than the glass transition point of the matrix material, the matrix material and the surface layer generate stress due to different Young's moduliThe force is self-contracted to form a micro-nano folded structure. The precise regulation and control of the fold wavelength and the amplitude can be realized by controlling the irradiation energy, the flux, the fluence, the heat treatment temperature and the time, and the thickness of the surface layer can be adjusted from nano-scale to millimeter-scale. The method adopts irradiation of heavy ions, electrons and protons to construct the folds, is suitable for constructing a large-area, low-cost and controllable micro-nano fold structure, and solves the problems of reactive plasma etching (RIE) and ultraviolet/O (ultraviolet/oxygen) adopted 3 The problems of complex irradiation and laser irradiation methods and high cost can be solved, and the method can be applied to the fields of optical regulation, intelligent sensors, surface-enhanced Raman scattering, fluorescence enhancement effect, micro-nano robots, surface wettability, antifogging and deicing and surface dust prevention.
Drawings
FIG. 1 is an SEM image of argon ion irradiation for constructing a corrugated structure on a polystyrene substrate in example 1;
FIG. 2 is an SEM image of proton irradiation on a polystyrene substrate to construct a wrinkled structure in example 2.
Detailed Description
The first embodiment is as follows: the method for constructing the surface wrinkle structure of the high polymer material in the embodiment comprises the following steps:
1. pre-cleaning of the base material: carrying out ultrasonic washing on a thermoplastic polymer matrix material, and then drying the thermoplastic polymer matrix material by using high-purity nitrogen to obtain a cleaned matrix material;
2. carrying out irradiation treatment on the matrix: carrying out irradiation treatment on the cleaned matrix material by using heavy ions, electrons or protons to obtain an irradiated matrix material;
3. heating the irradiated substrate material to a glass transition temperature T g And performing heat treatment, then placing in air for cooling, and constructing a wrinkle structure on the surface of the matrix to finish the preparation.
According to the embodiment, heavy ion, electron and proton irradiation is carried out to enable the surface of the thermoplastic polymer matrix material to generate cross-linking to form a surface layer, and when the temperature is higher than the glass transition point of the matrix material, the matrix material and the surface layer generate stress due to different Young modulus so as to form a micro-nano wrinkle structure through self-contraction. Can be used forThe precise regulation and control of the fold wavelength and the amplitude are realized by controlling the irradiation energy, the flux, the fluence, the heat treatment temperature and the time, and the thickness of the surface layer is adjustable from nano-scale to millimeter-scale. The method adopts irradiation of heavy ions, electrons and protons to construct the folds, is suitable for constructing a large-area, low-cost and controllable micro-nano fold structure, and solves the problems of reactive plasma etching (RIE) and ultraviolet/O (ultraviolet/oxygen) adopted 3 The problems of complex irradiation and laser irradiation methods and high cost can be solved, and the method can be applied to the fields of optical regulation, intelligent sensors, surface-enhanced Raman scattering, fluorescence enhancement effect, micro-nano robots, surface wettability, antifogging and deicing and surface dust prevention.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: and carrying out ultrasonic washing by using absolute ethyl alcohol or deionized water or alternatively carrying out ultrasonic washing by using the absolute ethyl alcohol and the deionized water. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the thermoplastic polymer matrix material is polystyrene heat-shrinkable film (PS), polyester heat-shrinkable film (PET), polyethylene heat-shrinkable film (PE), polyvinyl chloride heat-shrinkable film (PVC), multi-layer co-extruded polyolefin heat-shrinkable film (POF), co-extruded polypropylene heat-shrinkable film (PP), polyvinylidene chloride heat-shrinkable film (PVDC) or o-phenylphenol heat-shrinkable film (OPP). The rest is the same as the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment and one of the first to third embodiments is: the heavy ions are argon ions, nitrogen ions, oxygen ions, silicon ions, helium ions, copper ions or gold ions, the energy range is eV-MeV, and the injection amount is 1 × 10 11 cm -2 ～5×10 14 cm -2 . The rest is the same as one of the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the energy range of electron irradiation is eV-MeV, and the fluence is 1 multiplied by 10 12 cm -2 ～5×10 15 cm -2 . The rest is the same as one of the first to fourth embodiments.
The sixth specific implementation mode: this embodiment mode andthe difference of one of the first to the fifth embodiments is that: the energy range of proton irradiation is eV-MeV, and the injection amount is 1 multiplied by 10 12 cm -2 ～5×10 15 cm -2 . The rest is the same as one of the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: and (4) carrying out heat treatment by adopting a drying oven, a muffle furnace or other heat treatment furnaces. The rest is the same as one of the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: the heat treatment temperature is higher than the glass transition point temperature of the matrix and lower than the melting point. The rest is the same as one of the first to seventh embodiments.
The specific implementation method nine: the difference between this embodiment and the first to eighth embodiments is: the heat treatment time is 1 s-30 min. The rest is the same as the first to eighth embodiments.
The effect of the invention is verified by the following examples:
example 1:
utilizing argon ion irradiation to construct a fold structure on a polystyrene matrix:
(1) Ultrasonically cleaning a polystyrene heat-shrinkable film in alcohol and deionized water, and drying by using high-purity nitrogen.
(2) Subjecting the polystyrene thermal shrinkage film to heat treatment at an energy of 50keV and a flux of 5 × 10 10 cm -2 ·s -1 Fluence of 5X 10 13 cm -2 The irradiation treatment is carried out under the irradiation condition of argon ions, so that the surface of the polystyrene heat-shrinkable film is crosslinked.
(3) And (3) carrying out heat treatment on the irradiated polystyrene heat-shrinkable film at 125 ℃ for 3min, and then placing the heat-shrinkable film in air for cooling and self-shrinking to generate a wrinkle structure. SEM images of argon ion irradiation to build a wrinkled structure on a polystyrene substrate as shown in fig. 1, it can be seen from fig. 1 that this example successfully built a wrinkled structure on a polystyrene substrate. The calculated surface layer thickness was 86nm.
Example 2
Utilizing proton irradiation to construct a fold structure on a polystyrene matrix:
(1) Ultrasonically cleaning a polystyrene heat-shrinkable film in alcohol and deionized water, and drying by using high-purity nitrogen.
(2) Subjecting the polystyrene thermal shrinkage film to heat treatment at an energy of 50keV and a flux of 1 × 10 11 cm -2 ·s -1 The fluence is 5X 10 14 cm -2 The irradiation treatment is carried out under the proton irradiation condition to generate crosslinking on the surface of the polystyrene.
(3) And (3) carrying out heat treatment on the irradiated polystyrene heat-shrinkable film at 135 ℃ for 2min, and then placing the heat-shrinkable film in air for cooling and self-shrinking to generate a wrinkle structure. An SEM image of a fold structure formed on a polystyrene matrix by proton irradiation is shown in FIG. 2, and it can be seen from FIG. 2 that the fold structure is successfully formed on the polystyrene matrix in the embodiment, and the calculated surface layer thickness is 663nm.
Example 3
Utilizing proton irradiation to construct a fold structure on a polyester matrix:
(1) Ultrasonically cleaning the polyester heat-shrinkable film in alcohol and deionized water, and drying by using high-purity nitrogen.
(2) Heat-shrinkable polyester film was heated at an energy of 100keV and a flux of 1X 10 12 cm -2 ·s -1 Fluence of 1X 10 15 cm -2 The irradiation treatment is carried out under the proton irradiation condition to generate cross-linking on the surface of the polyester substrate.
(3) And (3) carrying out heat treatment on the irradiated polyester heat-shrinkable film at 160 ℃ for 4min, and then placing the film in air for cooling and self-shrinking to generate a wrinkle structure. The calculated surface layer thickness was 1.05 μm.
Example 4
Constructing a fold structure on a polyethylene matrix by utilizing electron irradiation:
(1) Ultrasonically cleaning the polyethylene heat-shrinkable film in alcohol and deionized water, and drying by using high-purity nitrogen.
(2) The polyethylene thermal shrinkage film is heated at the energy of 1MeV and the flux of 5 multiplied by 10 11 cm -2 ·s -1 Fluence of 5X 10 13 cm -2 The irradiation treatment is carried out under the electron irradiation condition to generate crosslinking on the surface of the polyethylene.
(3) And (3) carrying out heat treatment on the irradiated polyethylene heat-shrinkable film at 150 ℃ for 40s, and then placing the polyethylene heat-shrinkable film in air to cool and self-shrink to generate a wrinkle structure. The calculated surface layer thickness was 3.9mm.
According to the embodiments, the surface of the thermoplastic polymer matrix material is crosslinked to form the surface layer through heavy ion, electron and proton irradiation, and when the temperature is higher than the glass transition point of the matrix material, the matrix material and the surface layer generate stress due to different Young moduli, so that the micro-nano wrinkle structure is formed through self-contraction. The precise regulation and control of the fold wavelength and the amplitude can be realized by controlling the irradiation energy, the flux, the fluence, the heat treatment temperature and the time, and the thickness of the surface layer can be adjusted from nano-scale to millimeter-scale.
Claims (9)
1. A method for constructing a surface fold structure of a high polymer material is characterized by comprising the following steps:
1. pre-cleaning of the base material: carrying out ultrasonic washing on a thermoplastic polymer matrix material, and then drying the thermoplastic polymer matrix material by using high-purity nitrogen to obtain a cleaned matrix material;
2. carrying out irradiation treatment on a matrix: carrying out irradiation treatment on the cleaned matrix material by using heavy ions, electrons or protons to obtain an irradiated matrix material;
3. heating the irradiated substrate material to a glass transition temperature T g And performing heat treatment, then placing in air for cooling, and constructing a wrinkle structure on the surface of the matrix to finish the preparation.
2. The method for constructing a surface wrinkle structure of a polymer material as claimed in claim 1, wherein the ultrasonic washing is performed by absolute ethyl alcohol or deionized water, or alternatively by absolute ethyl alcohol and deionized water.
3. The method for constructing a surface wrinkle structure on a polymer material as claimed in claim 1, wherein the thermoplastic polymer substrate is a polystyrene heat-shrinkable film, a polyester heat-shrinkable film, a polyethylene heat-shrinkable film, a polyvinyl chloride heat-shrinkable film, a multi-layer co-extruded polyolefin heat-shrinkable film, a co-polypropylene heat-shrinkable film, a polyvinylidene chloride heat-shrinkable film or an o-phenylphenol heat-shrinkable film.
4. The method according to claim 1, wherein the heavy ions are argon ions, nitrogen ions, oxygen ions, silicon ions, helium ions, copper ions, or gold ions, the energy range is eV-MeV, and the flux is 1 x 10 8 cm -2 ·s -1 ～1×10 14 cm -2 ·s -1 Fluence of 1X 10 11 cm -2 ～5×10 14 cm -2 。
5. The method according to claim 1, wherein the electron irradiation energy range is eV-MeV, and the flux is 1X 10 8 cm -2 ·s -1 ～1×10 15 cm -2 ·s -1 Fluence of 1X 10 12 cm -2 ～5×10 15 cm -2 。
6. The method according to claim 1, wherein the proton irradiation energy is in the range of eV to MeV, and the flux is 1X 10 8 cm -2 ·s -1 ～1×10 15 cm -2 ·s -1 Fluence of 1X 10 12 cm -2 ～5×10 15 cm -2 。
7. The method according to claim 1, wherein the heat treatment is performed in a drying oven or a muffle furnace.
8. The method as claimed in claim 1, wherein the heat treatment temperature is higher than the glass transition point of the substrate and lower than the melting point.
9. The method as claimed in claim 1, wherein the heat treatment time is 1 s-30 min.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| US20080026329A1 (en) * | 2006-07-26 | 2008-01-31 | Ashkan Vaziri | Surface modification of polymer surface using ion beam irradiation |
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Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102199744A (en) * | 2010-03-26 | 2011-09-28 | 国家纳米科学中心 | Preparation method of film with micro-nano wrinkled patterns |
| ES2476465A1 (en) * | 2012-12-12 | 2014-07-14 | Consejo Superior de Investigaciones Cientficas (CSIC) | Method for producing polymer materials with structured surfaces, the materials thus produced and the applications thereof |
| CN104140092A (en) * | 2013-05-09 | 2014-11-12 | 国家纳米科学中心 | Wrinkled graphene lamella and making method thereof |
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