CN107880302B - Patterned polymer and preparation method thereof - Google Patents

Patterned polymer and preparation method thereof Download PDF

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Publication number
CN107880302B
CN107880302B CN201711375448.1A CN201711375448A CN107880302B CN 107880302 B CN107880302 B CN 107880302B CN 201711375448 A CN201711375448 A CN 201711375448A CN 107880302 B CN107880302 B CN 107880302B
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polymer
patterned
layer
silicone rubber
substrate layer
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CN107880302A (en
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何周坤
李秀云
喻永连
杨建�
唐昶宇
梅军
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Chengdu Science and Technology Development Center of CAEP
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Chengdu Science and Technology Development Center of CAEP
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Abstract

The invention discloses a patterned polymer laminar material which comprises at least three layers of laminated structures, namely a polymer substrate layer, a patterned structure layer and a surface packaging layer; the patterned structure layer is provided with dispersed bowl-shaped convex structures, grooves or porous structures; the surface packaging layer is a packaging layer which covers the surface of the patterned structural layer and keeps the shape of the patterned structural layer. The invention provides a novel large-area convex bowl-shaped patterning structure with a non-traditional porous structure, and simultaneously provides a composite material patterning technology based on a thermosetting polymer system and containing inorganic nano particles; the patterning structure layer is generated on the substrate layer in a bionic mode, and the upper packaging layer raw material is combined to form a stable packaging structure, so that the purpose of enhancing the performance of the patterning polymer material is achieved.

Description

Patterned polymer and preparation method thereof
Technical Field
The invention belongs to the technical field of material surface modification, relates to a modified hydrophilic or hydrophobic layer surface structure, and particularly relates to a polymer material with large-area patterning design. The patterned polymer surface structure has the characteristics of low cost and large-area preparation, and has more advantages compared with the existing patterned surface laminated structure.
Background
The wettability of the surface of the material, such as hydrophilicity or hydrophobicity, can realize the adjustment and change of the liquid contact angle by designing a unique structure through bionics and the difference of hydrophilicity and hydrophobicity of the material. Different surface wettabilities can be realized through different materials, and further different engineering application environment requirements can be met. Although the optimization of the surface wetting property of a part of the material can be realized through the hydrophily and hydrophobicity of the material, according to the research theory of bionics, the physical structure design of the surface of the material is also considered in order to realize the optimal regulation and control of the surface wetting property of the material, and the regular patterned structure is more favored due to the special application of the patterned structure, and meanwhile, the application field of the polymer material can be effectively expanded through the design of the patterned structure of the material and the effective regulation and control of the hydrophily and hydrophobicity of the surface.
At present, various technical means can be used for realizing the construction of a surface patterning structure, such as block copolymer self-assembly, femtosecond laser etching, 3D printing, a breathing pattern method and the like. However, the existing patterning technical means have one or more disadvantages of small patterning area, multi-step processing, high equipment cost, uncontrollable pattern structure and the like, so that a lot of problems to be solved exist in practical industrial application. For example, the breathing pattern method is mainly based on a dynamic template obtained by self-assembling water drops, and the cellular porous polymer membrane structure is prepared by comprehensively regulating and controlling various factors such as polymer type, solvent type, solution concentration, experiment temperature, environment humidity and the like. The method has the advantages of strong universality, low cost and the like, but the practical application of the method is limited because the control factors are complex, the area of the prepared patterned structure is small, the patterned structure is usually a porous structure, and the adopted system is only a thermoplastic pure polymer system generally.
Disclosure of Invention
The invention aims to overcome the defects of small patterning area, multi-step treatment, high equipment cost, uncontrollable pattern structure and the like in the conventional patterning technical means, provide a novel large-area convex bowl-shaped patterning structure with a non-traditional porous structure, and provide a composite material patterning technology based on a thermosetting polymer system and containing inorganic nanoparticles.
In order to achieve the above purpose, the invention provides the following technical scheme:
a patterned polymer laminar material comprises at least three layers of laminated structures, namely a polymer substrate layer, a patterned structure layer and a surface packaging layer.
The patterned structure layer has dispersed bowl-shaped raised structures, grooves or porous structures.
The surface packaging layer is a packaging layer which covers the surface of the patterned structural layer and keeps the shape of the patterned structural layer.
Preferably, the surface encapsulation layer is a continuous thin layer structure.
The patterned polymer layer material of the invention is used for preparing the patterned structure layer on the surface of the polymer substrate layer, and the patterned structure layer is used for designing the three-dimensional appearance of the polymer surface, thereby realizing different polymer surface appearances. And finally, the film-like surface packaging layer is sealed, and is matched with a hydrophilic or hydrophobic functional material to realize the effect of combining the microscopic morphology and the functional material, so that the bionic hydrophilic-hydrophobic wettability improvement and enhancement effect is achieved, the enhancement effect of breaking through the surface characteristics of general materials can be played, and the method has important practical application significance.
In the patterned structural layer in the patterned polymer of the present invention: the dispersed bowl-mounted convex structure is an independent annular structure with higher periphery and lower center. And secondly, forming a non-penetrating porous structure on the patterned structure layer, wherein the groove structures are distributed in a dispersed manner to form height drop distribution. And thirdly, the porous structure is a dispersed porous structure in the patterned structure layer, the porous structure is a porous structure with high peripheries and a continuous layer in the middle.
Further, the polymer substrate layer is a thermoplastic plastic film or sheet, a rubber elastic film or sheet.
Preferably, the material of the polymer substrate layer includes, but is not limited to, one or more of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyethylene terephthalate, polybutylene terephthalate, poly (p-xylylene chloride), poly (m-xylylene chloride), poly (o-xylylene chloride), polyimide, polytetrafluoroethylene, polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl phenyl silicone rubber, and methyl vinyl trifluoropropyl silicone rubber.
Further, the patterned structure layer is made of a second polymer, and 0-4 times of mass of hydrophobic inorganic nanoparticles are added into the second polymer. Preferably, the mass ratio of the second polymer to the inorganic nanoparticles is 90: 10-25: 75, and different patterning purposes can be achieved by changing the addition ratio of the inorganic nanoparticles, so that the inorganic nanoparticles generate different pattern shapes when the second polymer is cured to form a film layer structure. When the ratio of the second polymer to the inorganic nanoparticles is 100:0, indicates that no inorganic nanoparticles are added. Preferably, the inorganic nanoparticles are hydrophobically modified inorganic nanoparticles.
Preferably, the second polymer includes, but is not limited to, one of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyethylene terephthalate, polybutylene terephthalate, polychloro-p-xylene, polychloro-m-xylene, polychloro-o-xylene, polyimide, polytetrafluoroethylene, polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl phenyl silicone rubber, methyl vinyl trifluoropropyl silicone rubber.
Preferably, the molecular weight of the second polymer is 5000-100000 g/mol.
Preferably, the inorganic nanoparticles are one or more of calcium carbonate, silicon dioxide, titanium dioxide, carbon black, graphene, carbon nanotubes, montmorillonite and zinc oxide, and the size of the inorganic nanoparticles is 1-5000 nm. The inorganic nanoparticles are hydrophobic inorganic nanoparticles or inorganic nanoparticles modified to have hydrophobic properties. The inorganic nanoparticles have hydrophobicity, and the self-assembly molding of a bowl-shaped convex structure, a groove or a porous structure is realized through the hydrophobicity of the inorganic nanoparticles in the molding process of the patterned structure layer, so that the efficiency of the patterning molding is improved, and the large-area patternable treatment convenient for industrial production and preparation is realized.
Further, the inorganic nanoparticles are pre-soaked for 5-60 min by adopting a coupling agent with the mass concentration of 0.1-5.0%, and then dried for 5-60 min at the temperature of 20-90 ℃. The modified hydrophobic inorganic nano particles are more easily and uniformly dispersed with the second polymer to form a uniform and consistent patterned structural layer.
Preferably, the coupling agent is a silane coupling agent or a titanate coupling agent.
Preferably, the coupling agent is one or more of 3-aminopropyltriethoxysilane, 3-glycidoxypropyltrimethoxysilane, 3- (methacryloyloxy) propyltrimethoxysilane, bis (dioctyloxypyrophosphate) ethylene titanate and isopropyltris (dioctylpyrophosphate) titanate.
Furthermore, the patterned structure layer is made of raw materials with the concentration of 0.1-30.0%. The patterned structural layer is prepared by adopting the raw material liquid with the mass concentration, the raw material components comprise a second polymer and inorganic nano particles, the sum of the mass concentration of the second polymer and the inorganic nano particles in the solution is 0.1-30.0%, the balance of the components is a solvent, and the solvent volatilizes and disappears in the preparation and forming process. The patterning structure layer is made of polymer and inorganic nano particles, and the inorganic nano particles are uniformly distributed to form different patterning structures by adjusting the proportion of the polymer to the inorganic nano particles, so that the aim of designing the bionic surface structure is fulfilled.
Preferably, the patterned structural layer is made from a dope in which the second polymer is dissolved in the second solvent. Wherein 0-4 times of inorganic nanoparticles are added when the second polymer is dissolved. The second solvent corresponding to the second polymer is one or more of xylene, toluene, chloroform, tetrahydrofuran, m-cresol, methyl ethyl ketone, acetone, cyclohexane and dimethylacetamide.
Further, the material of the surface packaging layer is a third polymer or fluorine-containing silane.
Preferably, the third polymer is one or more of polyacrylic acid, chitosan quaternary ammonium salt, polyethylene glycol, ethyl hydroxyethyl cellulose, carbomer, polytetrafluoroethylene, polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl phenyl silicone rubber and methyl vinyl trifluoropropyl silicone rubber.
Preferably, the molecular weight of the third polymer is 5000-100000 g/mol.
Preferably, the fluorine-containing silane is one or more of 1H,1H,2H, 2H-perfluorooctyltrimethoxysilane, 1H,2H, 2H-perfluorooctyltriethoxysilane, 1H,2H, 2H-perfluorodecyltrimethoxysilane and 1H,1H,2H, 2H-perfluorodecyltriethoxysilane.
Preferably, the surface packaging layer is made of a third polymer or a solution containing fluorine silane, the mass concentration of the solution is 0.1-30.0%, and the balance is a solvent.
Preferably, the surface encapsulation layer is prepared from a solution of a third polymer or a fluorine-containing silane dissolved in a third solvent. The third solvent corresponding to the third polymer or the fluorine-containing silane is one or more of deionized water, methanol, ethanol, ethylene glycol, isopropanol, propanol, xylene, toluene, chloroform, tetrahydrofuran, methyl ethyl ketone, acetone, cyclohexane and dimethylacetamide. And selecting a proper third solvent for dissolving according to the characteristics of the material (a third polymer or fluorine-containing silane) of the surface packaging layer, so that the obtained feed liquid can be better molded on the surface of the patterned structural layer to obtain a film-shaped structure, and the morphological characteristics of the patterned structural layer are kept after the surface packaging layer is molded.
Further, the patterned polymeric layered material has the following characteristics: the contact angle of the water drop or the water-soluble liquid drop on the patterned polymer layered material is below 60 degrees or above 120 degrees.
Preferably, the water-soluble liquid drops include, but are not limited to, water-based paint, water-based ink, acid-base salt aqueous solution with pH of 1-13, sweat, blood and urine.
Further, the patterned polymeric layered material has the following characteristics: after the patterned polymer is subjected to one or more of ultrasonic strong damage for 120min, mechanical bending damage for 10000 times or mechanical friction for 10000 times, the contact angle of the liquid drop can still be kept below 60 degrees or above 120 degrees. The contact angle of the water drop or the water-soluble liquid drop on the surface of the patterned polymer can still be kept below 60 degrees or above 120 degrees. The patterned polymer layered material has extremely high structural stability, can resist high-strength mechanical abrasion damage, and keeps the surface hydrophilicity or hydrophobicity unchanged.
In order to prepare the patterned polymer, the invention also provides a preparation method, so as to better ensure that the surface pattern design of the patterned polymer material meets the design expectation and achieve good surface hydrophilic or hydrophobic property enhancement.
A method of making the above-described patterned polymer comprising the steps of:
(1) pretreatment of the polymer substrate layer: and cleaning a polymer substrate layer, wherein the polymer substrate layer is one of a thermoplastic plastic film or sheet and a rubber elastic film or sheet. Preferably, the polymer substrate layer is treated with a low temperature plasma after it is cleaned.
(2) Coating of the patterned structural layer: mixing a second polymer and hydrophobic inorganic nanoparticles, preparing a solution with the mass concentration of 0.1-30.0% by using a second solvent, and coating the polymer substrate layer; the mass ratio of the second polymer to the inorganic nanoparticles is 100: 0-20: 80;
(3) and (3) processing the patterned structural layer, wherein after the step (2) of coating, the patterned structural layer is processed for 30-180 min under the conditions that the temperature is 20-90 ℃ and the relative humidity is 20-100%.
(4) And (3) curing the surface packaging layer, namely dip-coating, spray-coating or spin-coating the polymer substrate layer processed in the step (3) with the raw material of the upper surface packaging layer, drying, then taking out and cleaning the polymer substrate layer after being processed in a super-thermal hydrogen device, and drying again to obtain the patterned polymer.
The preparation method comprises the steps of forming a patterned structure layer and curing the patterned structure layer in sequence, combining a second polymer and an inorganic nano particle material on the patterned structure layer, and processing a raw material coated on the patterned structure layer by using the conditions of temperature of 20-90 ℃ and relative humidity of 20-100% to form an excellent patterned structure so as to realize the design and printing of a bionic structure. And finally, combining an upper packaging layer raw material on the surface of the patterned structural layer, curing the patterned structural layer to form a thin layer structure with a continuous surface, and realizing a stable packaging structure while keeping the form of the patterned structural layer so as to achieve the purpose of enhancing the performance of the patterned polymer material.
The preparation method of the patterned polymer comprises the steps of pretreatment of a polymer base material layer, coating of a patterned structural layer, treatment of the patterned structural layer and curing treatment of a surface packaging layer. The patterned polymer has the advantages of no need of a physical template, regular and controllable pattern structure, large pattern size area and the like.
The method for preparing the patterned polymer has the advantages of strong universality, simple process, easy actual production, low production cost and the like, and can meet the actual application requirements of surface waterproof/anti-fouling, self-cleaning, low-cost polymer patterned templates and the like in the fields of electronic industry, printing industry, microfluid preparation, biomedicine and the like.
Further, step (1) is the pretreatment of the polymer substrate layer. In the process of cleaning the polymer substrate layer, soaking the porous substrate layer in ethanol for 5-60 min, and then drying at the temperature of 20-90 ℃ for 5-60 min; then soaking the mixture in deionized water for 5-60 min, and then drying the mixture at the temperature of 20-90 ℃ for 5-60 min. And then treating the mixture for 2 to 10 seconds by using low-temperature plasma.
Further, step (2) patterns the application of the structural layer. Mixing a second polymer and hydrophobic inorganic nanoparticles, and preparing a solution with the mass concentration of 0.1-30.0% by using a second solvent, wherein the mass ratio of the second polymer to the inorganic nanoparticles is 100: 0-20: 80; and (3) dip-coating for 5-3600 s to coat on the polymer substrate layer pretreated in the step (1), and taking out for later use.
Further, the step (3) is a process of patterning the structural layer. And (3) treating the polymer substrate layer coated in the step (2) for 30-180 min under the conditions that the temperature is 20-90 ℃ and the relative humidity is 20-100%.
And (4) further, curing the surface packaging layer. And preparing a surface packaging layer raw material solution by adopting a third polymer or fluorine-containing silane, wherein the mass concentration of the solution is 0.1-30.0%, and the balance is a third solvent. Coating the polymer substrate layer subjected to the patterning structure layer treatment in the step (3) by dip-coating for 5-3600 s or spray-coating for 2-180 s, drying at 20-90 ℃ for 5-120 min, treating in a super-thermal hydrogen device with voltage of 100-300V and vacuum degree of 0.05-0.15 Pa for 5-120 s, taking out, soaking in ethanol for 5-60 min, and drying at 20-90 ℃ for 5-60 min; and soaking the polymer in deionized water for 5-60 min, and drying the polymer at the temperature of 20-90 ℃ for 5-60 min to obtain the patterned polymer.
Preferably, in step 4, the surface packaging layer is a third polymer or fluorine-containing silane molded film layer or film.
Preferably, the third polymer is one or more of polyacrylic acid, chitosan quaternary ammonium salt, polyethylene glycol, ethyl hydroxyethyl cellulose, carbomer, polytetrafluoroethylene, polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl phenyl silicone rubber and methyl vinyl trifluoropropyl silicone rubber.
Preferably, the fluorine-containing silane is one or more of 1H,1H,2H, 2H-perfluorooctyltrimethoxysilane, 1H,2H, 2H-perfluorooctyltriethoxysilane, 1H,2H, 2H-perfluorodecyltrimethoxysilane and 1H,1H,2H, 2H-perfluorodecyltriethoxysilane.
Compared with the prior art, the invention has the beneficial effects that:
1. the patterned polymer layer material of the invention prepares the patterned structure layer on the surface of the polymer substrate layer, designs the three-dimensional morphology of the polymer surface by utilizing the patterned structure layer, overcomes the defects of small patterning area, multi-step treatment, high equipment cost, uncontrollable pattern structure and the like existing in the prior patterning technical means, and realizes different polymer surface morphologies.
2. The invention realizes the effect of combining the micro-morphology and the functional material by sealing the surface packaging layer and matching with the hydrophilic or hydrophobic functional material, has the effect of improving and enhancing the hydrophilic and hydrophobic wettability of bionics, can exert the enhancement effect of breaking through the surface characteristics of common materials, and has important practical application significance.
3. The invention provides a novel large-area convex bowl-shaped patterning structure with a non-traditional porous structure, and also provides a composite material patterning technology based on a thermosetting polymer system and containing inorganic nanoparticles. The patterning structure layer is generated on the substrate layer in a bionic mode, and the upper packaging layer raw material is combined to form a stable packaging structure, so that the purpose of enhancing the performance of the patterning polymer material is achieved.
Description of the drawings:
FIG. 1: scanning Electron microscopy of Large area porous patterned surface results (example 3)
FIG. 2: contact angle of water drop on Large area porous patterned surface 0 ° (example 3)
FIG. 3: scanning Electron microscopy of Large area porous patterned surface results (example 4)
FIG. 4: scanning Electron microscopy of Large area groove patterned surface results (example 5)
FIG. 5: scanning Electron microscopy of Large area groove patterned surface results (example 6)
FIG. 6: scanning Electron microscopy of Large area dispersed bowl-mounted convex patterned surface (example 7)
FIG. 7: contact angle of water drop on large area of the bowl-shaped raised patterned surface was 156 ° (example 7)
FIG. 8: scanning Electron microscopy of Large area dispersed bowl-mounted convex patterned surface (example 9)
FIG. 9: contact angle of water drop on large area dispersed bowl-mounted convex patterned surface 125 ° (example 9)
FIG. 10: scanning Electron microscopy of Large area dispersed bowl-mounted convex patterned surface (example 10)
FIG. 11: scanning Electron microscope results for Large area dispersed bowl-mounted convex patterned surfaces (example 11)
Detailed Description
The present invention is described in detail below by way of examples, and it should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention.
Example 1:
patterned polymeric layered materials
The patterned polymer layer material has a three-layer laminated structure of a polymer substrate layer of polyethylene, polypropylene and silica 80:20, and a polyacrylic surface encapsulation layer. The patterned structure layer has discrete bowl-shaped raised structures. The surface packaging layer is a continuous thin layer covering the surface of the patterned structural layer, and the shape of the patterned structural layer is reserved.
Example 2:
preparation of coupling agent pretreated inorganic nanoparticles
The inorganic nanoparticles are pre-soaked for 5-60 min by adopting a coupling agent with the mass concentration of 0.1-5.0%, and then dried for 5-60 min at the temperature of 20-90 ℃ to obtain the coupling agent modified inorganic nanoparticles for later use. The specific preparation raw materials and parameters are as follows:
Figure BDA0001514456840000071
Figure BDA0001514456840000081
example 3:
preparation of patterned Polymer layered Material
A patterned polymeric layered material was prepared according to the following steps:
in the process of cleaning the polyethylene base material layer, soaking the base material layer in ethanol for 10min, and then drying at the temperature of 30 ℃ for 60 min; soaking in deionized water for 10min, and drying at 30 deg.C for 60 min. And then treated with low temperature plasma for 10 s.
Step (2) a second polymer polypropylene having a molecular weight of 5000g/mol and the coupling agent-treated inorganic nanoparticles of number 201 in example 2 were mixed in a mass ratio of 90:10, and a solution having a mass concentration of 30.0% was prepared with toluene (second solvent). Then, the polymer substrate layer pretreated in the step (1) was coated by dip coating for 10 seconds and then taken out.
And (3) treating the polymer substrate layer coated in the step (2) for 30min at the temperature of 30 ℃ and the relative humidity of 90%.
And (4) preparing a surface packaging layer raw material solution with the mass concentration of 0.5% by using a third polymer with the molecular weight of 100000g/mol as polyacrylic acid and deionized water (a third solvent). Coating the polymer substrate layer subjected to the patterning structure layer treatment in the step (3) by dip-coating 3600s, drying at the temperature of 30 ℃ for 120min, treating in a super-thermal hydrogen device with the voltage of 300V and the vacuum degree of 0.15Pa for 10s, taking out, soaking in ethanol for 10min, and drying at the temperature of 30 ℃ for 60 min; then soaking the substrate in deionized water for 10min, and then drying the substrate at the temperature of 30 ℃ for 60min to obtain the patterned polymer.
< test >
The surface morphology of the prepared patterned polymer is observed by an electron microscope, and the result is shown in fig. 1, and the surface of the layered material has remarkable porous patterned morphology performance and meets the design expectation. The contact angle of the liquid drop on the surface of the material is tested, and as a result, the contact angle of the liquid drop on the surface of the patterned layered material is 0 degrees, as shown in fig. 2, compared with the layered thin film material made of the non-patterned surface packaging layer raw material, the contact angle of the liquid drop is obviously reduced, and the property of the layered material is superior to the hydrophilicity of the material which is not subjected to the patterning treatment.
Example 4:
preparation of patterned Polymer layered Material
A patterned polymeric layered material was prepared according to the following steps:
the cleaning process of the polyvinyl chloride base material layer in the step (1) is to soak the base material in ethanol for 20min and then dry the base material at the temperature of 40 ℃ for 50 min; soaking in deionized water for 20min, and drying at 40 deg.C for 50 min. And then treated with low temperature plasma for 8 s.
Step (2) the second polymer polystyrene having a molecular weight of 80000g/mol and the coupling agent-treated particles of number 202 in example 2 were mixed in a mass ratio of 80:20, and a solution having a mass concentration of 20.0% was prepared with tetrahydrofuran (second solvent). Then, the polymer substrate layer pretreated in the step (1) was coated by dip coating for 60 seconds and then taken out.
And (3) treating the polymer substrate layer coated in the step (2) for 60min under the conditions that the temperature is 30 ℃ and the relative humidity is 80%.
And (4) preparing a surface packaging layer raw material solution with the mass concentration of 0.1% by using a third polymer with the molecular weight of 10000g/mol as polyethylene glycol and ethanol (a third solvent). Coating the polymer base material layer subjected to the patterning structure layer treatment in the step (3) by spraying for 180s, drying at 40 ℃ for 90min, treating in a super-thermal hydrogen device with the voltage of 250V and the vacuum degree of 0.15Pa for 30s, taking out, soaking in ethanol for 20min, and drying at 40 ℃ for 50 min; then soaking the substrate in deionized water for 20min, and then drying the substrate for 50min at the temperature of 40 ℃ to obtain the patterned polymer.
< test >
The surface morphology of the prepared patterned polymer was observed with an electron microscope, and the results are shown in fig. 3, where the surface of the layered material had significant porous patterned morphology, which was in line with design expectations. The contact angle of the liquid drop on the surface of the water-based ink is tested, and the contact angle of the water-based ink on the surface of the patterned layered material is 0 degrees, compared with the layered thin film material made of the non-patterned surface packaging layer raw material, the contact angle of the liquid drop is obviously reduced, and the property of the layered material is superior to the hydrophilicity of the common non-patterned material through the patterning treatment.
Example 5:
preparation of patterned Polymer layered Material
A patterned polymeric layered material was prepared according to the following steps:
the method comprises the following steps that (1) in the process of cleaning the polystyrene substrate layer, the substrate is soaked in ethanol for 30min and then dried at the temperature of 50 ℃ for 50 min; then soaking in deionized water for 30min, and drying at 50 deg.C for 50 min. And then treated with low temperature plasma for 8 s.
Step (2) the second polymer polybutylene terephthalate having a molecular weight of 50000g/mol and the coupling agent-treated particles of the number 203 in example 2 were mixed in a mass ratio of 70:30, and m-cresol (second solvent) was used to prepare a solution having a mass concentration of 10.0%. Then, the polymer substrate layer pretreated in the step (1) is coated by dip coating for 120s, and then taken out.
And (3) treating the polymer substrate layer coated in the step (2) for 90min at the temperature of 50 ℃ and the relative humidity of 60%.
And (4) preparing a surface packaging layer raw material solution with the mass concentration of 5.0% by using (a third solvent) isopropanol and adopting a third polymer with the molecular weight of 20000g/mol as the polyethylene hydroxyethyl cellulose. Coating the polymer substrate layer subjected to the patterning structure layer treatment in the step (3) on a dip-coating layer for 1200s, drying at 50 ℃ for 70min, treating in a super-thermal hydrogen device with the voltage of 200V and the vacuum degree of 0.1Pa for 60s, taking out, soaking in ethanol for 30min, and drying at 50 ℃ for 50 min; and then soaking the substrate in deionized water for 30min, and then drying the substrate for 50min at the temperature of 50 ℃ to obtain the patterned polymer.
< test >
The surface morphology of the prepared patterned polymer was observed with an electron microscope, and the results are shown in fig. 4, where the surface of the layered material had significant groove patterned morphology performance, which was in line with design expectations. The contact angle of the liquid drop on the surface of the material is tested, and the contact angle of the aqueous solution of hydrogen chloride with the pH value of 2 on the surface of the patterned layered material is 0 degrees, compared with the layered thin film material made of the non-patterned surface packaging layer raw material, the contact angle of the liquid drop is obviously reduced, and the property of the layered material is superior to the hydrophilicity of the material which is not subjected to the patterning treatment.
Example 6:
preparation of patterned Polymer layered Material
A patterned polymeric layered material was prepared according to the following steps:
the method comprises the following steps that (1) in the process of cleaning a polybutylene terephthalate substrate layer, the substrate is soaked in ethanol for 40min and then dried at the temperature of 50 ℃ for 30 min; then soaking in deionized water for 40min, and drying at 50 deg.C for 30 min. And then treated with low temperature plasma for 10 s.
Step (2) the second polymer polybutylene terephthalate having a molecular weight of 20000g/mol and the coupling agent-treated particles of number 204 in example 2 were mixed in a mass ratio of 60:40, and a solution having a mass concentration of 5.0% was prepared using (second solvent) m-cresol. Then, the polymer substrate layer pretreated in the step (1) was coated by dip coating for 600s, and then taken out.
And (3) treating the polymer substrate layer coated in the step (2) for 120min at the temperature of 70 ℃ and the relative humidity of 40%.
And (4) preparing a surface packaging layer raw material solution with the mass concentration of 8.0% by using a third polymer with the molecular weight of 50000g/mol as carbomer and using (a third solvent) propanol. Coating the polymer base material layer subjected to the patterning structure layer treatment in the step (3) by spraying for 90s, drying at 40 ℃ for 60min, treating in a super-thermal hydrogen device with the voltage of 150V and the vacuum degree of 0.1Pa for 60s, taking out, soaking in ethanol for 40min, and drying at 50 ℃ for 30 min; and soaking the substrate in deionized water for 40min, and then drying the substrate at the temperature of 50 ℃ for 30min to obtain the patterned polymer.
< test >
The surface morphology of the prepared patterned polymer was observed with an electron microscope, and the results are shown in fig. 5, where the surface of the layered material had significant groove patterned morphology performance, which was in line with design expectations. The contact angle of the liquid drop on the surface of the material is tested, and the contact angle of the sodium chloride aqueous solution with the pH value of 7 on the surface of the patterned layered material is 0 degrees, compared with the layered thin film material made of the non-patterned surface packaging layer raw material, the contact angle of the liquid drop is obviously reduced, and the property of the layered material is superior to the hydrophilicity of the material which is not subjected to the patterning treatment.
Example 7:
preparation of patterned Polymer layered Material
A patterned polymeric layered material was prepared according to the following steps:
in the process of cleaning the polychlorinated p-xylene base material layer, the base material layer is soaked in ethanol for 50min and then dried at the temperature of 60 ℃ for 30 min; soaking in deionized water for 50min, and drying at 60 deg.C for 30 min. And then treated with low temperature plasma for 6 s.
Step (2) polyvinylidene fluoride, a second polymer having a molecular weight of 20000g/mol, and the coupling agent-treated particles of number 205 in example 2 were mixed in a mass ratio of 50:50, and a solution having a mass concentration of 5.0% was prepared with dimethylacetamide (a second solvent). Then, the polymer substrate layer pretreated in the step (1) is coated by dip coating 1200s, and then taken out.
And (3) treating the polymer substrate layer coated in the step (2) for 180min under the conditions that the temperature is 80 ℃ and the relative humidity is 30%.
And (4) preparing a surface packaging layer raw material solution with the mass concentration of 10.0% by using a third polymer with the molecular weight of 20000g/mol as polyvinylidene fluoride and dimethyl acetamide as a (third solvent). Coating the polymer base material layer subjected to the patterning structure layer treatment in the step (3) by dip coating for 600s, drying at the temperature of 60 ℃ for 60min, treating in a super-thermal hydrogen device with the voltage of 150V and the vacuum degree of 0.05Pa for 90s, taking out, soaking in ethanol for 50min, and drying at the temperature of 60 ℃ for 30 min; and then soaking the substrate in deionized water for 50min, and then drying the substrate for 30min at the temperature of 60 ℃ to obtain the patterned polymer.
< test >
The surface morphology of the prepared patterned polymer was observed with an electron microscope, and the results are shown in fig. 6, where the surface of the layered material had a significantly dispersed patterned morphology of bowl-shaped protrusions, which was in line with design expectations. The contact angle of the liquid drop on the surface of the material is tested, and as a result, the contact angle of the sodium hydroxide aqueous solution with the pH value of 12 on the surface of the patterned layered material is 156 degrees, as shown in fig. 7, compared with the layered thin film material made of the non-patterned surface packaging layer raw material, the contact angle of the liquid drop is obviously improved, and the patterning treatment enables the property of the layered material to be superior to the hydrophobicity of the common non-patterned material.
Example 8:
preparation of patterned Polymer layered Material
A patterned polymeric layered material was prepared according to the following steps:
in the process of cleaning the polyimide substrate layer, the substrate is soaked in ethanol for 60min and then dried at the temperature of 70 ℃ for 20 min; soaking in deionized water for 60min, and drying at 70 deg.C for 20 min. And then treated with low temperature plasma for 8 s.
Step (2) A second polymer, dimethylsilicone rubber having a molecular weight of 50000g/mol and the coupling agent-treated particles of No. 206 of example 2 were mixed in a mass ratio of 50:50, and a solution having a mass concentration of 3.0% was prepared using toluene (second solvent). Then, the polymer substrate layer pretreated in the step (1) was coated by dip coating 2400s, and then taken out.
And (3) treating the polymer substrate layer coated in the step (2) for 180min under the conditions that the temperature is 90 ℃ and the relative humidity is 60%.
And (4) preparing a surface packaging layer raw material solution with the mass concentration of 15.0% by using a third polymer (dimethyl silicon rubber) with the molecular weight of 5000g/mol and toluene (a third solvent). Coating the polymer base material layer subjected to the patterning structure layer treatment in the step (3) on a spraying layer for 30s, drying at 70 ℃ for 40min, treating in a super-thermal hydrogen device with the voltage of 100V and the vacuum degree of 0.05Pa for 120s, taking out, soaking in ethanol for 60min, and drying at 70 ℃ for 20 min; and then soaking the substrate in deionized water for 60min, and then drying the substrate at the temperature of 70 ℃ for 20min to obtain the patterned polymer.
< test >
The surface morphology of the prepared patterned polymer is observed by an electron microscope, and the result is similar to that shown in fig. 6, and the surface of the layered material has remarkable dispersed bowl-shaped raised patterned morphological expression, which meets the design expectation. The contact angle of the liquid drop on the surface of the layered material is tested, and the contact angle of the liquid drop on the surface of the patterned layered material is 132 degrees, compared with the layered thin film material made of the non-patterned surface packaging layer raw material, the contact angle of the liquid drop is obviously improved, and the characteristic of the layered material is superior to the hydrophobicity of the common non-patterned material through the patterning treatment.
Example 9:
preparation of patterned Polymer layered Material
A patterned polymeric layered material was prepared according to the following steps:
the cleaning process of the polyvinylidene fluoride substrate layer in the step (1) is that the substrate is soaked in ethanol for 60min and then dried at the temperature of 90 ℃ for 10 min; then soaking in deionized water for 60min, and drying at 90 deg.C for 10 min. And then treated with low temperature plasma for 8 s.
Step (2) a second polymer methyl vinyl silicone rubber having a molecular weight of 100000g/mol and the coupling agent-treated particle of number 201 in example 2 were mixed in a mass ratio of 40:60, and a solution having a mass concentration of 1.0% was prepared with (second solvent) cyclohexane. And (3) coating the polymer substrate layer pretreated in the step (1) by dipping 3600s, and then taking out.
And (3) treating the polymer substrate layer coated in the step (2) for 120min at the temperature of 60 ℃ and the relative humidity of 60%.
And (4) preparing a surface packaging layer raw material solution with the mass concentration of 20.0% by using a third polymer with the molecular weight of 10000g/mol as methylvinyl phenyl silicone rubber and xylene (a third solvent). Coating the polymer base material layer subjected to the patterning structure layer treatment in the step (3) on a dip-coating layer for 120s, drying the polymer base material layer at the temperature of 90 ℃ for 20min, treating the polymer base material layer in a super-thermal hydrogen device with the voltage of 200V and the vacuum degree of 0.05Pa for 90s, taking out the polymer base material layer, soaking the polymer base material layer in ethanol for 60min, and drying the polymer base material layer at the temperature of 90 ℃ for 10 min; and then soaking the substrate in deionized water for 60min, and then drying the substrate at the temperature of 90 ℃ for 10min to obtain the patterned polymer.
< test >
The surface morphology of the prepared patterned polymer was observed with an electron microscope, and the results are shown in fig. 8, where the surface of the layered material had a significantly dispersed patterned morphology of bowl-shaped protrusions, which was in line with design expectations. The contact angle of the liquid drop on the surface of the material is tested, and as a result, the contact angle of the liquid drop on the surface of the patterned layered material is 125 degrees, as shown in fig. 9, compared with the layered thin film material made of the non-patterned surface packaging layer raw material, the contact angle of the liquid drop is obviously improved, and the patterning treatment enables the property of the layered material to be superior to the hydrophobicity of the material which is not subjected to the common patterning treatment.
Example 10:
preparation of patterned Polymer layered Material
A patterned polymeric layered material was prepared according to the following steps:
the method comprises the following steps that (1) in the process of cleaning the methyl vinyl silicone rubber substrate layer, the substrate is soaked in ethanol for 30min and then dried at the temperature of 70 ℃ for 30 min; then soaking in deionized water for 30min, and drying at 70 deg.C for 30 min. And then treated with low temperature plasma for 4 s.
Step (2) the second polymer methylvinylsilicone rubber having a molecular weight of 80000g/mol and the coupling agent-treated particles of number 202 in example 2 were mixed in a mass ratio of 30:70, and a solution having a mass concentration of 1.0% was prepared with (second solvent) cyclohexane. Then, the polymer substrate layer pretreated in the step (1) is coated by dip coating 1200s, and then taken out.
And (3) treating the polymer substrate layer coated in the step (2) for 90min under the conditions that the temperature is 40 ℃ and the relative humidity is 40%.
And (4) preparing a surface packaging layer raw material solution with the mass concentration of 30.0% by using (a third solvent) ethanol by using fluorine-containing silane 1H,1H,2H, 2H-perfluorooctyl trimethoxy silane. Coating the polymer base material layer subjected to the patterning structure layer treatment in the step (3) by spraying for 60s, drying at 70 ℃ for 50min, treating in a super-thermal hydrogen device with the voltage of 200V and the vacuum degree of 0.1Pa for 60s, taking out, soaking in ethanol for 30min, and drying at 70 ℃ for 30 min; and then soaking the substrate in deionized water for 30min, and then drying the substrate at the temperature of 70 ℃ for 30min to obtain the patterned polymer.
< test >
The surface morphology of the prepared patterned polymer was observed with an electron microscope, and the results are shown in fig. 10, where the surface of the layered material had a significantly dispersed patterned morphology of bowl-shaped protrusions, which was in line with design expectations. The contact angle of the liquid drop on the surface of the material is tested, and the contact angle of the aqueous solution of hydrogen chloride with the pH value of 2 on the surface of the patterned layered material is 135 degrees, so that the contact angle of the liquid drop is obviously improved compared with the layered thin film material prepared from the non-patterned surface packaging layer raw material, and the characteristic of the layered material is superior to the hydrophobicity of the common non-patterned material through the patterning treatment.
Example 11:
preparation of patterned Polymer layered Material
A patterned polymeric layered material was prepared according to the following steps:
the method comprises the following steps that (1) in the process of cleaning a methyl vinyl trifluoropropyl silicone rubber substrate layer, the substrate is soaked in ethanol for 50min and then dried at the temperature of 60 ℃ for 50 min; then soaking in deionized water for 50min, and drying at 60 deg.C for 50 min. And then treated with low temperature plasma for 6 s.
Step (2) a second polymer methylvinylphenyl silicone rubber having a molecular weight of 5000g/mol and the coupling agent-treated particles of number 204 in example 2 were mixed in a mass ratio of 20:80, and a solution having a mass concentration of 0.5% was prepared with xylene (second solvent). Then, the polymer substrate layer pretreated in the step (1) was coated by dip coating for 600s, and then taken out.
And (3) treating the polymer substrate layer coated in the step (2) for 60min under the conditions that the temperature is 30 ℃ and the relative humidity is 80%.
And (4) preparing a surface packaging layer raw material solution with the mass concentration of 30.0% by adopting fluorine-containing silane 1H,1H,2H, 2H-perfluorodecyl triethoxysilane and using (a third solvent) toluene. Coating the polymer base material layer subjected to the patterning structure layer treatment in the step (3) on a dip-coating layer for 30s, drying the polymer base material layer at the temperature of 50 ℃ for 90min, treating the polymer base material layer in a super-thermal hydrogen device with the voltage of 300V and the vacuum degree of 0.1Pa for 20s, taking out the polymer base material layer, soaking the polymer base material layer in ethanol for 50min, and drying the polymer base material layer at the temperature of 60 ℃ for 50 min; and then soaking the substrate in deionized water for 50min, and then drying the substrate for 50min at the temperature of 60 ℃ to obtain the patterned polymer.
< test >
The surface morphology of the prepared patterned polymer was observed with an electron microscope, and the results are shown in fig. 11, where the surface of the layered material had a significantly dispersed patterned morphology of bowl-shaped protrusions, which was in line with design expectations. The contact angle of the liquid drop on the surface of the material is tested, and the contact angle of the sodium hydroxide aqueous solution with the pH value of 12 on the surface of the patterned layered material is 138 degrees, compared with the layered thin film material made of the non-patterned surface packaging layer raw material, the contact angle of the liquid drop is obviously improved, and the patterning treatment enables the property of the layered material to be superior to the hydrophobicity of the common non-patterned material.

Claims (6)

1. A patterned polymer laminar material comprises at least three layers of laminated structures, namely a polymer substrate layer, a patterned structure layer and a surface packaging layer;
the patterned structure layer is provided with dispersed bowl-shaped convex structures, grooves or porous structures;
the surface packaging layer covers the surface of the patterned structural layer, and the shape of the patterned structural layer is reserved;
the material of the surface packaging layer is a third polymer or fluorine-containing silane;
the patterned polymeric layered material has the following characteristics: the contact angle of the water drop or the water-soluble liquid drop on the patterned polymer laminar material is below 60 degrees or above 120 degrees;
the patterned polymer layered material is prepared by the following method:
(1) pretreatment of the polymer substrate layer: cleaning a polymer substrate layer, wherein the polymer substrate layer is one of a thermoplastic plastic film or sheet and a rubber elastic film or sheet;
(2) coating of the patterned structural layer: mixing a second polymer and hydrophobic inorganic nanoparticles, preparing a solution with the mass concentration of 0.1-30.0% by using a second solvent, and coating the polymer substrate layer; hydrophobic inorganic nanoparticles which are 0-4 times of the mass of the second polymer are added into the second polymer, and the situation that the inorganic nanoparticles are 0 is not included; the second solvent is one or more of xylene, toluene, chloroform, tetrahydrofuran, m-cresol, methyl ethyl ketone, acetone, cyclohexane and dimethylacetamide;
(3) treating the patterned structural layer, wherein after the coating in the step 2, the patterned structural layer is treated for 30-180 min under the conditions that the temperature is 20-90 ℃ and the relative humidity is 20-100%;
(4) and (3) curing the surface packaging layer, namely dip-coating, spray-coating or spin-coating the polymer substrate layer processed in the step (3) with the upper surface packaging layer raw material, drying, then taking out and cleaning after processing in a super-thermal hydrogen device, and drying again to obtain the patterned polymer.
2. The patterned polymeric laminate of claim 1, wherein the polymeric substrate layer is a thermoplastic film or sheet, a rubber elastic film or sheet;
the material of the polymer substrate layer is selected from one or more of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyethylene glycol terephthalate, polybutylene terephthalate, poly (p-xylylene chloride), poly (m-xylylene chloride), poly (o-xylylene chloride), polyimide, polytetrafluoroethylene, polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl phenyl silicone rubber and methyl vinyl trifluoropropyl silicone rubber.
3. The patterned polymeric layer material of claim 1, wherein the second polymer is selected from one of polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyethylene terephthalate, polybutylene terephthalate, polychloro-p-xylene, polychloro-m-xylene, polychloro-o-xylene, polyimide, polytetrafluoroethylene, polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl phenyl silicone rubber, methyl vinyl trifluoropropyl silicone rubber;
the molecular weight of the second polymer is 5000-100000 g/mol;
the inorganic nano particles are one or more of calcium carbonate, silicon dioxide, titanium dioxide, carbon black, graphene, carbon nano tubes, montmorillonite and zinc oxide, and the size of the inorganic nano particles is 1-5000 nm.
4. The patterned polymer layered material according to claim 1, wherein the inorganic nanoparticles are pre-soaked with a coupling agent with a mass concentration of 0.1-5.0% for 5-60 min, and then dried at 20-90 ℃ for 5-60 min.
5. The patterned polymeric layered material of claim 4, wherein the coupling agent is a silane coupling agent or a titanate coupling agent.
6. The patterned polymer layered material according to claim 1, wherein the third polymer is one or more selected from polyacrylic acid, chitosan quaternary ammonium salt, polyethylene glycol, ethyl hydroxyethyl cellulose, carbomer, polytetrafluoroethylene, polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl phenyl silicone rubber, and methyl vinyl trifluoropropyl silicone rubber;
the molecular weight of the third polymer is 5000-100000 g/mol;
the fluorine-containing silane is one or more of 1H,1H,2H, 2H-perfluorooctyltrimethoxysilane, 1H,2H, 2H-perfluorooctyltriethoxysilane, 1H,2H, 2H-perfluorodecyltrimethoxysilane and 1H,1H,2H, 2H-perfluorodecyltriethoxysilane.
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