CN107880302A - A kind of patterned polymer and preparation method thereof - Google Patents

A kind of patterned polymer and preparation method thereof Download PDF

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Publication number
CN107880302A
CN107880302A CN201711375448.1A CN201711375448A CN107880302A CN 107880302 A CN107880302 A CN 107880302A CN 201711375448 A CN201711375448 A CN 201711375448A CN 107880302 A CN107880302 A CN 107880302A
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polymer
layer
patterned
pattern
shape material
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CN107880302B (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 kind of patterned polymer layer shape material, the patterned polymer layer shape material includes at least trilaminate structure, respectively polymer substrate, pattern structural layer and surface encapsulation layer；The pattern structural layer has scattered bowl-shape bulge-structure, groove or loose structure；The surface encapsulation layer is to be covered in pattern structure layer surface, and retains the encapsulated layer of pattern structural layer shape.The present invention provides a kind of New Type Large Area of non-traditional loose structure raised bowl-shape pattern structure, while provides composite patterning techniques a kind of based on thermoset polymer system and containing inorganic nano-particle；Structure sheaf bionical generation on substrate layer is will be patterned into, and combines upper encapsulated layer raw material, forms stable encapsulating structure, reaches the purpose of enhancing patterned polymer material property.

Description

A kind of patterned polymer and preparation method thereof
Technical field
The invention belongs to material surface modifying technology field, is related to a kind of hydrophilic or hydrophobic layer surface texture of modification, special It is not related to a kind of polymeric material with large area patternization design.The patterned polymer surface texture of the present invention has low Cost, can large area prepare the characteristics of, have more advantage compared to existing patterned surface layer structure.
Background technology
The wetability of material surface, such as hydrophily or hydrophobicity, the unique structure of bionic design and material can be passed through The difference of material hydrophobe itself come realize the adjustment of Liquid contact angle change.Different surfaces can be realized by different materials Wetability, and then meet different engineer applied environmental requirements.Although material can be realized by the hydrophilic and hydrophobic of material in itself The optimization of part surface wettability, but according to bionic research theory, want to realize optimal material surface wetting characteristics Regulation and control, should also be considered material surface physical design, and wherein regular pattern structure because its special application and More favored, while polymeric material can effectively be expanded by the Effective Regulation of material patterned structure design and surface hydrophobe The application field of material.
Having multiple technologies means at present can realize that patterned surface structure is constructed, such as Self-Assembling of Block Copolymer, Femtosecond laser etching, 3D printing, breathing pattern method etc..But these existing patterning techniques means exist patterned area it is small, Or one or more weak points such as multi-step is handled or equipment cost height or patterning are uncontrollable are needed, so as to cause Many urgent problems to be solved also be present in actual industrialization application.Such as breathing pattern method, it is mainly based upon self assembly water droplet and obtains The dynamic template arrived, carried out by many factors such as type of polymer, solvent species, solution concentration, experimental temperature, ambient humidities Comprehensive regulation, so as to which cellular porous polymer membrane structure be prepared.It is excellent that this method has that versatile, cost is low etc. Gesture, but because its governing factor is complicated, it is small that pattern structure area is prepared, is usually loose structure, the system one of use As be only thermoplasticity straight polymer system the deficiencies of, so as to limit its practical application.
The content of the invention
Present invention aims to overcome that patterned area to be present small or need at multi-step for existing patterning techniques means The deficiencies of reason or equipment cost height or uncontrollable patterning, while a kind of New Type Large Area of non-traditional loose structure is provided Raised bowl-shape pattern structure, while provide a kind of based on thermoset polymer system and containing the compound of inorganic nano-particle Material patterned technology.
In order to realize foregoing invention purpose, the invention provides following technical scheme：
A kind of patterned polymer layer shape material, the patterned polymer layer shape material include at least trilaminate knot Structure, respectively polymer substrate, pattern structural layer and surface encapsulation layer.
The pattern structural layer has scattered bowl-shape bulge-structure, groove or loose structure.
The surface encapsulation layer is to be covered in pattern structure layer surface, and retains the encapsulation of pattern structural layer shape Layer.
Preferably, the surface encapsulation layer is continuous laminate structure.
Patterned polymer layer shape material of the present invention prepares pattern structural layer in polymeric substrate layer surface, utilizes pattern Change structure sheaf to be designed the stereoscopic pattern of polymer surfaces, realize different polymer surfaces patterns.Finally with film sample Surface encapsulation layer is closed, and is coordinated hydrophily or hydrophobic function material, is realized that microscopic appearance and functional material be combined with each other Effect, the effect that there is the close and distant wettability of bionics to improve enhancing, can give play to and break through general material surface characteristic Humidification, have important practical application of significance.
In patterned polymer of the present invention in pattern structural layer：1. scattered bowl dress bulge-structure is independent one by one , the higher ring-type of surrounding and central relatively low graphic structure.2. groove be formed in pattern structural layer it is nonpenerative porous Structure, these groove structure dispersed distributions, form high low head distribution.3. loose structure be in pattern structural layer disperse it is more Pore structure, loose structure are the loose structures run through between surrounding senior middle school, and the high part of surrounding is continuous stratiform.
Further, the polymer substrate is thermoplastic plastic membrane or piece, caoutchouc elasticity film or piece.
Preferably, the material of the polymer substrate includes but is not limited to polyethylene, polypropylene, polyvinyl chloride, polyphenyl Ethene, polyethylene terephthalate, polybutylene terephthalate (PBT), Parylene C, polychlorostyrene for meta-xylene, Poly- chloro-o-xylene, polyimides, polytetrafluoroethylene (PTFE), polyvinylidene fluoride, dimethyl silicone rubber, methyl ethylene silicon rubber One or more in glue, methyl vinyl phenyl silicon rubber, methyl ethylene trifluoro propyl silicon rubber.
Further, the pattern structural layer is made up of second polymer, and 0~4 times is added with the second polymer Quality hydrophobic inorganic nano-particle.Preferably, the mass ratio of second polymer and inorganic nano-particle is 90:10~25:75, Adding proportion by changing inorganic nano-particle can realize different patterning purposes so that inorganic nano-particle is poly- second Compound produces different pattern forms when being formed by curing film layer structure.When second polymer and the ratio of inorganic nano-particle For 100：When 0, show not add inorganic nano-particle.Preferably, the inorganic nano-particle is the inorganic of hydrophobic modification Nano-particle.
Preferably, the second polymer include but is not limited to polyethylene, polypropylene, polyvinyl chloride, polystyrene, poly- pair PET, polybutylene terephthalate (PBT), Parylene C, polychlorostyrene are adjacent for meta-xylene, polychlorostyrene generation Dimethylbenzene, polyimides, polytetrafluoroethylene (PTFE), polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl silicone rubber, methyl second One kind in alkenyl phenyl siloxane rubber, methyl ethylene trifluoro propyl silicon rubber.
Preferably, the molecular weight of the second polymer is 5000~100000g/mol.
Preferably, the inorganic nano-particle is calcium carbonate, silica, titanium dioxide, carbon black, graphene, carbon nanometer One or more in pipe, montmorillonite, zinc oxide, its size are 1~5000nm.The inorganic nano-particle is all hydrophobic nothing Machine nano-particle, or by being modified as the inorganic nano-particle of hydrophobic property.Inorganic nano-particle has hydrophobicity, in pattern During changing structure formable layer, bowl-shape bulge-structure, groove or porous knot are realized by the hydrophobicity of inorganic nano-particle The self-assembled molding of structure, the efficiency of patterning shaping is improved, realized at the large area patternable for being easy to industrialized production to prepare Reason.
Further, the inorganic nano-particle uses mass concentration to carry out immersion 5 in advance for 0.1~5.0% coupling agent ~60min, 5~60min is then dried at a temperature of 20~90 DEG C.Modified hydrophobic inorganic nano-particle is obtained, is more held Easily and second polymer is dispersed comes, and forms the pattern structural layer of uniformity.
Preferably, the coupling agent is silane coupler or titanate coupling agent.
Preferably, the coupling agent is 3- aminopropyl triethoxysilanes, 3- glycydoxy trimethoxies Silane, 3- (methacryloxypropyl) propyl trimethoxy silicane, Di(dioctylpyrophosphato) ethylene titanate and isopropyl One or more in base three (dioctylphyrophosphoric acid acyloxy) titanate esters.
Further, pattern structural layer uses concentration to be made up of 0.1~30.0% raw material.Pattern structural layer is using above-mentioned Prepared by the material liquid of mass concentration, material composition includes second polymer and inorganic nano-particle, and both are in the solution Mass concentration sum is 0.1~30.0%, and surplus composition is solvent, and solvent volatilizees during shaping is prepared and disappeared.Patterning The material of structure sheaf is polymer and inorganic nano-particle, is adjusted by both ratios so that inorganic nano-particle uniformly divides Cloth forms different pattern structures, and then bionics surface structure design purpose.
Preferably, the pattern structural layer is made of the feed liquid as obtained by being dissolved in the second solvent second polymer 's.Wherein, 0~4 times of inorganic nano-particle is added when second polymer dissolves.Correspondingly the second solvent of second polymer is One kind in dimethylbenzene, toluene, chloroform, tetrahydrofuran, metacresol, methyl ethyl ketone, acetone, hexamethylene, dimethyl acetamide It is or a variety of.
Further, the material of the surface encapsulation layer is third polymer or fluorine containing silane.
Preferably, the third polymer is polyacrylic acid, chitosan quaternary ammonium salt, polyethylene glycol, ethyl-hydroxyethyl fiber Element, carbomer, polytetrafluoroethylene (PTFE), polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl silicone rubber, methyl ethylene benzene One or more in base silicon rubber, methyl ethylene trifluoro propyl silicon rubber.
Preferably, the molecular weight of the third polymer is 5000~100000g/mol.
Preferably, described fluorine containing silane is 1H, 1H, 2H, 2H- perfluoro capryls trimethoxy silane, 1H, 1H, 2H, 2H- Perfluoro capryl triethoxysilane, 1H, 1H, 2H, 2H- perfluoro decyls trimethoxy silane, 1H, 1H, 2H, 2H- perfluoro decyls three One or more in Ethoxysilane.
Preferably, the surface encapsulation layer is made of the solution of third polymer or fluorine containing silane, and the quality of solution is dense Spend for 0.1~30.0%, surplus is solvent.
Preferably, the surface encapsulation layer is the material as obtained by being dissolved in the 3rd solvent third polymer or fluorine containing silane Made of liquid.3rd solvent of corresponding third polymer or fluorine containing silane is deionized water, methanol, ethanol, ethylene glycol, isopropyl One kind in alcohol, propyl alcohol, dimethylbenzene, toluene, chloroform, tetrahydrofuran, methyl ethyl ketone, acetone, hexamethylene, dimethyl acetamide It is or a variety of.Carried out according to the 3rd solvent that the selection of the characteristic of the material (third polymer or fluorine containing silane) of surface encapsulation layer is suitable Dissolving, it is ensured that gained feed liquid can preferably shaping obtains film like structures in pattern structure layer surface so that surface encapsulation Retain the shape characteristic of pattern structural layer after formable layer.
Further, the patterned polymer layer shape material has following characteristic：Water droplet or water-soluble drop are patterning Liquid-drop contact angle on polymer-layered material reaches less than 60 ° or more than 120 °.
Preferably, the water-soluble drop includes but is not limited to water paint, water-based ink, the acid-alkali salt that pH is 1~13 The aqueous solution, sweat, blood, urine.
Further, the patterned polymer layer shape material has following characteristic：Patterned polymer surpasses by 120min After one or more of destructions in sound strong destruction, 10000 mechanical bends destructions or 10000 mechanical friction, drop connects Feeler remains to be kept for less than 60 ° or more than 120 °.Including contact angle water droplet or water-soluble drop on patterned polymer surface Remain to be kept for less than 60 ° or more than 120 °.The patterned polymer layer shape material of the present invention has high structural stability, energy The mechanical wear for being resistant to high intensity is destroyed, and holding surface hydrophily or hydrophobicity are constant.
In order to which above-mentioned patterned polymer is prepared, present invention also offers a kind of preparation method, preferably to protect The picture on surface design of card patterned polymer material meets expected design, reaches good surface hydrophilic or hydrophobic performance increases By force.
A kind of method for preparing above-mentioned patterned polymer, comprises the following steps：
(1) pretreatment of polymer substrate：Polymer substrate's cleaning is clean, and the polymer substrate is thermoplastic One kind in property plastic foil or piece, caoutchouc elasticity film or piece.Preferably, with low temperature etc. after polymer substrate's cleaning is clean Gas ions processing.
(2) coating of pattern structural layer：Second polymer and hydrophobic inorganic nano-particle are mixed, matched somebody with somebody with the second solvent The solution that mass concentration is 0.1~30.0% is made, is coated on polymer substrate；Second polymer and inorganic nano-particle Mass ratio be 100:0~20:80；
(3) processing of pattern structural layer, after step 2 coating, temperature be 20~90 DEG C and relative humidity be 20~ 30~180min is handled under the conditions of 100%.
(4) curing process of surface encapsulation layer, in polymer substrate's dip-coating, spraying or the spin coating after step 3 is handled Surface encapsulation layer raw material, dry, take out cleaning after then being handled in superthermal hydrogen storage equipment, dry again, obtain described pattern Fluidized polymer.
Preparation method of the present invention will be patterned into the formation of structure sheaf and the solidification of pattern structural layer is carried out successively respectively, and Upper second polymer and inorganic nano-particle material are combined in pattern structural layer, utilizes 20~90 DEG C of temperature and relative humidity The raw material of 20~100% condition pattern Processing structure sheaf coating, is allowed to form excellent pattern structure, realizes bionical knot The design printing of structure.Upper encapsulated layer raw material finally is combined in pattern structure layer surface, cured pattern structure sheaf, forms surface Continuous laminate structure, while pattern structural layer form is retained, stable encapsulating structure is realized, reach enhancing patterning The purpose of polymeric material performance.
The preparation method of patterned polymer of the present invention includes the pretreatment of polymer substrate, the painting of pattern structural layer Cover, the processing of pattern structural layer, the curing process of surface encapsulation layer.Patterned polymer of the present invention has without thing Manage template, the advantages that patterning is regular controllable, pattern dimension area is big.
The method that the present invention prepares the patterned polymer, with universality is strong, technique is simply easy to actual production, life Low cost and other advantages are produced, the surface waterproofing in the fields such as electronics industry, printing industry, microfluid preparations, bio-medical/resist can be met The practical application requests such as dirt, automatically cleaning, the polymer patterning template of low cost.
Further, the pretreatment of step (1) polymer substrate.Being during polymer substrate's cleaning is clean will be more Hole base material soaks 5~60min with ethanol, and 5~60min is then dried at a temperature of 20~90 DEG C；Then 5 are soaked with deionized water ~60min, 5~60min is then dried at a temperature of 20~90 DEG C.Then 2~10s of Low Temperature Plasma Treating is used.
Further, the coating of step (2) pattern structural layer.Second polymer and hydrophobic inorganic nano-particle are mixed, The matter of solution, wherein second polymer and inorganic nano-particle that mass concentration is 0.1~30.0% is configured to the second solvent Amount ratio is 100:0~20:80；Then, the polymeric substrate pre-processed by step (1) is coated in by 5~3600s of dip-coating On layer, then take out standby.
Further, the processing of step (3) pattern structural layer.It will exist by the polymer substrate after step (2) coating Temperature be 20~90 DEG C and relative humidity be 20~100% under the conditions of handle 30~180min.
Further, the curing process of step (4) surface encapsulation layer.Surface is configured to using third polymer or fluorine containing silane Encapsulated layer material solution, the mass concentration of solution is 0.1~30.0%, and surplus is the 3rd solvent.By 5~3600s of dip-coating or Spray 2~180s to be coated on the polymer substrate by the processing of step (3) pattern structural layer, then in 20~90 DEG C of temperature Degree is lower to dry 5~120min, is then 100~300V in voltage, vacuum is to locate in 0.05~0.15Pa superthermal hydrogen storage equipment Taking-up soaks 5~60min with ethanol after managing 5~120s, and 5~60min is then dried at a temperature of 20~90 DEG C；Then spend from Sub- water soaks 5~60min, and it is that described patterning polymerization is prepared that 5~60min is then dried at a temperature of 20~90 DEG C Thing.
Preferably, step 4, the surface encapsulation layer is third polymer or the film layer or film of fluorine containing silane shaping.
Preferably, the third polymer is polyacrylic acid, chitosan quaternary ammonium salt, polyethylene glycol, ethyl-hydroxyethyl fiber Element, carbomer, polytetrafluoroethylene (PTFE), polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl silicone rubber, methyl ethylene benzene One or more in base silicon rubber, methyl ethylene trifluoro propyl silicon rubber.
Preferably, described fluorine containing silane is 1H, 1H, 2H, 2H- perfluoro capryls trimethoxy silane, 1H, 1H, 2H, 2H- Perfluoro capryl triethoxysilane, 1H, 1H, 2H, 2H- perfluoro decyls trimethoxy silane, 1H, 1H, 2H, 2H- perfluoro decyls three One or more in Ethoxysilane.
Compared with prior art, beneficial effects of the present invention：
1. patterned polymer layer shape material of the present invention prepares pattern structural layer in polymeric substrate layer surface, figure is utilized Case structure sheaf is designed to the stereoscopic pattern of polymer surfaces, overcomes existing patterning techniques means patterned area to be present It is small or need multi-step to handle or the deficiencies of equipment cost is high or patterning is uncontrollable, realize different polymer surfaces Pattern.
2. the present invention is closed with surface encapsulation layer, coordinate hydrophily or hydrophobic function material, realize microscopic appearance The effect being be combined with each other with functional material, the effect that there is the close and distant wettability of bionics to improve enhancing, can give play to breakthrough The humidification of general material surface characteristic, has important practical application of significance.
3. the present invention provides a kind of New Type Large Area of non-traditional loose structure raised bowl-shape pattern structure, provide simultaneously Composite patterning techniques a kind of based on thermoset polymer system and containing inorganic nano-particle.It will be patterned into structure Layer bionical generation on substrate layer, and upper encapsulated layer raw material is combined, stable encapsulating structure is formed, reaches enhancing patterning polymerization The purpose of thing material property.
Brief description of the drawings：
Fig. 1：The SEM result (embodiment 3) on large area porous design surface
Fig. 2：Contact angle 0 ° (embodiment 3) of the water droplet on large area porous design surface
Fig. 3：The SEM result (embodiment 4) on large area porous design surface
Fig. 4：The SEM result (embodiment 5) on large area groove pattern surface
Fig. 5：The SEM result (embodiment 6) on large area groove pattern surface
Fig. 6：The SEM result (embodiment 7) on the scattered bowl dress raised design surface of large area
Fig. 7：Contact angle 156 ° (embodiments 7) of the water droplet on the bowl dress raised design surface that large area is disperseed
Fig. 8：The SEM result (embodiment 9) on the scattered bowl dress raised design surface of large area
Fig. 9：Contact angle 125 ° (embodiments 9) of the water droplet on the bowl dress raised design surface that large area is disperseed
Figure 10：The SEM result (embodiment 10) on the scattered bowl dress raised design surface of large area
Figure 11：The SEM result (embodiment 11) on the scattered bowl dress raised design surface of large area
Embodiment
Make specific be described in detail to the present invention below by embodiment, it is necessary to it is pointed out here that, following examples are only used for The present invention is made and is further illustrated by, it is impossible to is interpreted as limiting the scope of the invention, the technology in the field Some nonessential modifications and adaptations that personnel make according to present invention to this, are regarded as protection scope of the present invention.
Embodiment 1：
Patterned polymer layer shape material
Patterned polymer layer shape material has trilaminate structure, the respectively polymer substrate of polyethylene, poly- third Alkene and silica 80：20 pattern structural layer and polyacrylic acid surface encapsulation layer.The pattern structural layer has scattered Bowl-shape bulge-structure.The surface encapsulation layer is the continuous thin layer for being covered in pattern structure layer surface, and retains patterning The encapsulated layer of structure sheaf shape.
Embodiment 2：
Prepare the inorganic nano-particle of coupling agent pretreatment
Inorganic nano-particle uses mass concentration to carry out 5~60min of immersion in advance for 0.1~5.0% coupling agent, then 5~60min is dried at a temperature of 20~90 DEG C, obtains the inorganic nano-particle of coupling agent modification, it is standby.Specific preparing raw material And parameter is as follows：
Embodiment 3：
Prepare patterned polymer layer shape material
Patterned polymer layer shape material is prepared according to following steps：
Step (1) will be that base material ethanol is soaked into 10min during the cleaning totally of polyethylene substrate layer, then 30 60min is dried at a temperature of DEG C；Then 10min is soaked with deionized water, 60min is then dried at a temperature of 30 DEG C.Then with low Isothermal plasma handles 10s.
Coupling of the step (2) by molecular weight for numbering 201 in 5000g/mol second polymer polypropylene and embodiment 2 The inorganic nano-particle of agent processing is according to 90:10 mass ratio mixing, is configured to mass concentration and is with (the second solvent) toluene 30.0% solution.Then, it is coated in by dip-coating 10s on the polymer substrate pre-processed by step (1), Ran Houqu Go out.
Step (3) is 30 DEG C in temperature by the polymer substrate after step (2) coating and relative humidity is 90% Under the conditions of handle 30min.
It for 100000g/mol third polymer is polyacrylic acid that step (4), which uses molecular weight, with (the 3rd solvent) go from Sub- water is configured to the surface encapsulation layer material solution that mass concentration is 0.5%.It is coated in by dip-coating 3600s and passes through step (3) On the polymer substrate of pattern structural layer processing, 120min is then dried at a temperature of 30 DEG C, is then 300V in voltage, Taking-up ethanol soaks 10min after 10s is handled in the superthermal hydrogen storage equipment that vacuum is 0.15Pa, is then dried at a temperature of 30 DEG C 60min；Then 10min is soaked with deionized water, it is that described patterning is prepared that 60min is then dried at a temperature of 30 DEG C Polymer.
＜ tests ＞
The patterned polymer configuration of surface being prepared using electron microscope observation, as a result as shown in figure 1, stratiform material The surface of material has significant porous design morphologic appearance, meets expected design.The liquid-drop contact angle on its surface is tested, as a result Water droplet is 0 ° in the contact angle of patterning stratiform material surface, as shown in Fig. 2 the surface encapsulation layer raw material with non-patterned processing Manufactured laminar film material is compared, and liquid-drop contact angle is significantly reduced, and shows that patterned process causes the property of stratified material Material hydrophilic of fine quality in common non-patterned processing.
Embodiment 4：
Prepare patterned polymer layer shape material
Patterned polymer layer shape material is prepared according to following steps：
Step (1) will be that base material ethanol is soaked into 20min, Ran Hou during the cleaning totally of polyvinyl chloride base material layer 50min is dried at a temperature of 40 DEG C；Then 20min is soaked with deionized water, 50min is then dried at a temperature of 40 DEG C.Then use Low Temperature Plasma Treating 8s.
Idol of the step (2) by molecular weight for numbering 202 in 80000g/mol second polymer polystyrene and embodiment 2 Join the particle of agent processing according to 80:20 mass ratio mixing, is configured to mass concentration and is with (the second solvent) tetrahydrofuran 20.0% solution.Then, it is coated in by dip-coating 60s on the polymer substrate pre-processed by step (1), Ran Houqu Go out.
Step (3) is 30 DEG C in temperature by the polymer substrate after step (2) coating and relative humidity is 80% Under the conditions of handle 60min.
It for 10000g/mol third polymer is polyethylene glycol that step (4), which uses molecular weight, with (the 3rd solvent) ethanol It is configured to the surface encapsulation layer material solution that mass concentration is 0.1%.It is coated in by spraying 180s by step (3) patterning On the polymer substrate of structure sheaf processing, 90min is then dried at a temperature of 40 DEG C, is then 250V in voltage, vacuum 20min is soaked to handle taking-up ethanol after 30s in 0.15Pa superthermal hydrogen storage equipment, 50min is then dried at a temperature of 40 DEG C； Then 20min is soaked with deionized water, it is that described patterning polymerization is prepared that 50min is then dried at a temperature of 40 DEG C Thing.
＜ tests ＞
The patterned polymer configuration of surface being prepared using electron microscope observation, as a result as shown in figure 3, stratiform material The surface of material has significant porous design morphologic appearance, meets expected design.The liquid-drop contact angle on its surface is tested, as a result Water-based ink is 0 ° in the contact angle of patterning stratiform material surface, and made of the surface encapsulation layer raw material of non-patterned processing Laminar film material is compared, and liquid-drop contact angle is significantly reduced, and shows patterned process so that the property of stratified material is better than The material hydrophilic of common non-patterned processing.
Embodiment 5：
Prepare patterned polymer layer shape material
Patterned polymer layer shape material is prepared according to following steps：
Step (1) will be that base material ethanol is soaked into 30min, Ran Hou during the cleaning totally of polystyrene base material layer 50min is dried at a temperature of 50 DEG C；Then 30min is soaked with deionized water, 50min is then dried at a temperature of 50 DEG C.Then use Low Temperature Plasma Treating 8s.
Second polymer polybutylene terephthalate (PBT) and embodiment 2 of the step (2) by molecular weight for 50000g/mol The particle of the coupling agent treatment of middle numbering 203 is according to 70:30 mass ratio mixing, matter is configured to (the second solvent) metacresol Measure the solution that concentration is 10.0%.Then, the polymer substrate pre-processed by step (1) is coated in by dip-coating 120s On, then take out.
Step (3) is 50 DEG C in temperature by the polymer substrate after step (2) coating and relative humidity is 60% Under the conditions of handle 90min.
It for 20000g/mol third polymer is poly- ethylhydroxyethylcellulose that step (4), which uses molecular weight, with the (the 3rd Solvent) isopropanol be configured to mass concentration be 5.0% surface encapsulation layer material solution.By dip-coating 1200s coated in process On the polymer substrate of step (3) pattern structural layer processing, 70min is then dried at a temperature of 50 DEG C, then in voltage For 200V, taking-up ethanol soaks 30min after handling 60s in the superthermal hydrogen storage equipment that vacuum is 0.1Pa, then in 50 DEG C of temperature Lower dry 50min；Then soak 30min with deionized water, then dried at a temperature of 50 DEG C 50min be prepared it is described Patterned polymer.
＜ tests ＞
The patterned polymer configuration of surface being prepared using electron microscope observation, as a result as shown in figure 4, stratiform material The surface of material has significant groove pattern morphologic appearance, meets expected design.The liquid-drop contact angle on its surface is tested, as a result The hydrochloride aqueous solution that pH is 2 is 0 ° in the contact angle of patterning stratiform material surface, and the surface encapsulation of non-patterned processing Laminar film material made of layer raw material is compared, and liquid-drop contact angle is significantly reduced, and shows that patterned process causes stratiform material The property of material is better than the material hydrophilic of common non-patterned processing.
Embodiment 6：
Prepare patterned polymer layer shape material
Patterned polymer layer shape material is prepared according to following steps：
Step (1) will be to soak base material with ethanol during the cleaning totally of polybutylene terephthalate (PBT) substrate layer 40min, 30min is then dried at a temperature of 50 DEG C；Then 40min is soaked with deionized water, is then dried at a temperature of 50 DEG C 30min.Then Low Temperature Plasma Treating 10s is used.
Second polymer polybutylene terephthalate (PBT) and embodiment 2 of the step (2) by molecular weight for 20000g/mol The particle of the coupling agent treatment of middle numbering 204 is according to 60:40 mass ratio mixing, matter is configured to (the second solvent) metacresol Measure the solution that concentration is 5.0%.Then, it is coated in by dip-coating 600s on the polymer substrate pre-processed by step (1), Then take out.
Step (3) is 70 DEG C in temperature by the polymer substrate after step (2) coating and relative humidity is 40% Under the conditions of handle 120min.
It for 50000g/mol third polymer is carbomer that step (4), which uses molecular weight, is matched somebody with somebody with (the 3rd solvent) propyl alcohol The surface encapsulation layer material solution that mass concentration is 8.0% is made.It is coated in by spraying 90s by step (3) patterning knot On the polymer substrate of structure layer processing, 60min is then dried at a temperature of 40 DEG C, is then 150V in voltage, vacuum is Taking-up soaks 40min with ethanol after 60s is handled in 0.1Pa superthermal hydrogen storage equipment, and 30min is then dried at a temperature of 50 DEG C；So 40min is soaked with deionized water afterwards, it is that described patterned polymer is prepared that 30min is then dried at a temperature of 50 DEG C.
＜ tests ＞
The patterned polymer configuration of surface being prepared using electron microscope observation, as a result as shown in figure 5, stratiform material The surface of material has significant groove pattern morphologic appearance, meets expected design.The liquid-drop contact angle on its surface is tested, as a result The sodium-chloride water solution that pH is 7 is 0 ° in the contact angle of patterning stratiform material surface, and the surface encapsulation of non-patterned processing Laminar film material made of layer raw material is compared, and liquid-drop contact angle is significantly reduced, and shows that patterned process causes stratiform material The property of material is better than the material hydrophilic of common non-patterned processing.
Embodiment 7：
Prepare patterned polymer layer shape material
Patterned polymer layer shape material is prepared according to following steps：
Step (1) will be that base material ethanol is soaked into 50min during the cleaning totally of Parylene C substrate layer, Then 30min is dried at a temperature of 60 DEG C；Then 50min is soaked with deionized water, 30min is then dried at a temperature of 60 DEG C. Then Low Temperature Plasma Treating 6s is used.
Molecular weight is numbering 205 in 20000g/mol second polymer polyvinylidene fluoride and embodiment 2 by step (2) Coupling agent treatment particle according to 50:50 mass ratio mixing, quality is configured to (the second solvent) dimethyl acetamide Concentration is 5.0% solution.Then, it is coated in by dip-coating 1200s on the polymer substrate pre-processed by step (1), Then take out.
Step (3) is 80 DEG C in temperature by the polymer substrate after step (2) coating and relative humidity is 30% Under the conditions of handle 180min.
It for 20000g/mol third polymer is polyvinylidene fluoride that step (4), which uses molecular weight, with (the 3rd solvent) Dimethyl acetamide is configured to the surface encapsulation layer material solution that mass concentration is 10.0%.By dip-coating 600s coated in process On the polymer substrate of step (3) pattern structural layer processing, 60min is then dried at a temperature of 60 DEG C, then in voltage For 150V, taking-up ethanol soaks 50min after handling 90s in the superthermal hydrogen storage equipment that vacuum is 0.05Pa, then in 60 DEG C of temperature Degree is lower to dry 30min；Then soak 50min with deionized water, then dried at a temperature of 60 DEG C 30min be prepared it is described Patterned polymer.
＜ tests ＞
The patterned polymer configuration of surface being prepared using electron microscope observation, as a result as shown in fig. 6, stratiform material The surface of material has significantly scattered bowl dress raised design morphologic appearance, meets expected design.Test the drop on its surface Contact angle, the sodium hydrate aqueous solution that as a result pH is 12 is 156 ° in the contact angle of patterning stratiform material surface, such as Fig. 7 institutes Show, with the surface encapsulation layer raw material of non-patterned processing made of laminar film material compare, liquid-drop contact angle is significantly carried Height, show that patterned process causes the property of stratified material to be better than the material hydrophobic of common non-patterned processing.
Embodiment 8：
Prepare patterned polymer layer shape material
Patterned polymer layer shape material is prepared according to following steps：
Step (1) will be that base material ethanol is soaked into 60min, Ran Hou during polyimide substrate layer cleaning totally 20min is dried at a temperature of 70 DEG C；Then 60min is soaked with deionized water, 20min is then dried at a temperature of 70 DEG C.Then use Low Temperature Plasma Treating 8s.
Molecular weight is numbering 206 in 50000g/mol second polymer dimethyl silicone rubber and embodiment 2 by step (2) Coupling agent treatment particle according to 50:50 mass ratio mixing, is configured to mass concentration and is with (the second solvent) toluene 3.0% solution.Then, it is coated in by dip-coating 2400s on the polymer substrate pre-processed by step (1), Ran Houqu Go out.
Step (3) is 90 DEG C in temperature by the polymer substrate after step (2) coating and relative humidity is 60% Under the conditions of handle 180min.
It for 5000g/mol third polymer is dimethyl silicone rubber that step (4), which uses molecular weight, with (the 3rd solvent) first Benzene is configured to the surface encapsulation layer material solution that mass concentration is 15.0%.Pass through step (3) pattern by spraying 30s and being coated in On the polymer substrate for changing structure sheaf processing, 40min is then dried at a temperature of 70 DEG C, is then 100V in voltage, vacuum Spend in the superthermal hydrogen storage equipment for 0.05Pa taking-up ethanol after handling 120s and soak 60min, then dried at a temperature of 70 DEG C 20min；Then 60min is soaked with deionized water, it is that described patterning is prepared that 20min is then dried at a temperature of 70 DEG C Polymer.
＜ tests ＞
The patterned polymer configuration of surface being prepared using electron microscope observation, as a result similar to shown in Fig. 6, layer The surface of shape material has significantly scattered bowl dress raised design morphologic appearance, meets expected design.Test its surface Liquid-drop contact angle, as a result urine is 132 ° in the contact angle of patterning stratiform material surface, and the surface envelope of non-patterned processing Laminar film material made of dress layer raw material is compared, and liquid-drop contact angle is significantly improved, and shows that patterned process causes stratiform The property of material is better than the material hydrophobic of common non-patterned processing.
Embodiment 9：
Prepare patterned polymer layer shape material
Patterned polymer layer shape material is prepared according to following steps：
Step (1) will be that base material ethanol is soaked into 60min during the cleaning totally of polyvinylidene fluoride substrate layer, so 10min is dried at a temperature of 90 DEG C afterwards；Then 60min is soaked with deionized water, 10min is then dried at a temperature of 90 DEG C.So Low Temperature Plasma Treating 8s is used afterwards.
Step (2) by molecular weight be 100000g/mol second polymer methyl vinyl silicone rubber and embodiment 2 in compile The particle of numbers 201 coupling agent treatment is according to 40:60 mass ratio mixing, it is dense to be configured to quality with (the second solvent) hexamethylene Spend the solution for 1.0%.Then, it is coated in by dip-coating 3600s on the polymer substrate pre-processed by step (1), so After take out.
Step (3) is 60 DEG C in temperature by the polymer substrate after step (2) coating and relative humidity is 60% Under the conditions of handle 120min.
It for 10000g/mol third polymer is methyl vinyl phenyl silicon rubber that step (4), which uses molecular weight, with ( Three solvents) dimethylbenzene be configured to mass concentration be 20.0% surface encapsulation layer material solution.By dip-coating 120s coated in warp Cross on the polymer substrate of step (3) pattern structural layer processing, 20min is then dried at a temperature of 90 DEG C, then in electricity Press as 200V, taking-up ethanol soaks 60min after handling 90s in the superthermal hydrogen storage equipment that vacuum is 0.05Pa, then at 90 DEG C At a temperature of dry 10min；Then 60min is soaked with deionized water, 10min is then dried at a temperature of 90 DEG C is prepared institute The patterned polymer stated.
＜ tests ＞
The patterned polymer configuration of surface being prepared using electron microscope observation, as a result as shown in figure 8, stratiform material The surface of material has significantly scattered bowl dress raised design morphologic appearance, meets expected design.Test the drop on its surface Contact angle, as a result water droplet patterning stratiform material surface contact angle be 125 °, as shown in figure 9, with non-patterned processing Laminar film material made of surface encapsulation layer raw material is compared, and liquid-drop contact angle is significantly improved, and shows that patterned process makes The property for obtaining stratified material is better than the material hydrophobic of common non-patterned processing.
Embodiment 10：
Prepare patterned polymer layer shape material
Patterned polymer layer shape material is prepared according to following steps：
Step (1) will be to soak base material with ethanol during the cleaning totally of methyl vinyl silicone rubber substrate layer 30min, 30min is then dried at a temperature of 70 DEG C；Then 30min is soaked with deionized water, is then dried at a temperature of 70 DEG C 30min.Then Low Temperature Plasma Treating 4s is used.
Step (2) by molecular weight be 80000g/mol second polymer methyl vinyl silicone rubber and embodiment 2 in compile The particle of numbers 202 coupling agent treatment is according to 30:70 mass ratio mixing, it is dense to be configured to quality with (the second solvent) hexamethylene Spend the solution for 1.0%.Then, it is coated in by dip-coating 1200s on the polymer substrate pre-processed by step (1), so After take out.
Step (3) is 40 DEG C in temperature by the polymer substrate after step (2) coating and relative humidity is 40% Under the conditions of handle 90min.
Step (4) uses fluorine containing silane 1H, 1H, 2H, 2H- perfluoro capryl trimethoxy silane, with (the 3rd solvent) ethanol It is configured to the surface encapsulation layer material solution that mass concentration is 30.0%.It is coated in by spraying 60s by step (3) patterning On the polymer substrate of structure sheaf processing, 50min is then dried at a temperature of 70 DEG C, is then 200V in voltage, vacuum 30min is soaked to handle taking-up ethanol after 60s in 0.1Pa superthermal hydrogen storage equipment, 30min is then dried at a temperature of 70 DEG C； Then 30min is soaked with deionized water, it is that described patterning polymerization is prepared that 30min is then dried at a temperature of 70 DEG C Thing.
＜ tests ＞
The patterned polymer configuration of surface being prepared using electron microscope observation, as a result as shown in Figure 10, stratiform The surface of material has significantly scattered bowl dress raised design morphologic appearance, meets expected design.Test the liquid on its surface Contact angle is dripped, the hydrochloride aqueous solution that as a result pH is 2 is 135 ° in the contact angle of patterning stratiform material surface, and non-patterned Laminar film material made of the surface encapsulation layer raw material of processing is compared, and liquid-drop contact angle is significantly improved, and shows to pattern Processing causes the property of stratified material to be better than the material hydrophobic of common non-patterned processing.
Embodiment 11：
Prepare patterned polymer layer shape material
Patterned polymer layer shape material is prepared according to following steps：
Step (1) will be by base material ethanol during the cleaning totally of methyl ethylene trifluoro propyl silicon rubber substrate layer 50min is soaked, 50min is then dried at a temperature of 60 DEG C；Then 50min is soaked with deionized water, then at a temperature of 60 DEG C Dry 50min.Then Low Temperature Plasma Treating 6s is used.
In second polymer methyl vinyl phenyl silicon rubber and embodiment 2 that molecular weight is 5000g/mol by step (2) The particle of the coupling agent treatment of numbering 204 is according to 20:80 mass ratio mixing, quality is configured to (the second solvent) dimethylbenzene Concentration is 0.5% solution.Then, it is coated in by dip-coating 600s on the polymer substrate pre-processed by step (1), so After take out.
Step (3) is 30 DEG C in temperature by the polymer substrate after step (2) coating and relative humidity is 80% Under the conditions of handle 60min.
Step (4) uses fluorine containing silane 1H, 1H, 2H, 2H- perfluoro decyl triethoxysilane, with (the 3rd solvent) toluene It is configured to the surface encapsulation layer material solution that mass concentration is 30.0%.It is coated in by dip-coating 30s and is patterned by step (3) On the polymer substrate of structure sheaf processing, 90min is then dried at a temperature of 50 DEG C, is then 300V in voltage, vacuum 50min is soaked to handle taking-up ethanol after 20s in 0.1Pa superthermal hydrogen storage equipment, 50min is then dried at a temperature of 60 DEG C； Then 50min is soaked with deionized water, it is that described patterning polymerization is prepared that 50min is then dried at a temperature of 60 DEG C Thing.
＜ tests ＞
The patterned polymer configuration of surface being prepared using electron microscope observation, as a result as shown in figure 11, stratiform The surface of material has significantly scattered bowl dress raised design morphologic appearance, meets expected design.Test the liquid on its surface Contact angle is dripped, the sodium hydrate aqueous solution that as a result pH is 12 is 138 ° in the contact angle of patterning stratiform material surface, and non-figure Laminar film material made of the surface encapsulation layer raw material of caseization processing is compared, and liquid-drop contact angle is significantly improved, and shows figure Caseization, which is handled, causes the property of stratified material to be better than the material hydrophobic of common non-patterned processing.

Claims (10)

1. a kind of patterned polymer layer shape material, the patterned polymer layer shape material includes at least trilaminate structure, Respectively polymer substrate, pattern structural layer and surface encapsulation layer；
The pattern structural layer has scattered bowl-shape bulge-structure, groove or loose structure；
The surface encapsulation layer is to be covered in pattern structure layer surface, and retains the encapsulated layer of pattern structural layer shape.
2. patterned polymer layer shape material according to claim 1, it is characterised in that the polymer substrate is thermoplastic Property plastic foil or piece, caoutchouc elasticity film or piece；
The material of the polymer substrate includes but is not limited to polyethylene, polypropylene, polyvinyl chloride, polystyrene, poly- to benzene Naphthalate, polybutylene terephthalate (PBT), Parylene C, polychlorostyrene are for meta-xylene, polychlorostyrene generation neighbour two Toluene, polyimides, polytetrafluoroethylene (PTFE), polyvinylidene fluoride, dimethyl silicone rubber, methyl vinyl silicone rubber, ethylene methacrylic One or more in base phenyl siloxane rubber, methyl ethylene trifluoro propyl silicon rubber.
3. patterned polymer layer shape material according to claim 1, it is characterised in that the pattern structural layer is by second Polymer is made, and 0 ~ 4 times of quality hydrophobic inorganic nano-particle is added with the second polymer.
4. patterned polymer layer shape material according to claim 3, it is characterised in that the second polymer is included but not It is limited to polyethylene, polypropylene, polyvinyl chloride, polystyrene, polyethylene terephthalate, polybutylene terephthalate Ester, Parylene C, polychlorostyrene are for meta-xylene, poly- chloro-o-xylene, polyimides, polytetrafluoroethylene (PTFE), poly- inclined difluoro Ethene, dimethyl silicone rubber, methyl vinyl silicone rubber, methyl vinyl phenyl silicon rubber, methyl ethylene trifluoro propyl silicon One kind in rubber；
The molecular weight of the second polymer is 5000 ~ 100000 g/mol；
The inorganic nano-particle is calcium carbonate, silica, titanium dioxide, carbon black, graphene, CNT, montmorillonite, oxygen Change the one or more in zinc, its size is 1 ~ 5000 nm.
5. patterned polymer layer shape material according to claim 1, it is characterised in that the inorganic nano-particle uses matter Measure the coupling agent that concentration is 0.1 ~ 5.0% and carry out 5 ~ 60 min of immersion in advance, 5 ~ 60 are then dried at a temperature of 20 ~ 90 DEG C min。
6. patterned polymer layer shape material according to claim 5, it is characterised in that the coupling agent is silane coupler Or titanate coupling agent.
7. patterned polymer layer shape material according to claim 1, it is characterised in that the material of the surface encapsulation layer is Third polymer or fluorine containing silane.
8. patterned polymer layer shape material according to claim 1, it is characterised in that the third polymer is polypropylene Acid, chitosan quaternary ammonium salt, polyethylene glycol, ethylhydroxyethylcellulose, carbomer, polytetrafluoroethylene (PTFE), polyvinylidene fluoride, diformazan One in base silicon rubber, methyl vinyl silicone rubber, methyl vinyl phenyl silicon rubber, methyl ethylene trifluoro propyl silicon rubber Kind is several；
The molecular weight of the third polymer is 5000 ~ 100000 g/mol；
Described fluorine containing silane is 1H, 1H, 2H, 2H- perfluoro capryls trimethoxy silane, 1H, 1H, 2H, the second of 2H- perfluoro capryls three TMOS, 1H, 1H, 2H, 2H- perfluoro decyls trimethoxy silane, 1H, 1H, 2H, in 2H- perfluoro decyl triethoxysilanes One or more.
9. patterned polymer layer shape material according to claim 1, it is characterised in that the patterned polymer layer shape material Material has following characteristic：The liquid-drop contact angle of water droplet or water-soluble drop on patterned polymer layer shape material reach 60 ° with It is lower or more than 120 °.
10. a kind of method for preparing above-mentioned patterned polymer, comprises the following steps：
（1）The pretreatment of polymer substrate：Polymer substrate's cleaning is clean, and the polymer substrate is thermoplasticity modeling Expect one kind in film or piece, caoutchouc elasticity film or piece；
（2）The coating of pattern structural layer：Second polymer and hydrophobic inorganic nano-particle are mixed, are configured to the second solvent Mass concentration is 0.1 ~ 30.0% solution, is coated on polymer substrate；The quality of second polymer and inorganic nano-particle Ratio is 100:0~20:80；
（3）The processing of pattern structural layer, after step 2 coating, in temperature be 20 ~ 90 DEG C and relative humidity is 20 ~ 100% 30 ~ 180 min are handled under part；
（4）The curing process of surface encapsulation layer, polymer substrate's dip-coating, spraying or spin coating upper surface after step 3 is handled Encapsulated layer raw material, dry, take out cleaning after then being handled in superthermal hydrogen storage equipment, dry again, obtain described patterning and gather Compound.
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