CN108424543A - The preparation method of the force-responsive type surface folding of controllable light transmittance - Google Patents
The preparation method of the force-responsive type surface folding of controllable light transmittance Download PDFInfo
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- C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
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- C08J7/0427—Coating with only one layer of a composition containing a polymer binder
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2401/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2401/08—Cellulose derivatives
- C08J2401/26—Cellulose ethers
- C08J2401/28—Alkyl ethers
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2427/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers
- C08J2427/02—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment
- C08J2427/04—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Derivatives of such polymers not modified by chemical after-treatment containing chlorine atoms
- C08J2427/06—Homopolymers or copolymers of vinyl chloride
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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Abstract
The present invention relates to the preparation methods of the force-responsive type surface folding of controllable light transmittance, etch to form one layer of hydrophilic layer by carrying out oxygen gas plasma to transparent elastic substrates；One layer of rigid compound coating solution, drying and forming-film are coated on the elastic substrates surface of etching；Stress is discharged after stretching the duplicature prepared.The gauffer of material surface rule is obtained by above method.The present invention changes elastic substrates hydrophily using ion etching, surface forms the fold with regular shape by pre-stretching after coating rigid molecule film forming, by applying differently strained its transmitance to visible light of measurement to fold, the reversible transition of 6% 90% a wide range of regulation and control wrinkled surface light transmittance is realized.This method operating method is applied widely, easy to operate, good reversibility, can large area prepare, have potential application value in smart window subdomains.
Description
Technical field
Present invention design is related to the material surface fold that a kind of pervasive method prepares force-responsive type rule, and utilizes stress
Change material surface fold pattern, to achieve the purpose that a wide range of (6%-90%) regulates and controls the regulation and control of visible light transmittance, belongs to
In intellectual material field.
Background technology
The strong scattering process that the fold of material surface has light, the fold pattern by changing surface can be effective
The light transmittance of ground controlled material itself has control material surface fold quantity, side using stress changes material surface pattern
To the advantages such as time of, strain, there is important application in intelligent window field.
1998, Ned Bowden et al. were put forward for the first time the side that fold is prepared on dimethyl silicone polymer (PDMS)
Method, by depositing layer of metal film on the PDMS of thermal expansion, the compression generated using PDMS cooling meats is formed on surface
Fold (Nature 1998,393:16-149).By Seung Goo Lee et al. form nanometer using template on PDMS
Column, the PDMS that pre-stretching is then handled with ultraviolet and ozone form rigid film, and being prepared for surface after release stress has nano-pillar to repair
The fold of decorations realizes that light transmittance modification scope is about 25%-91% based on intelligent window prepared by the principle.
Mainly there are two processes for the preparation of material surface fold：(1) the different double membrane structure of Young's modulus is prepared；(2)
Fold is formed by applying certain compression to existing duplicature.But make work in the existing method for preparing fold
Skill is relative complex, and applicable material is relatively single, the deficiencies of being susceptible to crackle in cyclic process and cause cycle life poor, and
And minimum light transmission rate is regulated and controled by fold and can only achieve 10% or more, highest transmitance is 90% hereinafter, significantly limiting pleat
The application of wrinkle in practice.
Chinese patent document CN105905868A discloses a kind of processing method of nanoscale rule pleated structure.This method
Include mainly：Stretchable base material is chosen and prepared, is pre-stretched the stretchable base material using fixture, is utilized
The plasma etching of fluorine base gas grows fluorocarbon polymer material on the base material after the pre-stretching, will grown fluorine
The base material of carbon polymer material discharges, and obtains nanoscale rule pleated structure.This method has been successfully prepared 500nm or less
Regular fold, still, the fold of the size range is unable to the optical property of controlled material itself, and is needed in preparation process
First by elastic substrates growing surface material in a stretched state, operation difficulty in preparation process is increased.
Invention content
In view of the deficiencies of the prior art, the present invention provides a kind of preparation of the force-responsive type surface folding of controllable light transmittance
Method.The present invention can be utilized by changing regulation and control of the thickness realization of the size and film that are pre-stretched to fold and amplitude
A wide range of regulation and control of the visible light transmittance from 6% to 90% are realized in the strain of very little, and large-sized can be prepared, in intelligence
The fields such as window have potential application.
Technical scheme is as follows：
A kind of preparation method of the force-responsive type surface folding of controllable light transmittance, including steps are as follows：
(1) transparent elastic substrates surface is aoxidized using oxygen gas plasma, one layer of substrate surface drop coating after oxidation
Rigid molecule solution simultaneously removes evaporation of the solvent, and rigid molecule film is formed in substrate surface；It is 50%- to be subsequently placed in relative humidity
1h or more in 80% environment obtains rigid film-substrate duplicature；
(2) it will prepare and return to reset condition, finally in the fold of surface formation rule.
, according to the invention it is preferred to, elastic substrates described in step (1) be silicone elastomer, polyamide elastomer,
Polyolefin elastomer or polyurethane elastomer.
Preferably, light transmittance >=90% of the elastic substrates.
, according to the invention it is preferred to, rigid molecule described in step (1) be polyvinyl alcohol (PVA), chitosan (CS),
Polyethylene (PS), hydroxyethyl cellulose (HEC), polyvinyl chloride (PVC), polyvinylpyrrolidone (PVP), polyurethane or acetic acid are fine
Dimension is plain (CA)；
Preferably, a concentration of 1-10wt% of the rigid molecule solution；The solvent is water or dimethylacetamide
Amine.
, according to the invention it is preferred to, step (1) aoxidizes transparent elastic substrates surface process using oxygen gas plasma
In：Oxygen flow is 5-25ml/min, radio-frequency power 50-100W, etch period 20-200s.
, according to the invention it is preferred to, the temperature for removing evaporation of the solvent in step (1) is 20-70 DEG C；
Preferably, the time being placed in the environment that relative humidity is 50%-80% is 1-5h；Environment temperature is 20-25 DEG C.
, according to the invention it is preferred to, the size that rigid film-substrate duplicature is cut in step (2) is the rectangular of 1cm*4cm
Shape film.
, according to the invention it is preferred to, apply the strain that pulling force makes rigid film-substrate duplicature generate strain in step (2)
Degree is 20%-100%.
Transmitance in the present invention refers both to normal direction transmitance.
Beneficial effects of the present invention are as follows：
1, in the released state, duplicature is in opaque state to fold produced by the present invention, to having formed the film of fold
Applying the stretching strain of very little can make duplicature be changed into fully transparent state by opaque state.
2, the present invention realizes a wide range of regulation and control of the visible light transmittance from 6% to 90% using the strain of very little.
3, the present invention uses O2Plasmon etching changes flexible substrates hydrophily, after surface coats rigid molecule film forming
The fold with regular shape is formed by pre-stretching, by applying differently strained its transmission to visible light of measurement to fold
Rate realizes the reversible transition of a wide range of regulation and control wrinkled surface light transmittance of 6%-90%.By the strain for changing pre-stretching
The fold with different cycles and amplitude can be formed, realization regulates and controls the different fold of light transmittance sensitivity.
4, this method operating method is applied widely, and large-sized can prepare.Easy to operate, good reversibility can
Prepared by large area, have potential application value in smart window subdomains.
Description of the drawings
Fig. 1 is polyvinyl alcohol/purple of the dimethyl silicone polymer duplicature fold under different stress prepared by embodiment 1
Outside-transmission spectrum.
Fig. 2 is the macro of intelligent window prepared by polyvinyl alcohol/dimethyl silicone polymer duplicature fold prepared by embodiment 1
See digital photograph.
Specific implementation mode：
With reference to specific embodiments and the drawings, the present invention is described further, but not limited to this.
Experimental method described in following embodiments is unless otherwise specified conventional method simultaneously；The reagent and material
Material, unless otherwise specified, commercially obtains.
Embodiment 1：
A kind of preparation method of force-responsive type PVA/PDMS film folds, including steps are as follows：
(1) it is 10 in mass ratio by dimethyl silicone polymer presoma and crosslinking agent:1 uniformly mixing, takes 9g mixed liquors to fall
Enter in 90mm culture dishes, be heating and curing after vacuum exclusion bubble at 80 DEG C 2h, obtains dimethyl silicone polymer elastic substrates；
The above-mentioned dimethyl silicone polymer being cured is put into O2Oxidation processes in the chamber of plasma etching machine, work
Condition is：Oxygen flow is 10ml/min, radio-frequency power 100W, etch period 20s；
Polyvinyl alcohol (PVA) water-soluble drop-coated of the 3wt% of 3g on etched dimethyl silicone polymer, is shaken up
And vacuum exclude bubble after at 50 DEG C drying and forming-film, the transparent state of duplicature prepared；It is placed in relative humidity RH=
1h in 50% room temperature environment；
(2) the rectangle film for cutting 1cm*4cm applies the strain that tensile stress makes it generate 30% at both ends, discharges stress
Fold can be formed in film surface afterwards, film is in integrally opaque state.
Embodiment 2：
A kind of preparation method of force-responsive type PVA/PDMS film folds, including steps are as follows：
(1) it is 10 in mass ratio by dimethyl silicone polymer presoma and crosslinking agent:1 uniformly mixing, takes 9g mixed liquors to fall
Enter in 90mm culture dishes, be heating and curing after vacuum exclusion bubble at 80 DEG C 2h, obtains dimethyl silicone polymer elastic substrates；It will
The above-mentioned dimethyl silicone polymer being cured is put into O2Oxidation processes in the chamber of plasma etching machine, operating condition are：Oxygen
Throughput is 10ml/min, radio-frequency power 100W, etch period 20s；
By the polyvinyl alcohol water solution drop coating of the 3wt% of 0.09g on etched dimethyl silicone polymer, shake up simultaneously
Vacuum exclude bubble after at 50 DEG C drying and forming-film, the transparent state of duplicature prepared；It is placed in the room temperature of RH=70%
In environment after 1h；
(2) the rectangle film for cutting 1cm*4cm applies the strain that tensile stress makes it generate 10% at both ends, discharges stress
Fold can be formed in film surface afterwards, film is in integrally opaque state.
Embodiment 3：
A kind of preparation method of force-responsive type polyvinylpyrrolidone/PDMS film folds, including steps are as follows：
(1) it is 10 in mass ratio by dimethyl silicone polymer presoma and crosslinking agent:1 uniformly mixing, takes 4.4g mixed liquors
It pours into 60mm culture dishes, be heating and curing after vacuum exclusion bubble at 80 DEG C 2h, obtains dimethyl silicone polymer elastic substrates；
The above-mentioned dimethyl silicone polymer being cured is put into O2Oxidation processes in the chamber of plasma etching machine, operating condition are：
Oxygen flow is 10ml/min, radio-frequency power 100W, etch period 20s；
By 0.1g polyvinyl chloride powders solvent in 5ml dimethylacetamide solutions, 1g mixing drop-coated is taken to carve
On the dimethyl silicone polymer of erosion, shakes up and drying and forming-film, the duplicature prepared are at 50 DEG C after vacuum exclusion bubble
Pellucidity is placed in the room temperature environment of RH=30% after 1h；
(2) the rectangle film for cutting 1cm*4cm applies the strain that tensile stress makes it generate 20% at both ends, discharges stress
Fold can be formed in film surface, film is integrally translucent state afterwards.
Embodiment 4：
A kind of preparation method of force-responsive type hydroxyethyl cellulose (HEC)/PDMS membrane fold, including step
It is as follows：
(1) it is 10 in mass ratio by dimethyl silicone polymer presoma and crosslinking agent:1 uniformly mixing, takes 9g mixed liquors to fall
Enter in 90mm culture dishes, be heating and curing after vacuum exclusion bubble at 80 DEG C 2h, obtains dimethyl silicone polymer elastic substrates；It will
The above-mentioned dimethyl silicone polymer being cured is put into O2Oxidation processes in the chamber of plasma etching machine, operating condition are：Oxygen
Throughput is 10ml/min, radio-frequency power 100W, etch period 20s；
By the hydroxyethyl cellulose aqueous solution drop coating of the 0.6wt% of 3g on etched dimethyl silicone polymer, shake
Drying and forming-film, the transparent state of duplicature prepared are placed in RH=40%'s at 50 DEG C after even and vacuum exclusion bubble
In room temperature environment after 1h；
(2) the rectangle film for cutting 1cm*4cm applies the strain that tensile stress makes it generate 30% at both ends, discharges stress
Fold can be formed in film surface afterwards, film is in integrally opaque state.
Comparative example 1,
As described in Example 1, it is 10 in mass ratio by dimethyl silicone polymer presoma and crosslinking agent:1 uniformly mixing, takes
9g mixed liquors pour into 90mm culture dishes, and be heating and curing after vacuum exclusion bubble at 80 DEG C 2h, obtains dimethyl silicone polymer
Elastic substrates；
The above-mentioned dimethyl silicone polymer being cured is put into O2Oxidation processes in the chamber of plasma etching machine, work
Condition is：Oxygen flow is 10ml/min, radio-frequency power 100W, etch period 20s；
Polyvinyl alcohol (PVA) water-soluble drop-coated of the 3wt% of 3g on etched dimethyl silicone polymer, is shaken up
And vacuum exclude bubble after at 50 DEG C drying and forming-film, the transparent state of duplicature prepared；It is placed in relative humidity RH=
1h in 30% room temperature environment；
The rectangle film for cutting 1cm*4cm applies the strain that tensile stress makes it generate 30% at both ends.
Since upper layer rigid film elasticity modulus is excessive, duplicature is easy to be broken, and cannot form fold.
Comparative example 2
As described in Example 1, it is 10 in mass ratio by dimethyl silicone polymer presoma and crosslinking agent:1 uniformly mixing, takes
9g mixed liquors pour into 90mm culture dishes, and be heating and curing after vacuum exclusion bubble at 80 DEG C 2h, obtains dimethyl silicone polymer
Elastic substrates；
The above-mentioned dimethyl silicone polymer being cured is put into O2Oxidation processes in the chamber of plasma etching machine, work
Condition is：Oxygen flow is 30ml/min, radio-frequency power 100W, etch period 20s；
Polyvinyl alcohol (PVA) water-soluble drop-coated of the 3wt% of 3g on etched dimethyl silicone polymer, is shaken up
And vacuum excludes after bubble that drying and forming-film, the duplicature prepared are translucent pellucidity at 50 DEG C, light transmittance is less than
80%.
Comparative example 3,
As described in Example 1, it is 10 in mass ratio by dimethyl silicone polymer presoma and crosslinking agent:1 uniformly mixing, takes
9g mixed liquors pour into 90mm culture dishes, and be heating and curing after vacuum exclusion bubble at 80 DEG C 2h, obtains dimethyl silicone polymer
Elastic substrates；
The above-mentioned dimethyl silicone polymer being cured is put into O2Oxidation processes in the chamber of plasma etching machine, work
Condition is：Oxygen flow is 10ml/min, radio-frequency power 100W, etch period 20s；
By the polyvinyl alcohol water solution drop coating of the 3wt% of 0.09g on etched dimethyl silicone polymer, shake up simultaneously
Vacuum exclude bubble after at 50 DEG C drying and forming-film, the transparent state of duplicature prepared；It is placed in the room temperature of RH=90%
In environment after 1h；
Cut 1cm*4cm rectangle film, both ends apply tensile stress make its generate 30% strain, discharge stress after by
It is too low in rigid film elasticity modulus, fold cannot be formed on the surfaces PDMS.
Test example：
The film both ends that fold has been formed to embodiment 1,2,3,4 apply tensile stress again, with the increase of membrane strain, film
The fold on surface fades away, and when fold completely disappears, fully transparent state is presented in film, discharges tensile stress caudacoria again again
It is changed into opaque state, due to passing through O2Plasma hydrophilic treated significantly enhances the combination of rigid film and the surfaces PDMS
Power, film are recycled thousands of times under opaque-pellucidity.
Such as Fig. 1 shows embodiment 1, fold formed with disappear when transmitted spectrum variation.
Claims (10)
1. a kind of preparation method of the force-responsive type surface folding of controllable light transmittance, including steps are as follows：
(1) transparent elastic substrates surface is aoxidized using oxygen gas plasma, one layer of rigidity of substrate surface drop coating after oxidation
Molecular solution simultaneously removes evaporation of the solvent, and rigid molecule film is formed in substrate surface；It is 50%-80% to be subsequently placed in relative humidity
Environment in 1h or more, obtain rigid film-substrate duplicature；
(2) rigid film prepared-substrate duplicature is cut to required size and fixes both ends, applying pulling force makes just
Property film-substrate duplicature generate strain after slowly discharge stress, so that rigid film-substrate duplicature is returned to reset condition, finally
The fold of formation rule on surface.
2. the preparation method of the force-responsive type surface folding of controllable light transmittance according to claim 1, which is characterized in that
Elastic substrates described in step (1) are silicone elastomer, polyamide elastomer, polyolefin elastomer or elastic polyurethane
Body.
3. the preparation method of the force-responsive type surface folding of controllable light transmittance according to claim 1, which is characterized in that
Light transmittance >=90% of elastic substrates described in step (1).
4. the preparation method of the force-responsive type surface folding of controllable light transmittance according to claim 1, which is characterized in that
Rigid molecule described in step (1) is polyvinyl alcohol (PVA), chitosan (CS), polyethylene (PS), hydroxyethyl cellulose
(HEC), polyvinyl chloride (PVC), polyvinylpyrrolidone (PVP) or polyurethane or cellulose acetate (CA).
5. the preparation method of the force-responsive type surface folding of controllable light transmittance according to claim 1, which is characterized in that
A concentration of 1-10wt% of rigid molecule solution described in step (1).
6. the preparation method of the force-responsive type surface folding of controllable light transmittance according to claim 1, which is characterized in that
Step (1) is aoxidized using oxygen gas plasma in transparent elastic substrates surface process：Oxygen flow is 5-25ml/min, radio frequency
Power is 50-100W, etch period 20-200s.
7. the preparation method of the force-responsive type surface folding of controllable light transmittance according to claim 1, which is characterized in that
The temperature for removing evaporation of the solvent in step (1) is 20-70 DEG C.
8. the preparation method of the force-responsive type surface folding of controllable light transmittance according to claim 1, which is characterized in that
The time being placed in step (1) in the environment that relative humidity is 50%-80% is 1-5h, and environment temperature is 20-25 DEG C.
9. the preparation method of the force-responsive type surface folding of controllable light transmittance according to claim 1, which is characterized in that
The size that rigid film-substrate duplicature is cut in step (2) is the rectangle film of 1cm*4cm.
10. the preparation method of the force-responsive type surface folding of controllable light transmittance according to claim 1, feature exist
In it is 20%-100% to apply pulling force in step (2) rigid film-substrate duplicature is made to generate the degree of strain of strain.
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| CN110133841A (en) * | 2019-05-15 | 2019-08-16 | 河南科技大学 | The adjustable film of light transmittance and light transmittance regulating device |
| CN110374481A (en) * | 2019-07-30 | 2019-10-25 | 开县金石教育服务有限责任公司 | From discoloration window and its indoor environment regulating system |
| CN110646870A (en) * | 2019-01-22 | 2020-01-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Film with adjustable and controllable light transmittance, preparation method and application thereof |
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| CN113736267A (en) * | 2021-09-27 | 2021-12-03 | 世晨材料技术(上海)有限公司 | Reversibly-stretched shading organic silicon film and preparation method thereof |
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| CN109561597A (en) * | 2018-12-12 | 2019-04-02 | 浙江清华柔性电子技术研究院 | The preparation method of automatically cleaning compliant conductive route and flexible apparatus with it |
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| CN110646870A (en) * | 2019-01-22 | 2020-01-03 | 中国科学院苏州纳米技术与纳米仿生研究所 | Film with adjustable and controllable light transmittance, preparation method and application thereof |
| CN110133841A (en) * | 2019-05-15 | 2019-08-16 | 河南科技大学 | The adjustable film of light transmittance and light transmittance regulating device |
| CN110374481A (en) * | 2019-07-30 | 2019-10-25 | 开县金石教育服务有限责任公司 | From discoloration window and its indoor environment regulating system |
| CN113174580A (en) * | 2021-04-15 | 2021-07-27 | 清华大学 | Humidity-based film wrinkle shape regulation and control method |
| CN113739715A (en) * | 2021-08-26 | 2021-12-03 | 西安交通大学 | Flexible strain sensor based on fold structure color and preparation method thereof |
| CN113736267A (en) * | 2021-09-27 | 2021-12-03 | 世晨材料技术(上海)有限公司 | Reversibly-stretched shading organic silicon film and preparation method thereof |
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