CN109762276A - A kind of high dielectric constant full stress-strain composite hydrophobic material and preparation method thereof - Google Patents
A kind of high dielectric constant full stress-strain composite hydrophobic material and preparation method thereof Download PDFInfo
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Abstract
The present invention relates to nanometer composite technology fields, it is desirable to provide a kind of high dielectric constant full stress-strain composite hydrophobic material and preparation method thereof.The composite hydrophobic material is with dimethyl silicone polymer and poly- (vinylidene-trifluoro-ethylene) for matrix, using polystyrene microsphere as packing material, is made by being blended with spin coating proceeding;In described matrix, the mass ratio of dimethyl silicone polymer and poly- (vinylidene-trifluoro-ethylene) is 2: 3, and the packing material accounts for 5~30wt% of full stress-strain composite hydrophobic material gross mass.Nano pipe/polyhenylethylene microballoon, which is added, in the present invention in having polymeric matrix can enhance interfacial polarization effect, construct micro- rough surface, improve the dielectric constant of composite material, and keep excellent hydrophobic performance.Preparation process is simple, and the operability and repeatability of method are high.By adjusting the addition content of PS, it is able to achieve dielectric, the performances such as the hydrophobic regulation of composite material, simultaneously because pure organic matter is compound, flexibility better performances.
Description
Technical field
The present invention relates to a kind of high dielectric constant full stress-strain composite hydrophobic materials and preparation method thereof, belong to nano combined skill
Art field.
Background technique
Electrowetting as a kind of novel actuation technology for regulating and controlling conductive drop using voltage, have modification scope it is wide,
Respond it is sensitive and the features such as can reuse, in all kinds of micro-fluidic chips, display component and focus variable liquid lens
With extensive use.Jie's Electrowetting device is usually made of substrate, electrode, dielectric layer, this 4 parts of conductive drop.Wherein, it is situated between
Electric layer suffers from very big influence to Electrowetting device driving voltage and manufacture craft, it can substantially eliminate Electrolysis
Occur, while increasing voltage to the modification scope of conductive drop, is greatly promoted electrowetting in the application of every field.It is logical
Often, the dielectric constant of Electrowetting device driving voltage and dielectric layer is inversely.Therefore, preparation have preferable hydrophobic performance and
The dielectric layer of high dielectric constant is of great significance to electrowetting performance is improved.However, most hydrophobic polymerization at present
The dielectric constant of object material is lower, causes driving voltage high, influences the stability of Jie's Electrowetting device.
Dimethyl silicone polymer (PDMS) is a kind of thermoset rubber, has excellent translucency, elasticity, plasticity and dredges
It is aqueous, and film-forming process is simple, is only achieved with by spin coating with a thickness of micron-sized film.However, Jie of pure PDMS material
Electric constant is lower (less than 3), limits it in the application in the fields such as Jie's Electrowetting device, micro-fluidic chip.Poly- (vinylidene-
Trifluoro-ethylene) (P (VDF-TrFE)) be the bipolymer for being copolymerized and being generated by vinylidene and trifluoro-ethylene, have compared with
High dielectric constant (7.6-17.6), dissolves in general organic solvent, easily forms a film.But hydrophobic property compared with other organic materials compared with
It is low, generally at 100 ° or so.
Summary of the invention
The problem to be solved in the present invention is that overcome the deficiencies of the prior art and provide a kind of high dielectric constant full stress-strain compound
Hydrophobic material and preparation method thereof.
In order to solve the technical problem, the technical scheme adopted by the invention is that:
Mention a kind of high dielectric constant full stress-strain composite hydrophobic material, the composite hydrophobic material be with dimethyl silicone polymer and
Poly- (vinylidene-trifluoro-ethylene) is matrix, using polystyrene microsphere as packing material, is made by being blended with spin coating proceeding;
In described matrix, the mass ratio of dimethyl silicone polymer and poly- (vinylidene-trifluoro-ethylene) is 2: 3, and the packing material accounts for
5~30wt% of full stress-strain composite hydrophobic material gross mass.
Invention further provides the preparation methods of aforementioned full stress-strain composite hydrophobic material, comprising the following steps:
(1) using poly- (vinylidene-trifluoro-ethylene) powder and polystyrene microsphere as solute, with n,N-Dimethylformamide
For solvent;Mixing and mechanical stirring are carried out, solution A is obtained;Dimethyl silicone polymer is added in isopropanol, mixes and machinery stirs
After mixing, solution B is obtained;
(2) solution A and solution are taken for 3: 2 by the mass ratio of poly- (vinylidene-trifluoro-ethylene) and dimethyl silicone polymer
B is uniformly mixed;Then it is added silicone elastomer curing agent, the mass ratio of curing agent and dimethyl silicone polymer is 1: 10;It will
Mixed solution is placed in 50 DEG C of stirred in water bath, is then stirred at room temperature, obtains suspension;Suspension is vacuumized except degassing
Bubble, obtains blend solution;
(3) blend solution is coated on clean ito glass conducting surface by spin-coating method, after drying at room temperature, at 80 DEG C
Under dry and remove residual solvent, obtain with high dielectric constant full stress-strain composite hydrophobic material existing for form membrane.
In the present invention, in step (1), the dosage of polystyrene microsphere is controlled, it is made to account for composite hydrophobic material gross mass
5~30wt%.
In the present invention, in step (1), the solvents mass ratio of solution A is 1: 10;The solvents quality of solution B
Than being 1: 5.
In the present invention, in the step (2), the time stirred in a water bath is 0.5 hour;Be stirred at room temperature when
Between be 24 hours;The time vacuumized is 1 hour.
In the present invention, in the step (3), it is 24 that the dry time, which is the time dry at 12 hours, 80 DEG C, at room temperature
Hour.
In the present invention, the polystyrene microsphere is prepared by following methods:
(1) in mass ratio 3: 200 polyvinylpyrrolidone and deionized water are taken, mixes simultaneously mechanical stirring;
(2) in the case where being continuously injected into nitrogen, styrene is warming up to 70 DEG C;Then (the 2- first of 2,2- azo two is added
Base propyl miaow) dihydrochloride, the mass ratio of additional amount and styrene is 1: 40;Lasting stirring, reacts 24 hours;
(3) reaction product is cleaned with ethyl alcohol, carries out centrifugation drying, obtain polystyrene microsphere.
Compared with prior art, the beneficial effects of the present invention are:
1, the present invention prepares the polystyrene PS microballoon that diameter is about 251nm by polymerisation in solution.By solution blending,
Spin-coating method prepares full stress-strain laminated film.Nano pipe/polyhenylethylene microballoon is added in having polymeric matrix can enhance interfacial polarization
Effect constructs micro- rough surface, improve composite material dielectric constant (at 1KHz, 33.86) dielectric constant reaches as high as, and
Keep excellent hydrophobic performance (123 °~133 ° of hydrophobic angle).
2, preparation process of the present invention is simple, and the operability and repeatability of method are high.By adjusting the addition content of PS,
It is able to achieve dielectric, the performances such as the hydrophobic regulation of composite material, simultaneously because pure organic matter is compound, flexibility better performances can
It is shown applied to electrowetting, the manufacture of the devices such as micro-fluidic chip, insulating substrate, there is wide development and application prospect.
Detailed description of the invention
Fig. 1 is the electromicroscopic photograph of polystyrene PS microballoon in the present invention.
Specific embodiment
Below with reference to embodiment and comparative example, the invention will be further described, and embodiment can make the professional skill of this profession
The present invention, but do not limit the invention in any way is more fully understood in art personnel.
Embodiment 1-8
(1) progress machinery in three-neck flask is added in 1.5g polyvinylpyrrolidone (PVP) and 100mL deionized water to stir
It mixes.Secondly, in the case where being continuously injected into nitrogen, by 10g styrene (C8H8) it is added to the three necks burning in the water-bath for being placed in 70 DEG C
Bottle.Then, 2, the 2- azo two of 0.25g (2- methyl-propyl miaow) dihydrochloride (AIBA) is added in reaction unit and is kept
Stirring 24 hours.Finally, by ethyl alcohol clean and be centrifuged drying obtain polystyrene microsphere (PS microballoon, partial size about 251nm, such as
Shown in Fig. 1).
(2) poly- (vinylidene-trifluoro-ethylene) powder (P (VDF-TrFE)) and PS microballoon are pressed into solvents mass ratio 1:
10 are dissolved in DMF (n,N-Dimethylformamide) and stir evenly, and obtain solution A.And by PDMS (dimethyl silicone polymer)
It is dissolved in isopropanol and is stirred evenly by solvents mass ratio 1: 5, obtain solution B.
(3) solution A and solution are taken for 3: 2 by the mass ratio of poly- (vinylidene-trifluoro-ethylene) and dimethyl silicone polymer
B is uniformly mixed;Silicone elastomer curing agent is added (mass ratio of curing agent and dimethyl silicone polymer is 1: 10).Then
Mixed solution is placed in 50 DEG C of stirred in water bath 0.5 hour, is then stirred at room temperature 24 hours.
(4) step (3) obtained suspension is vacuumized into 1 hour removing bubble under vacuum conditions, it will by spin coating
Blend solution is coated on clean ito glass conducting surface, is dried at room temperature for 12 hours, is continued 24 hours dry at 80 DEG C
To remove residual solvent, obtain with high dielectric constant full stress-strain composite hydrophobic material existing for form membrane.
The composite hydrophobic material is with dimethyl silicone polymer and poly- (vinylidene-trifluoro-ethylene) for matrix, with polyphenyl
Ethylene microballoon is packing material, is made by being blended with spin coating proceeding;In described matrix, dimethyl silicone polymer and poly- (inclined fluorine
Ethylene-trifluoroethylene) mass ratio be 2: 3.The preparation method the step of in (2), the additive amount of packing material is controlled, keeps PS micro-
Ball packing material accounts for 5wt%~30wt% of composite hydrophobic material gross mass (specific data are shown in Table 1).According to PS in step (2)
The difference of microballoon usage amount, PS microspheres amount is also different in blend solution used in spin coating.
Test mode:
With high dielectric constant full stress-strain composite hydrophobic material surface existing for form membrane, thickness is plated by vacuum coating equipment
The proof gold that degree is 100nm, diameter is 4mm carries out subsequent electrical performance testing as electrode.
Comparative example 9
(1) polydimethylsiloxane is dissolved in aqueous isopropanol by solvents mass ratio 1: 5, magnetic agitation 24
Hour;184 curing agent of Sygard (mass ratio of curing agent and dimethyl silicone polymer is 1: 10) is added in PDMS solution, then
It is stirred 0.5 hour in 50 DEG C of water-baths, is then stirred at room temperature 24 hours and obtains uniformly mixed clarified solution;
(2) clarified solution is vacuumized to 1 hour removing bubble under vacuum conditions, is later spun on clarified solution clean
It on the conducting surface of ito glass, is dried at room temperature for 12 hours, dries 24 hours at 80 DEG C then to remove residual solvent.
(3) it is plated by vacuum coating equipment in the film surface of ito glass with a thickness of 100nm, diameter is 4mm proof gold as electricity
Pole carries out subsequent electrical performance testing.
Comparative example 10
(1) P (VDF-TrFE) is dissolved in DMF (n,N-Dimethylformamide) solution by solvents mass ratio 1:5, magnetic
Power stirs 48 hours;
(2) clarified solution is vacuumized to 1 hour removing bubble under vacuum conditions, is then spun on clarified solution clean
It on the conducting surface of ito glass, is dried at room temperature for 12 hours, dries 24 hours at 80 DEG C then to remove residual solvent.
(3) it is plated by vacuum coating equipment in the film surface of ito glass with a thickness of 100nm, diameter is 4mm proof gold as electricity
Pole carries out subsequent electrical performance testing.
Comparative example 11
(1) polydimethylsiloxane is dissolved in aqueous isopropanol by solvents mass ratio 1: 5, magnetic agitation 24
Hour, obtain solution 1;And it is molten that P (VDF-TrFE) by solvents mass ratio 1:5 is dissolved in DMF (n,N-Dimethylformamide)
In liquid, magnetic agitation 24 hours, solution 2 is obtained;Solution 1 and solution 2 are mixed be added 184 curing agent of Sygard (curing agent with
The mass ratio of dimethyl silicone polymer is 1: 10), stirring 0.5 hour, be then stirred at room temperature 24 hours in 50 DEG C of water-baths
Obtain uniformly mixed clarified solution.
(2) clarified solution is vacuumized to 1 hour removing bubble under vacuum conditions, is then spun on clarified solution clean
It on the conducting surface of ito glass, is dried at room temperature for 12 hours, dries 24 hours at 80 DEG C then to remove residual solvent.
(3) it is plated by vacuum coating equipment in the composite film surface of ito glass with a thickness of 100nm, diameter is 4mm proof gold work
For electrode, subsequent electrical performance testing is carried out.
Table 1: the composition and performance table of different formulations in each embodiment
Implementation result
Fig. 1 is that the TEM of PS microballoon prepared by the present invention schemes, it can be seen that the PS Microsphere Size prepared is uniform, is uniformly dispersed,
Diameter is about 251nm.From table 1 it follows that compared with PDMS, P (VDF-TrFE) and PDMS/P (VDF-TrFE), this hair
Full stress-strain composite hydrophobic material dielectric constant with higher (reaching as high as 33.86) provided by bright and preferable hydrophobic angle
(reaching as high as 133.4 °), and the operability of method and repeatability are high, can be applied to electrowetting show, micro-fluidic chip,
The manufacture of the devices such as insulating substrate.
Claims (7)
1. a kind of high dielectric constant full stress-strain composite hydrophobic material, which is characterized in that the composite hydrophobic material is with poly dimethyl
Siloxanes and poly- (vinylidene-trifluoro-ethylene) are matrix, using polystyrene microsphere as packing material, by being blended and spin coating work
Skill is made;In described matrix, the mass ratio of dimethyl silicone polymer and poly- (vinylidene-trifluoro-ethylene) is 2: 3, the filling
Material accounts for 5~30wt% of full stress-strain composite hydrophobic material gross mass.
2. the preparation method of full stress-strain composite hydrophobic material described in claim 1, which comprises the following steps:
It (1) is molten with n,N-Dimethylformamide using poly- (vinylidene-trifluoro-ethylene) powder and polystyrene microsphere as solute
Agent obtains solution A after mixing and mechanical stirring;Dimethyl silicone polymer is added in isopropanol, after mixing simultaneously mechanical stirring,
Obtain solution B;
(2) solution A and solution B are taken for 3: 2 by the mass ratio of poly- (vinylidene-trifluoro-ethylene) and dimethyl silicone polymer, mixed
It closes uniform;Then it is added silicone elastomer curing agent, the mass ratio of curing agent and dimethyl silicone polymer is 1: 10;It will mixing
Solution is placed in 50 DEG C of stirred in water bath, is then stirred at room temperature, obtains suspension;Suspension is vacuumized into removing bubble, is obtained
To blend solution;
(3) blend solution is coated on clean ito glass conducting surface by spin-coating method, after drying at room temperature, is done at 80 DEG C
Dry removing residual solvent is obtained with high dielectric constant full stress-strain composite hydrophobic material existing for form membrane.
3. method according to claim 1, which is characterized in that in step (1), control the use of polystyrene microsphere
Amount, makes it account for 5~30wt% of composite hydrophobic material gross mass.
4. method according to claim 1, which is characterized in that in step (1), the solvents mass ratio of solution A
It is 1: 10;The solvents mass ratio of solution B is 1: 5.
5. method according to claim 1, which is characterized in that in the step (2), the time stirred in a water bath is
0.5 hour;The time being stirred at room temperature is 24 hours;The time vacuumized is 1 hour.
6. method according to claim 1, which is characterized in that in the step (3), the dry time is 12 at room temperature
Hour, the dry time is 24 hours at 80 DEG C.
7. according to method described in 1 to 6 any one of claims, which is characterized in that the polystyrene microsphere passes through
Following methods prepare:
(1) in mass ratio 3: 200 polyvinylpyrrolidone and deionized water are taken, mixes simultaneously mechanical stirring;
(2) in the case where being continuously injected into nitrogen, styrene is warming up to 70 DEG C;Then (the 2- methyl-prop of 2,2- azo two is added
Base miaow) dihydrochloride, the mass ratio of additional amount and styrene is 1: 40;Lasting stirring, reacts 24 hours;
(3) reaction product is cleaned with ethyl alcohol, carries out centrifugation drying, obtain polystyrene microsphere.
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Cited By (5)
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CN110564280A (en) * | 2019-08-20 | 2019-12-13 | 国电新能源技术研究院有限公司 | Double-component fluorine-containing hydrophobic coating and preparation and use methods thereof |
CN112920605A (en) * | 2020-11-10 | 2021-06-08 | 金冠电气股份有限公司 | Silicone rubber composite material for bonding polybutylene terephthalate |
CN113136042A (en) * | 2021-03-21 | 2021-07-20 | 浙江大学 | Triboelectric energy conversion device based on CTAB modified polystyrene composite P (VDF-TrFE) |
CN113307996A (en) * | 2021-05-20 | 2021-08-27 | 西安理工大学 | Preparation method of flexible composite membrane with hydrophobicity and low dielectric constant |
CN114146739A (en) * | 2021-12-17 | 2022-03-08 | 北京理工大学 | DMF dielectric layer film laminating method and system and digital microfluidic chip |
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Cited By (7)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110564280A (en) * | 2019-08-20 | 2019-12-13 | 国电新能源技术研究院有限公司 | Double-component fluorine-containing hydrophobic coating and preparation and use methods thereof |
CN112920605A (en) * | 2020-11-10 | 2021-06-08 | 金冠电气股份有限公司 | Silicone rubber composite material for bonding polybutylene terephthalate |
CN113136042A (en) * | 2021-03-21 | 2021-07-20 | 浙江大学 | Triboelectric energy conversion device based on CTAB modified polystyrene composite P (VDF-TrFE) |
CN113136042B (en) * | 2021-03-21 | 2021-12-07 | 浙江大学 | Triboelectric energy conversion device based on CTAB modified polystyrene composite P (VDF-TrFE) |
CN113307996A (en) * | 2021-05-20 | 2021-08-27 | 西安理工大学 | Preparation method of flexible composite membrane with hydrophobicity and low dielectric constant |
CN113307996B (en) * | 2021-05-20 | 2023-03-10 | 西安理工大学 | Preparation method of flexible composite membrane with hydrophobicity and low dielectric constant |
CN114146739A (en) * | 2021-12-17 | 2022-03-08 | 北京理工大学 | DMF dielectric layer film laminating method and system and digital microfluidic chip |
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