CN108117833A - Titanium dioxide/polymer composite dielectric hydrophobic material and preparation method - Google Patents
Titanium dioxide/polymer composite dielectric hydrophobic material and preparation method Download PDFInfo
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- C09D183/00—Coating compositions based on 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; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
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- C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
- C03C17/34—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions
- C03C17/42—Surface treatment of glass, not in the form of fibres or filaments, by coating with at least two coatings having different compositions at least one coating of an organic material and at least one non-metal coating
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/44—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the composition of the continuous phase
- C03C2217/445—Organic continuous phases
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- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/465—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase having a specific shape
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2217/00—Coatings on glass
- C03C2217/40—Coatings comprising at least one inhomogeneous layer
- C03C2217/43—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase
- C03C2217/46—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase
- C03C2217/47—Coatings comprising at least one inhomogeneous layer consisting of a dispersed phase in a continuous phase characterized by the dispersed phase consisting of a specific material
- C03C2217/475—Inorganic materials
- C03C2217/477—Titanium oxide
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- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C2218/00—Methods for coating glass
- C03C2218/10—Deposition methods
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- C03C2218/116—Deposition methods from solutions or suspensions by spin-coating, centrifugation
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
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Abstract
The present invention relates to nanocomposite technologies, it is desirable to provide a kind of titanium dioxide/polymer composite dielectric hydrophobic material and preparation method.The dielectric hydrophobic material is using dimethyl silicone polymer as polymeric matrix, using titanium dioxide nano thread as packing material, is made by blending and spin coating proceeding;The packing material accounts for 5~30wt% of dielectric hydrophobic material gross mass.The titanium dioxide nano thread that the present invention is prepared by hydro-thermal method, diameter is in 100 rans, and length is in 8 microns.By the titanium dioxide nano thread of the present invention for solution blending spin coating proceeding, the laminated film that titanium dioxide uniformly disperses can be prepared.The titanium dioxide nano thread of high length-diameter ratio can increase inorganic filler/polymer interface interaction zone, realize the enhancing of interfacial polarization effect, improve the dielectric constant of composite material, keep relatively low dielectric loss and excellent hydrophobic properties of the surface.Preparation process of the present invention is simple, and the operability and repeatability of method are high.
Description
Technical field
The present invention relates to a kind of titanium dioxide/polymer composite dielectric hydrophobic material and preparation methods, belong to nano combined
Field of material technology.
Background technology
Electrowetting is as a kind of new actuation technology for regulating and controlling conductive drop using voltage, and modification scope is wide, response
It is sensitive and can reuse, have in all kinds of micro-fluidic chips, display component and focus variable liquid lens extensive
Using.Jie's Electrowetting device is generally made of 4 parts --- substrate, electrode, dielectric layer, conductive drop.Its dielectric layer pair
The driving voltage and manufacture craft of required application suffer from very big influence, it can significantly eliminate the generation of Electrolysis,
Increase modification scope of the voltage to conductive drop simultaneously, be greatly promoted application of the electrowetting in every field.In general, electricity profit
The dielectric constant of wet device drive voltage and dielectric layer is inversely.Therefore, preparing has preferable hydrophobic performance and high dielectric
The dielectric layer of constant is of great significance to improving electrowetting performance.However, current most hydrophobic polymer material
Dielectric constant it is relatively low, cause driving voltage high, influence the stability of Jie's Electrowetting device.
Dimethyl silicone polymer (Polydimethylsiloxane, PDMS) is a kind of thermoset rubber, has excellent dredge
Aqueous, translucency, elasticity and plasticity, and glass transition temperature is low, film-forming process is simple, can be made by simple spin coating
Thickness is micron-sized film.But the dielectric constant of pure PDMS material is relatively low (be less than 3), limit its Jie's Electrowetting device,
The application in the fields such as micro-fluidic chip.
The content of the invention
The problem to be solved in the present invention is to overcome deficiency of the prior art, and it is compound to provide a kind of titanium dioxide/polymer
Dielectric hydrophobic material and preparation method.
To solve technical problem, the technical solution adopted in the present invention is:
A kind of titanium dioxide/polymer composite dielectric hydrophobic material is provided, which is with poly dimethyl silicon
Oxygen alkane is polymeric matrix, using titanium dioxide nano thread as packing material, is made by blending and spin coating proceeding;The filling material
Material accounts for 5~30wt% of dielectric hydrophobic material gross mass.
In the present invention, the packing material is prepared by following methods:
(1) it is without water glycol, 100 milliliters of concentration by 2.5 grams of titanium dioxide, 12.5 milliliters of absolute ethyl alcohols, 12.5 milliliters
The sodium hydroxide solution of 10 mol/Ls is placed in 200 milliliters of hydrothermal reaction kettles, and stirring after ten minutes, is ultrasonically treated 10 minutes, then
Stirring 10 minutes;Then reaction kettle is moved in air dry oven, when isothermal reaction 48 is small under the conditions of 180 DEG C;
(2) sediment is taken out after reaction, when small with the concentrated hydrochloric acid immersion 6 of 37wt%;Sediment after immersion is used
After deionized water washing repeatedly, 60 DEG C of oven dryings are moved to, obtain presoma H2Ti3O7;
(3) by presoma H2Ti3O7When calcination 2 is small in air, calcination temperature is 600 DEG C, and final obtain is used as filling material
The titanium dioxide nano thread of material.
The present invention also provides the preparation method of aforesaid titanium dioxide/polymer composite dielectric hydrophobic material, including following
Step:
(1) in mass ratio 1: 4 is dissolved in dimethyl silicone polymer in hexamethylene, when magnetic agitation 0.5 is small;Then two are added in
Titanium oxide nano wire, when ultrasonic disperse 0.5 is small;It is again 1 by the mass ratio of dimethyl silicone polymer and curing agent:10 add in
184 curing agent of Sygard, stirred in 50 DEG C of water-baths 0.5 it is small when after be changed to stir at room temperature 5 it is small when, be uniformly mixed
Suspension;
(2) by suspension vacuumize 1 it is small when to remove bubble after, be spun on clean ito glass;Move in baking oven
When 120 DEG C of constant temperature 2 are small, cured titanium dioxide nano thread/dimethyl silicone polymer composite dielectric hydrophobic material is obtained.
In the present invention, first ito glass is cleaned:Ito glass is positioned in beaker, is cleaned by ultrasonic 5 points with acetone
Clock, then be cleaned by ultrasonic 5 minutes with absolute ethyl alcohol, it moves into convection oven and dries.
Compared with prior art, the beneficial effects of the present invention are:
1st, the titanium dioxide nano thread that the present invention is prepared by hydro-thermal method, diameter exist in 100 rans, length
8 microns.By the titanium dioxide nano thread of the present invention for solution blending-spin coating proceeding, titanium dioxide can be prepared
Homodisperse laminated film.The titanium dioxide nano thread of high length-diameter ratio can increase inorganic filler/polymer interface interaction
Region realizes the enhancing of interfacial polarization effect, improves the dielectric constant of composite material, keep relatively low dielectric loss and excellent table
Face hydrophobic performance.
2nd, preparation process of the present invention is simple, and the operability and repeatability of method are high.By adjusting nano titania
The addition content of line can realize dielectric, the performances such as the hydrophobic regulation and control of composite material, while its glass transition temperature is very low,
Can be applied to electrowetting show, the manufacture of the devices such as micro-fluidic chip, there is wide development and application prospect.
Description of the drawings
Fig. 1 is the electromicroscopic photograph of titanium dioxide nano thread.
Fig. 2 is the XRD diagram of titanium dioxide nano thread collection of illustrative plates and titanium dioxide nano thread/dimethyl silicone polymer.
Specific embodiment
With reference to embodiment and comparative example, the invention will be further described, and embodiment can make the professional skill of this specialty
The present invention, but do not limit the invention in any way is more fully understood in art personnel.
Embodiment 1-6
(1) by 2.5 grams of titanium dioxide, 12.5 milliliters of absolute ethyl alcohols, 12.5 milliliters are without water glycol, 100 milliliters of concentration
10 mol/L sodium hydroxides are placed in 200 milliliters of hydrothermal reaction kettles, are stirred 10 minutes, are ultrasonically treated 10 minutes, are stirred for 10 points
Clock.Then reaction kettle is put into air dry oven when isothermal reaction 48 is small under the conditions of 180 DEG C;
(2) after reaction, sediment is taken out, when small with the concentrated hydrochloric acid immersion 6 of 37wt%, the sediment after immersion is used
Deionized water washing is multiple, moves to 60 DEG C of oven dryings, obtains presoma H2Ti3O7;
(3) by presoma H2Ti3O7When calcination 2 is small in air, calcination temperature is 600 DEG C, and 5 DEG C/min of heating rate is obtained
White more fluffy titania powder (its microstructure be wire, such as Fig. 1).
(4) in mass ratio 1: 4 is dissolved in dimethyl silicone polymer in hexamethylene, when magnetic agitation 0.5 is small;Then by dioxy
Change titanium nano wire packing material to disperse in the solution, when supersound process 0.5 is small;Add Sygard 184 curing agent (poly- diformazans
The mass ratio of radical siloxane and curing agent is 1:10);When stirring 0.5 is small in 50 DEG C of water-baths, it is small that 5 are stirred at room temperature afterwards
When, obtain uniformly mixed suspension;
(5) by the suspension vacuumize under vacuum conditions 1 it is small when to remove bubble, suspension is spun on washes afterwards
On the conducting surface of net ito glass, when 120 DEG C of constant temperature 2 are small in convection oven, cured titanium dioxide nano thread/poly- is obtained
Dimethyl siloxane composite dielectric hydrophobic material;
(6) thickness is plated as 50nm in composite film surface by vacuum coating equipment, a diameter of 1mm proof gold as electrode, into
The follow-up electrical performance testing of row.
In step (4), control the additive amount of packing material, make its account for shaping after dielectric hydrophobic material gross mass 5~
30wt%;
In step (5), ito glass should be cleaned first, and specific method is as follows:First ito glass is positioned in beaker
It is cleaned by ultrasonic 5 minutes with acetone, is cleaned by ultrasonic 5 minutes with absolute ethyl alcohol again afterwards, is moved into convection oven and dry.
Comparative example (embodiment 7)
(1) in mass ratio 1: 4 is dissolved in dimethyl silicone polymer in hexamethylene, when magnetic agitation 0.5 is small;It adds
(mass ratio of dimethyl silicone polymer and curing agent is 1 to 184 curing agent of Sygard:10);0.5 is stirred in 50 DEG C of water-baths
Hour, be stirred at room temperature afterwards 5 it is small when, obtain uniformly mixed clarified solution;
(5) clarified solution is vacuumized under vacuum conditions 1 it is small when to remove bubble, clarified solution is spun on afterwards clean
On the conducting surface of ito glass, when 120 DEG C of constant temperature 2 are small in convection oven, it is hydrophobic to obtain cured dimethyl silicone polymer dielectric
Material;
(6) thickness is plated as 50nm in composite film surface by vacuum coating equipment, a diameter of 1mm proof gold as electrode, into
The follow-up electrical performance testing of row.
Implementation result is verified
Fig. 1 is TiO prepared by the present invention2SEM figure, it can be seen that the TiO prepared2Linear, size uniformity, diameter is about
For 100nm, length is in 8 microns.Fig. 2 is titanium dioxide nano thread collection of illustrative plates and titanium dioxide nano thread/polydimethylsiloxanes
The XRD diagram of alkane, the TiO as can be seen from the figure prepared2Crystal form is anatase (PDF#21-1272).Table 1 gives embodiment system
The test performance of standby obtained laminated film.As can be seen from the table, the dielectric constant of laminated film is in inorganics filled amount
Reach maximum during 20wt%, be 7.01 (100Hz), keep relatively low dielectric loss (100Hz, dielectric loss 0.059).Meanwhile
Sample contact angle reaches 116.1 under the loading0.Compared with dielectric properties (100Hz Jie of pure polydimethyl siloxane material
Electric constant=2.33, dielectric loss 0.141), the dielectric hydrophobic material dielectric constant that the present invention prepares significantly improves, dielectric
Be lost it is relatively low, meet electric moistening display part application requirement.
Table 1
It should be noted that above-described embodiment is only illustrative of the invention and is not intended to limit the scope of the invention.In addition
It is to be understood that after reading the content taught by the present invention, those skilled in the art can make the present invention various changes or repair
Change, these equivalent forms also fall within the scope of the appended claims of the present application.
Claims (4)
1. a kind of titanium dioxide/polymer composite dielectric hydrophobic material, which is characterized in that the dielectric hydrophobic material is with poly- diformazan
Radical siloxane is polymeric matrix, using titanium dioxide nano thread as packing material, is made by blending and spin coating proceeding;It is described to fill out
Fill 5~30wt% that material accounts for dielectric hydrophobic material gross mass.
2. the dielectric hydrophobic material according to claims 1, which is characterized in that the packing material passes through following methods system
It is standby to obtain:
(1) 2.5 grams of titanium dioxide, 12.5 milliliters of absolute ethyl alcohols, 12.5 milliliters are rubbed without water glycol, 100 milliliters of concentration for 10
You/liter sodium hydroxide solution be placed in 200 milliliters of hydrothermal reaction kettles, stirring after ten minutes, be ultrasonically treated 10 minutes, be stirred for
10 minutes;Then reaction kettle is moved in air dry oven, when isothermal reaction 48 is small under the conditions of 180 DEG C;
(2) sediment is taken out after reaction, when small with the concentrated hydrochloric acid immersion 6 of 37wt%;By the sediment after immersion spend from
After sub- water washing is multiple, 60 DEG C of oven dryings are moved to, obtain presoma H2Ti3O7;
(3) by presoma H2Ti3O7When calcination 2 is small in air, calcination temperature is 600 DEG C, final to obtain as packing material
Titanium dioxide nano thread.
3. the preparation method of titanium dioxide described in claim 1/polymer composite dielectric hydrophobic material, which is characterized in that including
Following steps:
(1) in mass ratio 1: 4 is dissolved in dimethyl silicone polymer in hexamethylene, when magnetic agitation 0.5 is small;Then titanium dioxide is added in
Titanium nano wire, when ultrasonic disperse 0.5 is small;It is again 1 by the mass ratio of dimethyl silicone polymer and curing agent:10 add in Sygard
184 curing agent, stirred in 50 DEG C of water-baths 0.5 it is small when after be changed to stir at room temperature 5 it is small when, obtain uniformly mixed suspended
Liquid;
(2) by suspension vacuumize 1 it is small when to remove bubble after, be spun on clean ito glass;It moves in baking oven 120
When DEG C constant temperature 2 is small, cured titanium dioxide nano thread/dimethyl silicone polymer composite dielectric hydrophobic material is obtained.
4. according to the method described in claim 2, it is characterized in that, first ito glass is cleaned:Ito glass is positioned over
In beaker, it is cleaned by ultrasonic 5 minutes with acetone, then is cleaned by ultrasonic 5 minutes with absolute ethyl alcohol, is moved into convection oven and dry.
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN110563347A (en) * | 2019-10-11 | 2019-12-13 | 湖北大学 | Preparation method of high-temperature-resistant liquid and boiling water super-smooth coating based on flower-shaped titanium dioxide nanoparticles |
CN113372589A (en) * | 2021-04-28 | 2021-09-10 | 王登鑫 | Preparation method of PDMS film containing nano particles |
CN114773959A (en) * | 2022-05-31 | 2022-07-22 | 复旦大学 | High-performance transparent anticorrosive coating material and preparation method thereof |
CN117979673A (en) * | 2024-03-29 | 2024-05-03 | 西北工业大学 | Anti-corrosion transparent electromagnetic shielding film and preparation method and application thereof |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN110563347A (en) * | 2019-10-11 | 2019-12-13 | 湖北大学 | Preparation method of high-temperature-resistant liquid and boiling water super-smooth coating based on flower-shaped titanium dioxide nanoparticles |
CN110563347B (en) * | 2019-10-11 | 2022-04-19 | 湖北大学 | Preparation method of high-temperature-resistant liquid and boiling water super-smooth coating based on flower-shaped titanium dioxide nanoparticles |
CN113372589A (en) * | 2021-04-28 | 2021-09-10 | 王登鑫 | Preparation method of PDMS film containing nano particles |
CN114773959A (en) * | 2022-05-31 | 2022-07-22 | 复旦大学 | High-performance transparent anticorrosive coating material and preparation method thereof |
CN114773959B (en) * | 2022-05-31 | 2023-03-03 | 复旦大学 | High-performance transparent anticorrosive coating material and preparation method thereof |
CN117979673A (en) * | 2024-03-29 | 2024-05-03 | 西北工业大学 | Anti-corrosion transparent electromagnetic shielding film and preparation method and application thereof |
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