CN107974013A - Titanium dioxide/PVDF-TrFE laminated films and preparation method thereof - Google Patents
Titanium dioxide/PVDF-TrFE laminated films and preparation method thereof Download PDFInfo
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- CN107974013A CN107974013A CN201610915895.0A CN201610915895A CN107974013A CN 107974013 A CN107974013 A CN 107974013A CN 201610915895 A CN201610915895 A CN 201610915895A CN 107974013 A CN107974013 A CN 107974013A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L27/00—Compositions 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; Compositions of derivatives of such polymers
- C08L27/02—Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L27/12—Compositions 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; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
- C08L27/16—Homopolymers or copolymers or vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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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
- C08J2327/00—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
- C08J2327/02—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
- C08J2327/12—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 fluorine atoms
- C08J2327/16—Homopolymers or copolymers of vinylidene fluoride
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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Abstract
This application discloses a kind of titanium dioxide/PVDF TrFE laminated films, including PVDF TrFE matrixes and the titanium dioxide that is doped in PVDF TrFE matrixes, the doping of the titanium dioxide is 10~35%.A kind of titanium dioxide/PVDF TrFE preparation method of composite film is also disclosed, including：(1), nano-titanium dioxide powder is prepared；(2), the nano-titanium dioxide powder of preparation is dissolved in DMF, adds PVP and PVDF TrFE, 20~30min of ultrasonic disperse under the conditions of 40~60 DEG C；(3), the solvent flashing under the conditions of 70~85 DEG C；(4), when 110~140 DEG C of annealing 3~5 are small, titanium dioxide/PVDF TrFE laminated films are obtained.The dielectric constant of laminated film prepared by the present invention reaches 21.3；By XRD analysis, the appropriate doping of titanium dioxide can improve the crystallinity of PVDF TrFE films, and crystallization temperature has brought up to 138~139 DEG C.
Description
Technical field
This application involves a kind of dielectric material, more particularly to a kind of titanium dioxide/PVDF-TrFE laminated films and its system
Preparation Method.
Background technology
Energy storage material has extraordinary storage electric charge and uniformly electricity as a kind of extensive functional form material of application prospect
Field function.Capacitor is a kind of important energy storage material, is widely used in the every field such as aviation, household electrical appliances, traffic, communication.
Dielectric substance is one important part of capacitor, and the energy-storage property of dielectric substance has been largely fixed capacitance
The performance of device.
Single dielectric substance has been difficult to meet industrialized needs.Quality is good, pliability is good, is easily processed into
The high polymer matrix composite of type, dielectric properties is widely used in capacitor, sensor, manually because of its excellent performance
The fields such as muscle.
The content of the invention
It is an object of the invention to provide a kind of titanium dioxide/PVDF-TrFE laminated films and preparation method thereof, to overcome
Deficiency of the prior art.
To achieve the above object, the present invention provides following technical solution：
The embodiment of the present application discloses a kind of titanium dioxide/PVDF-TrFE laminated films, including PVDF-TrFE matrixes and
The titanium dioxide being doped in PVDF-TrFE matrixes, the doping of the titanium dioxide is 10~35%.
Correspondingly, disclosed herein as well is a kind of titanium dioxide/PVDF-TrFE preparation method of composite film, including：
(1), nano-titanium dioxide powder is prepared；
(2), the nano-titanium dioxide powder of preparation is dissolved in DMF, PVP and PVDF-TrFE is added, at 40~60 DEG C
Under the conditions of 20~30min of ultrasonic disperse；
(3), the solvent flashing under the conditions of 70~85 DEG C；
(4), when 110~140 DEG C of annealing 3~5 are small, titanium dioxide/PVDF-TrFE laminated films are obtained.
Preferably, in above-mentioned titanium dioxide/PVDF-TrFE preparation method of composite film, in the step (1), system
Standby nano-titanium dioxide powder method includes：
S1, using dihydric alcohol as solvent, nitrogen protection is lower to add titanium tetrachloride, stirs to being uniformly mixed, then adds rotation
Evaporator, is heated to 160~200 DEG C, adds deionized water rotary evaporation, 5~10min of reflux；
S2 and then cold bath cooling stop reaction, obtain the clear solution containing nano-titanium dioxide, are added dropwise into solution
Acetone, stirring obtain white precipitate；
S3, filter sediment, washed, being dried to obtain nano-titanium dioxide；
The nano-titanium dioxide of acquisition, be ground by s4, then when 400~800 DEG C of calcinings 2~3 are small, obtains nanometer
Titanium dioxide powder.
Preferably, in above-mentioned titanium dioxide/PVDF-TrFE preparation method of composite film, in step s1, by volume
Deionized water：Titanium tetrachloride=2~4：1.
Compared with prior art, the advantage of the invention is that：The dielectric constant of laminated film prepared by the present invention reaches
21.3；By XRD analysis, the appropriate doping of titanium dioxide can improve the crystallinity of PVDF-TrFE films, and crystallization temperature improves
To 138~139 DEG C.
Embodiment
The present invention is described further by the following example：According to following embodiments, the present invention may be better understood.
However, as it will be easily appreciated by one skilled in the art that embodiment described specific material ratio, process conditions and its result are only used
In the explanation present invention, without the present invention described in detail in claims should will not be limited.
Embodiment 1
In the present embodiment, titanium dioxide/PVDF-TrFE laminated films, including PVDF-TrFE matrixes and be doped in
Titanium dioxide in PVDF-TrFE matrixes, the doping of the titanium dioxide is 13%.
Titanium dioxide/PVDF-TrFE preparation method of composite film：
(1), the preparation of nano-titanium dioxide powder：
Using dihydric alcohol as solvent, nitrogen protection is lower to add titanium tetrachloride, stirs to being uniformly mixed, then adds rotary evaporation
Device, is heated to 200 DEG C, adds deionized water rotary evaporation, reflux 10min, by volume deionized water：Titanium tetrachloride=3：1；
Then cold bath cooling stops reaction, obtains the clear solution containing nano-titanium dioxide, third is added dropwise into solution
Ketone, stirring obtain white precipitate；
Sediment is filtered, washed, is dried to obtain nano-titanium dioxide；
The nano-titanium dioxide of acquisition is ground, then when 600 DEG C of calcinings 3 are small, obtains nanometer titanium dioxide titanium valve
Body.
(2), the nano-titanium dioxide powder of preparation is dissolved in DMF, PVP and PVDF-TrFE is added, in 60 DEG C of conditions
Lower ultrasonic disperse 30min；
(3), the solvent flashing under the conditions of 85 DEG C；
(4), when 140 DEG C of annealing 3 are small, titanium dioxide/PVDF-TrFE laminated films are obtained.
The dielectric constant of laminated film manufactured in the present embodiment reaches 21.3；By XRD analysis, the appropriate of titanium dioxide is mixed
The miscellaneous crystallinity that can improve PVDF-TrFE films, crystallization temperature have brought up to 139 DEG C.
Embodiment 2
In the present embodiment, titanium dioxide/PVDF-TrFE laminated films, including PVDF-TrFE matrixes and be doped in
Titanium dioxide in PVDF-TrFE matrixes, the doping of the titanium dioxide is 27%.
Titanium dioxide/PVDF-TrFE preparation method of composite film：
(1), the preparation of nano-titanium dioxide powder：
Using dihydric alcohol as solvent, nitrogen protection is lower to add titanium tetrachloride, stirs to being uniformly mixed, then adds rotary evaporation
Device, is heated to 200 DEG C, adds deionized water rotary evaporation, reflux 5min, by volume deionized water：Titanium tetrachloride=4：1；
Then cold bath cooling stops reaction, obtains the clear solution containing nano-titanium dioxide, third is added dropwise into solution
Ketone, stirring obtain white precipitate；
Sediment is filtered, washed, is dried to obtain nano-titanium dioxide；
The nano-titanium dioxide of acquisition is ground, then when 800 DEG C of calcinings 3 are small, obtains nanometer titanium dioxide titanium valve
Body.
(2), the nano-titanium dioxide powder of preparation is dissolved in DMF, PVP and PVDF-TrFE is added, in 40 DEG C of conditions
Lower ultrasonic disperse 30min；
(3), the solvent flashing under the conditions of 70 DEG C；
(4), when 120 DEG C of annealing 5 are small, titanium dioxide/PVDF-TrFE laminated films are obtained.
The dielectric constant of laminated film manufactured in the present embodiment reaches 20.8；By XRD analysis, the appropriate of titanium dioxide is mixed
The miscellaneous crystallinity that can improve PVDF-TrFE films, crystallization temperature have brought up to 137.5 DEG C.
Finally, it is to be noted that, term " comprising ", "comprising" or its any other variant be intended to it is non-exclusive
Property includes, so that process, method, article or equipment including a series of elements not only include those key elements, but also
Further include other elements that are not explicitly listed, or further include for this process, method, article or equipment it is intrinsic
Key element.
Claims (4)
1. a kind of titanium dioxide/PVDF-TrFE laminated films, it is characterised in that including PVDF-TrFE matrixes and be doped in
Titanium dioxide in PVDF-TrFE matrixes, the doping of the titanium dioxide is 10~35%.
2. titanium dioxide/PVDF-TrFE preparation method of composite film described in claim 1, it is characterised in that including：
(1), nano-titanium dioxide powder is prepared；
(2), the nano-titanium dioxide powder of preparation is dissolved in DMF, PVP and PVDF-TrFE is added, in 40~60 DEG C of conditions
20~30min of lower ultrasonic disperse；
(3), the solvent flashing under the conditions of 70~85 DEG C；
(4), when 110~140 DEG C of annealing 3~5 are small, titanium dioxide/PVDF-TrFE laminated films are obtained.
3. titanium dioxide according to claim 2/PVDF-TrFE preparation method of composite film, it is characterised in that：The step
Suddenly in (1), preparing nano-titanium dioxide powder method includes：
S1, using dihydric alcohol as solvent, nitrogen protection is lower to add titanium tetrachloride, stirs to being uniformly mixed, then adds rotary evaporation
Device, is heated to 160~200 DEG C, adds deionized water rotary evaporation, 5~10min of reflux；
S2 and then cold bath cooling stop reaction, obtain the clear solution containing nano-titanium dioxide, third is added dropwise into solution
Ketone, stirring obtain white precipitate；
S3, filter sediment, washed, being dried to obtain nano-titanium dioxide；
The nano-titanium dioxide of acquisition, be ground by s4, then when 400~800 DEG C of calcinings 2~3 are small, obtains nano-silica
Change titanium valve body.
4. titanium dioxide according to claim 3/PVDF-TrFE preparation method of composite film, it is characterised in that：Step s1
In, deionized water by volume：Titanium tetrachloride=2~4：1.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610915895.0A CN107974013A (en) | 2016-10-21 | 2016-10-21 | Titanium dioxide/PVDF-TrFE laminated films and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610915895.0A CN107974013A (en) | 2016-10-21 | 2016-10-21 | Titanium dioxide/PVDF-TrFE laminated films and preparation method thereof |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675728A (en) * | 2012-05-23 | 2012-09-19 | 江苏大学 | Ultrahydrophobic polypropylene/titanium dioxide composite film and preparation method thereof |
| CN104310468A (en) * | 2014-10-14 | 2015-01-28 | 吉林大学 | Method for preparing monodisperse titanium dioxide (B) nano particles |
| CN105037764A (en) * | 2015-08-03 | 2015-11-11 | 铜陵市胜达电子科技有限责任公司 | Polyimide high-dielectric composite film mixed with nano-titanium dioxide-loaded tin antimony oxide and used for capacitor and preparation method thereof |
-
2016
- 2016-10-21 CN CN201610915895.0A patent/CN107974013A/en not_active Withdrawn
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102675728A (en) * | 2012-05-23 | 2012-09-19 | 江苏大学 | Ultrahydrophobic polypropylene/titanium dioxide composite film and preparation method thereof |
| CN104310468A (en) * | 2014-10-14 | 2015-01-28 | 吉林大学 | Method for preparing monodisperse titanium dioxide (B) nano particles |
| CN105037764A (en) * | 2015-08-03 | 2015-11-11 | 铜陵市胜达电子科技有限责任公司 | Polyimide high-dielectric composite film mixed with nano-titanium dioxide-loaded tin antimony oxide and used for capacitor and preparation method thereof |
Non-Patent Citations (1)
| Title |
|---|
| XIWEN KUANG.ET.AL: "Effect of Calcination Temperature of TiO2 on the Crystallinity and the Permittivity of PVDF-TrFE/TiO2 Composites", 《APPLIED POLYMER》 * |
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Application publication date: 20180501 |