CN108003520A - A kind of preparation method of high dielectric property Kynoar titanium carbide nanosheet composite material - Google Patents

A kind of preparation method of high dielectric property Kynoar titanium carbide nanosheet composite material Download PDF

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CN108003520A
CN108003520A CN201711290938.1A CN201711290938A CN108003520A CN 108003520 A CN108003520 A CN 108003520A CN 201711290938 A CN201711290938 A CN 201711290938A CN 108003520 A CN108003520 A CN 108003520A
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kynoar
titanium carbide
composite material
high dielectric
dielectric property
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CN108003520B (en
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刘晓旭
李彦鹏
李娜
闫凯
岳东
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Datong Copolymerization Xi'an Technology Co ltd
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Heilongjiang University of Science and Technology
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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
    • C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
    • C08J5/18—Manufacture of films or sheets
    • 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
    • C08K7/00—Use of ingredients characterised by shape
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/20—Particle morphology extending in two dimensions, e.g. plate-like
    • 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
    • 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
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00—Applications
    • C08L2203/20—Applications use in electrical or conductive gadgets
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    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency

Abstract

A kind of preparation method of high dielectric property Kynoar titanium carbide nanosheet composite material, it is related to a kind of preparation method of polyvinylidene fluoride composite material.Dielectric constant the invention aims to solve the problems, such as existing Kynoar is low.Method：First, two-dimensional layer TiC nanometer sheets are prepared；2nd, it is compound, obtain the high dielectric property Kynoar titanium carbide nanosheet composite material that titanium carbide nanometer sheet mass fraction is 5%~20%.High dielectric property Kynoar titanium carbide nanosheet composite material prepared by the present invention can be applied to micro-electronic machining, integrated circuit, high efficiency energy-storage travelling wave tube field；The dielectric constant of high dielectric property Kynoar titanium carbide nanosheet composite material prepared by the present invention is 9.8~19.1.The present invention can obtain a kind of high dielectric property Kynoar titanium carbide nanosheet composite material.

Description

A kind of preparation of high dielectric property Kynoar titanium carbide nanosheet composite material Method
Technical field
The present invention relates to a kind of preparation method of polyvinylidene fluoride composite material.
Background technology
Nowadays, the trend of the just exponential rising of the efficiency of electronic product.With the fast lifting of this efficiency, generate New material with high-k.Compared with advanced low-k materials, high dielectric constant material can store more electricity Energy.Therefore, its application can be improved into efficiency in the electronic device.Electronic system usually by active original paper, such as integrated circuit, Formed with passive original paper.People increasingly increase the interest of passive original paper, because their usage amount is as electronics industry is to more It is H.D development and steady-state growth.Reduce the volume of high performance electronics, it would be desirable to integrated passive components, such as electricity Resistance, capacitance and inductance, their usage quantity exceed active integrated circuit original paper and take most of area of substrate.It is true On, ceramics and metal have higher hardness and good heat endurance and high dielectric property.However, their high density, Brittleness and challenging processing conditions hinder their uses as high dielectric material.On the other hand, polymer has The advantages of it is easy processing to have, mechanicalness is flexible and inexpensive.The mechanical flexibility and tunable performance of polymer matrix composite allow They become very attractive.But inorganic material is compared, high-molecular organic material usually has low-k, and scope is 2 ~5.Under special circumstances, although they have a fabulous physical attribute, the dielectric constant of pure polymer can more than 10, but still It is so very low, therefore these hinder them to be used as high dielectric material.So a key issue seek to increase substantially it is poly- Compound dielectric constant, while also to retain its excellent mechanical performance.
The content of the invention
Dielectric constant the invention aims to solve the problems, such as existing Kynoar is low, and provides a kind of high dielectric The preparation method of performance Kynoar titanium carbide nanosheet composite material.
A kind of preparation method of high dielectric property Kynoar titanium carbide nanosheet composite material, specifically by following step Suddenly complete：
First, two-dimensional layer TiC nanometer sheets are prepared：
1., by Ti3AlC2It is added in mixed acid solution, then low whipping speed is to be stirred under 100r/min~300r/min 0.5h~2h is reacted, adds sodium fluoride powder, then 10h~14h is reacted at being 35 DEG C~50 DEG C in temperature, obtains reaction solution；
Step 1 1. described in mixed acid solution be the concentrated sulfuric acid that mass fraction is 98% and mass fraction is 85% The mixed liquor of concentrated phosphoric acid, the body for the concentrated phosphoric acid that the concentrated sulfuric acid that mass fraction is 98% in mixed acid solution is 85% with mass fraction Product is than being 9:1；
Step 1 1. described in Ti3AlC2Quality and the volume ratio of mixed acid solution be (2g~4g):30mL；
Step 1 1. described in the quality of sodium fluoride powder and the volume ratio of mixed acid solution be (0.5g~2g): 30mL；
2., reaction solution is cooled to room temperature, then centrifuge in the case where centrifugal speed is 6000r/min~8000r/min 10min~ 20min, then supernatant is removed, obtain solid matter；Solid matter is cleaned 2 times~4 times first by distilled water, reuses nothing Water-ethanol is cleaned to the pH value of cleaning solution as neutrality, the solid matter after being cleaned；
3., add n,N-Dimethylformamide into the solid matter after cleaning, then under argon gas protection and ultrasonic power For ultrasound 3h~5h under 100W~500W, then centrifuge in the case where centrifugal speed is 3000r/min~4000r/min 10min~ 20min, then supernatant is taken, then centrifuge 10min, then taking precipitate matter in the case where centrifugal speed is 10000r/min；
Step 1 1. described in Ti3AlC2Quality and step 1 3. described in N,N-dimethylformamide volume Than for (2g~4g):100mL；
4., to step 1 3. in add n,N-Dimethylformamide in obtained deposit, it is 5mg/mL to obtain concentration The two-dimensional layer TiC nanometer sheet solution of~10mg/mL；
2nd,
1., Kynoar is placed in drying process 6h~9h in the baking oven that temperature is 70 DEG C~90 DEG C, obtain drying Kynoar；
2., that dry Kynoar is added to the two-dimensional layer TiC nanometer sheets that concentration is 5mg/mL~10mg/mL is molten In liquid, then stirring reaction 7h~9h in the case where temperature is 45 DEG C~55 DEG C and mixing speed is 100r/min, obtain thick mixing Solution B；
Step 2 2. described in drying Kynoar quality and concentration be 5mg/mL~10mg/mL two-dimensional layer The volume ratio of shape TiC nanometer sheet solution is (0.4g~0.95g):10mL；
3., by thick mixed solution B ultrasonic power be 100W~500W under ultrasound 3h~5h, obtain dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids；
4., by dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids drop to cleaning glass substrate On, make its natural casting film-forming, then 8h~12h are heat-treated for 70 DEG C~80 DEG C in temperature, then being placed in distilled water makes film natural Come off, then by film hang airing；
5., by the film dried temperature be 90 DEG C~100 DEG C at vacuum heat 8h~12h, obtain titanium carbide nanometer sheet Mass fraction is 5%~20% high dielectric property Kynoar titanium carbide nanosheet composite material；
Step 2 5. described in titanium carbide nanometer sheet mass fraction be 5%~20% high dielectric property Kynoar The thickness of titanium carbide nanosheet composite material is 100 μm~150 μm.
The principle of the present invention and advantage：
First, the present invention prepares high dielectric property Kynoar titanium carbide nanosheet composite material using solution casting method, High dielectric property Kynoar titanium carbide nanosheet composite material is provided simultaneously with high-k, low-dielectric loss, mechanicalness Can flexible, physico-chemical property stabilization excellent properties；
2nd, high dielectric property Kynoar titanium carbide nanosheet composite material prepared by the present invention can be applied to microelectronics Processing, integrated circuit, high efficiency energy-storage travelling wave tube field；
3rd, the dielectric constant of high dielectric property Kynoar titanium carbide nanosheet composite material prepared by the present invention is 9.8~19.1.
The present invention can obtain a kind of high dielectric property Kynoar titanium carbide nanosheet composite material.
Brief description of the drawings
Fig. 1 is the high dielectric property polyvinylidene fluoride olefinic carbon that titanium carbide nanometer sheet mass fraction prepared by embodiment one is 5% Change the SEM figures of titanium nanosheet composite material；
Fig. 2 is the high dielectric property polyvinylidene fluoride olefinic carbon that titanium carbide nanometer sheet mass fraction prepared by embodiment three is 15% Change the SEM figures of titanium nanosheet composite material；
Fig. 3 is dielectric constant curve, and A is the dielectric constant of pure Kynoar prepared by comparative example in Fig. 3, and B is The high dielectric property Kynoar titanium carbide nanometer sheet that titanium carbide nanometer sheet mass fraction prepared by embodiment one is 5% is compound The dielectric constant of material, C are that the high dielectric property that titanium carbide nanometer sheet mass fraction prepared by embodiment two is 10% gathers inclined fluorine The dielectric constant of ethene titanium carbide nanosheet composite material, D are that titanium carbide nanometer sheet mass fraction prepared by embodiment three is The dielectric constant of 15% high dielectric property Kynoar titanium carbide nanosheet composite material, E are carbon prepared by example IV Change the dielectric constant for the high dielectric property Kynoar titanium carbide nanosheet composite material that titanium nanometer sheet mass fraction is 20%.
Embodiment
Embodiment one：Present embodiment is a kind of high dielectric property Kynoar titanium carbide nanometer sheet composite wood What the preparation method of material was specifically realized by the following steps：
First, two-dimensional layer TiC nanometer sheets are prepared：
1., by Ti3AlC2It is added in mixed acid solution, then low whipping speed is to be stirred under 100r/min~300r/min 0.5h~2h is reacted, adds sodium fluoride powder, then 10h~14h is reacted at being 35 DEG C~50 DEG C in temperature, obtains reaction solution；
Step 1 1. described in mixed acid solution be the concentrated sulfuric acid that mass fraction is 98% and mass fraction is 85% The mixed liquor of concentrated phosphoric acid, the body for the concentrated phosphoric acid that the concentrated sulfuric acid that mass fraction is 98% in mixed acid solution is 85% with mass fraction Product is than being 9:1；
Step 1 1. described in Ti3AlC2Quality and the volume ratio of mixed acid solution be (2g~4g):30mL；
Step 1 1. described in the quality of sodium fluoride powder and the volume ratio of mixed acid solution be (0.5g~2g): 30mL；
2., reaction solution is cooled to room temperature, then centrifuge in the case where centrifugal speed is 6000r/min~8000r/min 10min~ 20min, then supernatant is removed, obtain solid matter；Solid matter is cleaned 2 times~4 times first by distilled water, reuses nothing Water-ethanol is cleaned to the pH value of cleaning solution as neutrality, the solid matter after being cleaned；
3., add n,N-Dimethylformamide into the solid matter after cleaning, then under argon gas protection and ultrasonic power For ultrasound 3h~5h under 100W~500W, then centrifuge in the case where centrifugal speed is 3000r/min~4000r/min 10min~ 20min, then supernatant is taken, then centrifuge 10min, then taking precipitate matter in the case where centrifugal speed is 10000r/min；
Step 1 1. described in Ti3AlC2Quality and step 1 3. described in N,N-dimethylformamide volume Than for (2g~4g):100mL；
4., to step 1 3. in add n,N-Dimethylformamide in obtained deposit, it is 5mg/mL to obtain concentration The two-dimensional layer TiC nanometer sheet solution of~10mg/mL；
2nd,
1., Kynoar is placed in drying process 6h~9h in the baking oven that temperature is 70 DEG C~90 DEG C, obtain drying Kynoar；
2., that dry Kynoar is added to the two-dimensional layer TiC nanometer sheets that concentration is 5mg/mL~10mg/mL is molten In liquid, then stirring reaction 7h~9h in the case where temperature is 45 DEG C~55 DEG C and mixing speed is 100r/min, obtain thick mixing Solution B；
Step 2 2. described in drying Kynoar quality and concentration be 5mg/mL~10mg/mL two-dimensional layer The volume ratio of shape TiC nanometer sheet solution is (0.4g~0.95g):10mL；
3., by thick mixed solution B ultrasonic power be 100W~500W under ultrasound 3h~5h, obtain dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids；
4., by dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids drop to cleaning glass substrate On, make its natural casting film-forming, then 8h~12h are heat-treated for 70 DEG C~80 DEG C in temperature, then being placed in distilled water makes film natural Come off, then by film hang airing；
5., by the film dried temperature be 90 DEG C~100 DEG C at vacuum heat 8h~12h, obtain titanium carbide nanometer sheet Mass fraction is 5%~20% high dielectric property Kynoar titanium carbide nanosheet composite material；
Step 2 5. described in titanium carbide nanometer sheet mass fraction be 5%~20% high dielectric property Kynoar The thickness of titanium carbide nanosheet composite material is 100 μm~150 μm.
Present embodiment step 1 3. in centrifugal speed be 3000r/min~4000r/min under centrifuge 10min~ 20min, is to remove the titanium carbide bulky grain for being stripped out, the supernatant obtained after centrifugation is the titanium carbide nanometer of thin layer Piece solution；10min, titanium carbide nanometer sheet, that is, TiC nanometers of two-dimensional layer of thin layer are centrifuged in the case where centrifugal speed is 10000r/min Piece is just precipitated out, and supernatant is n,N-Dimethylformamide；
Present embodiment step 1 3. in obtained deposit be two-dimensional layer TiC nanometer sheets, received to two-dimensional layer TiC N,N-Dimethylformamide is added in rice piece, the two-dimensional layer TiC nanometer sheets that concentration is 5mg/mL~10mg/mL can be made Solution.
The principle and advantage of present embodiment：
First, present embodiment prepares high dielectric property Kynoar titanium carbide nanometer sheet composite wood using solution casting method Material, high dielectric property Kynoar titanium carbide nanosheet composite material are provided simultaneously with high-k, low-dielectric loss, machinery The excellent properties that performance is flexible, physico-chemical property is stablized；
2nd, high dielectric property Kynoar titanium carbide nanosheet composite material prepared by present embodiment can be applied to micro- Electronics processing, integrated circuit, high efficiency energy-storage travelling wave tube field；
3rd, the dielectric constant of high dielectric property Kynoar titanium carbide nanosheet composite material prepared by present embodiment For 9.8~19.1.
Present embodiment can obtain a kind of high dielectric property Kynoar titanium carbide nanosheet composite material.
Embodiment two：Present embodiment is with one difference of embodiment：Step 1 1. in by Ti3AlC2 It is added in mixed acid solution, then low whipping speed is stirring reaction 0.5h~1h under 100r/min~200r/min, is added Sodium fluoride powder, then 10h~12h is reacted at being 45 DEG C~50 DEG C in temperature, obtain reaction solution.Other steps and specific embodiment party Formula one is identical.
Embodiment three：Present embodiment is with one of embodiment one or two difference：Step 1 1. in The Ti3AlC2Quality and the volume ratio of mixed acid solution be (2g~3g):30mL.Other steps and embodiment One or two is identical.
Embodiment four：Present embodiment is with one of embodiment one to three difference：Step 1 1. in The quality of the sodium fluoride powder and the volume ratio of mixed acid solution are (0.5g~1g):30mL.Other steps and specific reality It is identical to apply mode one to three.
Embodiment five：Present embodiment is with one of embodiment one to four difference：Step 1 1. in The Ti3AlC2Quality and step 1 3. described in the volume ratio of N,N-dimethylformamide be (2g~3g):100mL. Other steps are identical with embodiment one to four.
Embodiment six：Present embodiment is with one of embodiment one to five difference：Step 1 4. in To step 1 3. in add n,N-Dimethylformamide in obtained deposit, it is 5mg/mL~7.5mg/mL's to obtain concentration Two-dimensional layer TiC nanometer sheet solution.Other steps are identical with embodiment one to five.
Embodiment seven：Present embodiment is with one of embodiment one to six difference：Step 2 1. in Kynoar is placed in drying process 6h~8h in the baking oven that temperature is 80 DEG C~90 DEG C, obtains dry Kynoar. Other steps are identical with embodiment one to six.
Embodiment eight：Present embodiment is with one of embodiment one to seven difference：Step 2 2. in The quality of the Kynoar of the drying is the two-dimensional layer TiC nanometer sheet solution of 5mg/mL~10mg/mL with concentration Volume ratio is (0.4g~0.75g):10mL.Other steps are identical with embodiment one to seven.
Embodiment nine：Present embodiment is with one of embodiment one to eight difference：Step 2 4. in Dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids are dropped on the glass substrate of cleaning, make its nature Casting film-forming, then in temperature be 70 DEG C~75 DEG C heat treatment 8h~10h, then being placed in distilled water makes film come off naturally, then by film Hang airing.Other steps are identical with embodiment one to eight.
Embodiment ten：Present embodiment is with one of embodiment one to nine difference：Step 2 5. in Vacuum heat 8h~10h at being 95 DEG C~100 DEG C in temperature by the film dried, obtaining titanium carbide nanometer sheet mass fraction is 10%~20% high dielectric property Kynoar titanium carbide nanosheet composite material.Other steps and embodiment one It is identical to nine.
Embodiment one：Titanium carbide nanometer sheet mass fraction is 5% high dielectric property Kynoar titanium carbide nanometer sheet The preparation method of composite material, is specifically realized by the following steps：
First, two-dimensional layer TiC nanometer sheets are prepared：
1., by Ti3AlC2It is added in mixed acid solution, then low whipping speed is stirring reaction 1h under 200r/min, then add Enter sodium fluoride powder, then 12h is reacted at being 45 DEG C in temperature, obtain reaction solution；
Step 1 1. described in mixed acid solution be the concentrated sulfuric acid that mass fraction is 98% and mass fraction is 85% The mixed liquor of concentrated phosphoric acid, the body for the concentrated phosphoric acid that the concentrated sulfuric acid that mass fraction is 98% in mixed acid solution is 85% with mass fraction Product is than being 9:1；
Step 1 1. described in Ti3AlC2Quality and the volume ratio of mixed acid solution be 3g:30mL；
Step 1 1. described in the quality of sodium fluoride powder and the volume ratio of mixed acid solution be 1g:30mL；
2., reaction solution is cooled to room temperature, then centrifuge 15min in the case where centrifugal speed is 7000r/min, then remove supernatant Liquid, obtains solid matter；Solid matter is cleaned 3 times first by distilled water, reuses washes of absolute alcohol to cleaning solution PH value is neutrality, the solid matter after being cleaned；
3., add n,N-Dimethylformamide into the solid matter after cleaning, then under argon gas protection and ultrasonic power For ultrasound 4h under 300W, then 15min is centrifuged in the case where centrifugal speed is 4000r/min, then take supernatant, then be in centrifugal speed 10min, then taking precipitate matter are centrifuged under 10000r/min；
Step 1 1. described in Ti3AlC2Quality and step 1 3. described in N,N-dimethylformamide volume Than for 3g:100mL；
4., to step 1 3. in add n,N-Dimethylformamide in obtained deposit, it is 5mg/mL to obtain concentration Two-dimensional layer TiC nanometer sheet solution；
2nd,
1., Kynoar is placed in drying process 8h in the baking oven that temperature is 80 DEG C, obtain dry Kynoar；
2., dry Kynoar is added in the two-dimensional layer TiC nanometer sheet solution that concentration is 5mg/mL, then Temperature is 50 DEG C and mixing speed is stirring reaction 8h under 100r/min, obtains thick mixed solution B；
Step 2 2. described in drying Kynoar quality and concentration be 5mg/mL TiC nanometers of two-dimensional layer The volume ratio of piece solution is 0.95g:10mL；
3., by thick mixed solution B ultrasonic power be 300W under ultrasound 4h, obtain dispersed polyvinylidene fluoride Alkene-two-dimensional layer TiC nanometer sheet composite colloids；
4., by dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids drop to cleaning glass substrate On, make its natural casting film-forming, then in temperature be 75 DEG C of heat treatment 10h, then being placed in distilled water makes film come off naturally, then by film Hang airing；
5., by the film dried temperature be 100 DEG C at vacuum heat 10h, obtaining titanium carbide nanometer sheet mass fraction is 5% high dielectric property Kynoar titanium carbide nanosheet composite material.
Step 2 5. described in titanium carbide nanometer sheet mass fraction be 5% high dielectric property Kynoar titanium carbide The thickness of nanosheet composite material is 100 μm.
Embodiment two：Titanium carbide nanometer sheet mass fraction is 10% high dielectric property Kynoar titanium carbide nanometer sheet The preparation method of composite material, is specifically realized by the following steps：
First, two-dimensional layer TiC nanometer sheets are prepared：
1., by Ti3AlC2It is added in mixed acid solution, then low whipping speed is stirring reaction 1h under 200r/min, then add Enter sodium fluoride powder, then 12h is reacted at being 45 DEG C in temperature, obtain reaction solution；
Step 1 1. described in mixed acid solution be the concentrated sulfuric acid that mass fraction is 98% and mass fraction is 85% The mixed liquor of concentrated phosphoric acid, the body for the concentrated phosphoric acid that the concentrated sulfuric acid that mass fraction is 98% in mixed acid solution is 85% with mass fraction Product is than being 9:1；
Step 1 1. described in Ti3AlC2Quality and the volume ratio of mixed acid solution be 3g:30mL；
Step 1 1. described in the quality of sodium fluoride powder and the volume ratio of mixed acid solution be 1g:30mL；
2., reaction solution is cooled to room temperature, then centrifuge 15min in the case where centrifugal speed is 7000r/min, then remove supernatant Liquid, obtains solid matter；Solid matter is cleaned 3 times first by distilled water, reuses washes of absolute alcohol to cleaning solution PH value is neutrality, the solid matter after being cleaned；
3., add n,N-Dimethylformamide into the solid matter after cleaning, then under argon gas protection and ultrasonic power For ultrasound 4h under 300W, then 15min is centrifuged in the case where centrifugal speed is 4000r/min, then take supernatant, then be in centrifugal speed 10min, then taking precipitate matter are centrifuged under 10000r/min；
Step 1 1. described in Ti3AlC2Quality and step 1 3. described in N,N-dimethylformamide volume Than for 3g:100mL；
4., to step 1 3. in add n,N-Dimethylformamide in obtained deposit, it is 10mg/mL to obtain concentration Two-dimensional layer TiC nanometer sheet solution；
2nd,
1., Kynoar is placed in drying process 8h in the baking oven that temperature is 80 DEG C, obtain dry Kynoar；
2., dry Kynoar is added in the two-dimensional layer TiC nanometer sheet solution that concentration is 10mg/mL, then In the case where temperature is 50 DEG C and mixing speed is 100r/min, stirring reaction 8h, obtains thick mixed solution B；
Step 2 2. described in drying Kynoar quality and concentration be 10mg/mL two-dimensional layer TiC receive The volume ratio of rice piece solution is 0.9g:10mL；
3., by thick mixed solution B ultrasonic power be 300W under ultrasound 4h, obtain dispersed polyvinylidene fluoride Alkene-two-dimensional layer TiC nanometer sheet composite colloids；
4., by dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids drop to cleaning glass substrate On, make its natural casting film-forming, then in temperature be 75 DEG C of heat treatment 10h, then being placed in distilled water makes film come off naturally, then by film Hang airing；
5., by the film dried temperature be 100 DEG C at vacuum heat 10h, obtaining titanium carbide nanometer sheet mass fraction is 10% high dielectric property Kynoar titanium carbide nanosheet composite material.
Step 2 5. described in titanium carbide nanometer sheet mass fraction be 10% high dielectric property Kynoar be carbonized The thickness of titanium nanosheet composite material is 100 μm.
Embodiment three：Titanium carbide nanometer sheet mass fraction is 15% high dielectric property Kynoar titanium carbide nanometer sheet The preparation method of composite material, is specifically realized by the following steps：
First, two-dimensional layer TiC nanometer sheets are prepared：
1., by Ti3AlC2It is added in mixed acid solution, then low whipping speed is stirring reaction 1h under 200r/min, then add Enter sodium fluoride powder, then 12h is reacted at being 45 DEG C in temperature, obtain reaction solution；
Step 1 1. described in mixed acid solution be the concentrated sulfuric acid that mass fraction is 98% and mass fraction is 85% The mixed liquor of concentrated phosphoric acid, the body for the concentrated phosphoric acid that the concentrated sulfuric acid that mass fraction is 98% in mixed acid solution is 85% with mass fraction Product is than being 9:1；
Step 1 1. described in Ti3AlC2Quality and the volume ratio of mixed acid solution be 3g:30mL；
Step 1 1. described in the quality of sodium fluoride powder and the volume ratio of mixed acid solution be 1g:30mL；
2., reaction solution is cooled to room temperature, then centrifuge 15min in the case where centrifugal speed is 7000r/min, then remove supernatant Liquid, obtains solid matter；Solid matter is cleaned 3 times first by distilled water, reuses washes of absolute alcohol to cleaning solution PH value is neutrality, the solid matter after being cleaned；
3., add n,N-Dimethylformamide into the solid matter after cleaning, then under argon gas protection and ultrasonic power For ultrasound 4h under 300W, then 15min is centrifuged in the case where centrifugal speed is 4000r/min, then take supernatant, then be in centrifugal speed 10min, then taking precipitate matter are centrifuged under 10000r/min；
Step 1 1. described in Ti3AlC2Quality and step 1 3. described in N,N-dimethylformamide volume Than for 4g:100mL；
4., to step 1 3. in add n,N-Dimethylformamide in obtained deposit, it is 7.5mg/ to obtain concentration The two-dimensional layer TiC nanometer sheet solution of mL；
2nd,
1., Kynoar is placed in drying process 8h in the baking oven that temperature is 80 DEG C, obtain dry Kynoar；
2., dry Kynoar is added in the two-dimensional layer TiC nanometer sheet solution that concentration is 7.5mg/mL, then In the case where temperature is 50 DEG C and mixing speed is 100r/min, stirring reaction 8h, obtains thick mixed solution B；
Step 2 2. described in drying Kynoar quality and concentration be 7.5mg/mL two-dimensional layer TiC receive The volume ratio of rice piece solution is 0.425g:10mL；
3., by thick mixed solution B ultrasonic power be 300W under ultrasound 4h, obtain dispersed polyvinylidene fluoride Alkene-two-dimensional layer TiC nanometer sheet composite colloids；
4., by dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids drop to cleaning glass substrate On, make its natural casting film-forming, then in temperature be 75 DEG C of heat treatment 10h, then being placed in distilled water makes film come off naturally, then by film Hang airing；
5., by the film dried temperature be 100 DEG C at vacuum heat 10h, obtaining titanium carbide nanometer sheet mass fraction is 15% high dielectric property Kynoar titanium carbide nanosheet composite material.
Step 2 5. described in titanium carbide nanometer sheet mass fraction be 15% high dielectric property Kynoar be carbonized The thickness of titanium nanosheet composite material is 100 μm.
Example IV：Titanium carbide nanometer sheet mass fraction is 20% high dielectric property Kynoar titanium carbide nanometer sheet The preparation method of composite material, is specifically realized by the following steps：
First, two-dimensional layer TiC nanometer sheets are prepared：
1., by Ti3AlC2It is added in mixed acid solution, then low whipping speed is stirring reaction 1h under 200r/min, then add Enter sodium fluoride powder, then 12h is reacted at being 45 DEG C in temperature, obtain reaction solution；
Step 1 1. described in mixed acid solution be the concentrated sulfuric acid that mass fraction is 98% and mass fraction is 85% The mixed liquor of concentrated phosphoric acid, the body for the concentrated phosphoric acid that the concentrated sulfuric acid that mass fraction is 98% in mixed acid solution is 85% with mass fraction Product is than being 9:1；
Step 1 1. described in Ti3AlC2Quality and the volume ratio of mixed acid solution be 3g:30mL；
Step 1 1. described in the quality of sodium fluoride powder and the volume ratio of mixed acid solution be 1g:30mL；
2., reaction solution is cooled to room temperature, then centrifuge 15min in the case where centrifugal speed is 7000r/min, then remove supernatant Liquid, obtains solid matter；Solid matter is cleaned 3 times first by distilled water, reuses washes of absolute alcohol to cleaning solution PH value is neutrality, the solid matter after being cleaned；
3., add n,N-Dimethylformamide into the solid matter after cleaning, then under argon gas protection and ultrasonic power For ultrasound 3h~5h under 300W, then 15min is centrifuged in the case where centrifugal speed is 4000r/min, then take supernatant, then in centrifugal speed To centrifuge 10min, then taking precipitate matter under 10000r/min；
Step 1 1. described in Ti3AlC2Quality and step 1 3. described in N,N-dimethylformamide volume Than for 3g:100mL；
4., to step 1 3. in add n,N-Dimethylformamide in obtained deposit, it is 10mg/mL to obtain concentration Two-dimensional layer TiC nanometer sheet solution；
2nd,
1., Kynoar is placed in drying process 8h in the baking oven that temperature is 80 DEG C, obtain dry Kynoar；
2., dry Kynoar is added in the two-dimensional layer TiC nanometer sheet solution that concentration is 10mg/mL, then In the case where temperature is 50 DEG C and mixing speed is 100r/min, stirring reaction 8h, obtains thick mixed solution B；
Step 2 2. described in drying Kynoar quality and concentration be 10mg/mL two-dimensional layer TiC receive The volume ratio of rice piece solution is 0.4g:10mL；
3., by thick mixed solution B ultrasonic power be 300W under ultrasound 4h, obtain dispersed polyvinylidene fluoride Alkene-two-dimensional layer TiC nanometer sheet composite colloids；
4., by dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids drop to cleaning glass substrate On, make its natural casting film-forming, then in temperature be 75 DEG C of heat treatment 10h, then being placed in distilled water makes film come off naturally, then by film Hang airing；
5., by the film dried temperature be 100 DEG C at vacuum heat 10h, obtaining titanium carbide nanometer sheet mass fraction is 20% high dielectric property Kynoar titanium carbide nanosheet composite material.
Step 2 5. described in titanium carbide nanometer sheet mass fraction be 20% high dielectric property Kynoar be carbonized The thickness of titanium nanosheet composite material is 100 μm.
Comparative example：Kynoar is prepared according to the following steps：
1., Kynoar is placed in drying process 8h in the baking oven that temperature is 80 DEG C, obtain dry Kynoar；
2., dry Kynoar is added in n,N-Dimethylformamide, then in temperature for 50 DEG C and stirring speed Spend and react 8h for stirring under 100r/min, obtain Kynoar solution；
Step 2. described in drying the quality of Kynoar and the volume ratio of N,N-dimethylformamide be 0.95g:10mL；
4., by Kynoar solution ultrasonic power be 300W under ultrasound 4h, obtain dispersed Kynoar Colloid；
5., dispersed Kynoar colloid dropped on the glass substrate of cleaning, make its natural casting film-forming, then It is 75 DEG C of heat treatment 10h in temperature, then being placed in distilled water makes film come off naturally, then by film hang airing；
6., by the film dried temperature be 100 DEG C at vacuum heat 10h, obtain Kynoar；
Step 2 6. described in Kynoar thickness be 100 μm.
Fig. 1 is the high dielectric property polyvinylidene fluoride olefinic carbon that titanium carbide nanometer sheet mass fraction prepared by embodiment one is 5% Change the SEM figures of titanium nanosheet composite material；
From fig. 1, it can be seen that in high dielectric property Kynoar titanium carbide nanosheet composite material titanium carbide nanometer sheet matter When amount fraction is 5%, titanium carbide nanometer sheet is coated by polymer molecular chain, titanium carbide nanometer sheet dispersed phase pair in polyimides Uniformly, without obvious agglomeration.
Fig. 2 is the high dielectric property polyvinylidene fluoride olefinic carbon that titanium carbide nanometer sheet mass fraction prepared by embodiment three is 15% Change the SEM figures of titanium nanosheet composite material；
As can be seen from Figure 2, in high dielectric property Kynoar titanium carbide nanosheet composite material titanium carbide nanometer sheet matter When amount fraction is 15%, titanium carbide nanometer sheet is coated by polymer molecular chain, and titanium carbide nanometer sheet gathers inclined fluorine in high dielectric property Local bolus agglomerate is had begun in ethene titanium carbide nanosheet composite material to gather.
Fig. 3 is dielectric constant curve, and A is the dielectric constant of pure Kynoar prepared by comparative example in Fig. 3, and B is The high dielectric property Kynoar titanium carbide nanometer sheet that titanium carbide nanometer sheet mass fraction prepared by embodiment one is 5% is compound The dielectric constant of material, C are that the high dielectric property that titanium carbide nanometer sheet mass fraction prepared by embodiment two is 10% gathers inclined fluorine The dielectric constant of ethene titanium carbide nanosheet composite material, D are that titanium carbide nanometer sheet mass fraction prepared by embodiment three is The dielectric constant of 15% high dielectric property Kynoar titanium carbide nanosheet composite material, E are carbon prepared by example IV Change the dielectric constant for the high dielectric property Kynoar titanium carbide nanosheet composite material that titanium nanometer sheet mass fraction is 20%.
As can be seen from Figure 3, with titanium carbide nanometer sheet in high dielectric property Kynoar titanium carbide nanosheet composite material The increase of content, the dielectric constant of high dielectric property Kynoar titanium carbide nanosheet composite material dramatically increase, and work as Gao Jie When the mass fraction of titanium carbide nanometer sheet is 20% in electrical property Kynoar titanium carbide nanosheet composite material, its dielectric is normal Number has reached 19.1, and 2.5 times of about pure Kynoar dielectric constant, dielectric properties significantly improve.

Claims (10)

  1. A kind of 1. preparation method of high dielectric property Kynoar titanium carbide nanosheet composite material, it is characterised in that Yi Zhonggao What the preparation method of dielectric properties Kynoar titanium carbide nanosheet composite material was specifically realized by the following steps：
    First, two-dimensional layer TiC nanometer sheets are prepared：
    1., by Ti3AlC2It is added in mixed acid solution, then low whipping speed is that reaction is stirred under 100r/min~300r/min 0.5h~2h, adds sodium fluoride powder, then reacts 10h~14h at being 35 DEG C~50 DEG C in temperature, obtains reaction solution；
    Step 1 1. described in mixed acid solution be the concentrated sulfuric acid that mass fraction is 98% and the dense phosphorus that mass fraction is 85% The mixed liquor of acid, the volume ratio for the concentrated phosphoric acid that the concentrated sulfuric acid that mass fraction is 98% in mixed acid solution is 85% with mass fraction For 9:1；
    Step 1 1. described in Ti3AlC2Quality and the volume ratio of mixed acid solution be (2g~4g):30mL；
    Step 1 1. described in the quality of sodium fluoride powder and the volume ratio of mixed acid solution be (0.5g~2g):30mL；
    2., reaction solution is cooled to room temperature, then centrifuge in the case where centrifugal speed is 6000r/min~8000r/min 10min~ 20min, then supernatant is removed, obtain solid matter；Solid matter is cleaned 2 times~4 times first by distilled water, reuses nothing Water-ethanol is cleaned to the pH value of cleaning solution as neutrality, the solid matter after being cleaned；
    3., add n,N-Dimethylformamide into the solid matter after cleaning, then under argon gas protection and ultrasonic power is Ultrasound 3h~5h under 100W~500W, then 10min~20min is centrifuged in the case where centrifugal speed is 3000r/min~4000r/min, Supernatant is taken again, then centrifuges 10min, then taking precipitate matter in the case where centrifugal speed is 10000r/min；
    Step 1 1. described in Ti3AlC2Quality and step 1 3. described in the volume ratio of N,N-dimethylformamide be (2g~4g):100mL；
    4., to step 1 3. in add n,N-Dimethylformamide in obtained deposit, obtain concentration for 5mg/mL~ The two-dimensional layer TiC nanometer sheet solution of 10mg/mL；
    2nd,
    1., Kynoar is placed in drying process 6h~9h in the baking oven that temperature is 70 DEG C~90 DEG C, obtain drying it is poly- partially Vinyl fluoride；
    2., dry Kynoar is added to the two-dimensional layer TiC nanometer sheet solution that concentration is 5mg/mL~10mg/mL In, then stirring reaction 7h~9h in the case where temperature is 45 DEG C~55 DEG C and mixing speed is 100r/min, it is molten to obtain thick mixing Liquid B；
    Step 2 2. described in drying Kynoar quality and concentration be 5mg/mL~10mg/mL two-dimensional layer The volume ratio of TiC nanometer sheet solution is (0.4g~0.95g):10mL；
    3., by thick mixed solution B in the case where ultrasonic power is 100W~500W ultrasound 3h~5h, obtain dispersed poly- inclined Vinyl fluoride-two-dimensional layer TiC nanometer sheet composite colloids；
    4., by dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids drop to cleaning glass substrate on, Make its natural casting film-forming, then 8h~12h are heat-treated for 70 DEG C~80 DEG C in temperature, then being placed in distilled water makes film naturally de- Fall, then by film hang airing；
    5., by the film dried temperature be 90 DEG C~100 DEG C at vacuum heat 8h~12h, obtain titanium carbide nanometer tablet quality Fraction is 5%~20% high dielectric property Kynoar titanium carbide nanosheet composite material；
    Step 2 5. described in titanium carbide nanometer sheet mass fraction be 5%~20% high dielectric property Kynoar be carbonized The thickness of titanium nanosheet composite material is 100 μm~150 μm.
  2. A kind of 2. preparation side of high dielectric property Kynoar titanium carbide nanosheet composite material according to claim 1 Method, it is characterised in that step 1 1. in by Ti3AlC2Be added in mixed acid solution, then low whipping speed for 100r/min~ Stirring reaction 0.5h~1h, adds sodium fluoride powder under 200r/min, then reacted at being 45 DEG C~50 DEG C in temperature 10h~ 12h, obtains reaction solution.
  3. A kind of 3. preparation side of high dielectric property Kynoar titanium carbide nanosheet composite material according to claim 1 Method, it is characterised in that step 1 1. described in Ti3AlC2Quality and the volume ratio of mixed acid solution be (2g~3g):30mL.
  4. A kind of 4. preparation side of high dielectric property Kynoar titanium carbide nanosheet composite material according to claim 1 Method, it is characterised in that step 1 1. described in sodium fluoride powder quality and mixed acid solution volume ratio for (0.5g~ 1g):30mL。
  5. A kind of 5. preparation side of high dielectric property Kynoar titanium carbide nanosheet composite material according to claim 1 Method, it is characterised in that step 1 1. described in Ti3AlC2Quality and step 1 3. described in N,N-dimethylformamide Volume ratio is (2g~3g):100mL.
  6. A kind of 6. preparation side of high dielectric property Kynoar titanium carbide nanosheet composite material according to claim 1 Method, it is characterised in that step 1 4. in step 1 3. in add n,N-Dimethylformamide in obtained deposit, obtain Concentration is the two-dimensional layer TiC nanometer sheet solution of 5mg/mL~7.5mg/mL.
  7. A kind of 7. preparation side of high dielectric property Kynoar titanium carbide nanosheet composite material according to claim 1 Method, it is characterised in that step 2 1. in by Kynoar be placed in temperature be drying process 6h in 80 DEG C~90 DEG C of baking oven~ 8h, obtains dry Kynoar.
  8. A kind of 8. preparation side of high dielectric property Kynoar titanium carbide nanosheet composite material according to claim 1 Method, it is characterised in that step 2 2. described in quality and the concentration of Kynoar of drying be 5mg/mL~10mg/mL's The volume ratio of two-dimensional layer TiC nanometer sheet solution is (0.4g~0.75g):10mL.
  9. A kind of 9. preparation side of high dielectric property Kynoar titanium carbide nanosheet composite material according to claim 1 Method, it is characterised in that step 2 4. in dispersed Kynoar-two-dimensional layer TiC nanometer sheet composite colloids are dropped to it is clean On net glass substrate, make its natural casting film-forming, then 8h~10h are heat-treated for 70 DEG C~75 DEG C in temperature, then be placed in distillation Film is set to come off naturally in water, then by film hang airing.
  10. A kind of 10. preparation of high dielectric property Kynoar titanium carbide nanosheet composite material according to claim 1 Method, it is characterised in that step 2 5. in by the film dried temperature be 95 DEG C~100 DEG C at vacuum heat 8h~10h, obtain To the high dielectric property Kynoar titanium carbide nanosheet composite material that titanium carbide nanometer sheet mass fraction is 10%~20%.
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CN110828654A (en) * 2019-11-25 2020-02-21 齐鲁工业大学 Composite piezoelectric film and preparation method thereof
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CN115926345A (en) * 2022-12-14 2023-04-07 陕西科技大学 Polyvinylidene fluoride/calcium niobate nanosheet @ aluminum oxide composite material and preparation method and application thereof

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