CN110027270A - A kind of high dielectric flexible laminated film of sandwich structure and preparation method thereof - Google Patents
A kind of high dielectric flexible laminated film of sandwich structure and preparation method thereof Download PDFInfo
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- CN110027270A CN110027270A CN201910463704.5A CN201910463704A CN110027270A CN 110027270 A CN110027270 A CN 110027270A CN 201910463704 A CN201910463704 A CN 201910463704A CN 110027270 A CN110027270 A CN 110027270A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/04—Layered products comprising a layer of natural or synthetic rubber comprising rubber as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B25/00—Layered products comprising a layer of natural or synthetic rubber
- B32B25/20—Layered products comprising a layer of natural or synthetic rubber comprising silicone rubber
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B37/00—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding
- B32B37/06—Methods or apparatus for laminating, e.g. by curing or by ultrasonic bonding characterised by the heating method
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/005—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile
- B32B9/007—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising one layer of ceramic material, e.g. porcelain, ceramic tile comprising carbon, e.g. graphite, composite carbon
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B9/00—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00
- B32B9/04—Layered products comprising a layer of a particular substance not covered by groups B32B11/00 - B32B29/00 comprising such particular substance as the main or only constituent of a layer, which is next to another layer of the same or of a different material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B2250/00—Layers arrangement
- B32B2250/40—Symmetrical or sandwich layers, e.g. ABA, ABCBA, ABCCBA
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Abstract
The invention discloses high dielectric flexible laminated films of a kind of sandwich structure and preparation method thereof, the laminated film is made of three-decker stacking, and the three-decker is respectively as follows: the first outer layer with positive dielectric constant, the middle layer with negative permittivity and the second outer layer with positive dielectric constant；The middle layer is set between first outer layer and second outer layer.For the laminated film using organic silicon rubber as flexible substrate, carbon nanotube (CNTs) is functional stuffing.The present invention prepares the high dielectric flexible laminated film with sandwich structure by the method for in-situ polymerization, and the laminated film is while guaranteeing good flexibility, dielectric constant with higher.
Description
Technical field
The present invention relates to the preparation technical fields of composite material, and in particular to a kind of high dielectric flexible of sandwich structure is multiple
Close film and preparation method thereof.
Background technique
As electronic component develops to high-power, miniaturization, high frequency direction, the dielectric properties of capacitor are proposed
Requirements at the higher level, traditional plane-parallel capacitor have been difficult to satisfy the use demand.Currently, common dielectric substance has ceramics
Dielectric and two kinds of polymeric dielectric.Ceramic dielectric has high dielectric constant, however its disruptive field intensity is lower, be difficult into
One step improves its energy density；Compared to ceramic dielectric, polymeric dielectric have higher disruptive field intensity and preferably it is soft
Toughness, processability especially have important application value in the fields such as flexible electronic device and intelligent wearable device.No
It crosses, the dielectric constant of one-component polymer material is usually lower, limits its application and develops.Therefore, polymerization how is improved
The dielectric constant of object material becomes flexible electronic technical field urgent problem to be solved.
Chinese patent CN106497064A, by adding high dielectric ceramic material BaTiO in macromolecule matrix3(BTO)、
SrTiO3(STO), its dielectric constant is improved.However, due to the introducing of ceramic material, reduce composite material flexibility and
Disruptive field intensity is unfavorable for engineer application.In addition, Chinese patent CN108538643A, by the method for electro-deposition functional material
Graphene is attached on complete cotton knitted fabric and cotton knitwear, and it is thin that this method prepares the flexible compound with positive dielectric constant
Film.However, causing laminated film to be difficult to keep high dielectric constant in high band, in reality due to the directric relaxation behavior of material
There is certain limitation in.Chinese patent CN106218188A is using positive dielectric material and negative dielectric material as raw material, by two
Person obtains graphite/Kynoar block composite material of double-layer structure by hot press forming technology, significantly improves polymer
The dielectric constant of matrix.Since Kynoar belongs to ferroelectric polymers, there are ferroelectric hysteresis phenomenons, cause coercive field big, pole
Change reversion low-response, electromechanical conversion efficiency is low, to limit its application in flexible electronic device.
Summary of the invention
The purpose of the invention is to preferably meet flexible electronic device and technology, provide a kind of with Gao Jie
The fexible film composite material of electric constant.
In order to achieve the above object, the present invention provides a kind of preparations of the high dielectric flexible laminated film of sandwich structure
Method, the laminated film are made of three-decker stacking, and the three-decker is respectively as follows: the with positive dielectric constant
One outer layer, the middle layer with negative permittivity and the second outer layer with positive dielectric constant；The middle layer is set to
Between first outer layer and second outer layer；The preparation method comprises the steps of:
The presoma, curing agent and organic solvent of organic silicon rubber are uniformly mixed by step (1), obtain mixed solution；
Wherein, the organic solvent is equal with the quality of the presoma, the quality of the presoma and the curing agent
Than for 10:1；
The mixed solution and carbon nanotube are mixed to form slurry by step (2)；
When the quality of carbon nanotube and the mass percent of the mixed solution are 0.5%~2%, the slurry of formation is used for
Preparation first outer layer or second outer layer；
When the quality of carbon nanotube and the mass percent of the mixed solution are 3%, the slurry of formation is used to prepare institute
The middle layer stated；
The slurry for being used to prepare first outer layer is coated on plate by step (3), and coating is used to prepare after solidification
The slurry of the middle layer, re-coating is used to prepare slurry and the solidification of second outer layer after cured, obtains by having
The first outer layer, the middle layer with negative permittivity and the second outer layer institute with positive dielectric constant of positive dielectric constant
The laminated film of the sandwich structure of composition is laminated；
Step (4), the laminated film is removed from plate.
Preferably, the organic silicon rubber is dimethyl silicone polymer in step (1).
Preferably, the organic solvent is normal heptane in step (1).
Preferably, the plate refers to glass plate in step (3).
Preferably, the cured temperature is 80 DEG C~180 DEG C in step (3), the time is 1h~3h.
Preferably, the cured temperature is 120 DEG C, time 2h in step (3).
Preferably, the thickness of the middle layer, first outer layer and second outer layer be 0.1~
2mm。
Preferably, the thickness of the middle layer, first outer layer and second outer layer is
0.2mm。
The present invention also provides a kind of high dielectric flexible laminated films of sandwich structure, which can be by above method system
It is standby to obtain.
Compared with the existing technology, the invention has the following advantages:
(1) for the present invention using carbon nanotube as functional stuffing, obtaining has the flexibility of sandwich structure high dielectric property multiple
Film, laminated film dielectric constant with higher and disruptive field intensity are closed, overcomes making for electronic device to a certain extent
With limitation.
(2) negative dielectric properties are a kind of new physical properties, belong to Meta Materials scope, the present invention is based on negative dielectric material with
The sandwich structure design of positive dielectric material, obtains the flexible composite film with high dielectric value, has widened Meta Materials in electricity
The application space of sub- Material Field.
(3) develop with electronic component to miniaturization, high frequency and high-power direction, the height with high dielectric constant
Molecular material important in inhibiting in terms of meeting next-generation electronic equipment and system requirements.
(4) method of the invention has the characteristics that simple process, at low cost and be easy to large-scale production.
Detailed description of the invention
Jie for the flexible composite film that Fig. 1 is comparative example, embodiment 1, embodiment 2, embodiment 3, embodiment 4 are prepared
Electric spectrogram.
Specific embodiment
Below with reference to embodiment, technical scheme is described further, but person skilled in the art is aobvious
So various modifications easily can be made to these embodiments, and applied the general principles described here to other examples
Without having to go through creative labor.Therefore, the present invention includes but is not limited to embodiment here.Those skilled in the art according to
The embodiment of the present invention, the improvement and modification make to the present invention all should be within protection scope of the present invention.
In following comparative example or embodiment, carbon nanotube and the presoma containing dimethyl silicone polymer, curing agent and have
When the mass percent of the mixed solution of solvent is 0~2%, obtained material has positive dielectric constant；Carbon nanotube and mixed
When the mass percent for closing solution is 3%, obtained material has negative permittivity.The present invention select have large specific surface area,
Good conductivity, chemical stability be good, the carbon nanotube (CNTs) of the outstanding features such as environmental-friendly is as providing negative permittivity
Functive is added in dimethyl silicone polymer (organic silicon rubber) flexible substrate, by adjust content of carbon nanotubes and
Its distribution in the base obtains the functional layer with positive and negative dielectric constant respectively.Then, by positive dielectric layer material and
Negative dielectric layer material carries out structure design, prepares the flexible composite film with sandwich structure, and wherein interbed is negative dielectric
Layer, the upper and lower two layers positive dielectric layer for same component.
Embodiment 1
(1) presoma and each 2.5g of organic solvent normal heptane of dimethyl silicone polymer are weighed, then magnetic agitation
10min is uniformly mixed it.
(2) 0.25g curing agent is added, magnetic agitation 10min is uniformly mixed it, and it is molten to obtain the mixing that gross weight is 5.25g
Liquid.
(3) according to quality proportioning addition carbon nanotube is calculated into mixed solution, obtained slurry A, B is respectively used to prepare
Coating with positive and negative dielectric constant, wherein the carbon nanotube being added in slurry A be 0.0263g (carbon nanotube of addition with
The mass percent of mixed solution is 0.5%), to be used to prepare the upper and lower layer film with positive dielectric constant, that is, be used to prepare tool
There are the first outer layer and the second outer layer of positive dielectric constant.In order to guarantee the structural homogeneity of upper and lower double-layer films, above and below
The mass fraction of carbon nanotube in layer film is equal.The carbon nanotube that slurry B is added is the 0.1624g (carbon nanotube of addition
Mass ratio with mixed solution is 3%), to be used to prepare the intermediate layer film with negative permittivity.And slurry A, B magnetic force is stirred
10min is mixed, then sonic oscillation handles 10min.
(4) using successively coating, successively cured method, slurry A, B are respectively coated on to smooth, smooth glass plate
On, the flexible composite film of the sandwich structure of A-B-A type is made.At 400 μm, solidification temperature is the thickness control of monofilm
120 DEG C, curing time 2h.
(5) after the curing be complete, dimethyl silicone polymer/carbon nano tube flexible laminated film is shelled from plate glass
From.
The dielectric properties for the flexible composite film being prepared are measured using Agilent E4980AL test table.Knot
Fruit is as shown in figure 1 shown in the corresponding map of 0.5%-3%-0.5%, and dielectric constant is 50 or more.
Embodiment 2
(1) presoma and each 2.5g of organic solvent normal heptane of dimethyl silicone polymer are weighed, then magnetic agitation
10min is uniformly mixed it.
(2) 0.25g curing agent is added, magnetic agitation 10min is uniformly mixed it, and it is molten to obtain the mixing that gross weight is 5.25g
Liquid.
(3) according to quality proportioning addition carbon nanotube is calculated, obtained slurry A, B, which is respectively used to preparation, has positive and negative Jie
The coating of electric constant, wherein (carbon nanotube of addition and the mass ratio of mixed solution are slurry A addition 0.053g carbon nanotube
1%), preparation has the upper and lower layer film of positive dielectric constant, that is, is used to prepare the first outer layer with positive dielectric constant and the
Two outer layers；0.1624g carbon nanotube (mass ratio of the carbon nanotube of addition and mixed solution is 3%), preparation is added in slurry B
Intermediate layer film with negative permittivity.Slurry A, B magnetic agitation 10min, then sonic oscillation handles 10min.
(4) using successively coating, successively cured method, slurry A, B are respectively coated on to smooth, smooth glass plate
On, the flexible composite film of the sandwich structure of A-B-A type is made.At 400 μm, solidification temperature is the thickness control of monofilm
120 DEG C, curing time 2h.
(5) after the curing be complete, dimethyl silicone polymer/carbon nano tube flexible laminated film is shelled from plate glass
From.
The dielectric properties for the flexible composite film being prepared are measured using Agilent E4980AL test table.Knot
Fruit is as shown in figure 1 shown in the corresponding map of 1%-3%-1%, and dielectric constant is 50 or more.
Embodiment 3
(1) presoma and organic solvent normal heptane 2.5g of dimethyl silicone polymer are weighed, then magnetic agitation 10min,
It is uniformly mixed it.
(2) 0.25g curing agent is added, magnetic agitation 10min is uniformly mixed it, and it is molten to obtain the mixing that gross weight is 5.25g
Liquid.
(3) according to quality proportioning addition carbon nanotube is calculated, obtained slurry A, B, which is respectively used to preparation, has positive and negative Jie
The coating of electric constant, wherein (carbon nanotube of addition and the mass ratio of mixed solution are slurry A addition 0.08g carbon nanotube
1.5%), preparation has the upper and lower layer film of positive dielectric constant, that is, be used to prepare the first outer layer with positive dielectric constant and
Second outer layer；0.1624g carbon nanotube (mass ratio of the carbon nanotube of addition and mixed solution is 3%), system is added in slurry B
The standby intermediate layer film with negative permittivity.Slurry A, B distinguish magnetic agitation 10min, and then sonic oscillation handles 10min.
(4) using successively coating, successively cured method, slurry A, B are respectively coated on to smooth, smooth glass plate
On, the flexible composite film of the sandwich structure of A-B-A type is made.At 400 μm, solidification temperature is the thickness control of monofilm
120 DEG C, curing time 2h.
(5) after the curing be complete, dimethyl silicone polymer/carbon nano tube flexible laminated film is shelled from plate glass
From.
The dielectric properties for the flexible composite film being prepared are measured using Agilent E4980AL test table.Knot
Fruit is as shown in figure 1 shown in the corresponding map of 1.5%-3%-1.5%, and dielectric constant is 100 or more.
Embodiment 4
(1) presoma and organic solvent normal heptane 2.5g of dimethyl silicone polymer are weighed, then magnetic agitation 10min,
It is uniformly mixed it.
(2) 0.25g curing agent is added, magnetic agitation 10min is uniformly mixed it, and it is molten to obtain the mixing that gross weight is 5.25g
Liquid.
(3) according to quality proportioning addition carbon nanotube is calculated, obtained slurry A, B, which is respectively used to preparation, has positive and negative Jie
The coating of electric constant, wherein (carbon nanotube of addition and the mass ratio of mixed solution are slurry A addition 0.1071g carbon nanotube
2%), preparation has the upper and lower layer film of positive dielectric constant, that is, is used to prepare the first outer layer with positive dielectric constant and the
Two outer layers；0.1624g carbon nanotube (mass ratio of the carbon nanotube of addition and mixed solution is 3%), preparation is added in slurry B
Intermediate layer film with negative permittivity.Slurry A, B distinguish magnetic agitation 10min, and then sonic oscillation handles 10min.
(4) using successively coating, successively cured method, slurry A, B are respectively coated on to smooth, smooth glass plate
On, the flexible composite film of the sandwich structure of A-B-A type is made.At 400 μm, solidification temperature is the thickness control of monofilm
120 DEG C, curing time 2h.
(5) after the curing be complete, dimethyl silicone polymer/carbon nano tube flexible laminated film is shelled from plate glass
From.
The dielectric properties for the flexible composite film being prepared are measured using Agilent E4980AL test table.Knot
Fruit is as shown in figure 1 shown in the corresponding map of 2%-3%-2%, and dielectric constant is 250 or more.
Comparative example 1
(1) presoma and each 2.5g of organic solvent normal heptane of dimethyl silicone polymer are weighed, then magnetic agitation
10min is uniformly mixed it.
(2) 0.25g curing agent is added, magnetic agitation 10min is uniformly mixed it, and it is molten to obtain the mixing that gross weight is 5.25g
Liquid.
(3) according to quality proportioning addition carbon nanotube is calculated, obtained slurry A, B, which is respectively used to preparation, has positive and negative Jie
The coating of electric constant, wherein carbon nanotube is not added by slurry A, prepares the upper and lower layer film with positive dielectric constant, i.e., for making
Standby the first outer layer and the second outer layer with positive dielectric constant；0.1624g carbon nanotube is added in slurry B, and (carbon of addition is received
The mass ratio of mitron and mixed solution is 3%), to prepare the intermediate layer film with negative permittivity.And slurry A, B magnetic force is stirred
10min is mixed, then sonic oscillation handles 10min.
(4) using successively coating, successively cured method, slurry A, B are respectively coated on to smooth, smooth glass plate
On, the flexible composite film of the sandwich structure of A-B-A type is made.At 400 μm, solidification temperature is the thickness control of monofilm
120 DEG C, curing time 2h.
(5) after the curing be complete, dimethyl silicone polymer/carbon nano tube flexible laminated film is shelled from plate glass
From.
The dielectric properties for the flexible composite film being prepared are measured using Agilent E4980AL test table.Knot
Fruit is as shown in figure 1 shown in the corresponding map of 0%-3%-0%, and dielectric constant is less than 50.
In conclusion the high dielectric flexible laminated film with sandwich structure prepared in the present invention, has higher
Dielectric constant.High dielectric flexible laminated film of the invention can be improved disruptive field intensity while improving dielectric constant.This
The flexible composite film for inventing preparation has important answer in fields such as flexible electronic device, thin film capacitor and wearable devices
With value.
It is discussed in detail although the contents of the present invention have passed through above preferred embodiment, but it should be appreciated that above-mentioned
Description is not considered as limitation of the present invention.After those skilled in the art have read above content, for of the invention
A variety of modifications and substitutions all will be apparent.Therefore, protection scope of the present invention should be limited to the appended claims.
Claims (10)
1. a kind of preparation method of the high dielectric flexible laminated film of sandwich structure, which is characterized in that the laminated film
It is made of three-decker stacking, the three-decker is respectively as follows: the first outer layer with positive dielectric constant, has negative dielectric
The middle layer of constant and the second outer layer with positive dielectric constant；The middle layer be set to first outer layer and
Between second outer layer；The preparation method comprises the steps of:
The presoma, curing agent and organic solvent of organic silicon rubber are uniformly mixed by step (1), obtain mixed solution；Wherein,
The organic solvent is equal with the quality of the presoma, and the mass ratio of the presoma and the curing agent is
10:1；
The mixed solution and carbon nanotube are mixed to form slurry by step (2)；
When the quality of carbon nanotube and the mass percent of the mixed solution are 0.5%~2%, the slurry of formation is used to prepare
First outer layer or second outer layer；
When the quality of carbon nanotube and the mass percent of the mixed solution are 3%, the slurry of formation is used to prepare described
Middle layer；
The slurry for being used to prepare first outer layer is coated on plate by step (3), and coating is used to prepare described after solidification
The slurry of middle layer, re-coating is used to prepare slurry and the solidification of second outer layer after cured, obtains by having positive be situated between
The first outer layer, the middle layer with negative permittivity and the second outer layer with positive dielectric constant of electric constant are laminated
The laminated film of the sandwich structure of composition；
Step (4), the laminated film is removed from plate.
2. the preparation method of the high dielectric flexible laminated film of sandwich structure according to claim 1, which is characterized in that
In step (1), the organic silicon rubber is dimethyl silicone polymer.
3. the preparation method of the high dielectric flexible laminated film of sandwich structure according to claim 1, which is characterized in that
In step (1), the organic solvent is normal heptane.
4. the preparation method of the high dielectric flexible laminated film of sandwich structure according to claim 1, which is characterized in that
In step (3), the plate refers to glass plate.
5. the preparation method of the high dielectric flexible laminated film of sandwich structure according to claim 1, which is characterized in that
In step (3), the cured temperature is 80 DEG C~180 DEG C, and the time is 1h~3h.
6. the preparation method of the high dielectric flexible laminated film of sandwich structure according to claim 1, which is characterized in that
In step (3), the cured temperature is 120 DEG C, time 2h.
7. the preparation method of the high dielectric flexible laminated film of sandwich structure according to claim 1, which is characterized in that
The thickness of the middle layer, first outer layer and second outer layer is 0.1~2mm.
8. the preparation method of the high dielectric flexible laminated film of sandwich structure according to claim 1, which is characterized in that
The thickness of the middle layer, first outer layer and second outer layer is 0.2mm.
9. a kind of high dielectric flexible laminated film of sandwich structure, which is characterized in that the laminated film is by three-decker
Stacking composition, the three-decker are respectively as follows: the first outer layer with positive dielectric constant, with the centre of negative permittivity
Layer and the second outer layer with positive dielectric constant；The middle layer is set to first outer layer and described second
Between outer layer；First outer layer, the middle layer and second outer layer having by different proportion respectively
Machine silicon rubber and carbon nanotube are compounded to form.
10. the high dielectric flexible laminated film of sandwich structure according to claim 9, which is characterized in that described answers
The preparation method for closing film comprises the steps of:
The presoma, curing agent and organic solvent of organic silicon rubber are uniformly mixed by step (1), obtain mixed solution；Wherein,
The organic solvent is equal with the quality of the presoma, and the mass ratio of the presoma and the curing agent is
10:1；
The mixed solution and carbon nanotube are mixed to form slurry by step (2)；
When the quality of carbon nanotube and the mass percent of the mixed solution are 0.5%~2%, the slurry of formation is used to prepare
First outer layer or second outer layer；
When the quality of carbon nanotube and the mass percent of the mixed solution are 3%, the slurry of formation is used to prepare described
Middle layer；
The slurry for being used to prepare first outer layer is coated on plate by step (3), and coating is used to prepare described after solidification
The slurry of middle layer, re-coating is used to prepare slurry and the solidification of second outer layer after cured, obtains by having positive be situated between
The first outer layer, the middle layer with negative permittivity and the second outer layer with positive dielectric constant of electric constant are laminated
The laminated film of the sandwich structure of composition；
Step (4), the laminated film is removed from plate.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111710527A (en) * | 2020-07-08 | 2020-09-25 | 中南大学 | Organic-inorganic nano composite dielectric and preparation method thereof |
| CN112389038A (en) * | 2020-10-26 | 2021-02-23 | 上海海事大学 | High-dielectric and low-loss material based on capacitance and inductance synergistic effect and preparation method thereof |
| CN112615163A (en) * | 2020-12-08 | 2021-04-06 | 中国人民解放军海军工程大学 | Multilayer periodic wave-transparent structure based on ideal conductor filling |
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