CN105838001A - Preparation method of polyvinylidene fluoride composite material with high dielectric constant - Google Patents
Preparation method of polyvinylidene fluoride composite material with high dielectric constant Download PDFInfo
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Abstract
The invention discloses a preparation method of a polyvinylidene fluoride composite material with the high dielectric constant .The method comprises the steps of A, preparing a master batch through a co-precipitation method, wherein 100 parts by weight of polyvinylidene fluoride is dissolved into a N,N-dimethyl formamide solution to obtain a first solution, 1-5 parts by weight of iron-nitrogen alloy and 1-5 parts by weight of carbon nano tubes are dispersed into a N,N-dimethyl formamide solution to obtain a second solution, the first solution and the second solution are mixed to obtain a mixed solution, the mixed solution is poured into distilled water to enable polyvinylidene fluoride, carbon nano tubes and iron-nitrogen alloy to be subjected to co-precipitation in distilled water, precipitation is performed to obtain a three-phase composite material, the three-phase composite material is placed into a vacuum oven to be heated and dried, and the polyvinylidene fluoride/iron-nitrogen alloy/carbon nano tube master batch is obtained; B, performing melt blending, wherein the master batch obtained in the step A is subjected to extrusion granulation in a micro-extruder under the temperature of 190 DEG C for 6-10 min, and the polyvinylidene fluoride composite material is obtained .The prepared composite material is high in dielectric constant, low in dielectric loss, simple in technology and beneficial to mass production .
Description
Technical field
The present invention relates to the preparation method of the polyvinylidene fluoride-based composite of a kind of high-k.
Technical background
The exploitation of the novel dielectric material with high-k is that of current electronic material industry is important grinds
Study carefully field.In the electronics industry, energy-storage capacitor the highest for electronic device require have high-k,
Miniaturization, the easily requirement such as processing and excellent in mechanical performance.But traditional dielectric material is
Main, predominantly ferroelectric material, metal-oxide, nitride etc., although dielectric properties are excellent, but processing is tired
Difficulty is difficult to take into account good mechanical property simultaneously.Common high molecular polymer has light weight, and dielectric loss is low
And be prone to the advantages such as processing, but dielectric constant is the most on the low side.If preparing polymer-based dielectric material, its
Advantage is on the one hand polymeric material light weight, meets electronic device lightweight requirements;On the other hand, compare
For inorganic material, polymeric material is easily processed, and excellent in mechanical performance.The polymer base of application now
Dielectric material, mostly to add ceramic particle, but ceramic particle cannot be built well at material internal
Polarization networks, addition is relatively big, thus causes material to present fragility, processes the most difficult.Therefore, in order to
Realize material internal to polarize on a large scale, it is intended that fill out toward the internal conduction adding few content of polymeric material
Polarization networks built by material.Relative to other organic polymers, Kynoar has polymorphic microstructure,
Thus there is more excellent dielectric, piezoelectricity, ferroelectricity and pyroelectric.And CNT to be one the best
Conductive filler, electric charge can be freely-movable on one-dimensional CNT, and therefore CNT easily helps to gather
Interfacial polarization is there is in compound composite material after having built filler network.
In recent years, along with the further development of nanotechnology, polymer nanocomposite electrolyte receives and closes widely
Note.Polymer nanocomposite electrolyte is that inorganic filler is dispersed in polymer the compound of formation with nanoscale
System.Although but the dielectric constant of existing polymer nanocomposite dielectric composite is higher, but its dielectric is damaged
Consume higher, seriously constrain its development and application.So it is desirable that at polymer/conductive filler compound system
On the basis of, reduce its dielectric loss further, improve the application prospect of composite.Ceramic packing has
Preferably not there is while dielectric properties good electric conductivity, therefore it is proposed that, by adding pottery
Granule carrys out dispersed electro-conductive filler, make conductive filler can in polymeric matrix dispersed occur polarization and not
Mutually it is overlapped to form network and causes big Leakage Current.
Summary of the invention
It is an object of the invention to provide the preparation side of the polyvinylidene fluoride-based composite of a kind of high-k
Method, composite dielectric constant prepared by the method is high, and dielectric loss is low simultaneously;And its technique is simple, have
It is beneficial to large-scale production.
The present invention realizes its goal of the invention and be employed technical scheme comprise that, the polyvinylidene fluoride of a kind of high-k
The preparation method of thiazolinyl composite, the steps include:
A, coprecipitation prepare masterbatch: the Kynoar that 100 parts heavy is dissolved in N, N dimethylformamide
Solution obtains solution one, Fe-N Alloys and 15 parts of heavy CNTs of 15 parts of weights are scattered in N, N diformazan
Base formamide solvent obtains solution two;Solution one, solution two are mixed to obtain mixed solution;Mixed solution is poured into
Distilled water make N, N dimethylformamide be dissolved in distilled water, and Kynoar, CNT, ferrum nitrogen
Alloy is co-precipitated at distilled water, separates out and obtains Kynoar/CNT/Fe-N Alloys three-phase composite material
Material;
Again Kynoar/CNT/Fe-N Alloys three-phase composite material is put into vacuum drying oven heating, drying,
Obtain Kynoar/Fe-N Alloys/carbon nanotube masterbatch;Described Fe-N Alloys Fe(2‐19)N alloy powder;
B, melt blending: Kynoar/Fe-N Alloys/carbon nanotube masterbatch A step obtained squeezes miniature
Going out to carry out in machine temperature is 190 DEG C, and the time is the extruding pelletization of 6 10min, to obtain final product.
Compared with prior art, the invention has the beneficial effects as follows:
One, preparation method of the present invention is secondary operations blend method (solution is with melted), preparation side
Method is simple, can effectively ensure that dispersed in matrix material of filler simultaneously, can also promote filler simultaneously
Between interpenetrate diffusion so that two kinds of filler Fe-N Alloyses of 15 parts of weights and CNT, 100
The Kynoar matrix of part weight can be effectively formed dielectric Percolation network structure;Meanwhile, Fe-N Alloys can break
The mutual overlap joint of bad CNT so that it is cannot form effective conductive network, but adjacent CNT it
Between still can form micro-capacitance structure, therefore, while improving dielectric constant, make dielectric loss substantially drop
Low.The material that the present invention prepares, its dielectric constant values measured is all more than 150, and dielectric loss is all 1
Below.
Two, the present invention uses Fe-N Alloys and CNT as filler, and both rigidity are high, and modulus is big, fills out
Filling the composite modulus prepared by Kynoar to increase substantially, therefore the combination property of composite is excellent
Different.
Three, raw materials of the present invention is CNT, Fe-N Alloys and Kynoar, wherein CNT
With Kynoar raw material wide material sources, low cost, simple and easy to get.Preparation process is that secondary operations is blended (molten
Liquid is with melted), its mild condition, Device-General, preparation cost is low, beneficially large-scale promotion.
Further, the CNT of the present invention is diameter 0.5-200nm, the acidifying of length 100nm-50 μm
SWCN or acidifying multi-walled carbon nano-tubes.
The acidifying SWCN of this diameter and length or acidifying multi-walled carbon nano-tubes, by carboxyl grafting,
Can ensure that CNT has more preferable dispersion effect inside polymeric matrix, it is to avoid CNT exists
Polymeric matrix is piled up and bigger leakage current is occurred by internal generation.
Further, the Fe of the present invention(2‐19)The specific surface area of N alloy powder is 1.58m2/ g, saturated magnetization is strong
Degree is 80emu/g, a diameter of 300 400nm of powder.
Further, the Kynoar that 100 parts heavy is dissolved in DMF solution by the present invention
The concrete operations obtaining solution one are: solution temperature is 55-80 DEG C, and dissolution time is 20-40min, and adjoint
The stirring of 50-100r/min.
In this manner it is ensured that Kynoar can solve homogeneously in DMF solvent, formed
Kynoar/N,N-dimethylformamide solution.
Further, the Fe-N Alloys of 1-5 part weight and the CNT of 1-5 part weight are scattered in N, N-by the present invention
Solvent dimethylformamide obtains the concrete operations of solution two: temperature is 55-80 DEG C, and jitter time is 20-40
Min, and with the stirring of 50-100r/min.
So, beneficially Fe-N Alloys alloy powder and CNT are fast in DMF solution
Speed diffusion is the most dispersed, obtains Fe-N Alloys and CNT dispersed in DMF
Suspension.
Further, the present invention solution one, solution two are mixed the concrete operations of mixed solution are: 55-80 DEG C
At a temperature of, stirring 30min, more at room temperature, ultrasonic disperse 1-2h.
So, can guarantee that Kynoar will not be precipitated out due to the reduction of temperature from solvent, stir at this
Mixing speed and under the time, beneficially mixed solution is more uniformly distributed, and contribute to phase counterdiffusion between filler with
Infiltration.
Below in conjunction with detailed description of the invention, the present invention is described in further detail.
Detailed description of the invention
Embodiment one
A, coprecipitation prepare masterbatch: by 100 parts of heavy Kynoar, are dissolved in N, N dimethyl formyl
Obtaining solution one in amine aqueous solution, solution temperature during dissolving is 55 DEG C, and dissolution time is 20min, and with 50
The stirring of r/min;
It is 1.58m by specific surface area2/ g, saturation magnetization are 80emu/g, a diameter of 300 400nm
1 part of heavy Fe(2‐19)N alloy powder and diameter 0.5 200nm, 1 part heavy of length 100nm 50 μm
Acidifying SWCN is scattered in N, N solvent dimethylformamide and obtains solution two;Concrete operations during dispersion
Being: temperature is 55 DEG C, jitter time is 20min, and with the stirring of 50r/min
Solution one, solution two are mixed to obtain mixed solution;Concrete operations during mixing are: at a temperature of 55 DEG C,
Stirring 30min, more at room temperature, ultrasonic disperse 1h.
Then, being poured into by mixed solution in distilled water and make N, N dimethylformamide is dissolved in distilled water, and gathers
Vinylidene, CNT, Fe-N Alloys are co-precipitated at distilled water, separate out and obtain Kynoar/carbon
Nanotube/Fe-N Alloys three-phase composite material;
Again Kynoar/CNT/Fe-N Alloys three-phase composite material is put into vacuum drying oven heating, drying,
Obtain Kynoar/Fe-N Alloys/carbon nanotube masterbatch.
B, melt blending: Kynoar/Fe-N Alloys/carbon nanotube masterbatch is carried out in miniature extruder
Temperature is 190 DEG C, and the time is the extruding pelletization of 6min, to obtain final product.
The dielectric constant values of Kynoar/Fe-N Alloys/carbon nano tube compound material that this example prepares is 152,
Dielectric loss value is 0.2.
Embodiment two
A, coprecipitation prepare masterbatch: by 100 parts of heavy Kynoar, are dissolved in N, N dimethyl formyl
Obtaining solution one in amine aqueous solution, solution temperature during dissolving is 65 DEG C, and dissolution time is 30min, and with 70
The stirring of r/min;
It is 1.58m by specific surface area2/ g, saturation magnetization are 80emu/g, a diameter of 300 400nm
1 part of heavy Fe(2‐19)N alloy powder and diameter 0.5 200nm, 2 parts heavy of length 100nm 50 μm
Acidifying SWCN is scattered in N, N solvent dimethylformamide and obtains solution two;Concrete operations during dispersion
Being: temperature is 55 DEG C, jitter time is 20min, and with the stirring of 70r/min
Solution one, solution two are mixed to obtain mixed solution;Concrete operations during mixing are: at a temperature of 55 DEG C,
Stirring 30min, more at room temperature, ultrasonic disperse 1.5h.
Then, being poured into by mixed solution in distilled water and make N, N dimethylformamide is dissolved in distilled water, and gathers
Vinylidene, CNT, Fe-N Alloys are co-precipitated at distilled water, separate out and obtain Kynoar/carbon
Nanotube/Fe-N Alloys three-phase composite material;Again by Kynoar/CNT/Fe-N Alloys three-phase composite
Vacuum drying oven heating, drying put into by material, obtains Kynoar/Fe-N Alloys/carbon nanotube masterbatch;
B, melt blending: Kynoar/Fe-N Alloys/carbon nanotube masterbatch is carried out in miniature extruder
Temperature is 190 DEG C, and the time is the extruding pelletization of 10min, to obtain final product.
The dielectric constant values of Kynoar/Fe-N Alloys/carbon nano tube compound material that this example prepares is 168,
Dielectric loss value is 0.19.
Embodiment three
A, coprecipitation prepare masterbatch: by 100 parts of heavy Kynoar, are dissolved in N, N dimethyl formyl
Obtaining solution one in amine aqueous solution, solution temperature during dissolving is 80 DEG C, and dissolution time is 40min, and with 90
The stirring of r/min;
It is 1.58m by specific surface area2/ g, saturation magnetization are 80emu/g, a diameter of 300 400nm
2 parts of heavy Fe(2‐19)N alloy powder and diameter 0.5 200nm, 5 parts heavy of length 100nm 50 μm
Acidifying SWCN is scattered in N, N solvent dimethylformamide and obtains solution two;Concrete operations during dispersion
Being: temperature is 55 DEG C, jitter time is 30min, and with the stirring of 60r/min
Solution one, solution two are mixed to obtain mixed solution;Concrete operations during mixing are: at a temperature of 70 DEG C,
Stirring 30min, more at room temperature, ultrasonic disperse 1.5h.
Then, being poured into by mixed solution in distilled water and make N, N dimethylformamide is dissolved in distilled water, and gathers
Vinylidene, CNT, Fe-N Alloys are co-precipitated at distilled water, separate out and obtain Kynoar/carbon
Nanotube/Fe-N Alloys three-phase composite material;Again by Kynoar/CNT/Fe-N Alloys three-phase composite
Vacuum drying oven heating, drying put into by material, obtains Kynoar/Fe-N Alloys/carbon nanotube masterbatch;
B, melt blending: Kynoar/Fe-N Alloys/carbon nanotube masterbatch is carried out in miniature extruder
Temperature is 190 DEG C, and the time is the extruding pelletization of 8min, to obtain final product.
The dielectric constant values of Kynoar/Fe-N Alloys/carbon nano tube compound material that this example prepares is 231,
Dielectric loss value is 0.26.
Embodiment four
A, coprecipitation prepare masterbatch: by 100 parts of heavy Kynoar, are dissolved in N, N dimethyl formyl
Obtaining solution one in amine aqueous solution, solution temperature during dissolving is 70 DEG C, and dissolution time is 35min, and with 100
The stirring of r/min;
It is 1.58m by specific surface area2/ g, saturation magnetization are 80emu/g, a diameter of 300 400nm
5 parts of heavy Fe(2‐19)N alloy powder and diameter 0.5 200nm, 5 parts heavy of length 100nm 50 μm
Acidifying multi-walled carbon nano-tubes is scattered in N, N solvent dimethylformamide and obtains solution two;Concrete operations during dispersion
Being: temperature is 80 DEG C, jitter time is 40min, and with the stirring of 100r/min
Solution one, solution two are mixed to obtain mixed solution;Concrete operations during mixing are: at a temperature of 80 DEG C,
Stirring 30min, more at room temperature, ultrasonic disperse 2h.
Then, being poured into by mixed solution in distilled water and make N, N dimethylformamide is dissolved in distilled water, and gathers
Vinylidene, CNT, Fe-N Alloys are co-precipitated at distilled water, separate out and obtain Kynoar/carbon
Nanotube/Fe-N Alloys three-phase composite material;Again by Kynoar/CNT/Fe-N Alloys three-phase composite
Vacuum drying oven heating, drying put into by material, obtains Kynoar/Fe-N Alloys/carbon nanotube masterbatch;
B, melt blending: Kynoar/Fe-N Alloys/carbon nanotube masterbatch is carried out in miniature extruder
Temperature is 190 DEG C, and the time is the extruding pelletization of 7min, to obtain final product.
The Fe that the present invention uses(2-19)N alloy powder can be by document Materials and Design 90 (2016)
115-121“Preparation of high performance bulk Fe–N alloy by spark plasma
Sintering " method recorded prepares.
Table 1 is the embodiment of the present invention one, embodiment two, embodiment three, the polyvinylidene fluoride of embodiment four preparation
The dielectric constant values of alkene/Fe-N Alloys/carbon nano tube compound material.
Table 1 Kynoar/Fe-N Alloys/carbon nano tube compound material dielectric constant values
Component | Embodiment one | Embodiment two | Embodiment three |
Dielectric constant | 152 | 168 | 231 |
Table 2 is the embodiment of the present invention one, embodiment two, embodiment three and the polyvinylidene fluoride of embodiment four preparation
The dielectric loss value of alkene/Fe-N Alloys/carbon nano tube compound material.
Table 2 Kynoar/Fe-N Alloys/carbon nano tube compound material dielectric loss value
Component | Embodiment one | Embodiment two | Embodiment three |
Dielectric loss | 0.2 | 0.19 | 0.26 |
As can be seen from Table 1 and Table 2, the addition of CNT is greatly improved dielectric constant, pure
Kynoar dielectric constant is only 8, and the dielectric constant of the composite of the present invention is maintained at more than 150;
And the addition of Fe-N Alloys, effectively limits the dielectric loss of material, and its dielectric loss is below 0.26.
Visible, the composite of the present invention has higher dielectric constant, and dielectric loss is low simultaneously, is effectively increased material
The combination property of material, has widened the range of application of material.
Claims (6)
1. a preparation method for the polyvinylidene fluoride-based composite of high-k, the steps include:
A, coprecipitation prepare masterbatch: the Kynoar that 100 parts heavy is dissolved in N, N dimethylformamide
Solution obtains solution one, Fe-N Alloys and 15 parts of heavy CNTs of 15 parts of weights are scattered in N, N diformazan
Base formamide solvent obtains solution two;Solution one, solution two are mixed to obtain mixed solution;Mixed solution is poured into
Distilled water make N, N dimethylformamide be dissolved in distilled water, and Kynoar, CNT, ferrum nitrogen
Alloy is co-precipitated at distilled water, separates out and obtains Kynoar/CNT/Fe-N Alloys three-phase composite material
Material;
Again Kynoar/CNT/Fe-N Alloys three-phase composite material is put into vacuum drying oven heating, drying,
Obtain Kynoar/Fe-N Alloys/carbon nanotube masterbatch;Described Fe-N Alloys is Fe(2‐19)N alloyed powder
End;
B, melt blending: Kynoar/Fe-N Alloys/carbon nanotube masterbatch A step obtained squeezes miniature
Going out to carry out in machine temperature is 190 DEG C, and the time is the extruding pelletization of 6 10min, to obtain final product.
The preparation of the polyvinylidene fluoride-based composite of a kind of high-k the most according to claim 1
Method, it is characterised in that: described CNT is diameter 0.5-200nm, length 100nm-50 μm
Acidifying SWCN or acidifying multi-walled carbon nano-tubes.
The preparation of the polyvinylidene fluoride-based composite of a kind of high-k the most according to claim 1
Method, it is characterised in that: described Fe(2‐19)The specific surface area of N alloy powder is 1.58m2/ g, saturated magnetic
Change intensity is 80emu/g, a diameter of 300 400nm of powder.
The preparation of the polyvinylidene fluoride-based composite of a kind of high-k the most according to claim 1
Method, it is characterised in that: described is dissolved in DMF by the Kynoar that 100 parts are heavy
The concrete operations obtaining solution one in solution are: solution temperature is 55-80 DEG C, and dissolution time is 20-40min,
And with the stirring of 50-100r/min.
The preparation of the polyvinylidene fluoride-based composite of a kind of high-k the most according to claim 1
Method, it is characterised in that: the CNT of the described Fe-N Alloys by 1-5 part weight and 1-5 part weight is scattered in
DMF solvent obtains the concrete operations of solution two: temperature is 55-80 DEG C, and jitter time is
20-40min, and with the stirring of 50-100r/min.
The preparation of the polyvinylidene fluoride-based composite of a kind of high-k the most according to claim 1
Method, it is characterised in that: described solution one, solution two are mixed the concrete operations of mixed solution are:
At a temperature of 55-80 DEG C, stirring 30min, more at room temperature, ultrasonic disperse 1-2h.
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CN110527224A (en) * | 2019-09-04 | 2019-12-03 | 北京化工大学 | A kind of Kynoar base wave-absorbing material and preparation method thereof |
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Cited By (3)
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CN106751243A (en) * | 2016-12-05 | 2017-05-31 | 西南交通大学 | The preparation method of high dielectric constant and low dielectric loss polyvinylidene fluoride composite |
CN106751243B (en) * | 2016-12-05 | 2018-10-19 | 西南交通大学 | The preparation method of high dielectric constant and low dielectric loss polyvinylidene fluoride composite material |
CN110527224A (en) * | 2019-09-04 | 2019-12-03 | 北京化工大学 | A kind of Kynoar base wave-absorbing material and preparation method thereof |
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