CN110452421A - A kind of dielectric composite material based on core-shell structure filler - Google Patents
A kind of dielectric composite material based on core-shell structure filler Download PDFInfo
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Abstract
The invention belongs to dielectric composite material fields, and in particular to a kind of dielectric composite material based on core-shell structure filler.The specific technical proposal is: the dielectric composite material includes ceramic material and polymer, the ceramic material is core-shell structure, and in the core-shell structure, the dielectric constant of shell structure is less than the dielectric constant of nuclear structure.The present invention breaks through tradition and carries out surface coated Research Thinking to barium titanate, prepares BaTiO by two one-step hydrothermals as shell using paraelectric phase strontium titanates3‑SrTiO3Compound nucleocapsid filler prepares dielectric composite material with polymer matrix bluk recombination, reduces the interfacial polarization and residual polarization of composite material, increases anti-breakdown electric field, and then the energy storage density and efficiency of dielectric composite material greatly improved.Dielectric composite material provided by the invention can be widely applied in all kinds of capacitors.
Description
Technical field
The invention belongs to dielectric composite material fields, and in particular to a kind of dielectric composite wood based on core-shell structure filler
Material.
Background technique
In recent years, electronics technology development is maked rapid progress, and capacitor is widely used because of the power density with superelevation
In high power device, such as laser gun, radar, railgun, defibrillator and space station.But compared to fuel cell, lithium
The electrochemical energy storing devices such as ion battery, supercapacitor, the capacitor disadvantage low there are still energy density, so that its application
It is the big part of electronic component, re-quantization, it is expensive, it limits its application and develops.Therefore, the energy for improving capacitor is close
Degree, and then make device miniaturization, it is always the direction that researchers make great efforts.
Important component of the dielectric material as capacitor, according to its energy density (Ue) calculation formula:
Ue=∫ EdD=∫ ε0εrEdE。
Wherein, E, ε0, εrRespectively anti-breakdown electric field, permittivity of vacuum and the relative dielectric constant of material.It is found that wanting
The energy density of capacitor is improved, the relative dielectric constant and resistance for needing to improve dielectric material wear electric field value.
It is concentrated on inorganic ceramic filler/polymer composite systems currently, the field is largely studied, it is intended to will
The advantages of inorganic filler high dielectric constant, combines with the advantages of polymeric matrix highly resistance breakdown electric field, low-dielectric loss, with
Make dielectric composite material while obtaining high dielectric constant and anti-breakdown electric field, and then improves its energy storage density.
Representative of the barium titanate as traditional ferroelectric ceramics, since it is there are spontaneous polarization feature, the dielectric with superelevation is normal
Number, thus become the popular selection of filler in dielectric composite material.Researchers are about barium titanate filler to composite material dielectric
And the influence of energy-storage property has carried out a series of research work, for example, Tongji University Zhai Jiwei professor team has studied respectively
With BaTiO3Nanosphere and nano wire are as filler, to the affecting laws of PVDF base dielectric composite material energy storage density.Study table
It is bright, BaTiO3Ceramic packing can significantly improve the dielectric constant and energy storage density of composite material；With BaTiO3Filer content
Increase, the dielectric constant of composite material is gradually increased.
But due to BaTiO3The dielectric loss of ferroelectric ceramics itself is larger, with BaTiO in composite material3Ceramic packing
The increase of content not only can make the remanent polarization of composite material be gradually increased, and energy loss increases, can also be in the composite
The defects of introducing hole and crackle limits composite material energy storage density so that electric field value significant decrease is worn in the resistance of compound
Raising.
For this problem, researchers are from interface engineering angle, in BaTiO3It is normal that surface coats other low dielectrics
Several shell ceramics reduce the difference of dielectric constant between filler and polymer to form single-stage or multistage gradient interface to reduce
Loss, and then improve the energy storage density and efficiency of composite material.
For example, Lin et al. passes through in BaTiO3Nanofiber surface coats one layer of non-ferroelectric ceramics TiO2Shell utilizes
TiO2The characteristic of shell low-k and non-ferroelectric reduces the dielectric loss of composite material and the feelings of non-uniform electric
Condition, and then improve the energy storage density of composite material.Pan et al. is by the method for electrostatic spinning in BaTiO3Nanofiber surface draws
Enter Al2O3Dielectric ceramic layer improves the anti-breakdown electric field of composite material to reduce energy loss, obtains high energy storage density and effect
Rate.
Currently, the BaTiO studied3-SiO2, BaTiO3-Al2O3Equal nucleocapsids filler systems, it is this kind of with BaTiO3For core
The low-k ceramic shell system of preparation is improved between filler and polymeric matrix by introducing low-k shell
The mispairing of dielectric constant and composite material internal field concentrate, and reduce interfacial polarization, and then improve anti-breakdown electric field, improve
The energy storage density of composite material.But at the same time, the low-k shell ceramics and BaTiO of introducing3There is very big crystalline substance in core
The defects of body architectural difference, there are crackles, hole for nucleocapsid interface, these defects are likely to become the additional transmissions of electric charge carrier
Channel introduces additional interfacial polarization in dielectric composite material.
Therefore, how to provide it is a kind of improving anti-breakdown electric field while keeping low residual polarization, high storage is had both with acquisition
The dielectric composite material of energy density and energy storage efficiency, is still the difficult point of this field.
Summary of the invention
The object of the present invention is to provide a kind of dielectric composite materials for having both high energy storage density and energy storage efficiency.
For achieving the above object, the technical scheme adopted by the invention is that: a kind of dielectric composite material, the dielectric
Composite material includes ceramic material and polymer, and the ceramic material is core-shell structure, in the core-shell structure, Jie of shell structure
Electric constant is less than the dielectric constant of nuclear structure, and the material of the shell structure and nuclear structure is perovskite structure.
Preferably, in the core-shell structure, nuclear structural materials BaTiO3；Shell structure material is SrTiO3。
Preferably, the preparation method of the core-shell structure includes the following steps:
(1) by Ba (OH)2·8H2O is added in acetic acid solution, and dissolution is sufficiently stirred, obtains solution 1；
(2) by TiCl4It is added in ethanol solution, obtains solution 2；
(3) solution 1 and solution 2 are mixed, obtains precursor solution；
(4) solid NaOH is added in the precursor solution, mixes well, obtains intermediate liquid suspension；
(5) by Sr (OH)2·8H2O is dissolved in acetic acid solution, obtains solution 3；
(6) solution 3 is added in the intermediate liquid suspension, is mixed well, after hydro-thermal reaction, reaction product is washed
It washs, dry to get required core-shell structure.
Preferably, the volume of the core-shell structure is the 1%~3% of polymer volume.
Preferably, the preparation method of the dielectric composite material includes the following steps:
(1) core-shell material is added in organic solvent, ultrasonic disperse is simultaneously stirred well to uniformly；
(2) polymer is added in a solvent again, after fully dispersed, obtains dielectric composite material solution；
(3) the dielectric composite material solution curtain coating is formed, obtains the dielectric composite material.
Correspondingly, the application of the dielectric composite material in the capacitor.
The invention has the following advantages:
It is existing to BaTiO3The method that filler is handled is the material that one layer of low-k is directly coated on surface
Material is also easy to introduce at nucleocapsid interface simultaneously scarce although this method can reduce dielectric loss, improve anti-breakdown electric field
It falls into.And conventional method is broken through herein, by two one-step hydrothermals, make SrTiO3Epitaxial growth is in BaTiO3Surface prepares BaTiO3-
SrTiO3Nucleocapsid filler, is then combined dielectric composite material with polymeric matrix, the stored energy application for dielectric capacitor.
Wherein, the strontium titanates and barium titanate perovskite structure having the same and similar lattice constant used in the present invention.
Use has the strontium titanates of same crystal structure as shell with barium titanate, and in hydrothermal reaction process, strontium titanates can be along titanium
Sour barium surface grows shell, forms the less interface area of defect, can both improve the dielectric constant mispairing of filler and matrix, reduces
Interfacial polarization, and additional polarized generation can be reduced.Importantly, strontium titanates is paraelectric phase at room temperature, have low
Remanent polarization and dielectric loss are more advantageous to the energy storage efficiency for improving composite material compared with general advanced low-k materials.
The dielectric composite material prepared using the method provided by the present invention can effectively reduce the interfacial polarization of composite material and remain
Remaining polarization increases anti-breakdown electric field, and then improves the energy storage density and efficiency of dielectric composite material simultaneously.
Detailed description of the invention
Fig. 1 is BaTiO3-SrTiO3Scanning electron microscope (SEM) figure of nucleocapsid filler；
Fig. 2 is BaTiO3-SrTiO3Transmission electron microscope (TEM) figure of nucleocapsid filler；
Fig. 3 is BaTiO3-SrTiO3High-resolution-ration transmission electric-lens (HRTEM) figure of nucleocapsid filler；
Fig. 4 is BaTiO3-SrTiO3X-ray photoelectron spectroscopic analysis (XPS) figure of nucleocapsid filler；
Fig. 5 is the P-E loop schematic diagram of experimental group 1 of the present invention and control group 1；
Fig. 6 is pair of the anti-breakdown electric field of experimental group 1~3 of the present invention and control group 2, discharge energy density and energy storage efficiency
Than figure.
Specific embodiment
The present invention comprehensively considers the structure and performance characteristics of strontium titanates, and transformation carried out surface cladding to ceramic packing in the past
Research Thinking make SrTiO by two one-step hydrothermals3Epitaxial growth is in BaTiO3Surface prepares BaTiO3-SrTiO3Nucleocapsid is filled out
Material, and the nucleocapsid filler and polymeric matrix progress is compound, obtain a kind of new dielectric composite material.In lower content nucleocapsid
In the case where filler, the dielectric composite material is obtained better than straight polymer matrix and individually with BaTiO3For the dielectric of filler
The energy storage density of composite material.
Preparation method is described in detail combined with specific embodiments below.
Embodiment one: preparation BaTiO3-SrTiO3Nucleocapsid filler
The BaTiO3-SrTiO3Nucleocapsid filler is prepared using two one-step hydrothermals.By the Ba (OH) of 2.1809g2·8H2O adds
Enter in 16mL 1M acetic acid solution, dissolution is sufficiently stirred, obtains solution 1.Then by the TiCl of 0.8mL4It is added to the anhydrous second of 16mL
In alcoholic solution, solution 2 is obtained.
The solution 1 and solution 2 are mixed, precursor solution is obtained.Then the forerunner is added in 5.0g sheet NaOH
In liquid solution, mechanical stirring 10min is obtained containing BaTiO3The intermediate liquid suspension of nano particle and unreacted gel.
By 0.0967g Sr (OH)2·8H2O is dissolved in 24mL 1M acetic acid solution, obtains solution 3.The Ba (OH)2·
8H2O、TiCl4With Sr (OH)2·8H2The used in amounts of O guarantees that the molar ratio of Ba (Sr) and Ti are 1:1.
The solution 3 is added in intermediate liquid suspension, is uniformly mixed, and mixed suspension is transferred to instead
It answers in kettle, 200 degree of hydro-thermal reactions are washed twice with dehydrated alcohol for 24 hours, by reaction product, and dry 2h is at 80 DEG C to get required
BaTiO3-SrTiO3Nucleocapsid filler.
To the BaTiO of preparation3-SrTiO3Nucleocapsid filler carries out Electronic Speculum and lens scan, as a result as shown in Figures 1 to 3；And it is right
BaTiO3-SrTiO3Nucleocapsid filler carries out X-ray photoelectron spectroscopic analysis, as a result as shown in Figure 4.
Embodiment two: dielectric composite material is prepared
1, using n,N-Dimethylformamide (DMF) as solvent, with commercially available Kynoar-hexafluoropropylene copolymer
(hereinafter referred P (VDF-HFP)) is used as polymer, according to 1vol%, 2vol% and 3vol% of P (VDF-HFP) volume, respectively
Weigh the BaTiO of three groups of embodiments one preparation3-SrTiO3Nucleocapsid filler, as experimental group 1,2,3；And it is separately added into DMF solvent
In, ultrasonic disperse 30min, and 2h is stirred, with fully dispersed uniform.
Again in each group solvent, it is separately added into the solid P (VDF-HFP) of required quality, 12h is stirred at 50 DEG C, ultrasound
1h obtains the BaTiO of favorable dispersibility3-SrTiO3Nucleocapsid filler/P (VDF-HFP) solution.
It should be understood that obtaining BaTiO according to the above method3-SrTiO3Nucleocapsid filler/P (VDF-HFP) solution, this field
Technical staff can select the method being further dried according to actual needs, obtain required dielectric composite material, traveling of going forward side by side
One step application, such as the preparation for capacitor etc..The present embodiment for convenience carry out follow-up data measurement and by the solution into
Row the tape casting molding, and it is non-limiting can only use this method be dried, form.The specific method is as follows for the tape casting:
By solution drop on clean glass plate, the applicator (SZQ) of fixed height, curtain coating preparation BaTiO are utilized3-
SrTiO3/ P (VDF-HFP) composite material, at 60 DEG C it is dry for 24 hours, 200 DEG C of hot pressing 20min are done after quenching in mixture of ice and water
It is dry to get required each group dielectric composite material.
Under the same conditions simultaneously, by BaTiO3-SrTiO3Nucleocapsid filler replaces with the BaTiO of polymer 1vol%3, system
It is standby to obtain control group 1；With pure P (VDF-HFP) polymer as a control group 2.
2, it is compound to the dielectric of experimental group 1,2,3 and control group 1,2 under the same conditions, to be utilized respectively magnetron sputtering apparatus
The two sides of material carries out gold electrode sputtering；Sputtering power is 120W, sputters 100s.
Carry out breakdown test to the dielectric composite material of each experimental group: the voltage is since 100V, with the speed of 10kV/mm
Degree is continuously increased, until sample is breakdown；Utilize the P-E loop (polarization-electric field curve) of ferroelectricity analyzer test sample.Knot
Fruit is as shown in Figure 5,6.
Fig. 5 is the P-E loop figure of the dielectric composite material of experimental group 1 and control group 1.From fig. 5, it can be seen that identical
In the case where filer content, the residual polarization of control group 1 is bigger than experimental group 1, illustrates SrTiO3The introducing of shell can effectively subtract
The remanent polarization of small dielectric composite material.Putting for composite material can be obtained by carrying out integral calculation to the P-E loop of test
Electrical power densities.It is calculated, the composite material of experimental group 1 obtains 13.89J/cm under its anti-breakdown electric field3Electric discharge energy
Metric density, and under the same terms, discharge energy density of the control group 1 under its anti-breakdown electric field is 9.96J/cm3.It can obtain
Out, using BaTiO3-SrTiO3Core-shell structure material as filler, can effectively reduce dielectric composite material interfacial polarization and
Residual polarization obtains highly resistance breakdown electric field, and then obtains high discharge energy density and efficiency.
Fig. 6 is anti-breakdown electric field, discharge energy density and the energy storage efficiency comparison diagram of control group 2 and experimental group 1,2,3.Figure
A 6 uppermost curves are the change curve of anti-breakdown electric field, it can be seen that under low core-shell structure filler content
(1vol%, 2vol%, 3vol%), the dielectric composite material of experimental group 1,2,3 can be obtained higher than (pure P (the VDF- of control group 2
HFP) polymer) anti-breakdown electric field.A curve among Fig. 6 is the change curve of discharge energy density, it can be seen that real
The discharge energy density for testing group 1,2,3 is above control group 2.The bottom curve of Fig. 6 is the change curve of energy storage efficiency, when
When the content of nucleocapsid filler is 1vol% (experimental group 1), energy storage efficiency and pure P (VDF-HFP) are close, while obtaining high
Discharge energy density.
Claims (6)
1. a kind of dielectric composite material, it is characterised in that: the dielectric composite material includes ceramic material and polymer, the pottery
Ceramic material is core-shell structure, and in the core-shell structure, the dielectric constant of shell structure is less than the dielectric constant of nuclear structure, the shell knot
The material of structure and the material of nuclear structure are perovskite structure.
2. dielectric composite material according to claim 1, it is characterised in that: in the core-shell structure, nuclear structural materials are
BaTiO3；Shell structure material is SrTiO3。
3. dielectric composite material according to claim 2, it is characterised in that: the preparation method of the core-shell structure includes such as
Lower step:
(1) by Ba (OH)2·8H2O is added in acetic acid solution, and dissolution is sufficiently stirred, obtains solution 1；
(2) by TiCl4It is added in ethanol solution, obtains solution 2；
(3) solution 1 and solution 2 are mixed, obtains precursor solution；
(4) solid NaOH is added in the precursor solution, mixes well, obtains intermediate liquid suspension；
(5) by Sr (OH)2·8H2O is dissolved in acetic acid solution, obtains solution 3；
(6) solution 3 is added in the intermediate liquid suspension, is mixed well, after hydro-thermal reaction, reaction product is washed,
Drying is to get required core-shell structure.
4. dielectric composite material according to claim 1, it is characterised in that: the volume of the core-shell structure is polymeric acceptor
Long-pending 1%~3%.
5. dielectric composite material according to claim 1, it is characterised in that: the preparation method packet of the dielectric composite material
Include following steps:
(1) core-shell material is added in organic solvent, ultrasonic disperse is simultaneously stirred well to uniformly；
(2) polymer is added in a solvent again, after fully dispersed, obtains dielectric composite material solution；
(3) the dielectric composite material solution curtain coating is formed, obtains the dielectric composite material.
6. the application of dielectric composite material described in Claims 1 to 5 any one in the capacitor.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113527826A (en) * | 2021-06-04 | 2021-10-22 | 宁波大学 | Composite film of flaky core-shell structure doped with polyvinylidene fluoride copolymer and preparation method thereof |
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