CN109878176A - A kind of polymer based multilayer composite material and preparation method of high energy storage density - Google Patents
A kind of polymer based multilayer composite material and preparation method of high energy storage density Download PDFInfo
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- CN109878176A CN109878176A CN201910145712.5A CN201910145712A CN109878176A CN 109878176 A CN109878176 A CN 109878176A CN 201910145712 A CN201910145712 A CN 201910145712A CN 109878176 A CN109878176 A CN 109878176A
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Abstract
A kind of polymer based multilayer composite material and preparation method of high energy storage density, composite material is made of dielectric layers and the dielectric layer being arranged between dielectric layers, insulating layer is made of aluminium nitride and polyvinylidene fluoride composite material, and dielectric layer is made of potassium niobate and polyvinylidene fluoride composite material.Preparation method includes: 1) aluminium nitride powder to be added in Kynoar solution to be uniformly mixed, then obtained mixed solution is uniformly coated on substrate, takes off after vacuum drying, obtains insulating layer composite material film A；2) potassium niobate powder is added in Kynoar solution and is uniformly mixed, then obtained mixed solution is uniformly coated on substrate, taken off after vacuum drying, obtain dielectric layer composite material film K；3) using insulating layer composite material film A as outer layer, dielectric layer composite material film K is that internal layer carries out hot pressing.Preparation method of the present invention is simple, composite material disruptive field intensity with higher.
Description
Technical field
The invention belongs to dielectric capacitor fields, are the polymer based multilayer composite material and its system of a kind of high energy storage density
Preparation Method.
Background technique
Polymer-based dielectric capacitor is existed due to the cycle life of its high power density, quick efficiency for charge-discharge, length
Have in hybrid vehicle, Medical Devices and high power pulse electronic weaponry system grade high performance power electronic product huge
Development potentiality.However, the low energy density of polymer-based dielectric capacitor limits it as high performance capacitors in practical life
Generate the extensive use in living.So how to improve its energy density, have become the heat of polymer-based dielectric capacitor research
Point and emphasis.
For at present, the common matrix of polymer-based dielectric material is Kynoar (PVDF), is a kind of with pressure
Electrically with the organic matter of pyroelectricity, disruptive field intensity is up to 350MV/m.In addition, Kynoar is easily worked, be suitble to big face at
Film, and pass through different preparation methods, thus it is possible to vary the performance of polyvinylidene difluoride film, such as mechanical strength and hydrophilic and hydrophobic
(Li Liang, black a kind of polyvinylidene fluoride film of bull of woods and preparation method thereof, China, CN104226124A [P] .2014.12.24.).
However, the low dielectric constant of Kynoar limits the raising of its energy density, and then it is limited in high-performance dielectric electricity
The application of field of containers.In order to solve this problem, the ceramic material of high dielectric constant is introduced in polyvinylidene fluoride as filler
In alkene, to improve the energy storage density of Kynoar.Potassium niobate (KNbO3) it is a kind of important ferroelectricity with perovskite structure
Material is (Tc=435 DEG C of Curie temperature of ferroelectric of orthorhombic phase at room temperature；Under 1kHz, dielectric constant ≈ 300), recognized
To be a kind of ferroelectric material for having development potentiality.The compound polymer-based dielectric material for preparing of potassium niobate and Kynoar is had
Good prospect, Hou Yudong of Beijing University of Technology et al. is compound with Kynoar by potassium niobate, has prepared dielectric constant
(Hou Yudong, Ge Haiyan, Zhu Mankang wait a kind of potassium niobate of/gather inclined fluorine to higher, the lower polymer matrix composite of dielectric loss
The preparation method of ethylene high-dielectric composite material: China, CN102875939A [P] .2013.01.16.).Theoretically, this one
The composite material of system can be combined together the high dielectric constant of ceramics and the high breakdown field strength of polymer, prepare high-performance
Dielectric capacitor.But in actual operation, the introducing of ceramic packing potassium niobate can be such that the disruptive field intensity of matrix declines, and work as filler
Volume fraction increase when, field strength decline the phenomenon that it is particularly evident.For dielectric capacitor, energy storage density can use formula
Ue=∫ E dD indicates, so, the reduction of electric field strength has detrimental effect to the energy storage of capacitor, therefore, how to improve
Potassium niobate/polyvinylidene fluoride composite material disruptive field intensity is to be badly in need of the problem to be solved.Generally, multi-layer composite materials
Two adjacent layers of material will form strong potential barrier interface due to the difference of physicochemical properties, this globality to composite material
There can be important influence.Therefore, it is proposed to which the method by introducing insulating layer, enhances the interface pole between two interface of adjacent layer
Change, so that the disruptive field intensity of composite material can be improved, and then improve its energy storage density and optimization discharging efficiency, promotes it into one
The application of step.
Summary of the invention
It is an object of the invention to be directed to above-mentioned the problems of the prior art, a kind of polymer matrix of high energy storage density is provided
Multilayer materials and preparation method thereof can be improved the disruptive field intensity of composite material, and easy to operate, and reliable performance has
Effect.
To achieve the goals above, polymer based multilayer composite material of the invention is existed by dielectric layers and setting
Dielectric layer composition between dielectric layers, the insulating layer are made of aluminium nitride and polyvinylidene fluoride composite material, institute
The dielectric layer stated is made of potassium niobate and polyvinylidene fluoride composite material, and insulating layer and dielectric layer are membrane structure, the two
It is hot-forming.
Volume ratio shared by the filler of the dielectric layers is 1%, volume ratio shared by the filler of dielectric layer is 1%~
15%.
The preparation method of the polymer based multilayer composite material of high energy storage density of the present invention, comprising the following steps:
1) aluminium nitride powder and Kynoar powder are weighed for 1:99 by volume, prepares the poly- inclined of clear first
Vinyl fluoride solution makes its volume ratio 3%, and then aluminium nitride powder is added in Kynoar solution and is uniformly mixed, finally
Obtained mixed solution is uniformly coated on substrate, is taken off after vacuum drying, it is thin to obtain insulating layer composite material
Film A；
2) by volume for 1:99~15:85 weigh potassium niobate powder and with Kynoar powder, prepare clarification first
Transparent Kynoar solution makes its volume ratio 3%, and then potassium niobate powder is added in Kynoar solution and mixes
Uniformly, finally obtained mixed solution is uniformly coated on substrate, is taken off after vacuum dried, it is compound obtains dielectric layer
Material film K；
3) using insulating layer composite material film A as outer layer, dielectric layer composite material film K is internal layer, hot-forming.
The particle size range of aluminium nitride powder is 0.48 μm~2.17 μm in the step 1).
The particle size range of potassium niobate powder is 0.14 μm~0.73 μm in the step 2).
Kynoar solution the preparation method comprises the following steps: polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, 60
10-12h is stirred at a temperature of DEG C, obtains the Kynoar solution that the volume ratio of clear is 3%.
Aluminium nitride powder and potassium niobate powder are mixed with Kynoar solution by the ultrasonic vibration of 90min
Uniformly.
The substrate uses glass plate, and obtained mixed solution is uniformly coated on substrate using the tape casting,
After being dried in vacuo 8-10h at a temperature of 60 DEG C, respectively by insulating layer composite material film A and dielectric layer composite material film K
It takes off.
Volume ratio shared by the filler of the outer layer is 1%, and volume ratio shared by the filler of internal layer is 1%~15%.
Insulating layer composite material film A is put into mold with dielectric layer composite material film K and carries out by the step 3)
Hot pressing, hot pressing temperature are 190-200 DEG C, pressure 0.2-1MPa, hot pressing time 10-15min.
Compared with prior art, the present invention is with following the utility model has the advantages that multiple by introducing aluminium nitride and Kynoar
Insulating layer made of condensation material improves the disruptive field intensity of potassium niobate and polyvinylidene fluoride composite material, this is because in multilayer
In structural composite material, the potassium niobate with high dielectric constant/Kynoar dielectric layer and the nitridation with high breakdown field strength
Aluminium/Kynoar insulating layer is overlapped mutually, and significantly provides the comprehensive advantage of collaboration for electric field strength.Due to being situated between
The difference of dielectric property between electric layer and insulating layer, the electric field applied on the composite are re-distributed, and alleviate dielectric layer
In electric field strength make the disruptive field intensity of composite material to prevent the complete breakdown of multilayer materials under high voltages
It is greatly improved.By using insulating layer composite material film as outer layer, using dielectric layer composite material film as internal layer,
Hot-forming multilayer materials disruptive field intensity with higher, preparation method of the invention is easy to operate, composite material
Reliable performance is effective.
Detailed description of the invention
The polymer based multilayer composite structure schematic diagram of Fig. 1 high energy storage density of the present invention；
The scanning electron microscope (SEM) photograph of internal layer when volume ratio shared by Fig. 2 internal layer filler is 5%；
The scanning electron microscope (SEM) photograph of outer layer when volume ratio shared by Fig. 3 internal layer filler is 5%；
The scanning electron microscope (SEM) photograph of cross section when volume ratio shared by Fig. 4 internal layer filler is 5%；
Fig. 5 (a) potassium niobate/polyvinylidene fluoride composite material ferroelectric hysteresis loop；
The ferroelectric hysteresis loop of Fig. 5 (b) 3-layer composite material；
Fig. 6 (a) potassium niobate/polyvinylidene fluoride composite material energy storage density datagram；
The energy storage density datagram of Fig. 6 (b) 3-layer composite material；
Fig. 7 (a) potassium niobate/polyvinylidene fluoride composite material energy efficiency datagram；
The energy efficiency datagram of Fig. 7 (b) 3-layer composite material.
Specific embodiment
Present invention will be described in further detail below with reference to the accompanying drawings.
The present invention measures the micro- shape of prepared polymer matrix composite using FEI-Q25 scanning electron microscope
Looks.Prepared polymer matrix composite electric hysteresis is determined using 609B (Radiant Technologies) ferroelectricity work station
Loop line, and energy storage density and energy releasing efficiency are calculated on this basis.The above performance parameter all measures at room temperature.
Embodiment 1
It 1) is 1:99 according to the volume ratio of aluminium nitride and Kynoar, weighing aluminium nitride powder, (average grain diameter is 1.14 μ
And Kynoar powder m).Polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, 12h is stirred at 60 DEG C, obtains
The Kynoar solution that the volume ratio of clear is 3%；Then aluminium nitride powder is added in Kynoar solution,
Ultrasonic vibration 90min；Obtained mixed solution is uniformly coated on a glass using the tape casting, is dried in vacuo at 60 DEG C
After 10h, is gently taken off with tweezers, composite material film A can be obtained.
It 2) is 1:99 according to the volume ratio of potassium niobate and Kynoar, weighing potassium niobate powder, (average grain diameter is
330nm) and Kynoar powder.Polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, stirs 12h at 60 DEG C,
Obtain the solution for the Kynoar clear that volume ratio is 3%；It is molten that potassium niobate powder is then added to Kynoar
In liquid, ultrasonic vibration 90min；Obtained mixed solution is uniformly coated on glass plate using the tape casting, it is true at 60 DEG C
It after the dry 10h of sky, is gently taken off with tweezers, the composite material film K that potassium niobate volume ratio is 1% can be obtained.
3) using aluminium nitride/polyvinylidene fluoride composite material A as outer layer, potassium niobate volume ratio be 1% potassium niobate/gather inclined fluorine
Ethylene composite material is internal layer, is put into mold, is 200 DEG C in temperature, pressure is hot pressing 10min under conditions of 1MPa, is obtained
Composite A KA with three-decker, is named as 1-1-1 for dielectric film.
Embodiment 2
It 1) is that 1:99 weighs aluminium nitride powder (average grain diameter is 1.14 μ according to the volume ratio of aluminium nitride and Kynoar
And Kynoar powder m).Polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, 12h is stirred at 60 DEG C, obtains
The Kynoar solution that the volume ratio of clear is 3%；Then aluminium nitride powder is added in Kynoar solution,
Ultrasonic vibration 90min；Obtained mixed solution is uniformly coated on a glass using the tape casting, is dried in vacuo at 60 DEG C
After 10h, is gently taken off with tweezers, composite material film A can be obtained.
It 2) is 5:95 according to the volume ratio of potassium niobate and Kynoar, weighing potassium niobate powder, (average grain diameter is
330nm) and Kynoar powder.Polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, stirs 12h at 60 DEG C,
Obtain the solution for the Kynoar clear that volume ratio is 3%；It is molten that potassium niobate powder is then added to Kynoar
In liquid, ultrasonic vibration 90min；Obtained mixed solution is uniformly coated on glass plate using the tape casting, it is true at 60 DEG C
It after the dry 10h of sky, is gently taken off with tweezers, the composite material film K that potassium niobate volume ratio is 5% can be obtained.
3) using aluminium nitride/polyvinylidene fluoride composite material A as outer layer, potassium niobate volume ratio be 5% potassium niobate/gather inclined fluorine
Ethylene composite material is internal layer, is put into mold, is 200 DEG C in temperature, pressure is hot pressing 10min under conditions of 1MPa, is obtained
Composite A KA with three-decker, is named as 1-5-1 for dielectric film.
Implementation column 3
It 1) is 1:99 according to the volume ratio of aluminium nitride and Kynoar, weighing aluminium nitride powder, (average grain diameter is 1.14 μ
And Kynoar powder m).Polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, 12h is stirred at 60 DEG C, obtains
The Kynoar solution that the volume ratio of clear is 3%；Then aluminium nitride powder is added in Kynoar solution,
Ultrasonic vibration 90min；Obtained mixed solution is uniformly coated on a glass using the tape casting, is dried in vacuo at 60 DEG C
After 10h, is gently taken off with tweezers, composite material film A can be obtained.
It 2) is 10:90 according to the volume ratio of potassium niobate and Kynoar, weighing potassium niobate powder, (average grain diameter is
330nm) and Kynoar powder.Polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, stirs 12h at 60 DEG C,
Obtain the solution for the Kynoar clear that volume ratio is 3%；It is molten that potassium niobate powder is then added to Kynoar
In liquid, ultrasonic vibration 90min；Obtained mixed solution is uniformly coated on glass plate using the tape casting, it is true at 60 DEG C
It after the dry 10h of sky, is gently taken off with tweezers, the composite material film K that potassium niobate volume ratio is 10% can be obtained.
3) using aluminium nitride/polyvinylidene fluoride composite material A as outer layer, potassium niobate that potassium niobate volume ratio is 10%/poly- inclined
Fluoride composite material is internal layer, is put into mold, is 200 DEG C in temperature, pressure is hot pressing 10min under conditions of 1MPa, is obtained
To the composite A KA with three-decker, dielectric film is named as 1-10-1.
Embodiment 4
It 1) is 1:99 according to the volume ratio of aluminium nitride and Kynoar, weighing aluminium nitride powder, (average grain diameter is 1.14 μ
And Kynoar powder m).Polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, 12h is stirred at 60 DEG C, obtains
The Kynoar solution that the volume ratio of clear is 3%；Then aluminium nitride powder is added in Kynoar solution,
Ultrasonic vibration 90min；Obtained mixed solution is uniformly coated on a glass using the tape casting, is dried in vacuo at 60 DEG C
After 10h, is gently taken off with tweezers, composite material film A can be obtained.
It 2) is 15:85 according to the volume ratio of potassium niobate and Kynoar, weighing potassium niobate powder, (average grain diameter is
330nm) and Kynoar powder.Polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, stirs 12h at 60 DEG C,
Obtain the solution for the Kynoar clear that volume ratio is 3%；It is molten that potassium niobate powder is then added to Kynoar
In liquid, ultrasonic vibration 90min；Obtained mixed solution is uniformly coated on glass plate using the tape casting, it is true at 60 DEG C
It after the dry 10h of sky, is gently taken off with tweezers, the composite material film K that potassium niobate volume ratio is 15% can be obtained.
3) using aluminium nitride/polyvinylidene fluoride composite material A as outer layer, potassium niobate that potassium niobate volume ratio is 15%/poly- inclined
Fluoride composite material is internal layer, is put into mold, is 200 DEG C in temperature, pressure is hot pressing 10min under conditions of 1MPa, is obtained
To the composite A KA with three-decker, dielectric film is named as 1-15-1.
In view of embodiments above, in conjunction with attached drawing, now by potassium niobate/polyvinylidene fluoride composite material of single layer and three layers
The composite material of structure carries out structural characterization and electric performance test, and result compare it is as follows:
1) referring to figure 2-3, the internal layer of dielectric film 1-5-1 and superficies are smooth, in outer layer, a small amount of aluminium nitride without
It is regularly distributed in Kynoar；Internal layer potassium niobate ceramic packing slightly reunite, but on the whole it is evenly dispersed in the base；From
It can be seen that 3-layer composite material is tightly combined in Fig. 4, the significant deficiency that can not cause energy-storage property to decline, such as stomata,
Crackle.
2) referring to Fig. 5 (a), the disruptive field intensity of potassium niobate polyvinylidene fluoride composite material is in 280MV/m hereinafter, and with filling out
Material increases, and disruptive field intensity decreased significantly.Compared with Fig. 5 (a), three-decker polymer matrix composite in Fig. 5 (b)
Disruptive field intensity increases, maximum up to 400MV/m, this explanation, compared with single layer potassium niobate/Kynoar, with aluminium nitride/poly- inclined
Fluoride composite material is that the electric property of the composite material of the three-decker of insulating layer obtains the great improvement of band.
3) from Fig. 6 (a), it can be seen that potassium niobate/polyvinylidene fluoride composite material energy storage density of single layer is very low,
About 3J/cm3, for this numerical value far from the needs for meeting high-performance dielectric capacitor, this phenomenon is its low disruptive field intensity
Caused by.
Compared with Fig. 6 (a), potassium niobate/Kynoar composite wood relative to single layer can be seen that from Fig. 6 (b)
Material, using aluminium nitride/Kynoar as the 3-layer composite material of insulating layer, energy storage density is greatly improved, and is about 18J/
cm3, nearly 600% is improved, energy storage density can be improved in this explanation, the present invention really.
4) from Fig. 7 (a), it can be seen that the potassium niobate of single layer/polyvinylidene fluoride composite material inefficiency, and with
The increase of field strength and decline, stability is bad.It can be seen that potassium niobate/Kynoar relative to single layer from Fig. 7 (b)
Composite material, using aluminium nitride/Kynoar as the polymer matrix composite of the three-decker of insulating layer, efficiency has obviously
Improve, under the field strength of 400MV/m, is still able to maintain 65% discharging efficiency.
Claims (10)
1. a kind of polymer based multilayer composite material of high energy storage density, it is characterised in that: existed by dielectric layers and setting
Dielectric layer composition between dielectric layers, the insulating layer are made of aluminium nitride and polyvinylidene fluoride composite material, institute
The dielectric layer stated is made of potassium niobate and polyvinylidene fluoride composite material, and insulating layer and dielectric layer are membrane structure, the two
It is hot-forming.
2. according to the polymer based multilayer composite material of high energy storage density described in right 1, it is characterised in that: the dielectric layers
Filler shared by volume ratio be 1%, volume ratio shared by the filler of dielectric layer is 1%~15%.
3. a kind of preparation method of the polymer based multilayer composite material of high energy storage density, which comprises the following steps:
1) aluminium nitride powder and Kynoar powder are weighed for 1:99 by volume, prepares the polyvinylidene fluoride of clear first
Alkene solution makes its volume ratio 3%, and then aluminium nitride powder is added in Kynoar solution and is uniformly mixed, finally incites somebody to action
To mixed solution be uniformly coated on substrate, by vacuum drying after take off, obtain insulating layer composite material film A；
2) by volume for 1:99~15:85 weigh potassium niobate powder and with Kynoar powder, prepare clear first
Kynoar solution, make its volume ratio 3%, then will potassium niobate powder that mixing in Kynoar solution is added is equal
It is even, finally obtained mixed solution is uniformly coated on substrate, is taken off after vacuum dried, obtains dielectric layer composite wood
Expect film K；
3) using insulating layer composite material film A as outer layer, dielectric layer composite material film K is internal layer, hot-forming.
4. the preparation method of the polymer based multilayer composite material of high energy storage density according to claim 2, it is characterised in that:
The particle size range of aluminium nitride powder is 0.48 μm~2.17 μm in the step 1).
5. the preparation method of the polymer based multilayer composite material of high energy storage density according to claim 2, it is characterised in that:
The particle size range of potassium niobate powder is 0.14 μm~0.73 μm in the step 2).
6. the preparation method of the polymer based multilayer composite material of high energy storage density according to claim 2, which is characterized in that
Kynoar solution the preparation method comprises the following steps: polytetrafluoroethylene (PTFE) is added in n,N-Dimethylformamide, in 60 DEG C of temperature
Lower stirring 10-12h obtains the Kynoar solution that the volume ratio of clear is 3%.
7. the preparation method of the polymer based multilayer composite material of high energy storage density according to claim 2, it is characterised in that:
Aluminium nitride powder and potassium niobate powder are uniformly mixed with Kynoar solution by the ultrasonic vibration of 90min.
8. the preparation method of the polymer based multilayer composite material of high energy storage density according to claim 2, it is characterised in that:
The substrate uses glass plate, obtained mixed solution is uniformly coated on substrate using the tape casting, in 60 DEG C of temperature
After the lower vacuum drying 8-10h of degree, insulating layer composite material film A and dielectric layer composite material film K are taken off respectively.
9. the preparation method of the polymer based multilayer composite material of high energy storage density according to claim 2, it is characterised in that:
Volume ratio shared by the filler of outer layer is 1%, and volume ratio shared by the filler of internal layer is 1%~15%.
10. the preparation method of the polymer based multilayer composite material of high energy storage density, feature exist according to claim 2
In: insulating layer composite material film A and dielectric layer composite material film K are put into mold and carry out hot pressing by the step 3),
Hot pressing temperature is 190-200 DEG C, pressure 0.2-1MPa, hot pressing time 10-15min.
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| CN110556247A (en) * | 2019-09-11 | 2019-12-10 | 邯郸学院 | preparation method of sandwich-structure high-energy-storage low-conductivity polymer-based composite film |
| CN114347522A (en) * | 2022-01-27 | 2022-04-15 | 西安交通大学 | Sandwich polypropylene composite dielectric with high energy storage density and preparation method thereof |
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| CN107359051A (en) * | 2017-06-30 | 2017-11-17 | 同济大学 | A kind of high-energy-density sandwich structure flexible composite and preparation method thereof |
| CN108300153A (en) * | 2017-10-13 | 2018-07-20 | 深圳市峰泳科技有限公司 | High energy storage density dielectric substance and preparation method thereof |
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| CN102875939A (en) * | 2012-10-22 | 2013-01-16 | 北京工业大学 | Preparation method of potassium niobate/ polyvinylidene fluoride high-dielectric composite material |
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| CN114347522A (en) * | 2022-01-27 | 2022-04-15 | 西安交通大学 | Sandwich polypropylene composite dielectric with high energy storage density and preparation method thereof |
| CN114347522B (en) * | 2022-01-27 | 2023-01-03 | 西安交通大学 | Sandwich polypropylene composite dielectric with high energy storage density and preparation method thereof |
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