CN105860376B - A kind of dielectric composite material based on BNT monocrystal nanowires and preparation method thereof - Google Patents
A kind of dielectric composite material based on BNT monocrystal nanowires and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of dielectric composite material based on BNT monocrystal nanowires and preparation method thereof, the BNT nanometer monocrystalline wire materials that draw ratio is 20 50 are prepared by hydro-thermal method, it is combined again with vinylidene hexafluoropropylene copolymer after it is chemically modified with dopamine, obtains dielectric composite material.The dielectric composite material is realized under conditions of low ceramic phase content, obtains the anti-breakdown electric field for being up to 458kV/mm, higher than straight polymer P (VDF HFP) anti-breakdown electric field 398kV/mm, realizes 12.7J/cm3High-energy-density.
Description
Technical field
The present invention relates to a kind of dielectric composite material based on BNT monocrystal nanowires and preparation method thereof.
Background technology
Energy storage technology is widely applied to electronics industry, and wherein capacitor is due to its high-energy-density and efficiently
Charge/discharge rates and be widely used.In order to realize higher energy density, exploitation is with high-k, high dielectric strength
Dielectric material is most important.
Ceramic/polymer nano composite material is usually that (0 dimension structure nano ceramic powder is dispersed in the poly- of 3-dimensional connection to 0-3 types
In compound matrix).Theoretical according to percolation threshold, 0-3 type ceramic/polymer composites usually require compound more than 50vol%
Ceramic particle can just make its compound dielectric constant reach threshold value, but on the one hand the ceramic filler amount of high content destroys material
Pliability, on the other hand because inevitable defect and reunion substantially reduce the ability and machinery of the anti-breakdown electric field of compound
Performance.And 0 dimension structure nano ceramic powders be uniformly dispersed in polymer body, it is impossible to form continuous seepage flow radiating road
Footpath, limits the heat conductivility of compound.
The content of the invention
There is high-k, high anti-breakdown electric field, high-energy-density and good it is an object of the invention to provide one kind
The preparation method of the dielectric composite material based on BNT monocrystal nanowires of thermal conductivity, the present invention can be in low BNT nano wires content bar
Under part, the dielectric composite material with high-energy-density is obtained.
Another object of the present invention is to provide it is a kind of have high-k, high anti-breakdown electric field, high-energy-density and
The dielectric composite material based on BNT monocrystal nanowires of thermal conductive resin.
The technical scheme is that：
A kind of preparation method of the dielectric composite material based on BNT monocrystal nanowires, major diameter is prepared by hydro-thermal method
Than the BNT nanometer monocrystalline wire materials for 20-50, after it is chemically modified with dopamine again with biasfluoroethylene-hexafluoropropylene
Copolymer p (VDF-HFP) is combined, and obtains dielectric composite material.
The present invention includes following preferred technical scheme：
It is preferred that scheme in, a diameter of 80-100nm of the BNT monocrystal nanowires.
It is preferred that scheme in, the average lengths of the BNT monocrystal nanowires is 2-5 μm.
It is preferred that scheme in, the amine-modified BNT monocrystal nanowires of DOPA are relative to vinylidene fluoride-hexafluoropropylene copolymer
Volume fraction is 2%-13%.
It is preferred that scheme in, the amine-modified BNT monocrystal nanowires of DOPA are relative to vinylidene hexafluoropropylene copolymer
Volume fraction is 2%-5%.
It is preferred that scheme in, the thickness of the dielectric composite material is 10-20 μm.
It is preferred that scheme in, the preparation process of the BNT monocrystal nanowires is：By Bi (NO3)3·5H2O, NaNO3And Ti
(OC4H9)4CH is dissolved in respectively3COOH, deionized water and CH3CH2In OH, mixing adds 8-10mol/L NaOH solution above-mentioned
Mixed solution, stirring, obtain precursor solution, by precursor solution be put into polytetrafluoroethylene (PTFE) be liner stainless steel cauldron
In, sealing, keeping temperature is 150-180 DEG C, is reacted, and is cooled down, and is filtered, and cleaning is dried to obtain BNT monocrystal nanowires.
It is preferred that scheme in, the process of the amine-modified BNT monocrystal nanowires of DOPA is：By BNT nano wire ultrasonic disperses
In alcohol and the mixed solution of deionized water, reaction is centrifuged after reaction, and then vacuum drying adds dopamine hydrochloric acid
In saline solution, in 50-70 DEG C of stirring, centrifuge again, in 50-70 DEG C of vacuum drying, obtain the amine-modified BNT of DOPA mono-
Brilliant nano wire.
It is preferred that scheme in, the recombination process is：By the amine-modified NBT monocrystal nanowires of DOPA add vinylidene-
In hexafluoropropylene copolymer solution, after ultrasonic disperse, ball milling further disperses, and suspension flow casting molding is done at 70-90 DEG C
It is dry, composite sheets are obtained, then hot pressing obtains the dielectric composite material of densification under 180-200 DEG C, 15-20MPa.
It is preferred that scheme in, the concentration of the dopamine hydrochloride aqueous solution is 0.01-0.015mol/L.
The invention further relates to the dielectric composite material prepared by above-mentioned preparation method.
Wherein, vinylidene fluoride-hexafluoropropylene copolymer solution refers to that vinylidene fluoride-hexafluoropropylene copolymer is dissolved in acetone
With the mixed solution obtained in dimethylformamide (DMF).
Wherein, the volume ratio of acetone and dimethylformamide is most preferably 70:30.
The BNT is Bi0.5Na0.5TiO3。
For the effect for obtaining comprehensive high-k, high anti-breakdown electric field, high-energy-density and thermal conductive resin,
The most preferably amine-modified BNT monocrystal nanowires of DOPA are relative to the volume fraction of vinylidene hexafluoropropylene copolymer
2.37vol%.
Beneficial effects of the present invention
The present invention utilizes hydro-thermal reaction, obtains a diameter of 80-100nm, and average length is 2-5 μm of high length-diameter ratio (20-
50) BNT monocrystal nanowires, it is compound with P (VDF-HFP), and the dielectric composite material prepared can be in low ceramic phase
High dielectric constant and high anti-breakdown electric field are realized under conditions of content, high energy density is obtained.
The present invention obtains that defect in dielectric composite material is few, with excellent mechanical performance.
The monocrystal nanowire of the present invention can be formed in polymeric matrix to be dislocatedly distributed, so as to be easy in different direction shapes
Into Heat transmission approach, the good dielectric composite material of thermal conductivity is prepared.
In the present invention, BNT monocrystal nanowires/P (VDF-HFP) dielectric composite materials are in low ceramic phase content (2.73vol%
BNT monocrystal nanowires) under conditions of, obtain 458kV/mm anti-breakdown electric field, than pure P (VDF-HFP) polymer resist wear
Electric field is higher.
Energy density is up to 12.7J/cm3, it is three times higher more than pure P (VDF-HFP).
The dielectric composite material is realized in low ceramic phase content (particularly BNT nano wires content is 2.37vol%)
Under the conditions of, 458kV/mm anti-breakdown electric field is obtained, breakdown electric field 398kV/mm more anti-than straight polymer P (VDF-HFP) is higher, it is real
12.7J/cm is showed3High-energy-density.
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of BNT monocrystal nanowires prepared by embodiment 1.It can be seen that synthesized BNT nano wires
With very high draw ratio.
Fig. 2 is combined for the amine-modified BNT monocrystal nanowires of DOPA of different content with the compound obtained dielectrics of P (VDF-HFP)
The scanning electron microscope (SEM) photograph of material surface.(a) 2.37vol%, (b) 5.19vol%, (c) 12.73vol%.As can be seen that with BNT
The increase of monocrystal nanowire addition, the visible BNT monocrystal nanowires in its surface are also more and more, and they are uniformly embedded in poly-
In compound matrix, obvious reunite and other defects is not found.
Fig. 3 is combined for the amine-modified BNT monocrystal nanowires of DOPA of different content with the compound obtained dielectrics of P (VDF-HFP)
The anti-breakdown electric field of material.As can be seen that content obtains the anti-breakdown electric field 458kV/mm of highest when being 2.37vol%.
Fig. 4 is combined for the amine-modified BNT monocrystal nanowires of DOPA of different content with the compound obtained dielectrics of P (VDF-HFP)
The dielectric constant frequency spectrum of material.It can be seen that the dielectric constant of compound increases with the increase of BNT nano wire contents.
Fig. 5 is combined for the amine-modified BNT monocrystal nanowires of DOPA of different content with the compound obtained dielectrics of P (VDF-HFP)
The ferroelectric hysteresis loop under 300kV/mm electric fields of material.
Fig. 6 is energy density of the composite sample under not same electric field.It can be seen that when content is 2.37vol%, being combined
The energy density of thing is rapidly increased to 12.7J/cm3。
Specific embodiment
Embodiment 1
Hydrothermal Synthesiss BNT monocrystal nanowires
0.005mol Bi(NO3)3·5H2O and 0.01mol NaNO3It is dissolved separately in 7.5ml CH3COOH and 2.5ml are gone
In ionized water, 0.005mol Ti (OC4H9)4It is dissolved in 10ml CH3CH2In OH, by Bi (NO3)3·5H2O solution and NaNO3It is molten
Liquid adds Ti (OC4H9)4Mixed solution is made in solution.10mol/L 30ml NaOH solutions are added to above-mentioned mixed solution,
Magnetic agitation 1h obtains uniform precursor solution under normal temperature.It is liner that precursor solution is put into 100ml polytetrafluoroethylene (PTFE)
In stainless steel cauldron, sealing is put into incubator and 48h is incubated at 170 DEG C and is promoted using the pressure spontaneously formed in reactor
Reaction occurs.After soaking time terminates, room temperature is naturally cooled to.By obtained product deionized water suction filtration, cleaning, place into
BNT monocrystal nanowires are dried to obtain in 80 DEG C of drying box.
Embodiment 2
The preparation of the amine-modified BNT monocrystal nanowires of DOPA and P (VDF-HFP) dielectric composite material
The BNT nano wires for weighing 2.0g preparations are distributed to 95:In 5 (v/v) ethanol/water mixed solutions, at stirring and ultrasound
Reason, is collected by centrifugation sediment, and vacuum drying obtains the increased BNT monocrystal nanowires of the adsorbed hydroxyl content.Hydroxylated BNT is mono-
Brilliant nano wire is distributed in the 0.01mol/L dopamine hydrochloride aqueous solution, 60 DEG C of back flow reaction 10h, be cooled to after room temperature from
The heart, and deionized water thoroughly cleaning is used, collect powder 60 DEG C of dry 24h in vacuum drying chamber.
The dopamine that 2.37vol%, 5.19vol% and 12.73vol% are added into P (VDF-HFP) polymer solution is repaiied
After the BNT monocrystal nanowires adornd, ultrasonic disperse, ball milling further disperses for 2 days, scattered BNT/P (VDF-HFP) suspension
The flow casting molding on clean sheet glass, 24h is dried at 80 DEG C, composite sheets are obtained, then at 200 DEG C, 15MPa pressure strips
It is 10-20 μm, fine and close dielectric composite material that thickness is hot pressed under part.
Embodiment 3：
The electric performance test of dielectric composite material
The a diameter of 2mm of circular port is designed, hole center of circle spacing is 4mm metal mask plate, and metal mask plate is shaped as just
Square, the length of side is 30mm.The dielectric composite material suppressed is clipped in the middle of 2 metal mask plates, upper and lower surface is symmetrically sputtered
Gold electrode, upper and lower surface sputtering time is 10min, it is ensured that gold electrode has enough thickness.Tested using electric impedance analyzer
Its electric capacity draws dielectric constant, as a result as shown in Figure 4, it can be seen that the dielectric constant of compound is with BNT nano wire contents
Increase and increase, such as in 1kHz, when BNT nano wires content is respectively 0 in compound, 2.37,5.19 and 12.73vol%
When, its dielectric constant is respectively 6.9,13.1,16.9 and 21.7.Its ferroelectric hysteresis loop is tested using ferroelectricity analyzer.Detection
As a result it is as shown in Figure 5.Because BNT itself leakage currents are larger, thus in the compound BNT nano wires content to 12.73vol%
When, its ferroelectric hysteresis loop is substantially more fat than low content BNT nano wire dielectric composite materials, and remanent polarization substantially becomes big,
The energy of storage can not be discharged due to its major part is lost by loss.Therefore the amine-modified BNT monocrystal nanowires of DOPA and P
(VDF-HFP) maximum energy-density of dielectric composite material is shown and the general different feature of ceramic nano line, its energy
Metric density is higher in low content BNT nano wires, and when content increase, its energy density is reduced on the contrary.The amine-modified BNT of DOPA receives
When the content of rice noodles is 2.37vol%, the energy density 12.7J/cm of maximum is obtained3。
Claims (10)
1. a kind of preparation method of the dielectric composite material based on BNT monocrystal nanowires, it is characterised in that prepared by hydro-thermal method
Obtain draw ratio be 20-50 BNT nanometer monocrystalline wire materials, after it is chemically modified with dopamine again with vinylidene-
Hexafluoropropylene copolymer is combined, and obtains dielectric composite material.
2. preparation method according to claim 1, it is characterised in that a diameter of 80- of the BNT monocrystal nanowires
100nm。
3. preparation method according to claim 1, it is characterised in that the average length of the BNT monocrystal nanowires is 2-5
μm。
4. the preparation method according to claim any one of 1-3, it is characterised in that the amine-modified BNT nanometer monocrystallines of DOPA
Line is 2%-13% relative to the volume fraction of vinylidene fluoride-hexafluoropropylene copolymer.
5. the preparation method according to claim any one of 1-3, it is characterised in that the amine-modified BNT nanometer monocrystallines of DOPA
Line is 2%-5% relative to the volume fraction of vinylidene fluoride-hexafluoropropylene copolymer.
6. the preparation method according to claim any one of 1-3, it is characterised in that the thickness of the dielectric composite material is
10-20μm。
7. preparation method according to claim 1, it is characterised in that the preparation process of the BNT monocrystal nanowires is：Will
Bi(NO3)3·5H2O, NaNO3With Ti (OC4H9)4CH is dissolved in respectively3COOH, deionized water and CH3CH2In OH, mixing, by 8-
10mol/L NaOH solution adds above-mentioned mixed solution, and stirring obtains precursor solution, precursor solution is put into poly- four
PVF is in the stainless steel cauldron of liner, sealing, keeping temperature is 150-180 DEG C, is reacted, and is cooled down, and is filtered, and is cleaned, and is done
It is dry to obtain BNT monocrystal nanowires.
8. the preparation method according to claim 1 or 7, it is characterised in that the amine-modified BNT monocrystal nanowires of DOPA
Process is：By BNT monocrystal nanowires ultrasonic disperse in alcohol and the mixed solution of deionized water, reaction, centrifugation point after reaction
From then vacuum drying is added in the dopamine hydrochloride aqueous solution, in 50-70 DEG C of stirring, is centrifuged again, at 50-70 DEG C
Vacuum drying, obtains the amine-modified BNT monocrystal nanowires of DOPA.
9. preparation method according to claim 1, it is characterised in that the recombination process is：By the amine-modified BNT of DOPA
Monocrystal nanowire is added in vinylidene fluoride-hexafluoropropylene copolymer solution, and after ultrasonic disperse, ball milling further disperses, and will suspend
Liquid flow casting molding, in 70-90 DEG C of drying, obtains composite sheets, then hot pressing obtains densification under 180-200 DEG C, 15-20MPa
Dielectric composite material.
10. the dielectric composite material that the preparation method described in claim any one of 1-9 is prepared.
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