CN109400924A - The preparation method of the nano combined dielectric material of New Two Dimensional based on high energy storage efficiency - Google Patents
The preparation method of the nano combined dielectric material of New Two Dimensional based on high energy storage efficiency Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of nano combined dielectric material of the New Two Dimensional based on high energy storage efficiency.Common capacitor material has two class of polymer material and ferroelectric ceramic material, there is respective problem.The method of the present invention uses hydrothermal co-precipitation method to synthesize Zn first(1‑x)MxO@MoS2Nanometer powder, wherein Zn(1‑x)MxO nano particle is two-dimensional nano compounded mix, is handled ZnO nano particle, and the composite construction of other metallic particles Co, Ni or Fe formation is adulterated.Polymer is dissolved completely in polar solvent, polymer solution is formed.Then by Zn(1‑x)MxO@MoS2Nanometer powder is added in polymer solution, and stirring forms mixed liquor.Repeatedly by mixed liquor ultrasound, stirring reprocessing, suspension is formed, suspension is prepared into film, finally will obtain composite film material after film thermal insulating, quenching treatment.The laminated film of the method for the present invention preparation has the characteristics that good toughness, thickness are thin, dielectric constant is high, energy storage density is high, loss is small, and preparation method is simple, is easy to produce in enormous quantities.
Description
Technical field
The invention belongs to functional material preparation technical fields, and it is multiple to be related to a kind of New Two Dimensional nanometer based on high energy storage efficiency
Close the preparation method of dielectric material, specifically a kind of single layer MoS2Nanometer sheet removes the ZnO nano of other metallic particles of package doping
The preparation method of particle and polymer matrix composite high-performance dielectric foil material.
Background technique
With the development of information technology, in almost all of electronic equipment and microelectronic field, dielectric is all to Guan Chong
It wants, such as semiconductor field effect transistor, dynamic RAM and the ruler with capacitor material in printed wiring board
Very little size is reduced rapidly, and studies frivolous novel high dielectric medium material as current information functional material and microelectronic field
Advanced subject.Size is small but function still element can make device miniaturization, reduce cost, improve the electricity of electronic product
Gas performance.The effects of in this class component, capacitor is received extensive attention, it can play decoupling, bypass, filtering.Capacitor
Equipment material requires high dielectric constant, high polarization value, low dielectric loss and high electric-field intensity.Common capacitor material has polymerization
Two class of object material and ferroelectric ceramic material, polymer possess higher Young's modulus and high dielectric field strength, the breakdown field of polymer
By force close to 400MV/m, but dielectric constant is lower, influences energy storage density, such as common polymer composites polypropylene (PP)
Dielectric constant between 2~3, the dielectric constant of fluoropolymer PVDF is between 8~10.If improving Jie of polymer
Electric constant, one way in which are that inorganic particulate is added into polymer, such as graphene, molybdenum disulfide, zinc oxide, but such as
Inorganic particulate is only added in fruit, and the breakdown strength of polymer will be greatly reduced, therefore how weigh advantage between the two, preparation
It has provided high electric-field intensity and high potential moves, low residual polarization, low-loss high-dielectric composite material are very significant.In order to mention
The breakdown strength of polymer after height addition inorganic particulate, can be modified conducting particles.By modified inorganic particulate
It is compound as being carried out in filler addition polymer, this new structure design of polymer/novel composite nano filler is developed, is obtained
There must be the nanometer powder of high dielectric constant, and can be uniformly dispersed in inorganic particulate and form compound system in polymeric matrix.
Summary of the invention
The purpose of the invention is to overcome weak link present on the prior art, one provided is based on high energy storage efficiency
The nano combined dielectric material of New Two Dimensional preparation method.
Specific method of the present invention are as follows:
Step 1. synthesizes Zn using hydrothermal co-precipitation method(1-x)MxO@MoS2Nanometer powder, specific method are:
(1) polyetherimide (PEI) is added L and risen in deionized water and sufficiently dissolved, Zn is then added(1-x)MxO nanometers
, 1~4g polyetherimide, 0.5~2g Zn are added in every liter of deionized water(1-x)MxO nano particle；Add L/30~L/
20 liters of deionized water, ultrasound are simultaneously stirred to nano powder dispersion in deionized water, obtain polyetherimide and Zn(1-x)MxO
Mixed liquor, mixed liquor keep 0.5~1h, formed Zn(1-x)MxO-PEI mixed form solution；The Zn(1-x)MxO nanometers
Grain is two-dimensional nano compounded mix, is handled ZnO nano particle, and the composite construction of other metallic particles M formation is adulterated,
Other metallic particles are Co, Ni or Fe, x=0.1~0.8.
(2) by MoS2It is dissolved in deionized water, mixing liquid ultrasound simultaneously stirs 2~10 times, obtains MoS2Mixed liquor；Every liter
The MoS of 0.5~5g is added in deionized water2。
(3) MoS for rising L/30~L/202Mixed liquor pours into Zn(1-x)MxIn O-PEI mixed form solution, ultrasonic treatment
0.5~1h forms MoS2-PEI-Zn(1-x)MxO structure-solution.
(4) to MoS2-PEI-Zn(1-x)MxO structure-solution is centrifuged, and gained mixture passes through deionized water and second
Alcohol cleans 2~10 times and drying, obtains the Zn of core-shell structure(1-x)MxO@MoS2Nanometer powder.
Obtained Zn(1-x)MxO@MoS2Between 1~100nm, size is sufficiently small to fill out the partial size R of nanometer powder convenient for increasing
Contact area between material and polymer, is easy to scatter in the polymer, and then promotes the dielectric properties of film.
Step 2. adds a polymer in the polar solvent equipped with magnetic stirring apparatus, is sufficiently stirred, until be completely dissolved,
Form the polymer solution of clear；The polymer of 1~100g is added in every liter of polar solvent；
The polymer is Kynoar PVDF or P (VDF-CTFE), P (VDF-TrFE), P based on PVDF
(VDF-CTFE-TrFE), one of P (VDF-HFP)；
The polar solvent is the analysis pure solvent of DMF, NMP or DMAC.
Step 3. is by Zn(1-x)MxO@MoS2Nanometer powder is added in polymer solution, is put into magnetic stirring apparatus, stirring is extremely
Occur without precipitating, forms mixed liquor；The Zn of 0.1~10g is added in every liter of polymer solution(1-x)MxO@MoS2Nanometer powder.
Mixed liquor is put into ultrasonic machine 0.5~1h of ultrasound by step 4., and 0.5~1h is stirred for after taking-up, and so repeatedly 2~10
Secondary, last time is added dibenzoyl peroxide (BPO) before stirring and is used as crosslinking agent, forms suspension, and every liter of mixed liquor is added
The crosslinking agent of 0.5~2g.
Uniform suspension is coated on slide by step 5., or is cast out using casting machine and is answered with a thickness of 5~50 μm
Condensation material film heats 1~2h at 70~100 DEG C, makes solvent evaporating completely, obtain film.
Film is kept the temperature 0.5~3h by step 6. at 180~220 DEG C, is immediately put into -196~0 DEG C of low temperature environment
3~10min of middle quenching treatment, obtains composite film material.
The present invention handles ZnO nano particle, adulterates other metallic particles Zn(1-x)MxO forms composite construction, then uses
Single layer MoS2Flake nano powder is to Zn(1-x)MxO carries out being wrapped to form Zn(1-x)MxO@MoS2Nanometer core-shell structure, other metallic particles
For Co, Ni or Fe.It both overcomes in this way and only adds MoS2Cause film breakdown intensity to weaken significantly, while film material can be made again
The dielectric loss of material obtain certain reduction with this come make its energy storage efficiency improve.In addition common Kynoar PVDF is used
Deng being used as substrate, crosslinking agent is added and improves compatibility between filler and polymer, prepares with higher breakdown strength, higher
The composite film material of energy storage density and energy storage efficiency.
The present invention is by Zn(1-x)MxO nano particle and MoS2Nanometer sheet progress is compound, has prepared Zn(1-x)MxO@MoS2Shell core
The nanometer powder of structure uses this kind of nanometer powder as filler, compared to MoS2, not only it is improved breakdown strength, but also drop
Low dielectric loss, to improve the energy storage efficiency of thin-film material.
The present invention, can by the way of multiple circulation stirring and sonic oscillation during preparing composite material suspension
To further decrease the reunion of filler in the polymer, the dispersibility of filler is sufficiently improved, the quality of form film greatly improves.
Zn prepared by the present invention(1-x)MxO@MoS2Nanometer powder, generally between 1~100nm, size is small enough in increasing partial size
The filled contact area between polymer is easy to scatter in the polymer, and then promotes the dielectric properties of film.Above-mentioned
Under advantage synergistic effect, the performance of film obtains good effect.Laminated film prepared by the present invention has good toughness, thickness
Feature thin, dielectric constant is high, energy storage density is high, loss is small, preparation method is simple, is easy to produce in enormous quantities.
Detailed description of the invention
Fig. 1 is nanoscale Zn0.8Co0.2O@MoS2X-ray diffractogram (XRD)；
Fig. 2 (a) is nanoscale Zn0.8Co0.2O@MoS2The TEM of shell nuclear material schemes；
Fig. 2 (b) is nanoscale Zn0.8Co0.2O@MoS2The high-resolution TEM of shell nuclear material schemes；
Fig. 3 is Zn0.8Co0.2O nano particle and Zn0.8Co0.2O@MoS2The comparison Raman figure of core-shell structure；
Fig. 4 (a) is to utilize Zn0.8Co0.2The dielectric constant figure of the composite film material of O nano particle production；
Fig. 4 (b) is to utilize Zn0.8Co0.2The dielectric loss figure of the composite film material of O nano particle production；
Fig. 4 (c) is to utilize Zn0.8Co0.2The density that releases energy of the composite film material of O nano particle production, loss energy
Metric density and efficiency chart.
Specific embodiment
The preparation method of the nano combined dielectric material of New Two Dimensional based on high energy storage efficiency, this method first step are adopted first
Zn is synthesized with hydrothermal co-precipitation method(1-x)MxO@MoS2Nanometer powder.
Embodiment 1.
40g polyetherimide (PEI) is added in 10 liters of deionized waters first and is sufficiently dissolved, 10g is then added
Zn0.9Co0.1O nano particle adds the deionized water of 500ml, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water,
Obtain polyetherimide and Zn0.9Co0.1The mixed liquor of O is kept for 0.5 hour, forms Zn0.9Co0.1O-PEI mixed form solution；
By 2g MoS2It is dissolved in and being added in 500ml deionized water, mixing liquid ultrasound simultaneously stirs 2 times, obtains MoS2Mixed liquor.
Zn0.9Co0.1O nano particle is two-dimensional nano compounded mix, is handled ZnO nano particle, doping metals Co granulated
At.
Then the MoS of 500ml is taken2Mixed liquor pours into 15 liters of Zn0.9Co0.1In O-PEI mixed form solution, ultrasonic treatment
0.5 hour, form MoS2-PEI-Zn0.9Co0.1O structure-solution.
Finally to MoS2-PEI-Zn0.9Co0.1O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 3 times and drying, obtains the Zn of core-shell structure0.9Co0.1O@MoS2Nanometer powder.
Embodiment 2.
10g polyetherimide (PEI) is added in 10 liters of deionized waters first and is sufficiently dissolved, 5g is then added
Zn0.8Co0.2O nano particle adds the deionized water of 400ml, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water,
Obtain polyetherimide and Zn0.8Co0.2The mixed liquor of O is kept for 1 hour, forms Zn0.8Co0.2O-PEI mixed form solution；It will
2g MoS2It is dissolved in and being added in 400ml deionized water, mixing liquid ultrasound simultaneously stirs 3 times, obtains MoS2Mixed liquor.Zn0.8Co0.2O
Nano particle is two-dimensional nano compounded mix, is to handle ZnO nano particle, doping metals Co particle is formed.
Then the MoS of 400ml is taken2Mixed liquor pours into 14 liters of Zn0.8Co0.2In O-PEI mixed form solution, ultrasonic treatment
1 hour, form MoS2-PEI-Zn0.8Co0.2O structure-solution.
Finally to MoS2-PEI-Zn0.8Co0.2O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 4 times and drying, obtains the Zn of core-shell structure0.8Co0.2O@MoS2Nanometer powder.
Characterization test analysis is carried out to the powder of preparation, Fig. 1 is Zn0.8Co0.2O@MoS2The XRD diagram of nanometer powder, from
It can be seen that there is a wider peak at 15 ° or so in figure, this corresponds to 1T-MoS2(001) crystal face peak, this prove MoS2's
In the presence of.
Fig. 2 (a) and 2 (b) is nanoscale Zn0.8Co0.2O@MoS2The TEM of shell nuclear material schemes, and wherein Fig. 2 (b) is high-resolution
Rate TEM figure.From Fig. 2 (a) it can be seen that Zn0.8Co0.2O@MoS2The diameter grain of nanometer powder, can from Fig. 2 (b) between 10~20nm
To find out apparent crystal plane structure inside nano particle.
Fig. 3 is Zn0.8Co0.2O nano particle and Zn0.8Co0.2O@MoS2The comparison Raman figure of core-shell structure.Pass through comparison
Zn0.8Co0.2O and Zn0.8Co0.2O@MoS2Raman map, it can be clearly seen that former Zn0.8Co0.2It is located at 477cm in O-1Raman
Peak varies widely in core-shell structure, and the peak intensity that it corresponds to peak obviously weakens.Result explanation, works as Zn0.8Co0.2O nanometers
Particle surface coats MoS2It is formed after composite construction, MoS2For Zn0.8Co0.2The vibration mode of O produces bigger effect, i.e., and two
Very important interaction is produced between person.
Embodiment 3.
20g polyetherimide (PEI) is added in 10 liters of deionized waters first and is sufficiently dissolved, 20g is then added
Zn0.5Co0.5O nano particle adds the deionized water of 350ml, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water,
Obtain polyetherimide and Zn0.5Co0.5The mixed liquor of O is kept for 45 minutes, forms Zn0.5Co0.5O-PEI mixed form solution；It will
1g MoS2It is dissolved in and being added in 350ml deionized water, mixing liquid ultrasound simultaneously stirs 4 times, obtains MoS2Mixed liquor.Zn0.5Co0.5O
Nano particle is two-dimensional nano compounded mix, is to handle ZnO nano particle, doping metals Co particle is formed.
Then the MoS of 240ml is taken2Mixed liquor pours into 12 liters of Zn0.5Co0.5In O-PEI mixed form solution, ultrasonic treatment
1 hour, form MoS2-PEI-Zn0.5Co0.5O structure-solution.
Finally to MoS2-PEI-Zn0.5Co0.5O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 5 times and drying, obtains the Zn of core-shell structure0.5Co0.5O@MoS2Nanometer powder.
Embodiment 4.
7g polyetherimide (PEI) is added in 6 liters of deionized waters first and is sufficiently dissolved, 3g Zn is then added0.7Fe0.3O
Nano particle adds the deionized water of 200ml, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water, obtains polyethers
Acid imide and Zn0.7Fe0.3The mixed liquor of O is kept for 0.5 hour, forms Zn0.7Fe0.3O-PEI mixed form solution；By 1g MoS2
It is dissolved in and being added in 200ml deionized water, mixing liquid ultrasound simultaneously stirs 5 times, obtains MoS2Mixed liquor.Zn0.7Fe0.3O nanometers
Grain is two-dimensional nano compounded mix, is to handle ZnO nano particle, doping metals Fe particle is formed.
Then the MoS of 200ml is taken2Mixed liquor pours into 6 liters of Zn0.7Fe0.3In O-PEI mixed form solution, ultrasonic treatment
30 minutes, form MoS2-PEI-Zn0.7Fe0.3O structure-solution.
Finally to MoS2-PEI-Zn0.7Fe0.3O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 6 times and drying, obtains the Zn of core-shell structure0.7Fe0.3O@MoS2Nanometer powder.
Embodiment 5.
15g polyetherimide (PEI) is added in 15 liters of deionized waters first and is sufficiently dissolved, 10g is then added
Zn0.6Fe0.4O nano particle adds the deionized water of 500ml, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water,
Obtain polyetherimide and Zn0.6Fe0.4The mixed liquor of O is kept for 50 minutes, forms Zn0.6Fe0.4O-PEI mixed form solution；It will
1g MoS2It is dissolved in and being added in 500ml deionized water, mixing liquid ultrasound simultaneously stirs 6 times, obtains MoS2Mixed liquor.Zn0.6Fe0.4O
Nano particle is two-dimensional nano compounded mix, is to handle ZnO nano particle, doping metals Fe particle is formed.
Then the MoS of 500ml is taken2Mixed liquor pours into 15 liters of Zn0.6Fe0.4In O-PEI mixed form solution, ultrasonic treatment
50 minutes, form MoS2-PEI-Zn0.6Fe0.4O structure-solution.
Finally to MoS2-PEI-Zn0.6Fe0.4O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 7 times and drying, obtains the Zn of core-shell structure0.6Fe0.4O@MoS2Nanometer powder.
Embodiment 6.
30g polyetherimide (PEI) is added in 10 liters of deionized waters first and is sufficiently dissolved, 20g is then added
Zn0.4Fe0.6O nano particle adds the deionized water of 500ml, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water,
Obtain polyetherimide and Zn0.4Fe0.6The mixed liquor of O is kept for 1 hour, forms Zn0.4Fe0.6O-PEI mixed form solution；It will
0.5g MoS2It is dissolved in and being added in 500ml deionized water, mixing liquid ultrasound simultaneously stirs 7 times, obtains MoS2Mixed liquor.
Zn0.4Fe0.6O nano particle is two-dimensional nano compounded mix, is handled ZnO nano particle, doping metals Fe granulated
At.
Then the MoS of 500ml is taken2Mixed liquor pours into 10 liters of Zn0.4Fe0.6In O-PEI mixed form solution, ultrasonic treatment
0.5 hour, form MoS2-PEI-Zn0.4Fe0.6O structure-solution.
Finally to MoS2-PEI-Zn0.4Fe0.6O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 8 times and drying, obtains the Zn of core-shell structure0.4Fe0.6O@MoS2Nanometer powder.
Embodiment 7.
50g polyetherimide (PEI) is added in 50 liters of deionized waters first and is sufficiently dissolved, 30g is then added
Zn0.5Ni0.5O nano particle adds 2.5 liters of deionized water, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water,
Obtain polyetherimide and Zn0.5Ni0.5The mixed liquor of O is kept for 1 hour, forms Zn0.5Ni0.5O-PEI mixed form solution；It will
5g MoS2It is dissolved in and being added in 1.5 liters of deionized waters, mixing liquid ultrasound simultaneously stirs 8 times, obtains MoS2Mixed liquor.Zn0.5Ni0.5O
Nano particle is two-dimensional nano compounded mix, is to handle ZnO nano particle, doping metals Ni particle is formed.
Then 1.5 liters of MoS is taken2Mixed liquor pours into 45 liters of Zn0.5Ni0.5In O-PEI mixed form solution, ultrasonic treatment
1 hour, form MoS2-PEI-Zn0.5Ni0.5O structure-solution.
Finally to MoS2-PEI-Zn0.5Ni0.5O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 9 times and drying, obtains the Zn of core-shell structure0.5Ni0.5O@MoS2Nanometer powder.
Embodiment 8.
40g polyetherimide (PEI) is added in 10 liters of deionized waters first and is sufficiently dissolved, 20g is then added
Zn0.3Ni0.7O nano particle adds the deionized water of 400ml, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water,
Obtain polyetherimide and Zn0.3Ni0.7The mixed liquor of O is kept for 45 minutes, forms Zn0.3Ni0.7O-PEI mixed form solution；It will
2.5g MoS2It is dissolved in and being added in 500ml deionized water, mixing liquid ultrasound simultaneously stirs 9 times, obtains MoS2Mixed liquor.
Zn0.3Ni0.7O nano particle is two-dimensional nano compounded mix, is handled ZnO nano particle, doping metals Ni granulated
At.
Then 0.5 liter of MoS is taken2Mixed liquor pours into 10 liters of Zn0.3Ni0.7In O-PEI mixed form solution, ultrasonic treatment
40 minutes, form MoS2-PEI-Zn0.3Ni0.7O structure-solution.
Finally to MoS2-PEI-Zn0.3Ni0.7O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 10 times and drying, obtains the Zn of core-shell structure0.3Ni0.7O@MoS2Nanometer powder.
Embodiment 9.
20g polyetherimide (PEI) is added in 10 liters of deionized waters first and is sufficiently dissolved, 20g is then added
Zn0.2Ni0.8O nano particle adds the deionized water of 350ml, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water,
Obtain polyetherimide and Zn0.2Ni0.8The mixed liquor of O is kept for 35 minutes, forms Zn0.2Ni0.8O-PEI mixed form solution；It will
1.5g MoS2It is dissolved in and being added in 500ml deionized water, mixing liquid ultrasound simultaneously stirs 10 times, obtains MoS2Mixed liquor.
Zn0.2Ni0.8O nano particle is two-dimensional nano compounded mix, is handled ZnO nano particle, doping metals Ni granulated
At.
Then 0.5 liter of MoS is taken2Mixed liquor pours into 12 liters of Zn0.2Ni0.8In O-PEI mixed form solution, ultrasonic treatment
45 minutes, form MoS2-PEI-Zn0.2Ni0.8O structure-solution.
Finally to MoS2-PEI-Zn0.2Ni0.8O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 2 times and drying, obtains the Zn of core-shell structure0.2Ni0.8O@MoS2Nanometer powder.
Embodiment 10.
15g polyetherimide (PEI) is added in 12 liters of deionized waters first and is sufficiently dissolved, 6g is then added
Zn0.4Ni0.6O nano particle adds the deionized water of 400ml, and ultrasound is simultaneously stirred to nano powder dispersion in deionized water,
Obtain polyetherimide and Zn0.4Ni0.6The mixed liquor of O is kept for 0.5 hour, forms Zn0.4Ni0.6O-PEI mixed form solution；
By 0.5g MoS2It is dissolved in and being added in 600ml deionized water, mixing liquid ultrasound simultaneously stirs 3 times, obtains MoS2Mixed liquor.
Zn0.4Ni0.6O nano particle is two-dimensional nano compounded mix, is handled ZnO nano particle, doping metals Ni granulated
At.
Then the MoS of 600ml is taken2Mixed liquor pours into 12 liters of Zn0.4Ni0.6In O-PEI mixed form solution, ultrasonic treatment
0.5 hour, form MoS2-PEI-Zn0.4Ni0.6O structure-solution.
Finally to MoS2-PEI-Zn0.4Ni0.6O structure-solution is centrifuged, gained mixture by deionized water and
Ethyl alcohol cleans 4 times and drying, obtains the Zn of core-shell structure0.4Ni0.6O@MoS2Nanometer powder.
Obtained Zn(1-x)MxO@MoS2The partial size R of nanometer powder is between 1~100nm.
This method second step is added a polymer in polar solvent, and the polymer of clear is formed after being completely dissolved
Solution.
Embodiment 11.
The ratio of 1g is added according to every liter, it is pure that Kynoar PVDF is added to the analysis of the DMF equipped with magnetic stirring apparatus
It in solvent, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 12.
The ratio of 100g is added according to every liter, Kynoar PVDF is added to the analysis of the DMF equipped with magnetic stirring apparatus
It in pure solvent, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 13.
The ratio of 10g is added according to every liter, it is pure that Kynoar PVDF is added to the analysis of the DMF equipped with magnetic stirring apparatus
It in solvent, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 14.
The ratio of 1g is added according to every liter, it is pure that Kynoar PVDF is added to the analysis of the NMP equipped with magnetic stirring apparatus
It in solvent, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 15.
The ratio of 5g is added according to every liter, it is pure that Kynoar PVDF is added to the analysis of the NMP equipped with magnetic stirring apparatus
It in solvent, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 16.
The ratio of 15g is added according to every liter, it is pure that Kynoar PVDF is added to the analysis of the NMP equipped with magnetic stirring apparatus
It in solvent, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 17.
The ratio of 20g is added according to every liter, Kynoar PVDF is added to the analysis of the DMAC equipped with magnetic stirring apparatus
It in pure solvent, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 18.
The ratio of 50g is added according to every liter, Kynoar PVDF is added to the analysis of the DMAC equipped with magnetic stirring apparatus
It in pure solvent, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 19.
The ratio of 100g is added according to every liter, Kynoar PVDF is added to the analysis of the DMAC equipped with magnetic stirring apparatus
It in pure solvent, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 20.
The ratio of 30g is added according to every liter, the P (VDF-CTFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMF analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 21.
The ratio of 40g is added according to every liter, the P (VDF-CTFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMF analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 22.
The ratio of 50g is added according to every liter, the P (VDF-CTFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMF analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 23.
The ratio of 1g is added according to every liter, the P (VDF-CTFE) based on Kynoar PVDF is added to equipped with magnetic force
In the NMP analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 24.
The ratio of 2g is added according to every liter, the P (VDF-CTFE) based on Kynoar PVDF is added to equipped with magnetic force
In the NMP analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 25.
The ratio of 5g is added according to every liter, the P (VDF-CTFE) based on Kynoar PVDF is added to equipped with magnetic force
In the NMP analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 26.
The ratio of 10g is added according to every liter, the P (VDF-CTFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMAC analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 27.
The ratio of 50g is added according to every liter, the P (VDF-CTFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMAC analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 28.
The ratio of 100g is added according to every liter, the P (VDF-CTFE) based on Kynoar PVDF is added to equipped with magnetic
In the DMAC analysis pure solvent of power blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 29.
The ratio of 1g is added according to every liter, the P (VDF-TrFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMF analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 30.
The ratio of 100g is added according to every liter, the P (VDF-TrFE) based on Kynoar PVDF is added to equipped with magnetic
In the DMF analysis pure solvent of power blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 31.
The ratio of 10g is added according to every liter, the P (VDF-TrFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMF analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 32.
The ratio of 1g is added according to every liter, the P (VDF-TrFE) based on Kynoar PVDF is added to equipped with magnetic force
In the NMP analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 33.
The ratio of 5g is added according to every liter, the P (VDF-TrFE) based on Kynoar PVDF is added to equipped with magnetic force
In the NMP analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 34.
The ratio of 15g is added according to every liter, the P (VDF-TrFE) based on Kynoar PVDF is added to equipped with magnetic force
In the NMP analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 35.
The ratio of 20g is added according to every liter, the P (VDF-TrFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMAC analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 36.
The ratio of 50g is added according to every liter, the P (VDF-TrFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMAC analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 37.
The ratio of 25g is added according to every liter, the P (VDF-TrFE) based on Kynoar PVDF is added to equipped with magnetic force
In the DMAC analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 38.
The ratio of 1g is added according to every liter, the P (VDF-CTFE-TrFE) based on Kynoar PVDF is added to and is equipped with
In the DMF analysis pure solvent of magnetic stirring apparatus, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 39.
The ratio of 100g is added according to every liter, the P (VDF-CTFE-TrFE) based on Kynoar PVDF is added to dress
Have in the DMF analysis pure solvent of magnetic stirring apparatus, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 40.
The ratio of 15g is added according to every liter, the P (VDF-CTFE-TrFE) based on Kynoar PVDF is added to dress
Have in the DMF analysis pure solvent of magnetic stirring apparatus, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 41.
The ratio of 5g is added according to every liter, the P (VDF-CTFE-TrFE) based on Kynoar PVDF is added to and is equipped with
In the NMP analysis pure solvent of magnetic stirring apparatus, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 42.
The ratio of 30g is added according to every liter, the P (VDF-CTFE-TrFE) based on Kynoar PVDF is added to dress
Have in the NMP analysis pure solvent of magnetic stirring apparatus, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 43.
The ratio of 50g is added according to every liter, the P (VDF-CTFE-TrFE) based on Kynoar PVDF is added to dress
Have in the NMP analysis pure solvent of magnetic stirring apparatus, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 44.
The ratio of 1g is added according to every liter, the P (VDF-CTFE-TrFE) based on Kynoar PVDF is added to and is equipped with
In the DMAC analysis pure solvent of magnetic stirring apparatus, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 45.
The ratio of 10g is added according to every liter, the P (VDF-CTFE-TrFE) based on Kynoar PVDF is added to dress
Have in the DMAC analysis pure solvent of magnetic stirring apparatus, is sufficiently stirred, until being completely dissolved, the polymer for forming clear is molten
Liquid.
Embodiment 46.
The ratio of 100g is added according to every liter, the P (VDF-CTFE-TrFE) based on Kynoar PVDF is added to dress
Have in the DMAC analysis pure solvent of magnetic stirring apparatus, is sufficiently stirred, until being completely dissolved, the polymer for forming clear is molten
Liquid.
Embodiment 47.
The ratio of 1g is added according to every liter, the P (VDF-HFP) based on Kynoar PVDF is added to and is stirred equipped with magnetic force
It mixes in the DMF analysis pure solvent of device, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 48.
The ratio of 80g is added according to every liter, the P (VDF-HFP) based on Kynoar PVDF is added to equipped with magnetic force
In the DMF analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 49.
The ratio of 60g is added according to every liter, the P (VDF-HFP) based on Kynoar PVDF is added to equipped with magnetic force
In the DMF analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 50.
The ratio of 1g is added according to every liter, the P (VDF-HFP) based on Kynoar PVDF is added to and is stirred equipped with magnetic force
It mixes in the NMP analysis pure solvent of device, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 51.
The ratio of 15g is added according to every liter, the P (VDF-HFP) based on Kynoar PVDF is added to equipped with magnetic force
In the NMP analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 52.
The ratio of 35g is added according to every liter, the P (VDF-HFP) based on Kynoar PVDF is added to equipped with magnetic force
In the NMP analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 53.
The ratio of 20g is added according to every liter, the P (VDF-HFP) based on Kynoar PVDF is added to equipped with magnetic force
In the DMAC analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 54.
The ratio of 100g is added according to every liter, the P (VDF-HFP) based on Kynoar PVDF is added to equipped with magnetic force
In the DMAC analysis pure solvent of blender, it is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
Embodiment 55.
The ratio of 2g is added according to every liter, the P (VDF-HFP) based on Kynoar PVDF is added to and is stirred equipped with magnetic force
It mixes in the DMAC analysis pure solvent of device, is sufficiently stirred, until being completely dissolved, forms the polymer solution of clear.
This method third step is the Zn that will be prepared(1-x)MxO@MoS2Nanometer powder is added in polymer solution, and stirring is extremely
Occur without precipitating, forms mixed liquor.
Embodiment 56.
The ratio of 0.1g, Zn prepared by embodiment 1 are added according to every liter0.9Co0.1O@MoS2Nanometer powder is added to reality
In the polymer solution for applying the preparation of 11~55 either method of example, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
Embodiment 57.
The ratio of 0.2g, Zn prepared by embodiment 2 are added according to every liter0.8Co0.2O@MoS2Nanometer powder is added to reality
In the polymer solution for applying the preparation of 11~55 either method of example, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
Embodiment 58.
The ratio of 0.5g, Zn prepared by embodiment 3 are added according to every liter0.5Co0.5O@MoS2Nanometer powder is added to reality
In the polymer solution for applying the preparation of 11~55 either method of example, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
Embodiment 59.
The ratio of 0.8g, Zn prepared by embodiment 4 are added according to every liter0.7Fe0.3O@MoS2Nanometer powder is added to reality
In the polymer solution for applying the preparation of 11~55 either method of example, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
Embodiment 60.
The ratio of 1g, Zn prepared by embodiment 5 are added according to every liter0.6Fe0.4O@MoS2Nanometer powder is added to implementation
In the polymer solution of 11~55 either method of example preparation, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
Embodiment 61.
The ratio of 1.5g, Zn prepared by embodiment 6 are added according to every liter0.4Fe0.6O@MoS2Nanometer powder is added to reality
In the polymer solution for applying the preparation of 11~55 either method of example, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
Embodiment 62.
The ratio of 3g, Zn prepared by embodiment 7 are added according to every liter0.5Ni0.5O@MoS2Nanometer powder is added to implementation
In the polymer solution of 11~55 either method of example preparation, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
Embodiment 63.
The ratio of 5g, Zn prepared by embodiment 8 are added according to every liter0.3Ni0.7O@MoS2Nanometer powder is added to implementation
In the polymer solution of 11~55 either method of example preparation, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
Embodiment 64.
The ratio of 8g, Zn prepared by embodiment 9 are added according to every liter0.2Ni0.8O@MoS2Nanometer powder is added to implementation
In the polymer solution of 11~55 either method of example preparation, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
The 4th step of this method is stirred after mixed liquor to be put into ultrasonic machine ultrasound, and repeatedly, last time adds before stirring
Enter dibenzoyl peroxide (BPO) as crosslinking agent, forms suspension.
Embodiment 65.
The ratio of 10g, Zn prepared by embodiment 10 are added according to every liter0.4Ni0.6O@MoS2Nanometer powder is added to reality
In the polymer solution for applying the preparation of 11~55 either method of example, it is put into magnetic stirring apparatus, stirring occurs to without precipitating, forms mixing
Liquid.
The 4th step of this method is stirred after mixed liquor to be put into ultrasonic machine ultrasound, and repeatedly, last time adds before stirring
Enter dibenzoyl peroxide (BPO) as crosslinking agent, forms suspension.
Embodiment 66.
Mixed liquor prepared by embodiment 56 is put into ultrasonic machine ultrasound 0.5 hour, is stirred for 0.5 hour after taking-up, so
It is repeated 10 times, dibenzoyl peroxide (BPO) is added as crosslinking in the ratio that 1.3g is added according to every liter before stirring in last time
Agent forms suspension.
Embodiment 67.
Mixed liquor prepared by embodiment 57 is put into ultrasonic machine ultrasound 45 minutes, is stirred for after taking-up 1 hour, so repeats
9 times, the ratio that 0.5g is added according to every liter before stirring in last time is added dibenzoyl peroxide (BPO) and is used as crosslinking agent, shape
At suspension.
Embodiment 68.
Mixed liquor prepared by embodiment 58 is put into ultrasonic machine ultrasound 1 hour, is stirred for after taking-up 45 minutes, so repeats
8 times, the ratio that 1.5g is added according to every liter before stirring in last time is added dibenzoyl peroxide (BPO) and is used as crosslinking agent, shape
At suspension.
Embodiment 69.
Mixed liquor prepared by embodiment 59 is put into ultrasonic machine ultrasound 35 minutes, is stirred for after taking-up 0.5 hour, so weight
7 times multiple, the ratio that 1.8g is added according to every liter before stirring in last time is added dibenzoyl peroxide (BPO) and is used as crosslinking agent,
Form suspension.
Embodiment 70.
Mixed liquor prepared by embodiment 60 is put into ultrasonic machine ultrasound 0.5 hour, is stirred for after taking-up 35 minutes, so weight
6 times multiple, the ratio that 0.6g is added according to every liter before stirring in last time is added dibenzoyl peroxide (BPO) and is used as crosslinking agent,
Form suspension.
Embodiment 71.
Mixed liquor prepared by embodiment 61 is put into ultrasonic machine ultrasound 45 minutes, is stirred for after taking-up 45 minutes, so weight
2 times multiple, the ratio that 0.8g is added according to every liter before the 2nd stirring is added dibenzoyl peroxide (BPO) and is used as crosslinking agent, is formed
Suspension.
Embodiment 72.
Mixed liquor prepared by embodiment 62 is put into ultrasonic machine ultrasound 0.5 hour, is stirred for after taking-up 1 hour, so weight
3 times multiple, the ratio that 1.2g is added according to every liter before stirring in last time is added dibenzoyl peroxide (BPO) and is used as crosslinking agent,
Form suspension.
Embodiment 73.
Mixed liquor prepared by embodiment 63 is put into ultrasonic machine ultrasound 0.5 hour, is stirred for after taking-up 1 hour, so weight
4 times multiple, the ratio that 1.5g is added according to every liter before stirring in last time is added dibenzoyl peroxide (BPO) and is used as crosslinking agent,
Form suspension.
Embodiment 74.
Mixed liquor prepared by embodiment 64 is put into ultrasonic machine ultrasound 1 hour, is stirred for after taking-up 0.5 hour, so weight
5 times multiple, the ratio that 1g is added according to every liter before stirring in last time is added dibenzoyl peroxide (BPO) and is used as crosslinking agent, shape
At suspension.
Embodiment 75.
Mixed liquor prepared by embodiment 65 is put into ultrasonic machine ultrasound 1 hour, is stirred for after taking-up 0.5 hour, so weight
6 times multiple, the ratio that 2g is added according to every liter before stirring in last time is added dibenzoyl peroxide (BPO) and is used as crosslinking agent, shape
At suspension.
The 5th step of this method is that film is made in suspension.
Embodiment 76.
By 66~75 either method of embodiment prepare uniform suspension be coated on slide, coating thickness be 30 μm, 70
It is heated 2 hours at DEG C, makes solvent evaporating completely, obtain film.
Embodiment 77.
By 66~75 either method of embodiment prepare uniform suspension be coated on slide, coating thickness be 20 μm, 80
It is heated 45 minutes 1 hour at DEG C, makes solvent evaporating completely, obtain film.
Embodiment 78.
By 66~75 either method of embodiment prepare uniform suspension be coated on slide, coating thickness be 10 μm, 90
It is heated 30 minutes 1 hour at DEG C, makes solvent evaporating completely, obtain film.
Embodiment 79.
By 66~75 either method of embodiment prepare uniform suspension be coated on slide, coating thickness be 50 μm, 100
It is heated 30 minutes 1 hour at DEG C, makes solvent evaporating completely, obtain film.
Embodiment 80.
Uniform suspension prepared by 66~75 either method of embodiment is coated on slide, coating thickness is 5 μm, 75 DEG C
Lower heating 1 hour, makes solvent evaporating completely, obtains film.
Embodiment 81.
The suspension of 66~75 either method of embodiment preparation is cast out the composite wood with a thickness of 25 μm using casting machine
Expect film, is heated 30 minutes 1 hour at 70 DEG C, make solvent evaporating completely, obtain film.
Embodiment 82.
The suspension of 66~75 either method of embodiment preparation is cast out the composite wood with a thickness of 15 μm using casting machine
Expect film, is heated 2 hours at 80 DEG C, make solvent evaporating completely, obtain film.
Embodiment 83.
The suspension of 66~75 either method of embodiment preparation is cast out the composite material with a thickness of 5 μm using casting machine
Film heats 1 hour at 100 DEG C, makes solvent evaporating completely, obtain film.
Embodiment 84.
The suspension of 66~75 either method of embodiment preparation is cast out the composite wood with a thickness of 50 μm using casting machine
Expect film, is heated 2 hours at 100 DEG C, make solvent evaporating completely, obtain film.
Embodiment 85.
The suspension of 66~75 either method of embodiment preparation is cast out the composite wood with a thickness of 35 μm using casting machine
Expect film, is heated 20 minutes 1 hour at 85 DEG C, make solvent evaporating completely, obtain film.
The 6th step of this method is that composite film material is made in film.
Embodiment 86.
Film prepared by 76~85 either method of embodiment is kept the temperature 3 hours at 180 DEG C, is immediately put into -196 DEG C
Low temperature environment in be quenched 3 minutes, obtain composite film material.
Embodiment 87.
Film prepared by 76~85 either method of embodiment is kept the temperature 30 minutes 2 hours at 190 DEG C, is immediately put
Enter in -147 DEG C of low temperature environment and be quenched 5 minutes, obtains composite film material.
Embodiment 88.
Film prepared by 76~85 either method of embodiment is kept the temperature 2 hours at 200 DEG C, is immediately put into -98 DEG C
Low temperature environment in be quenched 7 minutes, obtain composite film material.
Embodiment 89.
Film prepared by 76~85 either method of embodiment is kept the temperature 1 hour at 210 DEG C, is immediately put into -49 DEG C
Low temperature environment in be quenched 8 minutes, obtain composite film material.
Embodiment 90.
Film prepared by 76~85 either method of embodiment is kept the temperature 30 minutes at 220 DEG C, is immediately put into 0 DEG C
It is quenched 10 minutes in low temperature environment, obtains composite film material.
To in embodiment utilize Zn0.8Co0.2The composite film material of O nano particle production carries out Electrical Analysis, wherein
Fig. 4 (a) is dielectric constant figure, and Fig. 4 (b) is dielectric loss figure, and Fig. 4 (c) is release energy density, loss of energy density and efficiency
Figure.
It can be seen that Zn from Fig. 4 (a) and Fig. 4 (b) figure0.8Co0.2O and Zn0.8Co0.2O@MoS2Manufactured thin-film dielectric is normal
Number is not much different, but Zn0.8Co0.2O@MoS2Manufactured film loss is obviously reduced.Found out from Fig. 4 (c) due to adding MoS2
Film breakdown intensity very little thus the density that releases energy is too small, and Zn0.8Co0.2O@MoS2Manufactured film compared to
Zn0.8Co0.2Film energy storage made of O is slightly promoted and efficiency is promoted from 68% or so to 80% or more, is promoted obvious.The party
Method Zn0.8Co0.2O@MoS2The high-performance dielectric material that nanometer powder and polymer are combined has high dielectric constant, height breakdown
Electric field, high energy storage density, low-loss feature.
Other nanometer powders Zn in this method(1-x)MxO@MoS2(metallic particles M is Co, Ni or Fe, x=0.1~0.8)
Also there is same performance, while the preparation method simple process being related to, selected materials performance is good, therefore the composite material prepared
Good reliability, toughness is high, can be mass-produced.
Claims (4)
1. the preparation method of the nano combined dielectric material of New Two Dimensional based on high energy storage efficiency, it is characterised in that this method is specific
It is as follows:
Step 1. synthesizes Zn using hydrothermal co-precipitation method(1-x)MxO@MoS2Nanometer powder, specific method are:
(1) polyetherimide is added L and risen in deionized water and sufficiently dissolved, Zn is then added(1-x)MxO nano particle, every liter is gone
1~4g polyetherimide, 0.5~2g Zn are added in ionized water(1-x)MxO nano particle；Add L/30~L/20 liter go from
Sub- water, ultrasound are simultaneously stirred to nano powder dispersion in deionized water, obtain polyetherimide and Zn(1-x)MxThe mixed liquor of O mixes
It closes liquid and keeps 0.5~1h, form Zn(1-x)MxO-PEI mixed form solution；
(2) by MoS2It is dissolved in deionized water, mixing liquid ultrasound simultaneously stirs 2~10 times, obtains MoS2Mixed liquor；Every liter go from
The MoS of 0.5~5g is added in sub- water2；
(3) MoS for rising L/30~L/202Mixed liquor pours into Zn(1-x)MxIn O-PEI mixed form solution, ultrasonic treatment 0.5~
1h forms MoS2-PEI-Zn(1-x)MxO structure-solution；
(4) to MoS2-PEI-Zn(1-x)MxO structure-solution is centrifuged, and gained mixture is clear by deionized water and ethyl alcohol
It washes 2~10 times and dry, obtains the Zn of core-shell structure(1-x)MxO@MoS2Nanometer powder；
Step 2. adds a polymer in the polar solvent equipped with magnetic stirring apparatus, is sufficiently stirred, until being completely dissolved, is formed
The polymer solution of clear；The polymer of 1~100g is added in every liter of polar solvent；
Step 3. is by Zn(1-x)MxO@MoS2Nanometer powder is added in polymer solution, is put into magnetic stirring apparatus, stirring is to without heavy
It forms sediment and occurs, form mixed liquor；The Zn of 0.1~10g is added in every liter of polymer solution(1-x)MxO@MoS2Nanometer powder；
Mixed liquor is put into ultrasonic machine 0.5~1h of ultrasound by step 4., and 0.5~1h is stirred for after taking-up, and so repeatedly 2~10 times,
Dibenzoyl peroxide is added as crosslinking agent in last time before stirring, form suspension, every liter of mixed liquor is added 0.5~2g's
Crosslinking agent；
Uniform suspension is coated on slide by step 5., or is cast out the composite wood with a thickness of 5~50 μm using casting machine
Expect film, heats 1~2h at 70~100 DEG C, make solvent evaporating completely, obtain film；
Film is kept the temperature 0.5~3h by step 6. at 180~220 DEG C, is immediately put into -196~0 DEG C of low temperature environment and is quenched
Fire 3~10min of processing, obtains composite film material.
2. the preparation method of the nano combined dielectric material of New Two Dimensional as described in claim 1 based on high energy storage efficiency,
It is characterized in that: Zn described in step 1(1-x)MxO nano particle is two-dimensional nano compounded mix, is carried out to ZnO nano particle
Processing, adulterates the composite construction of other metallic particles M formation, other metallic particles M is Co, Ni or Fe, x=0.1~0.8.
3. the preparation method of the nano combined dielectric material of New Two Dimensional as described in claim 1 based on high energy storage efficiency,
Be characterized in that: polymer described in step 2 is the Kynoar PVDF or P (VDF- based on Kynoar PVDF
CTFE), one of P (VDF-TrFE), P (VDF-CTFE-TrFE), P (VDF-HFP).
4. the preparation method of the nano combined dielectric material of New Two Dimensional as described in claim 1 based on high energy storage efficiency,
Be characterized in that: polar solvent described in step 2 is the analysis pure solvent of DMF, NMP or DMAC.
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| CN111218072A (en) * | 2020-02-29 | 2020-06-02 | 杭州电子科技大学 | High-dielectric high-energy-storage two-dimensional sheet strontium titanate composite material and preparation method thereof |
| CN115926345A (en) * | 2022-12-14 | 2023-04-07 | 陕西科技大学 | Polyvinylidene fluoride/calcium niobate nanosheet @ aluminum oxide composite material and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN110615956A (en) * | 2019-07-19 | 2019-12-27 | 杭州电子科技大学 | Preparation method of nano sandwich structure composite material based on high breakdown and high energy storage |
| CN110615956B (en) * | 2019-07-19 | 2021-10-29 | 杭州电子科技大学 | Preparation method of nano sandwich structure composite material based on high breakdown and high energy storage |
| CN111218072A (en) * | 2020-02-29 | 2020-06-02 | 杭州电子科技大学 | High-dielectric high-energy-storage two-dimensional sheet strontium titanate composite material and preparation method thereof |
| CN115926345A (en) * | 2022-12-14 | 2023-04-07 | 陕西科技大学 | Polyvinylidene fluoride/calcium niobate nanosheet @ aluminum oxide composite material and preparation method and application thereof |
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| CN109400924B (en) | 2021-03-23 |
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