CN109762278A - A kind of two-dimensional nano piece-polymer flexibility laminated film and preparation method thereof - Google Patents
A kind of two-dimensional nano piece-polymer flexibility laminated film and preparation method thereof Download PDFInfo
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- CN109762278A CN109762278A CN201910042726.4A CN201910042726A CN109762278A CN 109762278 A CN109762278 A CN 109762278A CN 201910042726 A CN201910042726 A CN 201910042726A CN 109762278 A CN109762278 A CN 109762278A
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Abstract
The present invention provides a kind of two-dimensional nano piece-polymer flexibility laminated film and preparation method thereof, is prepared by two-dimensional nano piece and polymeric matrix, the two-dimensional nano piece is by (Ca, Sr) with perovskite structure2(Nb,Ta)3O10Any one or more than one material in system is prepared, the polymer is Kynoar, any one or more than one material in Kynoar-trifluoro-ethylene, Kynoar-hexafluoropropene, epoxy resin, polypropylene, polyimides is prepared, and preparation process includes: high temperature sintering synthesis KCa2Nb3O10Material；Proton-exchange reaction synthesizes HCa2Nb3O10·1.5H2O material；Remove into two-dimensional nano piece；Flexible composite film product is prepared by the tape casting again.The present invention obtains the polymer matrix composite haveing excellent performance under lower inorganic matter additive amount to realize by adding two-dimensional nano piece into polymeric matrix, so that composite material be made to retain the good flexibility of polymeric matrix, improves laminated film disruptive field intensity.
Description
Technical field
The present invention relates to dielectric composite manufacturing technology fields, and in particular to a kind of two-dimensional nano piece-polymer flexible
Property laminated film and preparation method thereof.
Background technique
With the rapid development of the new high-tech industries such as Internet of Things, big data, new-energy automobile, intelligent terminal, whole world electricity
Container market realizes rapid growth, has been expanded to 20,900,000,000 dollars in 2017 via 17,300,000,000 dollars in 2012.According to not
Same application scenarios demand, has also derived the capacitor of different dielectric substances, and application currently on the market is more widely
Ceramic capacitor, aluminium electrolutic capacitor, tantalum electrolytic capacitor and thin film capacitor.Ceramic dielectric makes because of its dielectric constant height
With relatively wide, but its brittleness is big, loss is big, is not available and also can not be ignored in drawbacks such as printed circuit boards (PCB).In face of capacitor
Micromation, flexibility, passive development trend, single inorganic ceramic dielectric substance has been unable to satisfy requirement.Polymer
Dielectric substance because its flexibility is good, quality is small, it is easy to process, be easy large area film is made the characteristics of due to be widely used in film
Capacitor.Wherein, inorganic ceramic material has very high dielectric constant, but disruptive field intensity under high pressure is lower；And have
The disruptive field intensity of organic polymeric material is higher, but its dielectric constant is relatively low.Therefore, have good flexibility, quality smaller, easy
In processing and low-cost Organic-inorganic composite dielectric substance have received widespread attention.It is added into polymeric matrix
Inorganic ceramic material makes its dielectric constant while significantly improving with the high breakdown field strength of polymeric matrix.In electrical engineering
Field, this polymer-matrix composite dielectric material are a kind of good hv cable termination stress cone materials；In mechano-electronic
Field, this polymer-matrix composite dielectric material and organic circuit board have excellent compatibility, and are widely used in embedded-type electric
In the plate of road.In addition to this, along with the development of national smart grid and New Energy Industry, the capacitor of high power and large capacity is
As the great demand in new energy market, polymer matrix laminated film becomes the important of high-power components because of its high breakdown field strength
Element.
Existing research addition mainly into polymeric matrix has the ceramic particle of high dielectric constant to improve polymerization
The relative dielectric constant of object based composites, common ceramic particle have barium titanate (BaTiO3), titanium dioxide (TiO2), dioxy
Change zirconium (ZrO2) etc..But such scheme there are the problem of it is obvious, need the additive amount of higher inorganic ceramic particle that could be promoted
The volume fraction of the dielectric constant of composite material, inorganic ceramic particle is generally higher than 50%, this will make the flexibility of composite material
It substantially reduces.In addition, the disruptive field intensity that the addition of excessive inorganic component can cause defect to make laminated film reduces.Therefore, having must
The prior art is improved.
Summary of the invention
The object of the present invention is to provide a kind of two-dimensional nano piece-polymer flexibility laminated films and preparation method thereof, pass through
Two-dimensional nano piece is added into polymeric matrix obtains the polymer haveing excellent performance under lower inorganic matter additive amount to realize
Based composites improve laminated film disruptive field intensity so that composite material be made to retain the good flexibility of polymeric matrix.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of two-dimensional nano piece-polymer flexibility laminated film, is prepared by two-dimensional nano piece and polymeric matrix.
According to above scheme, the two-dimensional nano piece is by (Ca, Sr) with perovskite structure2(Nb,Ta)3O10In system
Any one or more than one material be prepared.
According to above scheme, the length and width of the two-dimensional nano piece is 0.1-1 μm, with a thickness of 1-2nm, described two
Nanometer sheet-polymer flexibility laminated film is tieed up with a thickness of 1-100 μm.
According to above scheme, the polymer is Kynoar (Polyvinylidene fluoride, PVDF), gathers
Vinylidene-trifluoro-ethylene (PVDF-TrFE), Kynoar-hexafluoropropene (PVDF-HFP), epoxy resin (Epoxy,
EP), polypropylene (PP), any one or more than one material in polyimides (PI) are prepared.
According to above scheme, the mass fraction of the two-dimensional nano piece is 0.1%-20%, the mass fraction of polymer is
80%-99.9%.
A kind of preparation method of two-dimensional nano piece-polymer flexibility laminated film, includes the following steps:
1) preparation has (Ca, the Sr) of perovskite structure2(Nb,Ta)3O10Two-dimensional nano piece；
2) two-dimensional nano piece and polymer composite membrane-forming.
According to above scheme, the Ca2Nb3O10The preparation of two-dimensional nano piece uses liquid phase stripping method, includes the following steps:
1) high temperature sintering synthesizes KCa2Nb3O10Material: oxide spinel potassium, calcium carbonate, niobium pentaoxide are needed in molar ratio
1:2:3 carry out mixed grinding 30-60min, then 1000-1300 DEG C at a temperature of be sintered 10-15h；
2) proton-exchange reaction synthesizes HCa2Nb3O10·1.5H2O material: by the KCa of synthesis2Nb3O10Material and concentration are 1
The nitric acid of~10mol/L is after 1:1 is mixed, to be placed on oscillator in molar ratio, carries out proton-exchange reaction 48-72h, filters,
Ultrapure water by obtained sample with resistivity greater than 18M Ω washes away the nitric acid of surface residual；
3) persursor material HCa2Nb3O10·1.5H2O is removed into two-dimensional nano piece: by the HCa of synthesis2Nb3O10·
1.5H2O material and tetrabutylammonium hydroxide solution (TBAOH, molecular formula C16H37NO) 1:1 mixes (i.e. TBA in molar ratio+:H+
=1:1), it is vibrated on mechnical oscillator and carries out within 10 days oscillation removing to get two-dimensional nano piece.
According to above scheme, the composite membrane-forming is prepared using casting technique, is included the following steps:
1) it by two-dimensional nano piece ultrasonic disperse into organic solvent n,N-Dimethylformamide (DMF) solution, is formed and is stablized
Then polymeric matrix is added in suspension, stir 24-48h, until sufficiently dissolution；
2) mixture of polymer and two-dimensional nano piece is cast into the film of required thickness, is dried at 40-80 DEG C, is received
Collect obtained laminated film.
The beneficial effects of the present invention are:
1) two-dimensional nano piece of the invention is made using the method for liquid phase removing, has inorganic perovskite structure special
Sign, polarization characteristic is obvious, thus dielectric constant with higher；
2) high dielectric constant of two-dimensional nano piece of the invention can be such that the specific gravity of the inorganic filler in composite material reduces,
Raising without influencing composite dielectric performance, this also makes laminated film remain good mechanical flexibility；
3) two-dimensional nano piece of the invention is dispersed in polymeric matrix, facilitates mentioning for laminated film disruptive field intensity
Height, this is beneficial to application of the laminated film in terms of high-voltage energy storage；
4) Novel compound film manufacture craft of the invention, by two-dimensional nano piece and high breakdown fields with high dielectric constant
Strong polymer is compound, and the laminated film of preparation has excellent mechanical property and electric property, is expected in composite dielectrics material
Material field is widely applied.
Detailed description of the invention
Fig. 1 is the two-dimensional nano piece AFM figure of the embodiment of the present invention 1；
Fig. 2 is the embodiment of the present invention 1, embodiment 2, the dielectric constant of 1 product of comparative example and dielectric loss with frequency
The relational graph of variation；
Fig. 3 is the relational graph that the dielectric displacement of the embodiment of the present invention 1,1 product of comparative example changes with extra electric field；
Fig. 4 is the profile scanning Electronic Speculum shape appearance figure of 1 finished product of the embodiment of the present invention.
Specific embodiment
Technical solution of the present invention is illustrated with embodiment with reference to the accompanying drawing.
Embodiment 1, is shown in Fig. 1 to Fig. 4:
The present invention provides a kind of two-dimensional nano piece-polymer flexibility laminated film, and preparation method includes the following steps:
1) preparation has the HCa of perovskite structure2Nb3O10Two-dimensional nano piece:
A) 1.4558g potassium carbonate (K is weighed2CO3), 4.0164g calcium carbonate (CaCO3) and 8.000g niobium pentaoxide
(Nb2O5) be placed in agate mortar and grind 60min, 1200 DEG C of high temperature furnace high temperature calcining 12h are put into, KCa is obtained2Nb3O10Sample
Product；
B) KCa of 2.5g synthesis is weighed2Nb3O10Powder is placed in the conical flask equipped with 100ml nitric acid (5mol/L), will be bored
Shape bottle, which is fixed on mini-vibrator, vibrates 72h, after the completion of proton-exchange reaction, filtering, by obtained sample ultrapure water (electricity
Resistance rate is greater than 18M Ω) nitric acid of surface residual is washed away to get two-dimensional nano piece persursor material HCa is arrived2Nb3O10·1.5H2O sample
Product；
C) the two-dimensional nano piece persursor material HCa of 1.0g synthesis is weighed2Nb3O10·1.5H2O powder is placed in equipped with 250ml
It is two-dimentional to get arriving by the fixed oscillation on the oscillator of conical flask 10 days in the conical flask of tetrabutylammonium hydroxide solution (TBAOH)
Emulsion after nanometer sheet removing；
2) two-dimensional nano piece and polymer composite membrane-forming:
D) the emulsion 1ml after measuring two-dimensional nano piece removing is freeze-dried, and group's wadding object of two-dimensional nano piece is obtained,
Its ultrasonic disperse is formed into stable suspension into 4ml DMF solution, then be added 0.396g PVDF, stirring 36h to sufficiently it is molten
Acquired solution is put into vacuum oven and stands 20min by Xie Hou, promotes the discharge of bubble；
E) mixture of PVDF and two-dimensional nano piece are cast into the film of required thickness, are subsequently placed in drying box,
12h (evaporation for being conducive to solvent) is stood at 40 DEG C, then keeps the temperature 10min at 200 DEG C, is put into quenching in ice water immediately
Obtain two-dimensional nano piece-polymer flexibility laminated film that two-dimensional nano piece filler is 1%.
Embodiment 2, is shown in Fig. 2:
The raw material of the present embodiment, preparation process substantially with embodiment 1, the difference is that: two wieners are measured in step d)
Emulsion 2ml after rice piece removing, finished product is two-dimensional nano piece-polymer flexibility THIN COMPOSITE that two-dimensional nano piece filler is 2%
Film.
Comparative example 1 is shown in Fig. 2 to Fig. 3:
The PVDF for weighing 0.5244g (mass fraction 10%) is dissolved in the DMF solution of 5ml, after stirring for 24 hours, gained is molten
Liquid, which is put into vacuum oven, stands 20min, promotes the discharge of bubble, then carry out curtain coating processing；Then the film of synthesis is put
Enter in drying box, stands 12h (evaporation for being conducive to solvent) at 40 DEG C；PVDF thin film is set to keep the temperature 10min at 200 DEG C again,
It is put into quenching in ice water immediately, pure PVDF thin film can be obtained.
Two-dimensional nano piece after the removing that 1 step c) of embodiment is obtained carries out AFM characterization, as a result as shown in Figure 1, two dimension
The thickness of nanometer sheet is 1.84nm, and length and width is between 0.2~0.5 μm.
Embodiment 1, embodiment 2 and 1 product of comparative example are tested, their dielectric constant and dielectric loss with
The relationship of frequency variation as shown in Fig. 2, be not added with the dielectric constant of the flexible PVDF thin film of two-dimentional filler between 10~11, and
Two-dimensional nano piece-polymer flexibility laminated film dielectric constant that two-dimentional filler preparation is added has apparent raising.Work as addition
When two-dimentional packing quality score is 1wt%, flexible composite film dielectric constant is between 12~13；When the two-dimentional packing quality of addition
When score is 2wt%, flexible composite film dielectric constant is between 13~14 (100Hz).It is two-dimentional when being added in terms of dielectric loss
When the mass fraction of filler is 1%, the dielectric loss of flexible composite film is consistent with pure PVDF thin film；When the two-dimentional filler of addition
When mass fraction is 2%, the purer PVDF thin film of the dielectric loss of flexible composite film has slightly elevated.
The relationship that the dielectric displacement of embodiment 1,1 product of comparative example changes with extra electric field as shown in figure 3, be powered on outside
When field intensity is 500kV/mm, the dielectric displacement for being not added with the flexible PVDF thin film of two-dimentional filler is 5.5mC/cm2, and it is added 1%
The dielectric displacement of the two-dimensional nano piece of two-dimentional filler-polymer flexibility laminated film is 6.5mC/cm2.Therefore, two-dimentional filler is added
The two-dimensional nano piece of preparation-polymer flexibility laminated film remanent polarization is higher than pure PVDF thin film, this is beneficial to thin
The raising of film energy storage density.
For the cross-section morphology of 1 product of embodiment as shown in scanning electron microscope Fig. 4, two-dimensional nano piece-polymer flexibility of preparation is multiple
Close film with a thickness of 10 μm.
Embodiment 3:
The raw material of the present embodiment, preparation process substantially with embodiment 1, the difference is that: polymer PVDF-HFP.
Embodiment 4:
The raw material of the present embodiment, preparation process substantially with embodiment 1, the difference is that: polymer EP.
Embodiment 5:
The raw material of the present embodiment, preparation process substantially with embodiment 1, the difference is that: polymer PP.
Embodiment 6:
The raw material of the present embodiment, preparation process substantially with embodiment 1, the difference is that: polymer PP, PI, EP's
The mixture of 1:1:1 in molar ratio.
The above embodiments are only used to illustrate and not limit the technical solutions of the present invention, although above-described embodiment to the present invention into
Gone detailed description, the related technical personnel of this field it is understood that can modify to the present invention or replace on an equal basis, but
Any modification and part replacement for not departing from spirit and scope of the invention should all be covered in scope of the presently claimed invention.
Claims (8)
1. a kind of two-dimensional nano piece-polymer flexibility laminated film, which is characterized in that by two-dimensional nano piece and polymer matrix system
It is standby to form.
2. two-dimensional nano piece according to claim 1-polymer flexibility laminated film, which is characterized in that two wiener
Rice piece is by (Ca, Sr) with perovskite structure2(Nb,Ta)3O10In system any one or more than one material preparation and
At.
3. two-dimensional nano piece according to claim 1-polymer flexibility laminated film, which is characterized in that two wiener
The length and width of rice piece is 0.1-1 μm, with a thickness of 1-2nm, the two-dimensional nano piece-polymer flexibility laminated film thickness
Degree is 1-100 μm.
4. two-dimensional nano piece according to claim 1-polymer flexibility laminated film, which is characterized in that the polymer
For Kynoar, Kynoar-trifluoro-ethylene, Kynoar-hexafluoropropene, epoxy resin, polypropylene, polyimides
In any one or more than one material be prepared.
5. two-dimensional nano piece according to claim 1-polymer flexibility laminated film, which is characterized in that two wiener
The mass fraction of rice piece is 0.1%-20%, the mass fraction of polymer is 80%-99.9%.
6. a kind of two-dimensional nano piece-polymer flexibility laminated film preparation method, includes the following steps:
1) preparation has (Ca, the Sr) of perovskite structure2(Nb,Ta)3O10Two-dimensional nano piece；
2) two-dimensional nano piece and polymer composite membrane-forming.
7. two-dimensional nano piece according to claim 6-polymer flexibility laminated film preparation method, which is characterized in that
The Ca2Nb3O10The preparation of two-dimensional nano piece uses liquid phase stripping method, includes the following steps:
1) high temperature sintering synthesizes KCa2Nb3O10Material: oxide spinel potassium, calcium carbonate, niobium pentaoxide are needed into 1:2:3 in molar ratio
Carry out mixed grinding 30-60min, then 1000-1300 DEG C at a temperature of be sintered 10-15h；
2) proton-exchange reaction synthesizes HCa2Nb3O10·1.5H2O material: by the KCa of synthesis2Nb3O10Material and concentration is 1~
The nitric acid of 10mol/L is after 1:1 is mixed, to be placed on oscillator in molar ratio, carries out proton-exchange reaction 48-72h, filters, will
Ultrapure water of the obtained sample with resistivity greater than 18M Ω washes away the nitric acid of surface residual；
3) persursor material HCa2Nb3O10·1.5H2O is removed into two-dimensional nano piece: by the HCa of synthesis2Nb3O10·1.5H2O material
1:1 is mixed in molar ratio with tetrabutylammonium hydroxide solution, is vibrated 10 days and is removed to get two wieners on mechnical oscillator
Rice piece.
8. two-dimensional nano piece according to claim 6-polymer flexibility laminated film preparation method, which is characterized in that
The composite membrane-forming is prepared using casting technique, is included the following steps:
1) by two-dimensional nano piece ultrasonic disperse into organic solvent n,N-Dimethylformamide solution, stable suspension is formed, so
After be added polymeric matrix, 24-48h is stirred, until sufficiently dissolution；
2) mixture of polymer and two-dimensional nano piece is cast into the film of required thickness, dries, collects at 40-80 DEG C
The laminated film arrived.
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Cited By (5)
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| CN111662515A (en) * | 2020-07-07 | 2020-09-15 | 西安交通大学 | Preparation method of polytetramethylene-pentene-titanium dioxide nanosheet composite film |
| CN112079384A (en) * | 2020-09-18 | 2020-12-15 | 武汉理工大学 | Method for ultrasonically stripping oxide nanosheets |
| CN114927345A (en) * | 2022-05-19 | 2022-08-19 | 江苏科技大学 | PVDF composite energy storage material and preparation method thereof |
| CN115322413A (en) * | 2022-05-20 | 2022-11-11 | 湘潭大学 | Flexible dielectric energy storage material and preparation method and application 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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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111662515A (en) * | 2020-07-07 | 2020-09-15 | 西安交通大学 | Preparation method of polytetramethylene-pentene-titanium dioxide nanosheet composite film |
| CN112079384A (en) * | 2020-09-18 | 2020-12-15 | 武汉理工大学 | Method for ultrasonically stripping oxide nanosheets |
| CN114927345A (en) * | 2022-05-19 | 2022-08-19 | 江苏科技大学 | PVDF composite energy storage material and preparation method thereof |
| CN115322413A (en) * | 2022-05-20 | 2022-11-11 | 湘潭大学 | Flexible dielectric energy storage material and preparation method and application thereof |
| CN115322413B (en) * | 2022-05-20 | 2023-08-15 | 湘潭大学 | Flexible dielectric energy storage material and preparation method and application 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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