CN106496684B - A kind of graphene-based dielectric elastomer composite material of multi-layer core-shell structure and preparation - Google Patents
A kind of graphene-based dielectric elastomer composite material of multi-layer core-shell structure and preparation Download PDFInfo
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Abstract
The invention discloses the graphene-based dielectric elastomer composite material of a kind of multi-layer core-shell structure for belonging to dielectric elastomer preparing technical field and preparations.The composite material includes elastomer matrix, cross-linking system, the graphene-based dielectric filler of multi-layer core-shell structure, wherein the graphene-based dielectric filler of multi-layer core-shell structure coats a strata DOPA amine layer by high dielectric ceramic filler surface, in one layer of graphene oxide of poly-dopamine surface grafting, graphene oxide layer is reduced to graphene layer and is formed.The graphene-based dielectric filler of a small amount of multi-layer core-shell structure is filled into dielectric elastomer, dielectric elastomer composite material is prepared.The preparation method effectively increases the dielectric constant of dielectric elastomer while keeping smaller dielectric loss, solves the problems such as required loading is high, Modulus of Composites is big and dielectric loss is big, electric breakdown strength is low when ceramic packing filled elastomer.
Description
Technical field
The invention belongs to dielectric elastomer preparing technical fields, and in particular to a kind of graphene-based dielectric of multi-layer core-shell structure
Elastic composite and preparation.
Background technology
Dielectric elastomer is with electroluminescent deformation is big, the response time is short, viscoelastic hysteresis loss is small, flexibility is well imitated with conversion
The high feature of rate is mainly used in the fields such as microrobot, micro-air-vehicles, artificial-muscle, plane loudspeaker.Dielectric at present
Elastomer there are dielectric constants it is low, dielectric loss is big, electroluminescent deformation is small the problems such as.
Improve dielectric elastomer dielectric constant method it is main there are two：First, addition high dielectric ceramic filler, this side
Although method can effectively improve dielectric elastomer dielectric constant, addition particle weight is larger, causes elasticity modulus to increase, material lacks
Fall into it is more, electric breakdown strength is low.Second is that addition conductive filler, such percolation-based threshold theory of method exceed when conductive filler reaches
When oozing threshold value, dielectric constant is maximum；But when conductive filler dosage meets or exceeds percolation threshold, dielectric elastomer formation is led
Electric pathway, dielectric loss are significantly increased, and electric breakdown strength is greatly reduced.
In patent CN103183847A, propose in the rubber emulsion be added graphene oxide water solution make graphene oxide with
Molecular level is dispersed in rubber matrix, and graphene oxide is reduced to graphene using in-situ heat restoring method, forms graphite
Alkene lamella wraps up the three-dimensional net structure of latex particle.The percolation threshold for this approach reducing elastic composite, improves
Dielectric constant reduces elasticity modulus, but since there are certain agglomeration, dielectric damages in elastomer matrix for graphene oxide
Consumption is still higher, and electric breakdown strength is relatively low.
In patent CN104031297A, proposition poly-dopamine layer cladding graphene oxide simultaneously distributes it to rubber latex
In, the graphene oxide layer for forming poly-dopamine organic coating wraps up latex particle isolation network structure.The preparation method drops
Low dielectric loss improves electric breakdown strength, but the poly-dopamine insulating layer of graphene oxide outer surface cladding can make Jie
The dielectric constant of electric elastomer is declined.
High-k, big electroluminescent deformation, low-dielectric loss and low elastic modulus can be taken into account by preparing a kind of particle, be
Such dielectric elastomer technical issues that need to address.
Invention content
In view of the deficiencies of the prior art, the present invention proposes a kind of graphene-based dielectric elastomeric bluk recombinations of multi-layer core-shell structure
Material and preparation.
Specific technical solution is as follows：
The preparation of the graphene-based dielectric elastomer composite material of multi-layer core-shell structure includes the following steps：
1) it uses trishydroxymethylaminomethane solid to adjust the pH to 8.5 of water, dopamine is added, obtains aqueous dopamine solution；
2) high dielectric ceramic particle is put into aqueous dopamine solution, mechanical agitation is after reaction, dilute with deionized water
It releases to neutral, suction filtration, vacuum drying, obtains solid poly-dopamine cladding high dielectric ceramic filler；
3) by graphene oxide ultrasonic disperse in deionized water, graphene oxide water solution is obtained；
4) in graphene oxide water solution, poly-dopamine is added and coats high dielectric ceramic filler, mechanical agitation, reaction knot
Shu Hou is diluted to neutral, suction filtration, vacuum drying with deionized water, obtains multi-layer core-shell structure graphite oxide alkenyl dielectric filler；
5) multi-layer core-shell structure graphite oxide alkenyl dielectric filler is put into the ammonia spirit of hydrazine hydrate, mechanical agitation,
After reaction, it is diluted to neutral, suction filtration, vacuum drying with deionized water, the graphene-based dielectric of multi-layer core-shell structure is made and fills out
Material；
6) the graphene-based dielectric filler of multi-layer core-shell structure is added in rubber matrix, vulcanizing agent, double roller mill is added
It is kneaded uniform, slice, rubber compound on machine to park, on vulcanizing press vulcanize, the graphene-based dielectric bullet of multi-layer core-shell structure is made
Elastomer composite material.
A concentration of 1.2-2mg/ml of aqueous dopamine solution in step 1).
High dielectric ceramic particle is nano barium phthalate, nano-titanium dioxide, nanometer lead magnesio-niobate in step 2).
High dielectric ceramic average particle size is 30-200nm in step 2).
Mechanical agitation is 25 DEG C of temperature, time 15-25h in step 2) and step 4).
Ultrasound condition is 800W, 6h in step 3).
A concentration of 0.4-1mg/ml of graphene oxide water solution in step 3).
A concentration of 0.005-0.015mg/ml of the ammonia spirit of hydrazine hydrate in step 5).
Mechanical agitation is 80-100 DEG C of temperature, time 1-3h in step 5).
The graphene-based dielectric filler of multi-layer core-shell structure is 1.5-5 mass parts in step 6), and rubber matrix is 100 mass
Part, vulcanizing agent is 0.5-2 mass parts.
Elastomer matrix described in step 6) is rubber；The rubber is natural rubber, silicon rubber, nitrile rubber, butyl
Rubber or acrylic rubber.
Vulcanizing agent described in step 6) is sulphur system and organic peroxide systems；The sulphur system is sulphur, oxygen
Change zinc and stearic acid；The organic peroxide systems are two (4- toluyls) peroxide, dibenzoyl peroxide, mistake
Aoxidize diisopropylbenzene (DIPB), 2,5- dimethyl -2,5- two (tert-butyl hydroperoxide) hexane.
Two-roll mill temperature is 20-60 DEG C in step 6)；The rubber compound storage period is 7-16h；Conditions of vulcanization is pressure
15Mpa, 160 DEG C of temperature, time 35min.
The graphene-based dielectric elastomer composite material of multi-layer core-shell structure prepared by the preparation method.
Beneficial effects of the present invention are：The preparation method of multi-layer core-shell particle proposed by the present invention selects poly-dopamine packet
High dielectric ceramic particle is covered, in poly-dopamine surface grafting graphene oxide, is restored using the method for electronation, makes appearance
The graphene easily reunited is grafted on the high dielectric ceramic particle surface of poly-dopamine cladding, and the dispersion of graphene has been significantly greatly increased
Property, reduce the dosage of graphene, and this method very simple environmental protection；By the graphene-based dielectric filler filling of multi-layer core-shell structure
Into rubber matrix, the dielectric constant of composite material is improved, dielectric loss is reduced, hence it is evident that improves electroluminescent deformation.
Description of the drawings
Fig. 1 (a) is the graphene-based dielectric elastomer composite material of multi-layer core-shell structure.
Fig. 1 (b) is the partial enlarged view of the graphene-based dielectric filler of multi-layer core-shell structure.
Label declaration：1- crosslinking points, the graphene-based dielectric filler of 2- multi-layer core-shell structures, 3- polymer molecular chains, 4- high
Dielectric ceramic particle, 5- poly-dopamines, 6- graphenes.
Specific implementation mode
With reference to embodiment, the invention will be further described, but the range that the present invention is protected is without being limited thereto.
Embodiment 1：
(1) by 20mg dopamines be added 100ml water in, and be added trishydroxymethylaminomethane solid (Tris) adjusting go from
The pH to 8.5 of sub- water, obtains dopamine solution；
(2) barium titanate particles that 1g grain sizes are 30nm are added in aqueous dopamine solution, mechanical agitation 18h at 25 DEG C,
After reaction, it is diluted to neutral, suction filtration, vacuum drying with deionized water, obtains poly-dopamine cladding barium titanate ceramics particle；
(3) by 0.5g graphene oxides ultrasonic disperse in 1000ml deionized waters, 800W ultrasonic disperse 6h are aoxidized
Graphene aqueous solution；
(4) the barium titanate ceramics particle that 1g poly-dopamines coat is added in graphene oxide water solution, machine at 25 DEG C
Tool stirs 16h, is diluted to neutral, vacuum filtration, vacuum drying with deionized water, obtains the poly-dopamine of graphene oxide modification
Coat high dielectric ceramic filler；
(5) 1.5g multi-layer core-shell structure graphite oxide alkenyl dielectric fillers are added to containing 0.9ml hydrazine hydrate 0.8ml ammonia
In the 100ml aqueous solutions of water, mechanical agitation 7h at 95 DEG C is diluted to neutral, vacuum filtration, vacuum drying with deionized water, obtains
To the graphene-based high dielectric core-shell particles of multi-layer core-shell structure；
(6) by the nitrile rubber of 100g, room temperature modeling is practiced on a mill, by the graphene-based dielectric of 1.5g multi-layer core-shell structures
Filler is added gradually in nitrile rubber, is then gradually added into 0.5g cumyl peroxides, and cutter is kneaded, beats triangle bag, make
Mixing it is uniform, slice, after rubber compound parks 7-16h, 15Mpa on vulcanizing press, 160 DEG C of vulcanization 35min obtain multilayer core
Shell structure graphene dielectric elastomer composite material.
(7) dielectric properties, elasticity modulus are carried out to obtained multi-layer core-shell structure graphene dielectric elastomer composite material
It is tested with electroluminescent deformation.Test result is shown in Table 1.
Dielectric constant is tested：Dielectric elastomer is tested at room temperature using U.S.'s Agilent E4980A impedance instrument, 20~
106Dielectric constant in frequency range.The dielectric constant for obtaining nitrile rubber dielectric elastomer composite material is shown in Table 1.
Elasticity modulus is tested：Stretching experiment is carried out using the puller system (3366) of Instron companies.Composite material diaphragm quilt
It is cut into the dumbbell shape batten of standard, thickness is in 1mm or so.At ambient temperature, with the rate of extension of 50mm/min to composite wood
Expect that batten carries out Mechanics Performance Testing, preceding 5% corresponding stress-strain data progress linear fit will be strained and obtain elasticity modulus.
Electroluminescent deformation and breakdown strength test：Flexible electrode is sprayed in the both sides of dielectric elastomeric body thin film with high-pressure spray gun,
A diameter of 11mm of flexible electrode, electrode are tested after being put into convection oven drying.Pass through bohr high voltage power supply (model 73030P)
Control applies voltage, while recording change in shape of the electrode zone of dielectric elastomer under electrical field stimulation with digital camera.Electricity
Pressure is continuously increased, until composite material is breakdown, voltage when record punctures and electroluminescent deformation amount.Test result is shown in Table 1.
Embodiment 2
The preparation method is the same as that of Example 1, the difference is that the middle addition dopamine dosage of step (1) is 33mg, graphite in step (6)
The dosage of alkenyl ceramic particle is 4.5g.Test result is shown in Table 1.
Embodiment 3
The preparation method is the same as that of Example 1, the difference is that the dosage of cumyl peroxide is 2g in step (6).Test result
It is shown in Table 1.
Embodiment 4
The preparation method is the same as that of Example 1, the difference is that high dielectric ceramic particle is the titanium dioxide of grain size 30nm in step (2)
Particle, and additive amount is 0.6g.Rubber matrix is silicon rubber, bis- (t-butyl peroxy of crosslinking agent 0.5g2,5- dimethyl -2,5-
Change) hexane.Test result is shown in Table 1.
Embodiment 5
Preparation method is with embodiment 4, the difference is that the dosage of graphene-based ceramic particle is 3.8g in step (6).Test
It the results are shown in Table 1.
Embodiment 6
Preparation method with embodiment 3, unlike in step (6) 2,5- dimethyl -2,5- bis- (tert-butyl hydroperoxide) oneself
The dosage of alkane is 2g.Test result is shown in Table 1.
Embodiment 7
The preparation method is the same as that of Example 1, the difference is that high dielectric ceramic particle is the magnoniobate of grain size 200nm in step (2)
Lead ceramic particle, and additive amount is 0.6g.Rubber matrix is butyl rubber, and crosslinking agent is 0.5g dibenzoyl peroxides.Test
It the results are shown in Table 1.
Embodiment 8
Preparation method is with embodiment 7, the difference is that the dosage of graphene-based ceramic particle is 3.8g in step (6).Test
It the results are shown in Table 1.
Embodiment 9
Preparation method is with embodiment 5, the difference is that the dosage of dibenzoyl peroxide is 2g in step (6).Test result
It is shown in Table 1.
Comparative example 1
By the nitrile rubber of 100g, room temperature modeling is practiced on a mill, and the barium titanate particles that 1.8g grain sizes are 30nm are gradually added
Entering into nitrile rubber, is then gradually added into 0.5g cumyl peroxides, cutter is kneaded, and beats triangle bag, is allowed to be kneaded uniformly,
Slice, after rubber compound parks 7-16h, 15Mpa on vulcanizing press, 160 DEG C of vulcanization 35min obtain Filled with Barium Titanate butyronitrile rubber
The dielectric elastomer of glue.
Dielectric properties, elasticity modulus and electroluminescent deformation test are carried out to obtained dielectric elastomer.Test result is shown in Table 1.
Comparative example 2
By the nitrile rubber of 100g, room temperature modeling is practiced on a mill, and the barium titanate particles that 1.8g grain sizes are 30nm are gradually added
Entering into nitrile rubber, is then gradually added into 0.5g cumyl peroxides, cutter is kneaded, and beats triangle bag, is allowed to be kneaded uniformly,
Slice, after rubber compound parks 7-16h, 15Mpa on vulcanizing press, 160 DEG C of vulcanization 35min obtain graphene filled silicon rubber
Dielectric elastomer.
Dielectric properties, elasticity modulus and electroluminescent deformation test are carried out to obtained dielectric elastomer.Test result is shown in Table 1.
The performance evaluation of 1 multi-layer core-shell structure graphene dielectric elastomer composite material of table
As seen from Table 1, the graphene-based dielectric filler of minimal amount of multi-layer core-shell structure is filled into dielectric elastomer matrix
In, the dielectric constant of elastomer is significantly raised, 83.7 is can reach at 100Hz, maximum electroluminescent deformation is up to 39.4%, maintains
Low elastic modulus and dielectric loss improve dielectric elastomer electric breakdown strength.
Claims (13)
1. a kind of preparation method of the graphene-based dielectric elastomer composite material of multi-layer core-shell structure, which is characterized in that including with
Lower step：
1) it uses trishydroxymethylaminomethane solid to adjust the pH to 8.5 of water, dopamine is added, obtains aqueous dopamine solution；
2) high dielectric ceramic particle is put into aqueous dopamine solution, mechanical agitation is diluted to deionized water after reaction
Neutral, suction filtration, vacuum drying obtain solid poly-dopamine cladding high dielectric ceramic filler；
3) by graphene oxide ultrasonic disperse in deionized water, graphene oxide water solution is obtained；
4) in graphene oxide water solution, poly-dopamine is added and coats high dielectric ceramic filler, mechanical agitation, reaction terminates
Afterwards, it is diluted to neutral, suction filtration, vacuum drying with deionized water, obtains multi-layer core-shell structure graphite oxide alkenyl dielectric filler；
5) multi-layer core-shell structure graphite oxide alkenyl dielectric filler is put into the ammonia spirit of hydrazine hydrate, 80-100 DEG C of machinery stirs
1-3h is mixed, after reaction, neutral, suction filtration, vacuum drying is diluted to deionized water, it is graphene-based that multi-layer core-shell structure is made
Dielectric filler；
6) the graphene-based dielectric filler of multi-layer core-shell structure is added in rubber matrix, addition vulcanizing agent, in two-roll mill
It is kneaded uniform, slice, rubber compound to park, on vulcanizing press vulcanize, the graphene-based dielectric elastomer of multi-layer core-shell structure is made
Composite material.
2. preparation method according to claim 1, which is characterized in that a concentration of 1.2- of aqueous dopamine solution in step 1)
2mg/ml。
3. preparation method according to claim 1, which is characterized in that high dielectric ceramic particle is nano barium titanate in step 2)
Barium, nano-titanium dioxide or nanometer lead magnesio-niobate.
4. preparation method according to claim 1, which is characterized in that high dielectric ceramic average particle size is in step 2)
30-200nm。
5. preparation method according to claim 1, which is characterized in that mechanical agitation is temperature in step 2) and step 4)
25 DEG C of degree, time 15-25h.
6. preparation method according to claim 1, which is characterized in that ultrasound condition is 800W, 6h in step 3).
7. preparation method according to claim 1, which is characterized in that graphene oxide water solution is a concentration of in step 3)
0.4-1mg/ml。
8. preparation method according to claim 1, which is characterized in that the ammonia spirit of hydrazine hydrate is a concentration of in step 5)
0.005-0.015mg/ml。
9. preparation method according to claim 1, which is characterized in that the graphene-based dielectric of multi-layer core-shell structure in step 6)
Filler is 1.5-5 mass parts, and rubber matrix is 100 mass parts, and vulcanizing agent is 0.5-2 mass parts.
10. preparation method according to claim 1, which is characterized in that rubber matrix described in step 6) be natural rubber,
Silicon rubber, nitrile rubber, butyl rubber or acrylic rubber.
11. preparation method according to claim 1, which is characterized in that vulcanizing agent described in step 6) be sulphur system or
Organic peroxide systems；The sulphur system is sulphur, zinc oxide and stearic acid；The organic peroxide systems are two
(4- toluyls) peroxide, two (tertiary fourth of dibenzoyl peroxide, cumyl peroxide or 2,5- dimethyl -2,5-
Base peroxidating) hexane.
12. preparation method according to claim 1, which is characterized in that two-roll mill temperature is 20-60 in step 6)
℃；The rubber compound storage period is 7-16h；Conditions of vulcanization is pressure 15Mpa, 160 DEG C of temperature, time 35min.
13. the graphene-based dielectric elastomeric bluk recombination of multi-layer core-shell structure prepared by any one of the claim 1-12 preparation methods
Material.
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| CN110564134A (en) * | 2019-07-30 | 2019-12-13 | 曹建康 | preparation method of polyurethane-based composite nitrile rubber dielectric elastomer |
| CN110713717A (en) * | 2019-11-23 | 2020-01-21 | 西北工业大学 | High-temperature-resistant dopamine-coated barium titanate/polyimide (BT @ PDA/PI) dielectric nano composite film |
| CN112745559B (en) * | 2020-12-23 | 2023-02-17 | 河南工业大学 | Polymer dielectric elastomer and preparation method and application thereof |
| CN112759807B (en) * | 2021-01-18 | 2022-05-24 | 中北大学 | High-thermal-conductivity three-dimensional graphene oxide composite functional particle modified natural rubber and preparation method thereof |
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