CN106496684A - 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 a kind of graphene-based dielectric elastomer composite material of multi-layer core-shell structure for belonging to dielectric elastomer preparing technical field and preparation.The composite includes the graphene-based dielectric filler of elastomer matrix, cross-linking system, multi-layer core-shell structure, wherein the graphene-based dielectric filler of multi-layer core-shell structure passes through one strata DOPA amine layer of high dielectric ceramic filler Surface coating, in one layer of graphene oxide of poly-dopamine surface grafting, graphene oxide layer is reduced to graphene layer and is formed.Graphene-based for a small amount of multi-layer core-shell structure dielectric filler is filled in dielectric elastomer, dielectric elastomer composite material is prepared.The preparation method effectively increases the dielectric constant of dielectric elastomer while less dielectric loss is kept, and solves that required loading during ceramic packing filled elastomer is high, Modulus of Composites is big and dielectric loss is big, the low problem of electric breakdown strength.
Description
Technical field
The invention belongs to dielectric elastomer preparing technical field, and in particular to a kind of graphene-based dielectric of multi-layer core-shell structure
Elastic composite and preparation.
Background technology
Dielectric elastomer has that electroluminescent deformation is big, response time is short, viscoelastic hysteresis loss is little, pliability is good with conversion effect
The characteristics of rate is high, is mainly used in the fields such as microrobot, micro-air-vehicles, artificial-muscle, plane microphone.Current dielectric
Elastomer has that dielectric constant is low, dielectric loss is big, electroluminescent deformation.
The method for improving dielectric elastomer dielectric constant mainly has two：One is to add high dielectric ceramic filler, this side
Although method can effectively improve dielectric elastomer dielectric constant, add particle weight larger, cause elastic modelling quantity increase, material to lack
Fall into many, electric breakdown strength low.Two is to add conductive filler, and the percolation-based threshold theory of this kind of method exceedes when conductive filler reaches
When oozing threshold value, dielectric constant is maximum；But when conductive filler consumption meets or exceeds percolation threshold, dielectric elastomer is formed and is led
Electric pathway, dielectric loss are significantly increased, and electric breakdown strength is greatly reduced.
In patent CN103183847A, propose in rubber latex add 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 method of reducing, forms graphite
Alkene lamella wraps up the three-dimensional net structure of latex particle.The percolation threshold of elastic composite is this approach reduced, is improve
Dielectric constant, reduces elastic modelling quantity, but as graphene oxide has certain agglomeration in elastomer matrix, dielectric is damaged
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, form the graphene oxide layer parcel latex particle isolation network structure of poly-dopamine organic coating.The preparation method drop
Low dielectric loss, improves electric breakdown strength, but the poly-dopamine insulating barrier of graphene oxide outer surface cladding can make Jie
The dielectric constant of electric elastomer has declined.
Prepare a kind of particle and can take into account high-k, big electroluminescent deformation, low-dielectric loss and low elastic modulus, be
Such dielectric elastomer technical issues that need to address.
Content of the invention
The present invention is directed to the deficiencies in the prior art, it is proposed that a kind of graphene-based dielectric elastomeric bluk recombination of multi-layer core-shell structure
Material and preparation.
Concrete technical scheme is as follows：
The preparation of the graphene-based dielectric elastomer composite material of multi-layer core-shell structure is comprised the following steps：
1) pH to 8.5 of water is adjusted with trishydroxymethylaminomethane solid, is added dopamine, is obtained aqueous dopamine solution；
2) high dielectric ceramic particle is put in aqueous dopamine solution, mechanical agitation, after reaction terminates, deionized water is dilute
Release to neutrality, sucking filtration, vacuum drying, obtain the poly-dopamine cladding high dielectric ceramic filler of solid-state；
3) by graphene oxide ultrasonic disperse in deionized water, graphene oxide water solution is obtained；
4) in graphene oxide water solution, poly-dopamine cladding high dielectric ceramic filler, mechanical agitation, reaction knot are added
Shu Hou, deionized water are diluted to neutrality, sucking filtration, vacuum drying, obtain multi-layer core-shell structure graphite oxide thiazolinyl dielectric filler；
5) multi-layer core-shell structure graphite oxide thiazolinyl dielectric filler is put in the ammonia spirit of hydrazine hydrate, mechanical agitation,
After reaction terminates, deionized water is diluted to neutrality, sucking filtration, vacuum drying, the graphene-based dielectric of multi-layer core-shell structure is obtained and fills out
Material；
6) graphene-based for multi-layer core-shell structure dielectric filler is added in rubber matrix, adds vulcanizing agent, double roller mill
Knead uniform, slice, elastomeric compound to park, vulcanize on vulcanizing press on machine, the graphene-based dielectric bullet of multi-layer core-shell structure is obtained
Elastomer composite material.
Step 1) in aqueous dopamine solution concentration be 1.2-2mg/ml.
Step 2) in high dielectric ceramic particle be nano barium phthalate, nano titanium oxide, nanometer lead magnesio-niobate.
Step 2) in high dielectric ceramic average particle size be 30-200nm.
Step 2) and step 4) in mechanical agitation be 25 DEG C of temperature, time 15-25h.
Step 3) in ultrasound condition be 800W, 6h.
Step 3) in graphene oxide water solution concentration be 0.4-1mg/ml.
Step 5) in hydrazine hydrate ammonia spirit concentration be 0.005-0.015mg/ml.
Step 5) in mechanical agitation be temperature 80-100 DEG C, time 1-3h.
Step 6) in the graphene-based dielectric filler of multi-layer core-shell structure be 1.5-5 mass parts, rubber matrix be 100 mass
Part, vulcanizing agent is 0.5-2 mass parts.
Step 6) described in elastomer matrix be rubber；The rubber is natural rubber, silicone rubber, nitrile rubber, butyl
Rubber or acrylate rubber.
Step 6) described in vulcanizing agent be sulfur system and organic peroxide systems；The sulfur system is sulfur, oxygen
Change zinc and stearic acid；The organic peroxide systems are two (4- toluyls) peroxide, dibenzoyl peroxide, mistake
Oxidation diisopropylbenzene (DIPB), 2,5- dimethyl -2,5- two (tert-butyl hydroperoxide) hexane.
Step 6) in two-roll mill temperature be 20-60 DEG C；The elastomeric 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, from poly-dopamine bag
High dielectric ceramic particle is covered, in poly-dopamine surface grafting graphene oxide, is reduced using the method for electronation, is made appearance
The Graphene that easily reunites 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 consumption of Graphene, and the method very simple environmental protection；Graphene-based for multi-layer core-shell structure dielectric filler is filled
The dielectric constant of composite in rubber matrix, is improve, 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.
Partial enlarged drawings of the Fig. 1 (b) for 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- are high
Dielectric ceramic particle, 5- poly-dopamines, 6- Graphenes.
Specific embodiment
With reference to embodiment, the invention will be further described, but the scope not limited to this protected by the present invention.
Embodiment 1：
(1) by 20mg dopamine add 100ml water in, and add trishydroxymethylaminomethane solid (Tris) adjust go from
The pH of sub- water obtains dopamine solution to 8.5；
(2) barium titanate particles by 1g particle diameters for 30nm are added in aqueous dopamine solution, mechanical agitation 18h at 25 DEG C,
After reaction terminates, deionized water is diluted to neutrality, sucking filtration, vacuum drying, 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 are coated is added in graphene oxide water solution, machine at 25 DEG C
Tool stirs 16h, and deionized water is diluted to neutrality, vacuum filtration, vacuum drying, obtains the poly-dopamine of graphene oxide modification
Cladding high dielectric ceramic filler；
(5) 1.5g multi-layer core-shell structure graphite oxide thiazolinyl 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, deionized water are diluted to neutrality, vacuum filtration, vacuum drying, obtain
Arrive 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 graphene-based for 1.5g multi-layer core-shell structures dielectric
Filler is added gradually in nitrile rubber, is then gradually added into 0.5g cumyl peroxides, and cutter kneads, beats triangle bag, make
Mixing uniform, slice, after elastomeric compound parks 7-16h, 15Mpa on vulcanizing press, 160 DEG C of sulfuration 35min obtain multilayer core
Shell structure Graphene dielectric elastomer composite material.
(7) the multi-layer core-shell structure Graphene dielectric elastomer composite material to obtaining carries out dielectric properties, elastic modelling quantity
Test with electroluminescent deformation.Test result is shown in Table 1.
Dielectric constant is tested：Dielectric elastomer is tested at room temperature using U.S. Agilent E4980A impedances instrument, 20～
106Dielectric constant in frequency range.The dielectric constant for obtaining nitrile rubber dielectric elastomer composite material is shown in Table 1.
Elastic modelling quantity is tested：Stretching experiment is carried out using the puller system (3366) of Instron companies.Composite diaphragm quilt
The dumbbell shape batten of standard is cut into, thickness is in 1mm or so.At ambient temperature, with the rate of extension of 50mm/min to composite wood
Material batten carries out Mechanics Performance Testing, front for strain 5% corresponding stress-strain data is carried out linear fit and obtains elastic modelling quantity.
Electroluminescent deformation and breakdown strength test：Flexible electrode is sprayed with high-pressure spray gun in the both sides of dielectric elastomeric body thin film,
A diameter of 11mm of flexible electrode, electrode are put into after convection oven is dried and test.By bohr high voltage power supply (model 73030P)
Control applied voltage, while record change of shape of the electrode zone of dielectric elastomer under electrical field stimulation with digital camera.Electricity
Pressure is continuously increased, until composite is breakdown, the voltage and electroluminescent deformation amount when record punctures.Test result is shown in Table 1.
Embodiment 2
Preparation method except for the difference that adds dopamine consumption for 33mg, graphite in step (6) with embodiment 1 in step (1)
The consumption of thiazolinyl ceramic particle is 4.5g.Test result is shown in Table 1.
Embodiment 3
With embodiment 1, except for the difference that in step (6), the consumption of cumyl peroxide is 2g to preparation method.Test result
It is shown in Table 1.
Embodiment 4
With embodiment 1, except for the difference that in step (2), high dielectric ceramic particle is the Titanium Dioxide of particle diameter 30nm to preparation method
Particle, and addition is 0.6g.Rubber matrix is silicone rubber, and cross-linking agent is 0.5g2,5- dimethyl -2, bis- (t-butyl peroxies of 5-
Change) hexane.Test result is shown in Table 1.
Embodiment 5
With embodiment 4, except for the difference that in step (6), the consumption of graphene-based ceramic particle is 3.8g to preparation method.Test
The results are shown in Table 1.
Embodiment 6
Preparation method with embodiment 3, except for the difference that 2,5- dimethyl -2 in step (6), 5- bis- (tert-butyl hydroperoxide) oneself
The consumption of alkane is 2g.Test result is shown in Table 1.
Embodiment 7
With embodiment 1, except for the difference that in step (2), high dielectric ceramic particle is the magnoniobate of particle diameter 200nm to preparation method
Lead ceramic particle, and addition is 0.6g.Rubber matrix is butyl rubber, and cross-linking agent is 0.5g dibenzoyl peroxides.Test
The results are shown in Table 1.
Embodiment 8
With embodiment 7, except for the difference that in step (6), the consumption of graphene-based ceramic particle is 3.8g to preparation method.Test
The results are shown in Table 1.
Embodiment 9
With embodiment 5, except for the difference that in step (6), the consumption of dibenzoyl peroxide is 2g to preparation method.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 barium titanate particles of the 1.8g particle diameters for 30nm are gradually added
Enter in nitrile rubber, be then gradually added into 0.5g cumyl peroxides, cutter is kneaded, and beats triangle bag, be allowed to mixing uniformly,
Slice, after elastomeric compound parks 7-16h, 15Mpa on vulcanizing press, 160 DEG C of sulfuration 35min obtain Filled with Barium Titanate butyronitrile rubber
The dielectric elastomer of glue.
The test of dielectric properties, elastic modelling quantity and electroluminescent deformation is carried out to the dielectric elastomer for obtaining.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 barium titanate particles of the 1.8g particle diameters for 30nm are gradually added
Enter in nitrile rubber, be then gradually added into 0.5g cumyl peroxides, cutter is kneaded, and beats triangle bag, be allowed to mixing uniformly,
Slice, after elastomeric compound parks 7-16h, 15Mpa on vulcanizing press, 160 DEG C of sulfuration 35min obtain Graphene filled silicon rubber
Dielectric elastomer.
The test of dielectric properties, elastic modelling quantity and electroluminescent deformation is carried out to the dielectric elastomer for obtaining.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, graphene-based for minimal amount of multi-layer core-shell structure dielectric filler is filled into dielectric elastomer matrix
In, the dielectric constant of elastomer is significantly raised, can reach 83.7 under 100Hz, and maximum electroluminescent deformation is up to 39.4%, maintains
Low elastic modulus and dielectric loss, improve dielectric elastomer electric breakdown strength.
Claims (14)
1. the preparation method of the graphene-based dielectric elastomer composite material of a kind of multi-layer core-shell structure, it is characterised in that include with
Lower step：
1) pH to 8.5 of water is adjusted with trishydroxymethylaminomethane solid, is added dopamine, is obtained aqueous dopamine solution；
2) high dielectric ceramic particle is put in aqueous dopamine solution, mechanical agitation, after reaction terminates, deionized water is diluted to
Neutrality, sucking filtration, vacuum drying, obtain the poly-dopamine cladding high dielectric ceramic filler of solid-state；
3) by graphene oxide ultrasonic disperse in deionized water, graphene oxide water solution is obtained；
4) in graphene oxide water solution, poly-dopamine cladding high dielectric ceramic filler is added, mechanical agitation, reaction terminate
Afterwards, deionized water is diluted to neutrality, sucking filtration, vacuum drying, obtains multi-layer core-shell structure graphite oxide thiazolinyl dielectric filler；
5) multi-layer core-shell structure graphite oxide thiazolinyl dielectric filler is put in the ammonia spirit of hydrazine hydrate, mechanical agitation, reaction
After end, deionized water is diluted to neutrality, sucking filtration, vacuum drying, and the graphene-based dielectric filler of multi-layer core-shell structure is obtained；
6) graphene-based for multi-layer core-shell structure dielectric filler is added in rubber matrix, adds vulcanizing agent, in two-roll mill
Mixing is uniform, slice, elastomeric compound are parked, vulcanize on vulcanizing press, and the graphene-based dielectric elastomer of multi-layer core-shell structure is obtained
Composite.
2. preparation method according to claim 1, it is characterised in that step 1) in the concentration of aqueous dopamine solution be 1.2-
2mg/ml.
3. preparation method according to claim 1, it is characterised in that step 2) in high dielectric ceramic particle be nano barium titanate
Barium, nano titanium oxide, nanometer lead magnesio-niobate.
4. preparation method according to claim 1, it is characterised in that step 2) in high dielectric ceramic average particle size be
30-200nm.
5. preparation method according to claim 1, it is characterised in that step 2) and step 4) in mechanical agitation be temperature
25 DEG C of degree, time 15-25h.
6. preparation method according to claim 1, it is characterised in that step 3) in ultrasound condition be 800W, 6h.
7. preparation method according to claim 1, it is characterised in that step 3) in graphene oxide water solution concentration be
0.4-1mg/ml.
8. preparation method according to claim 1, it is characterised in that step 5) in the ammonia spirit concentration of hydrazine hydrate be
0.005-0.015mg/ml.
9. preparation method according to claim 1, it is characterised in that step 5) in mechanical agitation be temperature 80-100
DEG C, time 1-3h.
10. preparation method according to claim 1, it is characterised in that step 6) in graphene-based Jie of multi-layer core-shell structure
Electric filler is 1.5-5 mass parts, and rubber matrix is 100 mass parts, and vulcanizing agent is 0.5-2 mass parts.
11. preparation methoies according to claim 1, it is characterised in that step 6) described in elastomer matrix be rubber；Institute
Rubber is stated for natural rubber, silicone rubber, nitrile rubber, butyl rubber or acrylate rubber.
12. preparation methoies according to claim 1, it is characterised in that step 6) described in vulcanizing agent be sulfur system and
Organic peroxide systems；The sulfur system is sulfur, zinc oxide and stearic acid；The organic peroxide systems are two
(4- toluyls) peroxide, dibenzoyl peroxide, cumyl peroxide, the two (tert-butyl groups of 2,5- dimethyl -2,5-
Peroxidating) hexane.
13. preparation methoies according to claim 1, it is characterised in that step 6) in two-roll mill temperature be 20-60
℃；The elastomeric compound storage period is 7-16h；Conditions of vulcanization be pressure 15Mpa, 160 DEG C of temperature, time 35min.
The graphene-based dielectric elastomeric bluk recombination of the multi-layer core-shell structure of preparation method preparation described in 14. any one of claim 1-13
Material.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265762A (en) * | 2018-08-30 | 2019-01-25 | 北京石油化工学院 | A kind of core-shell structure silver-based heat-conductivity rubber composite material and preparation method thereof |
| 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 |
| CN112745559A (en) * | 2020-12-23 | 2021-05-04 | 河南工业大学 | Polymer dielectric elastomer and preparation method and application thereof |
| CN112759807A (en) * | 2021-01-18 | 2021-05-07 | 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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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103183847A (en) * | 2013-04-12 | 2013-07-03 | 北京化工大学 | Graphene elastomer nano composite material with high dielectric constant and low dielectric loss and preparation method thereof |
| CN104031297A (en) * | 2014-07-03 | 2014-09-10 | 北京化工大学 | Graphene-based dielectric elastomer composite material and preparing method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103183847A (en) * | 2013-04-12 | 2013-07-03 | 北京化工大学 | Graphene elastomer nano composite material with high dielectric constant and low dielectric loss and preparation method thereof |
| CN104031297A (en) * | 2014-07-03 | 2014-09-10 | 北京化工大学 | Graphene-based dielectric elastomer composite material and preparing method thereof |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109265762A (en) * | 2018-08-30 | 2019-01-25 | 北京石油化工学院 | A kind of core-shell structure silver-based heat-conductivity rubber composite material and preparation method thereof |
| 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 |
| CN112745559A (en) * | 2020-12-23 | 2021-05-04 | 河南工业大学 | Polymer dielectric elastomer and preparation method and application thereof |
| CN112745559B (en) * | 2020-12-23 | 2023-02-17 | 河南工业大学 | Polymer dielectric elastomer and preparation method and application thereof |
| CN112759807A (en) * | 2021-01-18 | 2021-05-07 | 中北大学 | High-thermal-conductivity three-dimensional graphene oxide composite functional particle modified natural rubber and preparation method 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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