CN103146179B - Polyurethane elastomer composite material with low modulus and high dielectric constant, and preparation method of composite material - Google Patents
Polyurethane elastomer composite material with low modulus and high dielectric constant, and preparation method of composite material Download PDFInfo
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- CN103146179B CN103146179B CN201310111326.7A CN201310111326A CN103146179B CN 103146179 B CN103146179 B CN 103146179B CN 201310111326 A CN201310111326 A CN 201310111326A CN 103146179 B CN103146179 B CN 103146179B
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- elastomer
- polyurethane elastomer
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- 229920003225 polyurethane elastomer Polymers 0.000 title claims abstract description 44
- 239000002131 composite material Substances 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229920001971 elastomer Polymers 0.000 claims abstract description 9
- 239000000806 elastomer Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 36
- 239000011159 matrix material Substances 0.000 claims description 28
- 239000000945 filler Substances 0.000 claims description 26
- -1 polyoxyethylene Polymers 0.000 claims description 24
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 20
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 20
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical group C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- 229920002635 polyurethane Polymers 0.000 claims description 12
- 239000004814 polyurethane Substances 0.000 claims description 12
- 229920002725 thermoplastic elastomer Polymers 0.000 claims description 10
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 8
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 8
- 239000002904 solvent Substances 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 6
- 238000009423 ventilation Methods 0.000 claims description 6
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 4
- 235000011187 glycerol Nutrition 0.000 claims description 4
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 239000000203 mixture Substances 0.000 claims description 2
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 2
- 229920002595 Dielectric elastomer Polymers 0.000 abstract description 25
- 239000000463 material Substances 0.000 abstract description 10
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 9
- 239000001257 hydrogen Substances 0.000 abstract description 9
- 230000000694 effects Effects 0.000 abstract description 3
- 238000005516 engineering process Methods 0.000 abstract description 3
- 230000008859 change Effects 0.000 abstract description 2
- 230000003993 interaction Effects 0.000 abstract description 2
- 230000010287 polarization Effects 0.000 abstract description 2
- 125000004435 hydrogen atom Chemical group [H]* 0.000 abstract 1
- 239000004014 plasticizer Substances 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 10
- 238000005530 etching Methods 0.000 description 5
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 4
- 241000209094 Oryza Species 0.000 description 4
- 235000007164 Oryza sativa Nutrition 0.000 description 4
- 239000000919 ceramic Substances 0.000 description 4
- 230000005684 electric field Effects 0.000 description 4
- 238000009434 installation Methods 0.000 description 4
- 235000009566 rice Nutrition 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- 239000002041 carbon nanotube Substances 0.000 description 3
- 229910021393 carbon nanotube Inorganic materials 0.000 description 3
- 229920002981 polyvinylidene fluoride Polymers 0.000 description 3
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 description 2
- 229910002113 barium titanate Inorganic materials 0.000 description 2
- 239000011231 conductive filler Substances 0.000 description 2
- 150000003384 small molecules Chemical class 0.000 description 2
- 239000004902 Softening Agent Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 235000013409 condiments Nutrition 0.000 description 1
- 239000004020 conductor Substances 0.000 description 1
- 229920000547 conjugated polymer Polymers 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- 229920001746 electroactive polymer Polymers 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000004945 silicone rubber Substances 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a polyurethane elastomer composite material with a low modulus and a high dielectric constant, and a preparation method of the composite material, and belongs to the technical field of dielectric elastomer preparation. The composite material is added with small organic molecules which have a low dielectric constant and can form a hydrogen bond with a hydrogen proton, and the small organic molecules exist at a molecular level in the material so as to break down the interaction force among the molecular chains of an elastomer and change the movement capability and polarization capability of the molecular chains, and therefore, a dielectric elastomer composite material achieves a high dielectric effect. In addition, the added small organic molecules play a plasticizer role, thereby lowering the modulus of the composite material. The polyurethane elastomer composite material with the low modulus (2.10-0.23MPa) and the high dielectric constant (18-3500) can generate high electro-deformation under a very low outer field voltage, and the problem that the dielectric elastomer in the traditional method needs a high voltage to generate high electro-deformation is solved. Besides, the preparation method is simple, easy to operate, and easy to control in technology.
Description
Technical field:
The invention belongs to dielectric elastomer preparing technical field, particularly a kind of polyurethane elastomer molecular composite material and preparation method thereof of low modulus high-k.
Technical background:
Dielectric elastomer has that electroluminescent deformation is large, fast response time, energy density are high, modulus is low, electromechanical coupling factor is high and the advantage such as principle of work is simple.Therefore, the research and development of dielectric elastomer driver becomes focus nearly ten years.But the requirement of dielectric elastomer driver to high driving voltage (100kv/mm) greatly limit its application, particularly biomedical sector in some field.Therefore, dielectric elastomer be developed into the micro-drive technology of dependable performance, its key is the driving voltage reducing dielectric elastomer, makes it under lower electric field, produce enough large deformation.
The principle of work of dielectric elastomer driver can be formulated:
(in formula: S
zfor the deformation quantity of thickness direction; ε and ε
0be respectively relative permittivity and the permittivity of vacuum (8.85 × l of dielectric elastomer
-12f/m); E is for applying strength of electric field; Y is elastomeric Young's modulus) (RonPelrine, etal.High-speedelectricallyactuatedelastomerswithstrains greaterthan100%.Science, 2000.287:p.836-839.).
As can be seen from formula, when keeping SZ constant, wanting to reduce driving voltage, can reach by improving specific inductivity and reducing modulus.Improve specific inductivity and reduce modulus and become dielectric elastomer driver field problem demanding prompt solution.Elastomerics has snappiness, filling capacity that snappiness is good and high, but most of elastomerics polarity is little, and specific inductivity (ε) is low, and external electric field induction is more weak, can not directly as electroactive polymer.Currently mainly contain two kinds of methods to obtain the dielectric elastomer of high-k: in the middle of polymeric matrix, one, fill high dielectric ceramic to improve the specific inductivity of dielectric elastomer; Two, the specific inductivity of dielectric elastomer is improved by the conjugated polymers of filled conductive filler or high degree of polarization.But these two kinds of methods have weak point.
First, although stupalith has high-k (up to several thousand), stupalith bad mechanical property, and can not compatible current circuit integrated technology.After elastomerics adds high dielectric ceramic, although specific inductivity increases, the fragility of material increases simultaneously, and modulus obviously raises, or needs can produce deformation at higher voltages.Chinese patent application " dielectric elastomer material and preparation method thereof " (number of patent application 200810064238.5) proposes and adopts relaxor ferroelectric ceramics material and silicone rubber solution to be mixed and made into dielectric elastomer, and its specific inductivity can reach 80-360.But, because make the modulus of matrix material greatly increase a large amount of adding of ceramic powder, make dielectric elastomer need could produce deformation under very high voltage, strongly limit application.
And conductive filler material is when reaching certain loading level, the specific inductivity of dielectric elastomer increases sharply, and occur exceeding and ooze phenomenon, the dielectric loss of material also increases greatly, reduces electromechanical performance gain factor, is unfavorable for that dielectric elastomer produces large deformation.Chinese patent application " high-dielectric composite material containing carbon nanotube and preparation method thereof " (number of patent application: 03104776.9) adopt carbon nanotube CNT, barium titanate BaTiO
3with the matrix material that organic polyvinylidene difluoride (PVDF) (PVDF) is made, its specific inductivity can up to 450.But high-k depends on carbon nanotube CNT and barium titanate BaTiO
3add, but the volumetric usage of these fillers must control within the specific limits, otherwise when the electric conductivity of matrix material increases above the excess effusion value of material, can there is the transformation of isolator to conductor in matrix material.
Summary of the invention:
The object of this invention is to provide polyurethane elastomer molecular composite material of a kind of low modulus high-k and preparation method thereof.
With previous methods unlike, the present invention is not the specific inductivity that dielectric filler by adding high-k in dielectric elastomer improves dielectric elastomer, but by add low-k, can with the organic molecule of proton hydrogen evolution hydrogen bond, organic molecule is made to be present in material with molecular level, destroy the Interaction Force of elastomer molecules chain, change motor capacity and the polarizability of itself molecular chain, and then make dielectric elastomer composite material reach a kind of effect of high dielectric.Simultaneously organic molecule add the effect also serving softening agent, the modulus of matrix material is reduced.The polyurethane elastomer molecular composite material of this low modulus high-k can obtain high electroluminescent deformation under very low outer field voltage, solves the difficult problem that traditional method dielectric elastomerics needs to produce under high voltages large electroluminescent deformation.
Polyurethane elastomer molecular composite material of the present invention, its composition comprises: the elastomer matrix of 100 mass parts, the organic molecule filler of 5-50 mass parts.
Above-mentioned elastomer matrix is: Polyurethane Thermoplastic Elastomer.
Above-mentioned organic molecule filler is: polyoxyethylene glycol, glycerine or pyridine.
The molecular weight of described polyoxyethylene glycol is 200-15000.
The preparation method of above-mentioned polyurethane elastomer molecular composite material is: the elastomer matrix of 100 mass parts be dissolved in the good solvent of 1000-2000 mass parts, be stirred to dissolve under 40-80 DEG C of condition and obtain clear solution, then the organic molecule filler of 5-50 mass parts is added, continue heated and stirred to dissolving completely, solution is poured in mould, 4-7 hour is placed, obtained polyurethane elastomer molecular composite material under ventilation condition.
Described good solvent is tetrahydrofuran (THF), acetone, dimethyl formamide or N-Methyl pyrrolidone.
The specific inductivity at 1 hz of above-mentioned obtained polyurethane elastomer molecular composite material is 18-3500, and Young's modulus is 2.10-0.23Mpa.
The present invention selects polyurethane elastomer to be, containing a large amount of amino-NH-and carbonyl-COO-in urethane, both formed hydrogen bond at polyurethane molecular interchain as the reason of matrix, can form hydrogen bond again with the organic molecule filler added.
The consumption of organic molecule filler of the present invention can not be too high, otherwise easily occur the phenomenon that condiment is reunited in the composite, and if small molecules amount of filler too large, the matrix material obtained can because of too soft and cannot film forming.
The present invention by add in polyurethane elastomer can with the organic molecule filler of proton hydrogen evolution hydrogen bond, destroy the hydrogen bond in urethane, itself and urethane is made to form new hydrogen bond, filler is present in matrix material with molecular form, improve motor capacity and the polarizability of polyurethane molecular chain, obtain the molecular composite material with high-k.The specific inductivity of urethane is under 15(1Hz) left and right, the specific inductivity of small molecules filler is about 14, and the specific inductivity of the dielectric elastomer that the present invention obtains is about 3500, improves nearly 240 times.Be greatly improved simultaneously at specific inductivity, the modulus of matrix material does not only increase, also along with the increase of filler, in the trend reduced gradually.The molecular composite material of such low modulus (2.10-0.23MPa) high-k (18-3500) greatly reduces the requirement of material to strength of electric field, can be applied to the dielectric elastomer lower to voltage request and drive field, be a kind of novel advanced functional elastomer material.Simultaneously simple, easy to operate, the technique of preparation method easily controls.
Accompanying drawing illustrates:
Fig. 1 is the brittle failure face etching of the polyurethane elastomer molecular composite material of the low modulus high-k that embodiment 1-4 obtains and the scanning electron microscope (SEM) photograph of non-etched portions.(a1)-embodiment 1 does not etch brittle failure face, and (a2)-embodiment 1 etches brittle failure face; (b1)-embodiment 2 does not etch brittle failure face, and (b2)-embodiment 2 etches brittle failure face; (c1)-embodiment 3 does not etch brittle failure face, and (c2)-embodiment 3 etches brittle failure face; (d1)-embodiment 4 does not etch brittle failure face, and (d2)-embodiment 4 etches brittle failure face.
Embodiment:
Below by embodiment, the present invention will be further described, but not as limiting the scope of the invention.
Embodiment 1:
With polyurethane elastomer as matrix, using polyoxyethylene glycol as organic molecule filler, prepare the polyurethane elastomer molecular composite material of low modulus high-k, concrete operation step is: 100g Polyurethane Thermoplastic Elastomer is dissolved in the tetrahydrofuran (THF) of 1500g by (1), and 66 DEG C of heated and stirred are dissolved to clear solution; (2) molecular weight adding 5g is 600 polyoxyethylene glycol small molecules fillers, continues heated and stirred and dissolves completely to polyoxyethylene glycol; (3) solution is poured in the square mould that thickness is 2cm, length is 8cm, place 6 hours in ventilation installation, after the solvent in solution volatilizees completely, the polyurethane elastomer molecular composite material of obtained low modulus high-k.
The Polyurethane Thermoplastic Elastomer of above-mentioned use is
soft45A PAUR elastomerics.
The mensuration of specific inductivity: first, is cut into the disk of diameter 25mm rice by the polyurethane elastomer molecular composite material of obtained low modulus high-k, then adopt German Novocntrol Alpha-A high performance frequency analyser test at room temperature, 10
-2-10
6specific inductivity in the range of frequency of Hz, the specific inductivity data obtained are in table 1.
As shown in Figure 1, can be illustrated with comparing of non-etch profile by the etching of the polyurethane elastomer molecular composite material to obtained low modulus high-k, polyoxyethylene glycol does not form reunion in the middle of polyurethane elastomer matrix, but is present in the middle of matrix with molecular level.
Embodiment 2:
With polyurethane elastomer as matrix, using polyoxyethylene glycol as organic molecule filler, prepare the polyurethane elastomer molecular composite material of low modulus high-k, concrete operation step is: 100g Polyurethane Thermoplastic Elastomer is dissolved in 1800g tetrahydrofuran (THF) by (1), and 66 DEG C of heated and stirred are dissolved to clear solution; (2) molecular weight adding 15g is 600 polyoxyethylene glycol small molecules fillers, continues heated and stirred and dissolves completely to polyoxyethylene glycol; (3) solution is poured in the square mould that thickness is 2cm, length is 8cm, place 6 hours in ventilation installation, after the solvent in solution volatilizees completely, the polyurethane elastomer molecular composite material of obtained low modulus high-k.
The Polyurethane Thermoplastic Elastomer of above-mentioned use is
soft45A PAUR elastomerics.
The mensuration of specific inductivity: first, is cut into the disk of diameter 25mm rice by the polyurethane elastomer molecular composite material of obtained low modulus high-k, then adopt German Novocntrol Alpha-A high performance frequency analyser test at room temperature, 10
-2-10
6specific inductivity in the range of frequency of Hz, the specific inductivity data obtained are in table 1.
As shown in Figure 1, can be illustrated with comparing of non-etch profile by the etching of the polyurethane elastomer molecular composite material to obtained low modulus high-k, polyoxyethylene glycol does not form reunion in the middle of polyurethane elastomer matrix, but is present in the middle of matrix with molecular level.
Embodiment 3:
With polyurethane elastomer as matrix, using polyoxyethylene glycol as organic molecule filler, prepare the polyurethane elastomer molecular composite material of low modulus high-k, concrete operation step is: 100g Polyurethane Thermoplastic Elastomer is dissolved in 2000g acetone by (1), and 56 DEG C of heated and stirred are dissolved to clear solution; (2) molecular weight adding 30 mass parts is 200 polyoxyethylene glycol small molecules fillers, continues heated and stirred and dissolves completely to polyoxyethylene glycol; (3) solution is poured in the square mould that thickness is 2cm, length is 8cm, place 6 hours in ventilation installation, after the solvent in solution volatilizees completely, the polyurethane elastomer molecular composite material of obtained low modulus high-k.
The Polyurethane Thermoplastic Elastomer of above-mentioned use is
soft45A PAUR elastomerics.
The mensuration of specific inductivity: first, is cut into the disk of diameter 25mm rice by the polyurethane elastomer molecular composite material of obtained low modulus high-k, then adopt German Novocntrol Alpha-A high performance frequency analyser test at room temperature, 10
-2-10
6specific inductivity in the range of frequency of Hz, the specific inductivity data obtained are in table 1.
As shown in Figure 1, can be illustrated with comparing of non-etch profile by the etching of the polyurethane elastomer molecular composite material to obtained low modulus high-k, polyoxyethylene glycol does not form reunion in the middle of polyurethane elastomer matrix, but is present in the middle of matrix with molecular level.
Embodiment 4:
With polyurethane elastomer as matrix, using polyoxyethylene glycol as organic molecule filler, prepare the polyurethane elastomer molecular composite material of low modulus high-k, concrete operation step is: 100g Polyurethane Thermoplastic Elastomer is dissolved in 2000g acetone by (1), and 56 DEG C of heated and stirred are dissolved to clear solution; (2) adding 50g molecular weight is 1000 polyoxyethylene glycol small molecules fillers, continues heated and stirred and dissolves completely to polyoxyethylene glycol; (3) solution is poured in the square mould that thickness is 2cm, length is 8cm, place 6 hours in ventilation installation, after the solvent in solution volatilizees completely, the polyurethane elastomer molecular composite material of obtained low modulus high-k.
The Polyurethane Thermoplastic Elastomer of above-mentioned use is
soft45A PAUR elastomerics.
The mensuration of specific inductivity: first, is cut into the disk of diameter 25mm rice by the polyurethane elastomer molecular composite material of obtained low modulus high-k, then adopt German Novocntrol Alpha-A high performance frequency analyser test at room temperature, 10
-2~ 10
6specific inductivity in the range of frequency of Hz, the specific inductivity data obtained are in table 1.
As shown in Figure 1, can be illustrated with comparing of non-etch profile by the etching of the polyurethane elastomer molecular composite material to obtained low modulus high-k, polyoxyethylene glycol does not form reunion in the middle of polyurethane elastomer matrix, but is present in the middle of matrix with molecular level.
Embodiment 5:
Preparation method and testing method with example 1, unlike glycerine organic molecule filler being replaced with 5g.Test result is in table 2.
Embodiment 6:
Preparation method and testing method with example 1, unlike glycerine organic molecule filler being replaced with 50g.Test result is in table 2.
Comparative example 7:
Preparation method and testing method, with example 1, do not add organic molecule filler unlike in preparation process, namely pure polyurethane elastomer.Test result is in table 1.
Table 1
Table 2
Claims (4)
1. the preparation method of a polyurethane elastomer molecular composite material, it is characterized in that, its concrete preparation process is: the elastomer matrix of 100 mass parts be dissolved in the good solvent of 1000-2000 mass parts, be stirred to dissolve under 40-80 DEG C of condition and obtain clear solution, then add the organic molecule filler of 5-50 mass parts, continuing heated and stirred to dissolving completely, solution being poured in mould, 4-7 hour is placed, obtained polyurethane elastomer molecular composite material under ventilation condition.
2. the polyurethane elastomer molecular composite material for preparing of method according to claim 1, it is characterized in that, its composition comprises: the elastomer matrix of 100 mass parts, the organic molecule filler of 5-50 mass parts; Described elastomer matrix is: Polyurethane Thermoplastic Elastomer; Described organic molecule filler is: polyoxyethylene glycol, glycerine or pyridine; The molecular weight of described polyoxyethylene glycol is 200-15000.
3. preparation method according to claim 1, is characterized in that, described good solvent is tetrahydrofuran (THF), acetone, dimethyl formamide or N-Methyl pyrrolidone.
4. the polyurethane elastomer molecular composite material for preparing of method according to claim 1, is characterized in that, obtained polyurethane elastomer molecular composite material at 1 hz specific inductivity is 18-3500, and Young's modulus is 2.10-0.23Mpa.
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| CN104088150B (en) * | 2014-07-08 | 2016-03-02 | 北京化工大学 | A kind of interlocking structure full stress-strain dielectric elastomer material and preparation method thereof |
| WO2016176350A1 (en) * | 2015-04-27 | 2016-11-03 | The Regents Of The University Of Michigan | Durable icephobic surfaces |
| KR102042873B1 (en) * | 2015-09-25 | 2019-11-08 | 주식회사 엘지화학 | Pdms-urethane film for display and the manufacturing method thereby |
| KR102042302B1 (en) * | 2015-09-25 | 2019-11-07 | 주식회사 엘지화학 | Polyurethane film for display and the manufacturing method thereby |
| CN108034227A (en) * | 2017-12-12 | 2018-05-15 | 东莞市雄林新材料科技股份有限公司 | One kind has high dielectric property and durothermic TPU film and preparation method thereof |
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| CN101899177B (en) * | 2010-07-09 | 2011-08-10 | 北京化工大学 | High dielectric constant and low-modulus dielectric elastomer material and preparation method thereof |
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