CN105622871A - Crosslinked fluorine polymer based dielectric elastomer compound material and preparation method therefor - Google Patents
Crosslinked fluorine polymer based dielectric elastomer compound material and preparation method therefor Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F299/00—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers
- C08F299/02—Macromolecular compounds obtained by interreacting polymers involving only carbon-to-carbon unsaturated bond reactions, in the absence of non-macromolecular monomers from unsaturated polycondensates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F8/00—Chemical modification by after-treatment
- C08F8/42—Introducing metal atoms or metal-containing groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2800/00—Copolymer characterised by the proportions of the comonomers expressed
- C08F2800/20—Copolymer characterised by the proportions of the comonomers expressed as weight or mass percentages
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2810/00—Chemical modification of a polymer
- C08F2810/20—Chemical modification of a polymer leading to a crosslinking, either explicitly or inherently
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2810/00—Chemical modification of a polymer
- C08F2810/50—Chemical modification of a polymer wherein the polymer is a copolymer and the modification is taking place only on one or more of the monomers present in minority
Abstract
The invention discloses a crosslinked fluorine polymer based dielectric elastomer compound material and a preparation method therefor. The compound material comprises the following components in parts by mass: 60-90 parts of a fluorine polymer matrix, 8-40 parts of a functional crosslinker and 1-3 parts of a catalyst. The preparation method comprises the steps of adding 50-120 parts of a solvent into a flask, then adding 60-90 parts of an internal double bond-containing polyvinylidene fluoride copolymer, and performing strong stirring for 30 minutes; dropwise adding 8-40 parts of functional crosslinker molecules with strong stirring, and continuing to stir at the room temperature for 20-30 minutes; then dropwise adding 1-3 parts of the catalyst and stirring for reaction at 40-60 DEG C for 8-10 hours; after cooling to the room temperature, filtering a reaction solution, performing tape casting on a glass flat plate, putting the glass flat plate into a uniform heat environment, gradually heating to 60-100 DEG C, drying for 4-8 hours to remove the solvent, thereby obtaining a crosslinked fluorine polymer based dielectric elastomer compound material membrane on the glass flat plate. According to the method, the low-driving-voltage and high-electrodeformation total-organic dielectric elastomer compound material can be obtained by adopting the self-synthesized internal double bond-containing polyvinylidene fluoride copolymer as a matrix and the functional crosslinker molecules as a crosslinking unit.
Description
Technical field
The present invention relates to a kind of dielectric elastomer material, particularly to a kind of cross-linking type fluoropolymer base dielectric elastomer composite material and preparation method thereof.
Background technology
Novel high-performance electric drive material can convert electrical energy into mechanical energy, has a wide range of applications in intelligent drives and biologic medical field. Compared with piezoelectric ceramics and memorial alloy, electroactive polymer has the advantage such as low cost, structure easy-regulating, causes special concern.
Dielectric elastomer is the elastomeric material with high-k (K), electrode coated in dielectric elastomer film upper and lower surface and after applying external electric field, the deformation of about 10%��40% can be occurred to change its shape or volume, this process is along with the generation of stress and strain, thus converting electrical energy into mechanical energy. Dielectric elastomer has electromechanical conversion efficiency height, deformation is big and responds the Good All-around Properties such as rapid, has practical application in driver, electromotor and sensor etc.
For dielectric elastomer, its electroluminescent deformation size be proportional to dielectric constant K and be added in electric field intensity thereon square, therefore, improve dielectric constant K and breakdown strength EbThe two index is to improve the important channel of dielectric elastomer executor's efficiency. Meanwhile, the elastic modelling quantity Y of material also contributes to the size of electroluminescent deformation, and usual elastic modelling quantity is more little, and it is more little that material deforms upon required stress, and required driving voltage is also more low. Therefore, preparation is provided simultaneously with the elastomeric material of high dielectric constant and relatively low elastic modulus, is obtain excellent performance, the i.e. key point of the dielectric elastomer material of low driving voltage, big electroluminescent deformation characteristic.
Kynoar based copolymer material has higher dielectric constant values, but its glass transition temperature is higher, and elastic mould value is also relatively big, can not obtain bigger electroluminescent deformation directly as dielectric elastomer when therefore using. How carrying out composite modified to it is the study hotspot of association area. General, by adding inorganic high-permitivity ceramics to the K value that can improve composite in polymeric matrix, but owing to the elastic modelling quantity of composite also can increase simultaneously, therefore drive deformation increase inconspicuous; Secondly, the K value of composite can be greatly improved by adding organic conductor, but the increase of conductivity makes the E of compositebBeing substantially reduced, leakage conductance loss simultaneously increases, and causes that deformation increase is also inconspicuous.
Summary of the invention
In order to overcome the existing deficiency that dielectric elastomer material driving voltage is higher, electroluminescent deformation is less, it is an object of the invention to provide a kind of cross-linking type fluoropolymer base dielectric elastomer composite material and preparation method thereof, the method adopts the Kynoar based copolymer containing internal double bond synthesized voluntarily to be matrix, functional cross-link agent molecule is crosslink unit, it is possible to obtain low driving voltage, big electroluminescent deformation full stress-strain dielectric elastomer composite material; The dielectric elastomer material that the present invention relates to has relatively large deformation/displacement (about 30-300%) under low electric field, is expected to be applied to prepare the machine-electricity conversion driver parts such as artificial-muscle, micro-fluidic pump valve, speaker and sensitive tactile display.
In order to achieve the above object, technical scheme and approach are:
A kind of cross-linking type fluoropolymer base dielectric elastomer composite material, its raw material components includes according to the mass fraction: the catalyst of the fluoropolymer matrix of 60-90 part, the functional cross-link agent of 8-40 part weight and 1-3 part.
Described fluoropolymer matrix is Kynoar (PVDF) based copolymer, including by but be not limited to vinylidene (VDF) and trifluoro-ethylene (TrFE), CTFE (CTFE), tetrafluoroethene (TFE), hexafluoropropene (HFP), perfluoroethylene-propylene (copolymer) (FEP), hexafluoro-isobutene (TrFE), perfluoroalkyl vinyl ether (TrFE) monomer, two or more monomer therein by copolyreaction prepare; The copolymer that copolyreaction prepares includes gathering (vinylidene-CTFE) copolymer, poly-(vinylidene-trifluoro-ethylene-CTFE) copolymer, poly-(biasfluoroethylene-hexafluoropropylene) copolymer etc.; Fluoropolymer matrix also can be made up of one or more polymer in above-mentioned copolymer.
Described functional cross-link agent molecule, its molecular weight is between 100��100000, cross-linker molecules main chain is flexible low modulus structure, and molecular structure of chemistry includes but not limited to polysiloxanes, polyacrylate, polyisoprene, polyurethane, polyether-based polymers and derivant thereof. Cross-linker molecules also comprises and with the polar group of the internal double bond generation additive reaction in fluoropolymer matrix, can include but not limited to sulfydryl, amino, carboxyl etc.
Described catalyst, it is the little molecule containing activity hydroxy or macromole, for accelerating the chemical crosslink reaction between function cross-linker molecules and fluoropolymer matrix, it is typically include but is not limited to one or more in the hydroxy-containing compounds such as water, ethanol, isopropanol.
The preparation method of a kind of cross-linking type fluoropolymer base dielectric elastomer composite material, comprises the steps:
A () adds 50-120 part solvent in flask, solvent is intensive polar solvent, including ethyl acetate or oxolane or dimethylformamide, is subsequently adding the 60-90 part Kynoar based copolymer containing internal double bond, strong stirring 30min;
B (), after (a) dissolves, is added dropwise over 8-40 part functional cross-link agent molecule under strong stirring, continue stirring 20-30min under room temperature; Then 1-3 part catalyst it is gradually dropped, stirring reaction 8-10h at 40-60 DEG C;
C () is down to after room temperature until (b), reaction solution is filtered, curtain coating on glass plate immediately, glass plate is placed in uniform thermal environment, progressively it is warming up to 60-100 DEG C, dry 4-8h removes solvent, and namely glass plate prepares cross-linking type fluoropolymer base dielectric elastomer composite material film;
Described addition number is mass fraction.
The beneficial outcomes of the present invention is: carry out cross-linking reaction owing to employing has the flexible low modulus cross-linker molecules of functional group with the high-k fluo-copolymer containing internal double bond, the composite of preparation is not only benefited from the functional group (such as amino, carboxyl, sulfydryl etc.) introducing polarity and fluoropolymer K value is improved, and due to the interval action of flexible chain, the elastic mould value making composite is substantially reduced, and electroluminescent deformation/shift value is greatly improved.
Accompanying drawing explanation
Fig. 1 is for amino silicone functional cross-link agent molecule, prepare the process schematic of cross-linking type fluoropolymer base dielectric elastomer composite material, including the addition-crosslinked chemical process containing internal double bond fluo-copolymer of the synthesis containing internal double bond fluo-copolymer and the cross-linker molecules containing amino functional.
Fig. 2 is the machine-electricity conversion performance table of embodiment 1 dielectric elastic composite.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is elaborated.
Embodiment one
Its raw material components of the present embodiment calculates the catalyst including the fluoropolymer matrix of 90 parts, the functional cross-link agent of 9 parts of weight and 1 part according to the mass fraction.
The present embodiment preparation method, comprises the steps: addition 100ml ethyl acetate in the flask of 200ml, is subsequently adding the 9g poly-(vinylidene-CTFE) containing internal double bond, strong stirring 30min; After to be dissolved, under strong stirring, it is added dropwise over 0.9g amino silicone functional cross-link agent molecule (molecular weight is about 2000), under room temperature, continues stirring 30min; Then 0.1g catalyst water it is gradually dropped, stirring reaction 8h at 60 DEG C; After being down to room temperature, being filtered by reaction solution, curtain coating on glass plate immediately, glass plate is placed in uniform thermal environment, is progressively warming up to 80 DEG C, and dry 8h removes solvent. Namely glass plate prepares amino silicone addition-crosslinked fluoropolymer base dielectric elastomer composite material film.
After tested, the dielectric constant values of made cross-linking type fluoropolymer base dielectric elastomer composite material film is 16, and deformation values improves about 300% than uncrosslinked fluoropolymer. Fig. 2 lists the machine-electricity conversion performance test value of the molecule crosslinked fluoropolymer base dielectric elastomer composite material of different content amino silicone, including dielectric constant, Young's modulus, machine-electricity transition sensitive degree and deformation/shift value. Note: a-dielectric constant 100Hz; B-Young's modulus, DMA tests; *-dynamo-electric sensitivity; ��-deformation/shift value.
Embodiment two
Its raw material components of the present embodiment calculates the catalyst including the fluoropolymer matrix of 60 parts, the functional cross-link agent of 38 parts of weight and 2 parts according to the mass fraction.
The present embodiment preparation method, comprises the steps: addition 80ml dimethylformamide in the flask of 200ml, is subsequently adding the 6g poly-(vinylidene-trifluoro-ethylene-CTFE) containing internal double bond, strong stirring 30min; After to be dissolved, under strong stirring, it is added dropwise over 3.8g sulfydryl polyacrylate functional cross-link agent molecule (molecular weight is about 20000), under room temperature, continues stirring 30min; Then 0.2g catalyst ethanol it is gradually dropped, stirring reaction 8h at 50 DEG C; After being down to room temperature, being filtered by reaction solution, curtain coating on glass plate immediately, glass plate is placed in uniform thermal environment, is progressively warming up to 90 DEG C, and dry 8h removes solvent. Namely glass plate prepares polyacrylate cross-linking modified fluoropolymer base dielectric elastomer composite material film.
After tested, the dielectric constant values of made full stress-strain fluoropolymer base dielectric elastomer composite material film is 12, and deformation values improves about 110% than uncrosslinked fluoropolymer matrix.
Embodiment three
Its raw material components of the present embodiment includes according to the mass fraction: the fluoropolymer matrix of 77 parts, the functional cross-link agent of 20 parts of weight and 3 parts catalyst.
The present embodiment preparation method, comprises the steps: addition 120ml oxolane in the flask of 200ml, is subsequently adding the 7.7g poly-(biasfluoroethylene-hexafluoropropylene) containing internal double bond, strong stirring 30min; After to be dissolved, under strong stirring, it is gradually added 2g polyisoprene functional cross-link agent molecule (molecular weight is about 50000), under room temperature, continues stirring 30min; Then 0.3g catalyst benzoyl peroxide it is gradually dropped, stirring reaction 8h at 40 DEG C; After being down to room temperature, being filtered by reaction solution, curtain coating on glass plate immediately, glass plate is placed in uniform thermal environment, is progressively warming up to 60 DEG C, and dry 4h removes solvent. Namely glass plate prepares polyisoprene crosslinking fluoropolymer base dielectric elastomer composite material film.
After tested, the dielectric constant values of made cross-linking type fluoropolymer base dielectric elastomer composite material film is 15, and deformation values improves about 150% than uncrosslinked fluoropolymer matrix.
Claims (2)
1. a cross-linking type fluoropolymer base dielectric elastomer composite material, its raw material components includes according to the mass fraction: the catalyst of the fluoropolymer matrix of 60-90 part, the functional cross-link agent of 8-40 part weight and 1-3 part;
Described fluoropolymer matrix is Kynoar (PVDF) based copolymer, including by but be not limited to vinylidene (VDF) and trifluoro-ethylene (TrFE), CTFE (CTFE), tetrafluoroethene (TFE), hexafluoropropene (HFP), perfluoroethylene-propylene (copolymer) (FEP), hexafluoro-isobutene (TrFE), perfluoroalkyl vinyl ether (TrFE) monomer, two or more monomer therein by copolyreaction prepare; The copolymer that copolyreaction prepares includes gathering (vinylidene-CTFE) copolymer, poly-(vinylidene-trifluoro-ethylene-CTFE) copolymer, poly-(biasfluoroethylene-hexafluoropropylene) copolymer etc.; Fluoropolymer matrix also can be made up of one or more polymer in above-mentioned copolymer;
Described functional cross-link agent molecule, its molecular weight is between 100-100000, cross-linker molecules main chain is flexible low modulus structure, and molecular structure of chemistry includes but not limited to polysiloxanes, polyacrylate, polyisoprene, polyurethane, polyether-based polymers and derivant thereof; Cross-linker molecules also comprises and with the polar group of the internal double bond generation additive reaction in fluoropolymer matrix, can include but not limited to sulfydryl, amino, carboxyl;
Described catalyst, it is the little molecule containing activity hydroxy or macromole, for accelerating the chemical crosslink reaction between function cross-linker molecules and fluoropolymer matrix, it is typically include but is not limited to one or more in the hydroxy-containing compounds such as water, ethanol, isopropanol.
2., based on the preparation method of cross-linking type fluoropolymer base dielectric elastomer composite material a kind of described in claim 1, comprise the steps:
A () adds 50-120 part solvent in flask, solvent is intensive polar solvent, including ethyl acetate or oxolane or dimethylformamide, is subsequently adding the 60-90 part Kynoar based copolymer containing internal double bond, strong stirring 30min;
B (), after (a) dissolves, is added dropwise over 8-40 part functional cross-link agent molecule under strong stirring, continue stirring 20-30min under room temperature; Then 1-3 part catalyst it is gradually dropped, stirring reaction 8-10h at 40-60 DEG C;
C () is down to after room temperature until (b), reaction solution is filtered, curtain coating on glass plate immediately, glass plate is placed in uniform thermal environment, progressively it is warming up to 60-100 DEG C, dry 4-8h removes solvent, and namely glass plate prepares cross-linking type fluoropolymer base dielectric elastomer composite material film;
Described addition number is mass fraction;
Described fluoropolymer matrix, for Kynoar (PVDF) based copolymer, including by but be not limited to vinylidene (VDF) and trifluoro-ethylene (TrFE), CTFE (CTFE), tetrafluoroethene (TFE), hexafluoropropene (HFP), perfluoroethylene-propylene (copolymer) (FEP), hexafluoro-isobutene (TrFE), perfluoroalkyl vinyl ether (TrFE) monomer, two or more monomer therein by copolyreaction prepare; The copolymer that copolyreaction prepares includes gathering (vinylidene-CTFE) copolymer, poly-(vinylidene-trifluoro-ethylene-CTFE) copolymer, poly-(biasfluoroethylene-hexafluoropropylene) copolymer etc.; Fluoropolymer matrix also can be made up of one or more polymer in above-mentioned copolymer;
Described functional cross-link agent molecule, its molecular weight is between 100��100000, cross-linker molecules main chain is flexible low modulus structure, and molecular structure of chemistry includes but not limited to polysiloxanes, polyacrylate, polyisoprene, polyurethane, polyether-based polymers and derivant thereof; Cross-linker molecules also comprises and with the polar group of the internal double bond generation additive reaction in fluoropolymer matrix, can include but not limited to sulfydryl, amino, carboxyl.
Described catalyst, it is the little molecule containing activity hydroxy or macromole, for accelerating the chemical crosslink reaction between function cross-linker molecules and fluoropolymer matrix, it is typically include but is not limited to one or more in the hydroxy-containing compounds such as water, ethanol, isopropanol.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111094539A (en) * | 2017-09-15 | 2020-05-01 | Ａｇｃ株式会社 | Micro flow path chip |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111094539A (en) * | 2017-09-15 | 2020-05-01 | Ａｇｃ株式会社 | Micro flow path chip |
| CN111094539B (en) * | 2017-09-15 | 2024-03-22 | Ａｇｃ株式会社 | Microchannel chip |
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