CN110746629B - Electrically-driven shape memory polymer micro-layer composite material and preparation method thereof - Google Patents
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- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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Abstract
The invention discloses an electrically-driven shape memory polymer micro-layer composite material and a preparation method thereof, wherein the electrically-driven shape memory polymer micro-layer composite material comprises an elastic recovery layer and a drive conversion layer. The carbon fiber braided fabric is subjected to continuous dipping and baking to form a conductive driving conversion layer, and then an elastic recovery layer high molecular material is sprayed on one side of the conversion layer to form the electrically-driven shape memory polymer micro-layer composite material.
Description
Technical Field
The invention relates to the technical field of polymer composite materials and preparation thereof, in particular to an electrically-driven shape memory polymer micro-layer composite material and a preparation method thereof.
Background
The shape memory polymer material is an intelligent material capable of responding under external stimulus, and after the initial shape of the material is deformed, the material is sensed under the stimulus of external condition change, and corresponding adjustment is made to finally recover the original shape. The shape memory polymer has the advantages of large deformation amount, easiness in shaping, easiness in processing, adjustable response, light weight, low price, rich varieties and the like, so that the material has wide application prospects in the fields of intelligent sensing, biomedical treatment, aerospace, intelligent textile, self-repairing and the like.
The triggering mode of the shape memory polymer material is various, such as temperature, current, humidity, illumination, magnetic field, PH, and the like. At present, the temperature response type shape memory polymer material is most studied, firstly, the thermotropic shape memory polymer material with the original shape is heated to be above the glass transition or the melting point, and is molded into a temporary shape under certain external force, so that the temperature is reduced to be below the transition temperature, the stress is frozen, and the temporary shape is fixed; when the temperature rises to the transition temperature, the energy stored in the polymer is released, and the material is driven by entropy elasticity to return from the temporary shape to the original shape. However, in practical applications, the acquisition of the temperature field requires additional heating equipment, which is generally low in efficiency and requires a long heating time. In addition, the recovery process of the thermotropic shape memory polymer material is generally uncontrollable, and can only be directly recovered to the original shape from the temporary fixed shape, and the shape in the recovery process can not be controlled at will, so that the use efficiency is greatly reduced. The electro-shape memory polymer realizes the recovery of the temporary shape to the original shape by the loading of current. The electroluminescent shape memory polymer has advantages over the thermotropic shape memory polymer. Therefore, the preparation of the convenient and easy-to-use electro-shape memory polymer material, the improvement of the use efficiency and the control of the recovery process are hot spots of the field development and the future direction.
Patent CN201810069421.8 discloses a conductive shape memory fiber film, wherein the shape memory material is dissolved and spun, dried and then soaked in a conductive polymer to form a conductive shape memory film; patents CN201710232884.7 and CN201710924004.2 disclose a three-dimensional shape memory composite material, in which the former impregnates porous polymer material in conductive carbon solution, the latter impregnates it in nano silver wire solution, and finally impregnates the three-dimensional conductive pore structure in resin to form three-dimensional electrically-driven shape memory composite material; patent CN201710340831.7 discloses a multilayer anisotropic electro-shape memory polymer composite material, in which one of the recovery layer or the reversible layer is made into a conductive layer, and the other layer is made into an insulating layer, and they are stacked alternately.
The conductive materials currently used include carbon-based materials and metal particle materials, such as: the graphene powder, the carbon black, the carbon fiber powder, the carbon nano tube, the silver nano wire, the silver nano particle, the copper powder, the aluminum powder and the like, and the preparation method comprises melt blending, solution mixing and an impregnation method. The method has the problems of unstable resistance characteristics and large resistance after repeated use, and some methods are complicated and have extremely high cost, so that the method cannot be industrially produced.
Disclosure of Invention
In order to solve the technical problems that the resistance of the conventional conductive shape memory polymer material is unstable after repeated use, the resistance is increased after repeated use, the method is complex, the cost is high, and large-scale production cannot be realized, the invention provides an electrically-driven shape memory polymer micro-layer composite material and a preparation method thereof, and the problems in the background art are solved.
In order to achieve the purpose, the invention provides the following technical scheme: an electrically-driven shape memory polymer micro-layer composite material comprises an elastic recovery layer and a driving conversion layer, wherein the elastic recovery layer is made of an elastomer material, and the driving conversion layer is made of a rigid polymer material and a carbon fiber braided fabric.
Preferably, the thickness of the elastic recovery layer is 50-500um, and the thickness of the drive conversion layer is 50-500 um.
Preferably, the elastomer material of the elasticity recovering layer is one or a mixture of more of polyolefin thermoplastic elastomer, polyurethane thermoplastic elastomer, polyester elastomer or thermosetting rubber elastomer.
Preferably, the rigid polymer material is any one or a mixture of more of polycaprolactone, polyethylene terephthalate, polybutylene terephthalate, polycarbonate, polyethylene-vinyl acetate, polyimide, polyamide, polysulfone or polyphenylene sulfide, and the carbon fiber woven fabric is formed by a carbon fiber woven layer with vapor phase carbon fibers and graphene growing on the surface.
Preferably, the thickness of the carbon fiber braided fabric is 0.040-0.205mm, and the thickness of the carbon fiber braided layer is 0.03-0.20 mm.
Preferably, the diameter of the gas-phase carbon fiber on the surface of the carbon fiber braided fabric is 0.1-1um, and the thickness of the graphene on the surface of the carbon fiber braided fabric is 1-500 nm.
A preparation method of an electrically-driven shape memory polymer micro-layer composite material comprises the following steps:
s1, weaving the carbon fiber tows with the single-filament number of 1-12k into large-area continuous layers to form carbon fiber woven layers, and rolling;
s2, continuously growing vapor-phase carbon fibers on the surface of the carbon fiber woven layer by using a chemical vapor deposition method, introducing hydrogen gas at the temperature of 500 ℃ under the protection of N2, injecting liquid benzene into a reaction furnace body at the temperature of 1100 ℃, and continuously reacting for 3 hours to obtain the carbon fiber woven layer with the vapor-phase carbon fibers on the surface;
s3, continuously depositing a graphene film on the surface of the carbon fiber woven layer deposited with the vapor-phase carbon fibers and formed in the step S2 by a chemical vapor deposition method, and preparing the carbon fiber woven fabric at the preparation temperature of 550 ℃ in a continuous tunnel furnace, and rolling the carbon fiber woven fabric for later use;
s4, continuously dipping the continuous roll-shaped carbon fiber braided fabric prepared by the S3 in a drive conversion high polymer material solution by a dipping method, wherein the wiring speed is 0.0017-0.1666m/S, the baking temperature is 80-150 ℃, and the organic solvent is volatilized to obtain a conductive drive conversion layer;
and S5, spraying an elastic recovery polymer solution on one side of the conductive drive conversion layer prepared in the step S4, wherein the wiring speed is 0.0017-0.1666m/S, the baking temperature is 50-120 ℃, and the organic solvent is volatilized to obtain the electrically-driven shape memory polymer micro-layer composite material.
Preferably, the drive conversion polymer solution in step S4 is one or more of butanone, N-dimethylformamide, N-dimethylacetamide, dimethylsulfoxide, tetrahydrofuran, and N-methylpyrrolidone.
Preferably, the elastic recovery polymer solution in step S5 is one or more of butanone, N-dimethylformamide, N-dimethylacetamide, dimethylsulfoxide, tetrahydrofuran, and N-methylpyrrolidone.
The invention has the beneficial effects that: according to the electrically-driven shape memory polymer micro-layer composite material, the driving conversion layer skeleton conductive material is a carbon fiber braided fabric formed by longitudinally growing vapor-phase carbon fibers on the surface of a carbon fiber braided fabric through chemical vapor deposition and depositing and growing graphene on the surface of the carbon fiber braided fabric through a chemical vapor deposition method, and a conductive carbon-carbon composite material grows in gaps of the braided fabric, so that the conductive properties of the carbon-carbon composite material in the longitudinal, transverse and vertical directions are more excellent, a three-dimensional conductive network is formed, the electrically-driven shape memory polymer micro-layer composite material disclosed by the invention is excellent in conductive property, has excellent conductive property in a three-dimensional space, can quickly realize the driving and recovery of a polymer micro-layer, is greatly improved in sensitivity, and can be widely applied to the technical field of wearable. The preparation method provided by the invention is simple, low in cost, high in efficiency and capable of realizing continuous large-scale preparation.
Drawings
FIG. 1 is a cross-sectional view of an electrically driven shape memory polymer microlayer composite;
FIG. 2 is a flow chart of a method for preparing an electrically-driven shape memory polymer micro-layer composite material;
in the figure, the 1-elastic recovery layer, the 2-drive conversion layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Referring to fig. 1-2, the present invention provides a technical solution: an electrically-driven shape memory polymer micro-layer composite material comprises an elastic recovery layer (1) and a drive conversion layer (2), wherein the elastic recovery layer (1) is made of an elastomer material; the drive conversion layer (2) is made of a rigid polymer material and a carbon fiber braided fabric.
Further, the thickness of the elastic recovery layer (1) is 50-500um, and the thickness of the drive conversion layer (2) is 50-500 um.
Further, the elastomer material of the elasticity recovery layer (1) is one or a mixture of more of polyolefin thermoplastic elastomer, polyurethane thermoplastic elastomer, polyester elastomer or thermosetting rubber elastomer.
Further, the rigid polymer material is any one or a mixture of a plurality of polycaprolactone, polyethylene terephthalate, polybutylene terephthalate, polycarbonate, polyethylene-vinyl acetate, polyimide, polyamide, polysulfone or polyphenylene sulfide, and the carbon fiber braided fabric is formed by carbon fiber braided layers with vapor phase carbon fibers and graphene growing on the surfaces.
Further, the thickness of the carbon fiber braided fabric is 0.040-0.205mm, and the thickness of the carbon fiber braided layer is 0.03-0.20 mm.
Further, the diameter of the gas-phase carbon fiber on the surface of the carbon fiber braided fabric is 0.1-1um, and the thickness of the graphene on the surface of the carbon fiber braided fabric is 1-500 nm.
A preparation method of an electrically-driven shape memory polymer micro-layer composite material comprises the following steps:
s1, weaving the carbon fiber tows with the single-filament number of 1-12k into large-area continuous layers to form carbon fiber woven layers, and rolling;
s2, continuously growing vapor-phase carbon fibers on the surface of the carbon fiber woven layer by using a chemical vapor deposition method, introducing hydrogen gas at the temperature of 500 ℃ under the protection of N2, injecting liquid benzene into a reaction furnace body at the temperature of 1100 ℃, and continuously reacting for 3 hours to obtain the carbon fiber woven layer with the vapor-phase carbon fibers on the surface;
s3, continuously depositing a graphene film on the surface of the carbon fiber woven layer deposited with the vapor-phase carbon fibers and formed in the step S2 by a chemical vapor deposition method, and preparing the carbon fiber woven fabric at the preparation temperature of 550 ℃ in a continuous tunnel furnace, and rolling the carbon fiber woven fabric for later use;
s4, continuously dipping the continuous roll-shaped carbon fiber braided fabric prepared by the S3 in a drive conversion high polymer material solution by a dipping method, wherein the wiring speed is 0.0017-0.1666m/S, the baking temperature is 80-150 ℃, and the organic solvent is volatilized to obtain a conductive drive conversion layer;
and S5, spraying an elastic recovery polymer solution on one side of the conductive drive conversion layer prepared in the step S4, wherein the wiring speed is 0.0017-0.1666m/S, the baking temperature is 50-120 ℃, and the organic solvent is volatilized to obtain the electrically-driven shape memory polymer micro-layer composite material.
Further, the drive conversion polymer solution in step S4 is one or more of butanone, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, tetrahydrofuran, and N-methylpyrrolidone.
Further, the elastic recovery polymer solution in step S5 is one or more of butanone, N-dimethylformamide, N-dimethylacetamide, dimethylsulfoxide, tetrahydrofuran, and N-methylpyrrolidone.
The invention uses carbon fiber to weave a continuous conductive weaving layer, firstly deposits vapor carbon fiber on the surface of the weaving layer under the action of chemical vapor deposition, and then deposits graphene through chemical vapor to obtain a carbon fiber woven fabric, conductive carbon-carbon composite material grows in the gaps of the carbon fiber woven fabric, so that the conductivity of the carbon-carbon composite material in the longitudinal, transverse and vertical directions is more excellent, a three-dimensional conductive network is formed, the electrically-driven shape memory polymer micro-layer composite material has excellent conductivity, the three-dimensional space has excellent conductivity, the driving and restoring performance of the polymer micro-layer can be rapidly realized, the sensitivity is greatly improved, the invention can be widely applied to the technical field of wearable, the carbon fiber woven fabric forms a conductive driving conversion layer through continuous dipping and baking, and then sprays elastic restoring layer high molecular material on one side of the conversion layer to form the electrically-driven shape memory polymer micro-layer composite material, the preparation method provided by the invention is simple, low in cost, high in efficiency and capable of realizing continuous large-scale preparation.
Although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that various changes in the embodiments and/or modifications of the invention can be made, and equivalents and modifications of some features of the invention can be made without departing from the spirit and scope of the invention.
Claims (9)
1. An electrically-driven shape memory polymer micro-layer composite material comprises an elastic recovery layer (1) and a drive conversion layer (2), and is characterized in that: the elastic recovery layer (1) is made of an elastomer material; the drive conversion layer (2) is made of a rigid high polymer material and a carbon fiber braided fabric; the carbon fiber braided fabric is composed of a carbon fiber braided layer with vapor phase carbon fibers and graphene growing on the surface.
2. An electrically driven shape memory polymer microlayer composite as in claim 1 wherein: the thickness of elasticity restoration layer (1) is 50-500um, the thickness of drive conversion layer (2) is 50-500 um.
3. An electrically driven shape memory polymer microlayer composite as in claim 1 or 2 wherein: the elastomer material of the elasticity recovery layer (1) is one or a mixture of more of polyolefin thermoplastic elastomer, polyurethane thermoplastic elastomer, polyester elastomer or thermosetting rubber elastomer.
4. An electrically driven shape memory polymer microlayer composite as in claim 1 wherein: the rigid high polymer material is any one or a mixture of a plurality of polycaprolactone, polyethylene terephthalate, polybutylene terephthalate, polycarbonate, polyethylene-vinyl acetate, polyimide, polyamide, polysulfone or polyphenylene sulfide.
5. An electrically driven shape memory polymer microlayer composite as in claim 4 wherein: the thickness of the carbon fiber braided fabric is 0.040-0.205mm, and the thickness of the carbon fiber braided layer is 0.03-0.20 mm.
6. An electrically driven shape memory polymer microlayer composite as in claim 4 or 5 wherein: the diameter of the gas-phase carbon fiber on the surface of the carbon fiber braided fabric is 0.1-1um, and the thickness of the graphene on the surface of the carbon fiber braided fabric is 1-500 nm.
7. A method for preparing an electrically driven shape memory polymer microlayer composite as claimed in any of claims 1-6, wherein the method comprises the steps of: the method comprises the following steps:
s1, weaving the carbon fiber tows with the single-filament number of 1-12k into large-area continuous layers to form carbon fiber woven layers, and rolling;
s2, continuously growing vapor-phase carbon fibers on the surface of the carbon fiber woven layer by using a chemical vapor deposition method, introducing hydrogen gas at the temperature of 500 ℃ under the protection of N2, injecting liquid benzene into a reaction furnace body at the temperature of 1100 ℃, and continuously reacting for 3 hours to obtain the carbon fiber woven layer with the vapor-phase carbon fibers on the surface;
s3, continuously depositing a graphene film on the surface of the carbon fiber woven layer deposited with the vapor-phase carbon fibers and formed in the step S2 by a chemical vapor deposition method, and preparing the carbon fiber woven fabric at the preparation temperature of 550 ℃ in a continuous tunnel furnace, and rolling the carbon fiber woven fabric for later use;
s4, continuously dipping the continuous roll-shaped carbon fiber braided fabric prepared by the S3 in a drive conversion high polymer material solution by a dipping method, wherein the wiring speed is 0.0017-0.1666m/S, the baking temperature is 80-150 ℃, and the organic solvent is volatilized to obtain a conductive drive conversion layer;
and S5, spraying an elastic recovery polymer solution on one side of the conductive drive conversion layer prepared in the step S4, wherein the wiring speed is 0.0017-0.1666m/S, the baking temperature is 50-120 ℃, and the organic solvent is volatilized to obtain the electrically-driven shape memory polymer micro-layer composite material.
8. The method for preparing an electrically-driven shape memory polymer microlayer composite material as claimed in claim 7, wherein the method comprises the steps of: the solvent for driving the conversion polymer solution in step S4 is one or more of butanone, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, tetrahydrofuran, and N-methylpyrrolidone.
9. The method for preparing an electrically-driven shape memory polymer microlayer composite material as claimed in claim 7, wherein the method comprises the steps of: the solvent of the elastic recovery polymer solution in step S5 is one or more of butanone, N-dimethylformamide, N-dimethylacetamide, dimethyl sulfoxide, tetrahydrofuran, and N-methylpyrrolidone.
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