CN112724458B - Preparation method of graphene composite toughened porous gel electric actuating membrane - Google Patents
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Abstract
The invention relates to a preparation method of a graphene composite toughened porous gel electric actuating membrane, which is characterized by comprising the steps of preparing a 25mg/ml aqueous solution by selecting a natural polymer sodium alginate, doping and pouring a micro-nano green electrolyte 4ml of ionic liquid [ EMIm ] into the aqueous solution]BF 4 A plasticizer and a stimulus-responsive functional component as a solution of the gel electro-active membrane; preliminarily preparing a semi-finished product of the porous gel electric actuating membrane by adopting a freezing negative pressure casting forming method, so that the semi-finished product has a linear-oriented internal anisotropic three-dimensional layered structure; and immersing the semi-finished product of the porous gel electric actuating membrane in the graphene aqueous dispersion, carrying out composite strengthening and toughening on the semi-finished product of the porous gel electric actuating membrane, and heating and drying the semi-finished product of the porous gel electric actuating membrane to obtain the finished product of the porous gel electric actuating membrane with excellent mechanical property, conductivity and flexibility. The method has the advantages of being scientific and reasonable, simple and convenient to operate, strong in applicability, high in production efficiency and good in effect.
Description
Technical Field
The invention relates to a preparation method of a gel electric actuating membrane, in particular to a preparation method of a graphene composite strengthening and toughening porous gel electric actuating membrane.
Background
The bionic artificial muscle device is an intelligent electric actuator with great application prospect, and can replace a traditional driving system to reproduce the motion of an organism. In various intelligent construction materials, the gel has the advantages of wide response range, large volume deformation, high sensitivity and the like as an electric actuating membrane of a bionic artificial muscle device. However, the conventional gel electro-active membrane only generates volume change (simple contraction and expansion) based on the isotropic inner structure in response to external stimulus, and cannot be regarded as an ideal artificial muscle electro-active membrane because it lacks the ability of complex deformation. The gel electric actuating membrane with the anisotropic structure and reasonably and optimally designed in the bionic artificial muscle device is needed to be solved, so that the gel electric actuating membrane can obtain controllable complex deformation. Therefore, the preparation method of the graphene composite strengthened and toughened porous gel electric actuating membrane, which is simple and convenient to operate, high in production efficiency and widely applicable, is provided to construct a stimulation-responsive bionic artificial muscle device with an anisotropic structure, so that the bionic muscle movement which generates multidirectional bending, directional amplification deformation and rapid controllable actuation is realized. The method has very important scientific significance and engineering value for the method to go beyond the concept verification stage and advance to practical application.
Disclosure of Invention
The invention aims to overcome the defects of the prior art, provide a preparation method of a graphene composite toughened porous gel electric actuating membrane, and simultaneously provide optimized graphene aqueous dispersion concentration, ionic liquid doping amount and preparation method process parameters related to the preparation method, so as to obtain the gel electric actuating membrane for a bionic artificial muscle device, which has the advantages of light weight, low energy consumption, large deformation, high flexibility and high elasticity. Furthermore, explaining the effective preparation method mechanism and the electric actuation action mechanism of the obtained gel electric actuation film, the invention opens up a new space for the performance improvement and the application development of the electric actuation film.
The purpose of the invention is realized as follows: a preparation method of a graphene composite toughened porous gel electric actuating membrane is characterized by comprising the following steps:
(1) Preparing a gel electric actuating membrane solution: starting a magnetic stirrer, setting the temperature at 50 ℃ and the stirring speed at 50%, placing a beaker filled with 50ml of distilled water in the water environment, uniformly adding 1.25g of sodium alginate, and after completely dissolving, dropwise adding 4ml of ionic liquid [ EMIm ]]BF 4 Heating in water bath at 50 deg.C, stirring for 15min, adding 0.2g sodium dodecyl sulfate powder, adding 3ml glycerol dropwise, heating, stirring for 20min, mixing, and vibration defoaming in ultrasonic cleaning machine for 10min for 4-5 periods to obtain gel electrically-actuated membrane solution;
(2) Preparing a porous gel electric actuating membrane: pouring the solution of the gel electric actuating membrane after standing into a tray, placing a temperature sensor beside the tray, then immersing the solution of the gel electric actuating membrane into a cold trap together, covering a sealed glass cover above the cold trap, starting a freezing casting machine to set the temperature to be 60 ℃ below zero for refrigerating for 7 hours, placing the frozen ice-shaped gel electric actuating membrane which is frozen and formed in a primary forming way on a bracket above the cold trap, covering the glass cover, starting a vacuum pump to form an environment of secondary negative pressure freezing casting, enabling the low-temperature cold trap to automatically capture and adsorb water vapor sublimated from the ice-shaped gel electric actuating membrane which is formed in a primary forming way, and continuing for 20-24 hours to prepare a semi-finished product of the porous gel electric actuating membrane;
(3) Graphene composite strengthening and toughening treatment: preheating a vacuum constant-temperature drying oven at 50 ℃ for 30min on one side, putting the porous gel electric actuating membrane semi-finished product into a culture dish with the diameter of phi 12cm on the other side, uniformly casting 50ml of graphene water dispersion liquid subjected to secondary dispersion into the culture dish until the graphene water dispersion liquid is immersed in the gel electric actuating membrane semi-finished product, horizontally putting the graphene water dispersion liquid into the vacuum constant-temperature drying oven, setting the temperature at 50 ℃ and the vacuum degree at-0.090 MPa, standing for 4h, and naturally cooling and drying to obtain the porous gel electric actuating membrane finished product.
Further, the sodium alginate is analytically pure, 90%.
Further, the ionic liquid [ EMIm]BF 4 1-ethyl-3-methylimidazolium tetrafluoroborate, experimental reagent, 97%.
Further, the concentration of the graphene aqueous dispersion is 1.0%.
Further, the sodium lauryl sulfate is chemically pure.
Further, the glycerol is chemically pure and is more than or equal to 99.0%.
Furthermore, the sodium alginate concentration of the gel electric actuating membrane solution is 25mg/ml, and the thickness of the cast molding membrane is 0.8-1.0mm.
The preparation method of the graphene composite toughened porous gel electric actuating membrane has the advantages of simplicity and convenience in operation, strong applicability, high production efficiency and good effect. Further advantages are realized in that:
based on the purposes of green chemistry and sustainable development, hydrophilic ionic liquid [ EMIm ] is selected]BF 4 The modified sodium alginate solution is doped, so that the formed gel electric actuating membrane can be plasticized, the thermal stability of the gel electric actuating membrane is obviously enhanced, and the crystallinity is reduced; meanwhile, the number of conductive ions contained in the electric actuator is increased, and the electric actuating performance is improved accordingly. Then, rapidly freezing the water in the gel electric actuating membrane solution into ice by a freezing negative pressure casting molding method to form a frozen pre-molded ice-shaped gel electric actuating membrane; the ice is sublimated into water vapor to be removed through the negative pressure process, so as to cast and mold a semi-finished product of the porous gel electric actuating membrane, the chemical and physical properties of the gel electric actuating membrane, such as porous structure, colloidal property and the like, are well maintained, namely the change of the physical structure and the molecular structure is extremely small, the organizational structure and the appearance form of the gel electric actuating membrane are completely maintained, and the stimulation-responsive functional components in the solution raw material are well preserved, so that the porous gel electric actuating membrane with the unique characteristics of biological systematicness, such as three-dimensional ordered multi-scale and multi-level anisotropic structure, is obtained; then carrying out graphene composite strengthening and toughening treatment, cooling and drying to enable the prepared porous gel electric actuating membrane finished product to have an internal covalent cross-linking network and be tempered into an anisotropic structure with consistent height, so that the generated large specific surface areaHigh conductivity, high flexibility and high elasticity, and brings about large deformation, quick response and actuation and good mechanical property of the gel electric actuating membrane.
Drawings
FIG. 1 is a flow chart of a process for preparing a graphene composite toughened porous gel electro-active membrane according to the present invention;
FIG. 2 is a schematic of the macrostructure of the porous gel electroactive membrane of the invention;
FIG. 3 is a scanning electron microscope image of the internal microstructure of the porous gel electroactive film of the invention;
figure 4 is an XRD pattern of the gel electrically actuated membrane and functional components of the present invention, sodium alginate and ionic liquid.
Detailed Description
The invention is described in further detail below with reference to the accompanying drawings:
as shown in fig. 1, the preparation method of the graphene composite strengthened and toughened porous gel electric actuating membrane of the invention comprises three sequential processes: formulation of gel electroactive Membrane solutions, i.e. Ionic liquids [ EMIm]BF 4 Doping sodium alginate solution, preparing a porous gel electric actuating membrane (a freezing negative pressure casting molding method) and carrying out graphene composite strengthening and toughening treatment (direct blending soaking and heating drying treatment). In addition, the whole preparation method is simple and convenient to operate, high in production efficiency and widely applicable, so that the anisotropic-structure porous gel electric actuating membrane for the bionic artificial muscle device is light in weight, low in energy consumption, large in deformation, high in flexibility and high in elasticity.
(1) The preparation process of the gel electric actuating membrane solution comprises the following steps:
starting the magnetic stirrer, setting the temperature at 50 ℃ and the stirring speed at 50% of the maximum stirring speed, placing a beaker filled with 50ml of distilled water in a water bath environment on the magnetic stirrer, and heating to 50 ℃. 1.25g of sodium alginate powder was weighed out using an analytical balance and slowly dissolved in 50ml of distilled water at 50 ℃. After the sodium alginate is completely dissolved, 4ml of ionic liquid [ EMIm ] is dripped]BF 4 And heating and stirring in water bath at 50 deg.C for 15min. Then 0.2g of sodium dodecyl sulfate is added into the solution evenly, and the solution is heated and stirred continuously until the solution is heated and stirredAnd completely dissolving. Measuring 3ml of glycerol with a disposable rubber-tipped dropper, slowly dripping into the above solution, and continuously heating and stirring for 20min to ensure that the humectant is uniformly mixed. And then pouring a certain amount of water into an ultrasonic cleaning machine, setting the defoaming time to be 10min, placing the prepared solution in the ultrasonic cleaning machine for vibration defoaming, and repeating for 4-5 cycles. The solution after vibration defoaming treatment was slowly and uniformly poured into a horizontal glass mold 50mm × 50mm × 5mm using a glass rod, and then allowed to stand for 20min to ensure the solution level.
(2) The preparation process of the porous gel electric actuating membrane comprises the following steps:
the freeze-casting machine was started and the gel electroactive film solution after standing was placed in a tray, and a temperature sensor was placed next to it. And then placing the freezing molding frame in a cold trap, tightly covering a sealed glass cover above the freezing molding frame, setting the refrigerating function of a freezing casting machine to be 60 ℃ below zero, and freezing the gel electric actuating membrane solution in the cold trap for 7 hours. After the freezing forming is finished, the frozen and pre-formed ice-shaped gel electric actuating membrane is quickly taken out from the freezing chamber and is placed on a bracket above the freezing chamber, the bracket is a casting frame, a glass cover is immediately covered, and a vacuum pump is started to form a negative pressure vacuum internal environment. In addition, the refrigeration function of whole process, to keep the open mode all the time, then cryogenic cold trap catches and adsorbs the vapor that the sublimation came out by oneself. After 24 hours, the semi-finished product of the porous gel electric actuating membrane is prepared, and the drain valve is opened to drain water.
(3) The processing process of graphene composite strengthening and toughening comprises the following steps:
preheating at 50 deg.C, vacuum drying for 30min, placing the other side in a culture dish container of 12cm, and placing porous gel electric-actuated membrane semi-finished product. With reference to fig. 2 and 3, 50ml of the graphene aqueous dispersion after the second dispersion is extracted by a needle tube and is slowly and uniformly cast into a culture dish along a glass rod until the gel electroactive film semi-finished product is immersed. Then horizontally placing the culture dish in a vacuum constant temperature drying oven, setting the temperature at 50 ℃, the vacuum degree at-0.090 MPa, standing for 4h, closing a switch of the drying oven to carry out natural cooling and drying to obtain a finished product of the porous gel electric actuating membrane, wherein the casting thickness of the finished product is 0.8-1.0mm.
The specific working principle is as follows:
as can be seen from FIG. 4, the ionic liquid [ EMIm]BF 4 In sodium alginate solution, all ionizes to anions [ BF ] 4 ] - With cations [ EMIm] + . Part of anions and cations are strongly coordinated with hydroxyl in sodium alginate molecules through synergistic action to form a large number of hydrogen bonds, so that the sodium alginate molecules are further self-wound through the hydrogen bonds to form a gel polymer, and the plasticizing effect is achieved, so that the internal resistance is reduced, the specific capacitance is improved, and the elastic modulus is reduced. Meanwhile, the other part of the remaining anions and cations are retained in a three-dimensional network structure in the gel film, can move freely and are always in a disordered free state. Under the action of an external direct current electric field, the gel electric actuating membrane can generate directional migration, and the large deformation and the improvement of the response speed of the gel electric actuating membrane are facilitated.
Furthermore, the novel graphene composite toughened porous gel electric actuating membrane has a unique electric actuating mechanism, namely, the novel graphene composite toughened porous gel electric actuating membrane can show long-term practical performance and has stable electrochemical characteristics to water and air under the conditions of open air and dry non-external solvents. Specifically, under the action of an external direct current electric field, free cations in the electric actuating membrane can directionally migrate to the negative electrode interface of the electric actuating membrane; meanwhile, the free anions are continuously enriched to the interface of the positive terminal. When the accumulation amount of the charged ions is enough, the volume of the negative electrode side is expanded and is larger than that of the positive electrode side (a serious volume difference is generated) because the radius of the positive ions is obviously larger than that of the negative ions, and the actuation deflection effect of the gel electric actuation film is further promoted because the electrostatic repulsion action exists among the same-polarity ions.
While the present invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof as defined in the appended claims.
Claims (7)
1. A preparation method of a graphene composite toughened porous gel electric actuating membrane is characterized by comprising the following steps:
(1) Preparing a gel electric actuating membrane solution: starting the magnetic stirrer, setting the temperature at 50 deg.C and the stirring speed at 50% of the maximum stirring speed of the magnetic stirrer, placing 50ml of distilled water in a beaker in a water bath environment of the magnetic stirrer, uniformly adding 1.25g of sodium alginate, and dropping 4ml of ionic liquid [ EMIm ] after completely dissolving]BF 4 Heating in water bath at 50 deg.C, stirring for 15min, adding 0.2g sodium dodecyl sulfate powder, adding 3ml glycerol dropwise, heating, stirring for 20min, mixing, and vibration defoaming in ultrasonic cleaning machine for 10min for 4-5 periods to obtain gel electrically-actuated membrane solution;
(2) Preparing a porous gel electric actuating membrane: pouring the solution of the gel electric actuating membrane after standing into a tray, placing a temperature sensor beside the tray, then immersing the solution of the gel electric actuating membrane into a cold trap together, covering a sealed glass cover above the cold trap, starting a freezing casting machine to set the temperature to be 60 ℃ below zero for refrigerating for 7 hours, placing the frozen ice-shaped gel electric actuating membrane which is frozen and formed in a primary forming way on a bracket above the cold trap, covering the glass cover, starting a vacuum pump to form an environment of secondary negative pressure freezing casting, enabling the low-temperature cold trap to automatically capture and adsorb water vapor sublimated from the ice-shaped gel electric actuating membrane which is formed in a primary forming way, and continuing for 20-24 hours to prepare a semi-finished product of the porous gel electric actuating membrane;
(3) Graphene composite strengthening and toughening treatment: preheating a vacuum constant-temperature drying oven at 50 ℃ for 30min, putting the porous gel electric actuating membrane semi-finished product into a culture dish with the diameter of phi 12cm on the other side, uniformly casting 50ml of graphene aqueous dispersion subjected to secondary dispersion into the culture dish until the gel electric actuating membrane semi-finished product is immersed, horizontally placing the culture dish into the vacuum constant-temperature drying oven, setting the temperature at 50 ℃ and the vacuum degree at-0.090 MPa, standing for 4h, and naturally cooling and drying to obtain the porous gel electric actuating membrane finished product.
2. The method for preparing the graphene composite strengthened and toughened porous gel electric actuating membrane according to claim 1, wherein the sodium alginate is analytically pure, 90%.
3. The method for preparing the graphene composite toughened porous gel electroactive membrane as claimed in claim 1, wherein the ionic liquid [ EMIm]BF 4 1-ethyl-3-methylimidazolium tetrafluoroborate, experimental reagent, 97%.
4. The method for preparing the graphene composite toughened porous gel electric actuating film as claimed in claim 1, wherein the concentration of the graphene aqueous dispersion is 1.0%.
5. The method for preparing the graphene composite toughened porous gel electric actuating membrane as claimed in claim 1, wherein the sodium dodecyl sulfate is chemically pure.
6. The method for preparing the graphene composite toughened porous gel electric actuating membrane according to claim 1, wherein the glycerol is chemically pure and is not less than 99.0%.
7. The method for preparing the graphene composite toughened porous gel electric actuating film as claimed in claim 1, wherein the sodium alginate concentration of the gel electric actuating film solution is 25mg/ml, and the thickness of the cast film is 0.8-1.0mm.
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