CN115216056B - Hydrogel material with bionic pore structure and preparation method and application thereof - Google Patents
Hydrogel material with bionic pore structure and preparation method and application thereof Download PDFInfo
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
- C08J9/286—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/0066—Use of inorganic compounding ingredients
- C08J9/0071—Nanosized fillers, i.e. having at least one dimension below 100 nanometers
- C08J9/0076—Nanofibres
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- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K9/00—Screening of apparatus or components against electric or magnetic fields
- H05K9/0073—Shielding materials
- H05K9/0081—Electromagnetic shielding materials, e.g. EMI, RFI shielding
- H05K9/009—Electromagnetic shielding materials, e.g. EMI, RFI shielding comprising electro-conductive fibres, e.g. metal fibres, carbon fibres, metallised textile fibres, electro-conductive mesh, woven, non-woven mat, fleece, cross-linked
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- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/022—Hydrogel, i.e. a gel containing an aqueous composition
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
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- C—CHEMISTRY; METALLURGY
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C—CHEMISTRY; METALLURGY
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- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2389/00—Characterised by the use of proteins; Derivatives thereof
Abstract
The invention discloses a hydrogel material with a bionic pore structure, and a preparation method and application thereof, and the hydrogel material comprises the following steps: the MXene waste precipitate remained after the MAX phase is etched and stripped is used as a filler, and is mixed with a water-soluble polymer material, and a metal nanowire is added into the mixture, and the mixture is obtained after uniform mixing; placing the obtained mixture in a cold source at the temperature of minus 196 ℃ to minus 20 ℃ for directional freezing; and (3) putting the product obtained after directional freezing into a salt solution, and carrying out salting-out treatment to obtain the hydrogel material with the bionic pore structure. The hydrogel material has a cellular bionic pore structure which is arranged in a directional way, is excellent in mechanical property, super-flexibility and stretchability, and excellent in electromagnetic shielding property and electromechanical sensing property, and is simple in preparation method, low in production energy consumption and cost, and capable of realizing large-scale industrial application.
Description
Technical Field
The invention belongs to the technical field of electromagnetic shielding materials, and relates to a hydrogel material with a bionic pore structure, a preparation method and application thereof.
Background
The statements herein merely provide background information related to the present disclosure and may not necessarily constitute prior art.
The rapid development of wireless communication technology brings convenience to people, and simultaneously, the generated electromagnetic interference or radiation can interrupt or interfere the normal operation of electronic equipment to influence data transmission, so that the wireless communication technology has very important significance for effectively protecting the electronic equipment from electromagnetic waves. The conventional metal shielding material and the porous foam/aerogel shielding have the common problems of brittleness and poor flexibility, and cannot meet the requirements of miniaturization, light weight and wearability, so that the application of the metal shielding material is limited.
The hydrogel is a porous material composed of a cross-linked polymer skeleton and water-rich pores, has excellent flexibility, elasticity and fatigue resistance, particularly has excellent tensile property, is expected to replace metal films and porous foam/aerogel, and becomes a new generation of electromagnetic shielding material. As a high molecular polymer, a hydrogel material needs to be compounded with a high conductive material to perform efficient electromagnetic shielding. Compared with materials such as carbon nano tubes and graphene, the transition metal carbide MXene nano-sheet has high conductivity close to metal, large specific surface area and anisotropy, and is more suitable for being used as conductive filler.
However, the current method for preparing MXene nanoplatelets has low productivity and low dispersion concentration (about 5 wt%), which is disadvantageous for increasing the content thereof in the hydrogel, which further limits the increase of the conductivity of the hydrogel, and causes a great amount of waste precipitation (80-90%) generated during the preparation process, resulting in a great amount of waste.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide the hydrogel material with the bionic pore structure, the preparation method and the application thereof, wherein the hydrogel material has the cellular bionic pore structure which is arranged in a directional way, has excellent mechanical property, super flexibility and stretchability, and has excellent electromagnetic shielding property and electromechanical sensing property, the preparation method is simple, the production energy consumption and the cost are low, and the large-scale industrialized application can be realized.
In order to achieve the above object, the present invention is realized by the following technical scheme:
in a first aspect, the present invention provides a method for preparing a hydrogel material having a biomimetic pore structure, comprising the steps of:
the MXene waste precipitate remained after the MAX phase is etched and stripped is used as a filler, and is mixed with a water-soluble polymer material, and a metal nanowire is added into the mixture, and the mixture is obtained after uniform mixing;
placing the obtained mixture in a cold source at the temperature of minus 196 ℃ to minus 20 ℃ for directional freezing;
and (3) putting the product obtained after directional freezing into a salt solution, and carrying out salting-out treatment to obtain the hydrogel material with the bionic pore structure.
In a second aspect, the invention provides a hydrogel material with a bionic pore structure, which is prepared by the preparation method.
In a third aspect, the invention provides application of the hydrogel material with the bionic pore structure in electromagnetic shielding and electromechanical sensing.
The beneficial effects achieved by one or more embodiments of the present invention described above are as follows:
1) The hydrogel material with the bionic pore structure prepared based on the MXene waste precipitate provided by the invention adopts the MXene waste precipitate left after the MXene is obtained by etching and stripping of MAX phase as a filler, and metal nanowires are added into the material, and the solid phase of the waste precipitate mainly consists of unetched MAX and multiple layers of MXene, and also has conductivity and high solid content (about 30-40 wt%) which are comparable to those of metals.
The prepared hydrogel material forms a conductive network by unetched MAX, unpeeled multilayer MXene and metal nano wires, and when in directional freezing, the inside of the hydrogel material is provided with an internal pore structure which is arranged in a directional way, and the high water content provides strong polarization loss, so that the hydrogel material has excellent electromagnetic shielding performance and can have shielding effectiveness exceeding 40dB under X, ka, K and Ku wave bands (8.2-40 GHz).
2) The hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation can further amplify multiple reflection of the material on electromagnetic waves due to the honeycomb bionic pore structure in the hydrogel material, and is further beneficial to improving the shielding performance of the material.
3) The hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation has excellent mechanical properties, super flexibility and stretchability, and is widely applied to motion detection.
4) The hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation is based on the waste material, does not need special atmosphere, pressure and temperature, does not need complex instruments and equipment, has simple preparation process and low cost, and can effectively improve the utilization rate of raw materials.
Drawings
The accompanying drawings, which are included to provide a further understanding of the invention and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention.
FIG. 1 is a scanning electron microscope image of a hydrogel material with a biomimetic pore structure prepared based on MXene waste precipitation provided in example 1;
FIG. 2 is an optical image of a flexible display of a hydrogel material with a biomimetic pore structure prepared based on MXene waste precipitation as provided in example 1;
FIG. 3 is a cross-sectional scanning electron microscope image of the hydrogel material with a biomimetic pore structure prepared based on MXene waste precipitation provided in example 1;
FIG. 4 is a graph of electromagnetic shielding performance at 8.2-40GHz of a hydrogel material with a biomimetic pore structure prepared based on MXene waste precipitation provided in example 3;
FIG. 5 is a graph showing the relationship between electromagnetic shielding performance and directional pore structure of a hydrogel material with a biomimetic pore structure prepared based on MXene waste precipitation in the X-band provided in example 2;
fig. 6 is a graph of the motion detection sensing performance of the hydrogel material with a biomimetic pore structure prepared based on MXene waste precipitation provided in example 4.
Detailed Description
It should be noted that the following detailed description is illustrative and is intended to provide further explanation of the invention. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
In a first aspect, the present invention provides a method for preparing a hydrogel material having a biomimetic pore structure, comprising the steps of:
the MXene waste precipitate remained after the MAX phase is etched and stripped is used as a filler, and is mixed with a water-soluble polymer material, and a metal nanowire is added into the mixture, and the mixture is obtained after uniform mixing;
placing the obtained mixture in a cold source at the temperature of minus 196 ℃ to minus 20 ℃ for directional freezing;
and (3) putting the product obtained after directional freezing into a salt solution, and carrying out salting-out treatment to obtain the hydrogel material with the bionic pore structure.
The dispersing concentration of the MXene nano-sheets is very low (about 5wt percent), so that the content of the MXene in the hydrogel is difficult to improve on the premise of ensuring the strength of the hydrogel, and the conductivity of the hydrogel is difficult to further improve; on the other hand, the low yield of the MXene nano-sheets causes 80-90% of raw materials to be wasted, and high cost is added. The solid content of the MXene waste precipitate is high (30-40%), so that the content of the conductive filler in the hydrogel can be increased, the conductivity can be improved, and the preparation and use cost of the MXene can be reduced.
In some embodiments, the MAX phase is selected from Ti 3 AlC 2 、Ti 3 AlCN、Ti 2 One or at least two of AlC.
Preferably, the etching liquid adopted in the etching is HF solution or LiF/HCl solution.
Further preferably, the etching time is 4-36 hours and the etching temperature is 25-50 ℃.
In some embodiments, the stripping is mechanical stripping at a speed of 1000-3000rpm for a stripping time of 10-40min;
the rotational speed of the centrifugal treatment is 3000-5000rpm, and the time is 5-10min.
In some embodiments, the water-soluble polymeric material is selected from any one or a combination of at least two of cellulose, hydroxymethyl cellulose, carboxymethyl cellulose, lignin, starch, hydroxymethyl starch, starch acetate, vegetable gums, animal gums, polyacrylamide, polyvinylpyrrolidone, aqueous polyurethane, polyacrylic acid, polyacrylate, polyvinyl alcohol (PVA), polyaniline, polylactic acid, polymaleic anhydride, or polyethylene glycol.
In some embodiments, the metal nanowires are aqueous dispersions of metal nanowires selected from one or a combination of at least two of silver nanowire aqueous dispersions, copper nanowire aqueous dispersions, or nickel nanowire aqueous dispersions.
Preferably, the metal nanowires are added in an amount of 0.01-2wt% based on the total solids in the mixture.
In some embodiments, the MXene waste precipitate comprises 1% -90% of the total solids in the mixture. For example, it may be: 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19%, 20%, 21%, 22%, 23%, 24%, 25%, 26%, 27%, 28%, 29%, 30%, 31%, 32%, 33%, 34%, 35%, 36%, 37%, 38%, 39%, 40%, 41%, 42%, 43%, 44%, 45%, 46%, 47%, 48%, 49%, 50%, 51%, 52%, 53%, 54%, 55%, 56%, 57%, 58%, 59%, 60%, 61%, 62%, 63%, 64%, 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73%, 74%, 75%, 76%, 77%, 78%, 79%, 80%, 81%, 82%, 83%, 84%, 85%, 86%, 87%, 88%, 89%, 90%.
Preferably, the MXene waste precipitate is 10% to 80%, more preferably 20% to 70%, and even more preferably 30% to 60% of the total solids in the mixture.
In some embodiments, the salt solution is selected from one or at least two of sodium chloride, calcium chloride, copper chloride, sodium citrate, sodium sulfate, sodium nitrate, sodium acetate, potassium sulfate, potassium carbonate, or potassium chloride.
Preferably, the salt solution contains 15-40wt% of salt.
Further preferably, the salting-out treatment time is 2 to 48 hours.
In a second aspect, the invention provides a hydrogel material with a bionic pore structure, which is prepared by the preparation method.
In a third aspect, the invention provides application of the hydrogel material with the bionic pore structure in electromagnetic shielding and electromechanical sensing.
The invention is further illustrated below with reference to examples.
Example 1
The hydrogel material with the bionic pore structure, which is prepared based on MXene waste precipitation, is prepared by the following method:
(1) 2g of Ti 3 AlC 2 Added to a solution of LiF (3.2 g) and HCl (30 mL) of 6M concentration, stirred at 35℃for 24h; after the reaction is finished, washing the mixture to be neutral by deionized water, and collecting an upper MXene nano-sheet dispersion liquid after mechanical stripping for 30min at a rotating speed of 2500rpm and centrifugal treatment for 10min at 4000rpm, wherein a lower precipitate is MXene waste precipitate;
(2) Uniformly mixing the MXene waste precipitate, silver nanowire dispersion liquid and polyvinyl alcohol (polymerization degree 2400) aqueous solution, wherein the total solid content is 20wt%, the mass fraction of the MXene waste precipitate is 20wt%, and the mass fraction of the silver nanowire is 1wt%; pouring the mixed liquid into a mould, and placing the mould into a cold source at the temperature of minus 80 ℃ for directional freezing;
(3) And (3) putting the sample obtained in the step (2) into a sodium acetate solution, wherein the content of sodium acetate is 20wt%, salting out for 48 hours, and cleaning to obtain the hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation.
The MXene-based waste precipitate was subjected to a morphological test by a scanning electron microscope (SEM, SU-70, hitachi), the SEM of which is shown in FIG. 1.
The optical picture of the flexibility (bending, curling) of the hydrogel material with the biomimetic pore structure prepared based on the MXene waste precipitation is shown in fig. 2.
The hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation was freeze-dried, and the microscopic morphology test was performed on the hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation provided in this example by a scanning electron microscope (SEM, SU-70, hitachi), and the obtained scanning electron microscope image is shown in fig. 3, which shows that the hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation has a regular and highly oriented pore structure inside, and the pore width is 4-5 μm.
Example 2
(1) 0.5g of Ti 3 AlC 2 Added to a solution of LiF (0.5 g) and HCl (20 mL) at a concentration of 4.5M, stirred at 40℃for 24h; after the reaction is completed, washing the mixture to be neutral by deionized water, and collecting an upper MXene nano-sheet dispersion liquid after mechanical stripping for 30min at a rotating speed of 2500rpm and centrifugal treatment for 10min at 4000rpm, wherein the lower precipitate is the MXene waste precipitate.
(2) Uniformly mixing the MXene waste precipitate, silver nanowire dispersion liquid and TEMPO oxidized cellulose dispersion liquid, wherein the total solid content is 20wt%, and the mass fraction of the MXene waste precipitate is 80wt%; pouring the mixed liquid into a mould, and placing the mould into a cold source at the temperature of-196 ℃ for directional freezing;
(3) And (3) placing the sample obtained in the step (2) into a sodium citrate solution, wherein the content of sodium citrate is 25wt%, salting out for 12 hours, and cleaning to obtain the hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation.
Example 3
(1) 0.5g of Ti 3 AlC 2 Added to a solution of LiF (0.5 g) and HCl (20 mL) at a concentration of 4.5M, and stirred at 35℃for 24h; after the reaction is completed, washing the mixture to be neutral by deionized water, and collecting an upper MXene nano-sheet dispersion liquid after mechanical stripping for 30min at a rotating speed of 2500rpm and centrifugal treatment for 10min at 4000rpm, wherein the lower precipitate is the MXene waste precipitate.
(2) Uniformly mixing the MXene waste precipitate, silver nanowire dispersion liquid and polyvinyl alcohol (polymerization degree 1700) aqueous solution, wherein the total solid content is 20wt%, the mass fraction of the MXene waste precipitate is 80wt%, pouring the mixed liquid into a mold, and placing the mold into a cold source at-196 ℃ for directional freezing;
(3) And (3) putting the sample obtained in the step (2) into a sodium chloride solution, wherein the content of sodium chloride is 25wt%, salting out for 24 hours, and cleaning to obtain the hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation.
The electromagnetic shielding performance of the MXene-based polyvinyl alcohol hydrogel material provided in this embodiment was measured using a vector network analyzer (VNA, agilent 8517A), and the obtained electromagnetic shielding performance graph is shown in fig. 4, and the MXene composite film material can have shielding performance exceeding 40dB under the X, ka, K and Ku bands (8.2-40 GHz), and can attenuate electromagnetic waves by more than 99.99%, which is far exceeding the requirement of commercial 20 dB. Fig. 5 shows that the directional pore structure significantly improves the electromagnetic shielding performance of the hydrogel, wherein pe-SE is the performance when the incident electromagnetic wave is perpendicular to the directional pore structure, and pa-SE is the performance when the incident electromagnetic wave is parallel to the directional pore structure, so that the influence of the bionic directional pore structure on the electromagnetic shielding performance of the hydrogel can be seen.
Example 4
(1) 1.2g of Ti 3 AlC 2 Added to a solution of LiF (2.4 g) and HCl (40 mL) of 5M concentration, stirred at 35℃for 24h; after the reaction is completed, washing the mixture to be neutral by deionized water, and collecting an upper MXene nano-sheet dispersion liquid after mechanical stripping for 20min and rotating speed of 1500rpm and centrifugal treatment for 15min and 3500rpm, wherein the lower precipitate is the MXene waste precipitate.
(2) Uniformly mixing the MXene waste precipitate, silver nanowire dispersion liquid and gelatin aqueous solution, wherein the total solid content is 20wt%, and the mass fraction of the MXene waste precipitate is 60wt%; pouring the mixed liquid into a mould, and placing the mould into a cold source at the temperature of minus 20 ℃ for directional freezing;
(3) And (3) placing the sample obtained in the step (2) into an ammonium sulfate solution, wherein the content of ammonium sulfate is 25wt%, salting out for 24 hours, and cleaning to obtain the hydrogel material with the bionic pore structure prepared based on the MXene waste precipitation.
The resistance change of the MXene-based polyvinyl alcohol hydrogel material is measured by adopting a TH26011CS test system and a double-probe method, so that the sensing performance of the MXene-based polyvinyl alcohol hydrogel material is obtained, and as shown in FIG. 6, the MXene-based polyvinyl alcohol hydrogel material is shown to be used as a sensor for bending joints of fingers, which shows that the MXene-based polyvinyl alcohol hydrogel material can be used as an excellent electromechanical sensor for motion detection.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. The application of the hydrogel material with the bionic pore structure in electromagnetic shielding and electromechanical sensing is characterized in that:
the preparation method of the hydrogel material with the bionic pore structure comprises the following steps:
taking the MXene waste precipitate remained after the MAX phase is etched, stripped and centrifuged to obtain MXene as a filler, mixing with a water-soluble high polymer material, adding metal nanowires into the mixture, and uniformly mixing to obtain a mixture;
placing the obtained mixture in a cold source at the temperature of minus 196 ℃ to minus 20 ℃ for directional freezing;
putting the product obtained after directional freezing into a salt solution for salting out treatment to obtain a hydrogel material with a bionic pore structure;
wherein the MXene waste sediment accounts for 20-80% of the total solid content in the mixture; the added metal nano wires account for 0.01-2wt% of the total solids in the mixture.
2. The use according to claim 1, characterized in that: the MAX phase is selected from Ti 3 AlC 2 、Ti 3 AlCN、Ti 2 One or at least two of AlC.
3. The use according to claim 1, characterized in that: the etching liquid adopted in the etching is HF solution or LiF/HCl solution;
the etching time is 4-36h, and the etching temperature is 25-50 ℃.
4. The use according to claim 1, characterized in that: the stripping adopts mechanical stripping, the rotating speed of the mechanical stripping is 1000-3000rpm, and the stripping time is 10-40min;
the rotational speed of the centrifugal treatment is 3000-5000rpm, and the time is 5-10min.
5. The use according to claim 1, characterized in that: the water-soluble polymer material is selected from any one or a combination of at least two of cellulose, hydroxymethyl cellulose, carboxymethyl cellulose, lignin, starch, hydroxymethyl starch, acetic acid starch, vegetable gum, animal glue, polyacrylamide, polyvinylpyrrolidone, aqueous polyurethane, polyacrylic acid, polyacrylate, polyvinyl alcohol, polyaniline, polylactic acid, polymaleic anhydride or polyethylene glycol.
6. The use according to claim 1, characterized in that: the metal nanowire is an aqueous dispersion of the metal nanowire, and is selected from one or a combination of at least two of an aqueous dispersion of silver nanowire, an aqueous dispersion of copper nanowire or an aqueous dispersion of nickel nanowire.
7. The use according to claim 1, characterized in that: the MXene waste precipitate accounts for 30% -60% of the total solids in the mixture.
8. The use according to claim 1, characterized in that: the salt solution is selected from one or at least two of sodium chloride, calcium chloride, copper chloride, sodium citrate, sodium sulfate, sodium nitrate, sodium acetate, potassium sulfate, potassium carbonate or potassium chloride;
the mass percentage of salt in the salt solution is 15-40 wt%;
the salting-out treatment time is 2-48h.
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