CN112768113B - Preparation method of responsive nanocomposite polymer conductive film - Google Patents
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Abstract
The invention discloses a preparation method of a responsive nanocomposite polymer conductive film, which comprises the steps of firstly compositing small molecules containing functional groups with a metal nanomaterial in a dynamic covalent bond mode to obtain a nanocomposite, and then carrying out free radical polymerization reaction in the presence of polymerizable monomers to obtain nanocomposite organogel; the precursor solution formed by mixing the nanocomposite organic gel and the conductive metal nanowire is coated on a substrate, and the responsive nanocomposite polymer conductive film is obtained after drying. The network aperture structure of the nano composite polymer conductive film has certain level regularity, so that the nano composite polymer film shows driving responsiveness in organic solvent vapor; in addition, the invention utilizes the doping and mixing of the functional nano material and the organic gel solution to endow the nano composite polymer film with conductive performance, thereby the nano composite polymer conductive film has potential application in the aspects of physical sensing and detection, environmental monitoring and the like.
Description
Technical Field
The invention relates to a preparation method of a responsive nanocomposite polymer conductive film, belonging to the technical field of nanometer materials.
Background
Polymer films have been one of the directions of intense research in the film field. Because of the unique inherent low density, flexibility, commercial availability, surface structure, flexibility, optical transparency, and excellent mechanical, thermodynamic and physicochemical properties, polymer films are widely used in the fields of mass separation, energy storage, physical/mechanical sensing and detection, environmental monitoring, food safety, biological medicine, and the like.
In recent years, a novel film formed by compounding a high molecular polymer and a metal nano material is developed, and because the film can accord with the unique property of the metal nano material, people begin to research and develop the metal nano composite polymer film in depth, and the film is mainly applied to the fields of optoelectronics, biomedicine and the like. The preparation of such composite films generally involves two links: firstly, synthesizing a metal nano material, dispersing the metal nano material in a dissolved polymer or monomer, and performing solvent evaporation or polymerization reaction to form the metal nano polymer composite film. The preparation method has the main advantages that the functional nano particles are compounded in the high polymer film, so that the basic performances of the film such as strength, stretching and the like are greatly improved, and meanwhile, due to the addition of the functional nano particles, the film is endowed with excellent performances such as self-repairing, near infrared light heating and the like, so that the high polymer film has more functional application prospects.
The functional nano composite polymer film material, especially the responsive nano composite polymer film material, has very rapid mechanical motion transformation to external stimulus environment, good hydrophobicity, high response driving performance and strong circulation stability, and has important application value in the fields of responsive materials, drivers, actuators, sensor development and the like, so that the functional nano composite polymer film material is always paid attention to in scientific, technical and industrial fields. However, since such materials are still in the beginning of design and synthetic preparation. Limitations on the structure of the nano material and the type of the polymer in the preparation process, requirements on the structure of the film in the test process and the like make the nano material difficult to be widely applied. Therefore, it is very significant to study a method that can simply and rapidly prepare a responsive nanocomposite polymer conductive film.
Disclosure of Invention
The invention aims to provide a preparation method of a responsive nano composite polymer conductive film, which takes dynamic coordination and intermolecular pi-pi interaction as a crosslinking mode to obtain the nano composite polymer conductive film with organic solvent response.
The invention relates to a preparation method of a responsive nano composite polymer conductive film, which comprises the steps of firstly compositing small molecules containing functional groups with a metal nano material in a dynamic covalent bond mode to obtain a nano composite; then, the nanocomposite is subjected to free radical polymerization reaction rapidly under the stimulation of external environment by adding an initiator in the presence of a polymerizable monomer, so that nanocomposite organogel can be obtained; after the nano composite organic gel is dissolved in an organic solvent, a precursor solution formed by mixing the nano composite organic gel and the conductive metal nanowire is coated on a substrate, and the solvent is dried, so that the responsive nano composite polymer conductive film is finally obtained.
The responsiveness of the nanocomposite polymer conductive film is mainly derived from the interaction between the porous structure, the pore size gradient and the solvent molecules and the film high molecular chain material. The network pore diameter structure of the nano composite polymer conductive film has certain level regularity, and shows that the network pore diameter near the upper surface side of air is small, the network pore diameter near the lower surface side of a substrate is large, and the regularity is increased from the upper surface to the lower surface. The organic nanocomposite film exhibits structural layer regularity such that the nanocomposite polymer film exhibits driving responsiveness in organic solvent vapor, such as acetone, methylene chloride, chloroform, and the like. In addition, the invention utilizes the doping and mixing of the functional nano material and the organic gel solution to endow the nano composite polymer film with conductive performance, thereby leading the nano composite polymer conductive film to have potential application in the aspects of physical sensing and detection, environmental monitoring and the like.
The preparation method of the responsive nano composite polymer conductive film comprises the following steps:
step 1: functional surface modification of gold nanoparticles
Adding a functional modifier into the metal nano material dispersion liquid, and performing ultrasonic treatment at room temperature for 30s to enable thiol small molecules to be adsorbed on the surfaces of the metal nano particles successfully, so as to obtain the surface modified functional metal nano particle dispersion liquid;
the metal nano material is a gold nano particle material with a zero-dimensional sphere.
The functional modification body is a functional small molecule containing sulfhydryl and benzene ring, preferably 2-mercaptobenzimidazole, and the mass-volume ratio of the added mass to the volume of the metal nano material dispersion liquid is 5mg/mL.
The concentration of the functional metal nanoparticle dispersion liquid is 0.1-1.0mg/mL.
Step 2: preparation of nanocomposite organogels
Under the protection of nitrogen, adding a liquid organic monomer and a photoinitiator into the surface-modified functional metal nanoparticle dispersion liquid obtained in the step 1, uniformly mixing by ultrasound, placing in a vacuum drying oven, removing dissolved oxygen in the solution, placing in an ultraviolet lamp box for polymerization reaction for 30min, and cooling to room temperature to obtain the nanocomposite organogel. In the step, the functional metal nano particles with the modified surfaces are used as a cross-linking agent in the polymerization process, and the nano composite organogel with unique performance can be formed without adding other cross-linking agents.
The organic monomer is phenyl methacrylate, and the added volume of the organic monomer is 80% of the volume of the mixed organic gel reaction solution.
The photoinitiator comprises benzoin and derivatives thereof, preferably 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone, and the addition mass of the photoinitiator is 0.1% of the mass of the metal nano material dispersion liquid.
The flow rate of nitrogen was controlled at 0.5mL/s, and the vacuum oven temperature was set at ambient temperature 25 ℃.
Step 3: preparation of nanocomposite polymer conductive films
Dissolving the newly prepared nano composite organic gel in an organic solvent, and dissolving the linear high polymer chains from the nano composite organic gel by utilizing the thermal dilution and the solubility of the nano composite organic gel to form a linear high polymer chain solution which is uniformly dispersed in the organic solvent; then mixing the metal nanoparticle solution with the linear high polymer chain solution to form a precursor solution; then the precursor solution is uniformly coated on a substrate, the substrate is placed in a vacuum drying oven, the organic solvent in the organic film is removed, and then the organic film is separated from the substrate, so that the self-supporting and responsive nano composite polymer conductive film can be obtained.
The organic solvent comprises N, N-dimethylformamide or dichloromethane, and the ratio of the added volume of the organic solvent to the volume of the nano composite organic gel is 10:1.
The concentration of the metal nano particles in the mixed precursor solution is 5mg/mL, and the metal nano particles are one-dimensional linear silver nano wires.
The substrate is a float soda-lime glass sheet or a silicon sheet; the vacuum oven temperature was set at 70 ℃.
In step 1, the preparation process of the metal nano material dispersion liquid is as follows:
5mL of 3 mM chloroauric acid solution and 45mL of deionized water are added into a 100mL round-bottom flask, the mixture is heated to 100 ℃ in an oil bath, the temperature is kept constant for 10min, 1mL of 38.7mM/L sodium citrate solution is added into the round-bottom flask, and the mixture is reacted at constant temperature for 5min to obtain a wine-red gold nanoparticle solution.
In step 3, the preparation process of the metal nanoparticle solution is as follows:
adding 5.86g of polyvinylpyrrolidone into 190mL of glycerol, uniformly stirring, and then standing in a 90 ℃ environment for 5min to completely dissolve the polyvinylpyrrolidone; then cooling to 50 ℃, sequentially adding 1.58g of silver nitrate solution in 10mL of glycerol and 59mg of sodium chloride solution in 0.5mL of deionized water, stirring uniformly, and then heating to 210 ℃; and after heating, adding 200mL of deionized water, cooling to room temperature, standing for precipitation, removing the upper layer of solution, redispersing the bottom layer of precipitate of deionized water, washing with ethanol, centrifuging, and dispersing into the aqueous solution to obtain the metal nano material dispersion liquid with the nanowire morphology.
The beneficial effects of the invention are as follows:
the invention uses functional micromolecules containing sulfhydryl and benzene ring to modify the surface of metal nano material to functionalize the metal nano material in the process of preparing the responsive nano composite polymer conductive film, and the surface modification process of the metal is to successfully functionalize the surface of the gold nano particle material after the surface functional modification by utilizing the adsorption effect of gold atoms on the surface of gold nano particles to sulfur atoms on the functional micromolecules containing sulfhydryl. The organic gel is formed by pi-pi interaction between benzene rings on small molecules functionalized on the surface of the gold nanoparticle material and benzene rings on a polyphenyl methacrylate chain. Because the existence of N, N-dimethylformamide molecules can destroy pi-pi interaction between benzene rings on small molecules functionalized on the surfaces of gold nanoparticle materials and benzene rings on the polyphenyl methacrylate chains, gelled polyphenyl methacrylate chains fall off from the organogel and are freely dispersed in the N, N-dimethylformamide. And mixing the silver nanowire solution with the linear high polymer chain solution to form a precursor solution. In the film coating and drying process, the precursor solution is converted into the organic film. The network pore diameter structure of the prepared responsive nano composite polymer conductive film has certain level regularity by utilizing the difference between upper and lower interfaces in the precursor solution drying film forming process, the network pore diameter of the side close to the upper surface of air is small, the network pore diameter of the side close to the lower surface of a substrate is large, and the regularity is increased from the upper surface to the lower surface. The organic nano composite conductive film shows a hierarchical regular structure, and the adsorption of the vapor molecules of the solvent to the surface pores of the conductive film causes the change of local volume to cause driving movement, so that the nano composite polymer conductive film shows responsiveness in the vapor of the organic solvent. After the conductive film is removed, the solvent in the film is quickly volatilized due to the fact that the upper surface side is close to the air, the residual amount of the solvent in the holes is less, the lower surface is close to the substrate, the solvent in the conductive film is difficult to volatilize compared with the upper surface side, and a large amount of solvent remains in the film. After the responsive nano composite polymer conductive film is uncovered, the upper surface side has a large aperture, the solvent in the hole is less, the hole starts to shrink, and the aperture is reduced; the pore diameter of the lower surface is almost unchanged due to the fact that a large amount of solvent exists in the pore diameter. Because the pore sizes of the upper surface and the lower surface are different, the conductive film naturally bends towards the small pore size direction. When the conductive film is placed in an acetone vapor environment, solvent molecules diffuse to the upper and lower surfaces of the porous film at a relatively high rate, and the upper and lower surface regions are expanded due to expansion strain generated by the interaction of the solvent with the polymer chains in the film, and the increase of the osmotic pressure of the solvent at the upper surface causes more expansion than at the bottom. The acetone solvent molecules and the polymer chains in the film have strong interaction, so that the conductive film is bent in the opposite direction from the upper surface to the lower surface, and the conductive film of the responsive nanocomposite polymer can be stretched and straightened in the organic solvent. The pore gradient produces a gradient of interaction between the solvent and the polymer chains within the membrane, thereby producing a modulus gradient, which in turn alters the curvature of the membrane drive response.
In summary, the invention provides a preparation method of a responsive nano composite polymer conductive film, which controls the hierarchical regularity of the network pore structure of the nano composite polymer conductive film, and shows that the network pore size near the upper surface of air is small, the network pore size near the lower surface of a substrate is large, and the regular pore size gradient is shown from the upper surface to the lower surface. Silver nanowires are arranged in the polymer film in a lap joint manner, so that the nano composite polymer film is endowed with conductive performance. The method provides a theoretical basis for preparing the responsive polymer conductive film material, and the responsive nano composite polymer conductive film of the type has a wide application prospect in the aspects of a driver, a responder, a sensor and the like and can be applied to a plurality of fields as an intelligent material.
Drawings
FIG. 1 is an optical photograph of a nanocomposite organogel. From fig. 1, it can be seen that the organogel is transparent and exhibits a uniform reddish brown color, indicating that the organogel polymerization process is uniform and stable.
Fig. 2 is an optical photograph of a nanocomposite organogel dissolution process. From fig. 2, it can be seen that the organogel has good degradation performance, and the solution obtained after degradation is clear and uniform without precipitation.
Fig. 3 is an optical photograph of a nanocomposite polymer conductive film. As can be seen from fig. 3, the silver nanowire composite conductive film has high transparency and simultaneously has conductive performance.
Fig. 4 is an optical photograph of a responsive nanocomposite polymer conductive film responsive to an organic solvent. It can be seen from fig. 4 that the film exhibited rapid actuation of the acetone stimulus. Responsiveness to orientation in organic solvents. The oriented curled film can respond quickly after being placed in the steam environment of organic solvent, and can be flat after being stretched. After removal of the vapor environment of the organic solvent, the film rapidly curls again. This process is repeatable.
Fig. 5 is a scanning electron micrograph of a responsive nanocomposite polymer conductive film.
Detailed Description
The reagent raw materials and the equipment used in the invention are all commercial products and can be purchased through the market.
Example 1: preparation of metal nanomaterial dispersion
1. To a 100mL round bottom flask was added 0.6mL of 0.2m/L chloroauric acid and 48.4mL of deionized water, heated to 100 ℃ in an oil bath, stirred at constant temperature for 10min to mix well, then 1mL of 10% sodium citrate solution by mass was added, stirring was continued for 5min at 100 ℃, heat source was removed rapidly and cooled to room temperature. Transferring the solution into a beaker, adding 10mL of polyvinylpyrrolidone solution with mass fraction of 3%, washing with N, N-dimethylformamide, centrifuging, and dispersing into the N, N-dimethylformamide solution to obtain the metal nano material dispersion liquid with the shape of the wine red particles.
2. 5.86g of polyvinylpyrrolidone is added into 190mL of glycerol, stirred uniformly and then placed in a 90 ℃ environment for 5min to dissolve the polyvinylpyrrolidone completely. Then the temperature is reduced to 50 ℃, 1.58g of silver nitrate solution which is prepared by dissolving silver nitrate in 10mL of glycerol and 59mg of sodium chloride solution which is prepared by dissolving sodium chloride in 0.5mL of deionized water are sequentially added, and the temperature is raised to 210 ℃ after uniform stirring. After the heating was completed, 200mL of deionized water was added, and the mixture was cooled to room temperature and allowed to stand for precipitation. And removing the upper layer solution, re-dispersing the bottom layer precipitate with deionized water, washing with ethanol, centrifuging, and dispersing into the aqueous solution to obtain the metal nano material dispersion liquid with the nanowire morphology.
Example 2:
1. surface modification of metal nanomaterials
Mixing 0.235mol/L of the metal nanomaterial dispersion liquid with the particle morphology prepared in the step 1 of the example 1 with the functional modification 2-mercaptobenzimidazole respectively, wherein the added mass of the functional modification is 0.1% of that of the metal nanomaterial dispersion liquid, and carrying out ultrasonic treatment for 30s at room temperature to obtain a metal nanomaterial dispersion liquid with a modified surface;
2. preparation of organogels
Sequentially adding an organic monomer phenyl methacrylate and a photoinitiator 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone into the surface-modified metal nano material dispersion liquid obtained in the step 1 under the protection of nitrogen, carrying out ultrasonic treatment for 30s to uniformly mix the materials, and placing the materials in a vacuum drying oven for standing to remove oxygen dissolved in the solution; then placing the mixture in an ultraviolet lamp box for polymerization reaction for 25min, and cooling the mixture to room temperature to obtain the nano composite organic gel. The added volume of the organic monomer phenyl methacrylate is 80% of the volume of the mixed organic gel reaction liquid dispersion liquid. The flow rate of nitrogen was controlled at 0.7mL/s. The added mass of the photoinitiator 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone is 0.1 percent of the mass of the metal nano material dispersion liquid.
In the step, the surface-modified metal nano material is used as a responsive cross-linking agent to crosslink to form a gel network structure, and the cross-linking agent is not added, namely the surface-modified metal nano material is used as the cross-linking agent in the polymerization process.
Example 3: preparation of responsive nanocomposite polymer conductive films
The newly prepared nano composite organic gel is placed in N, N-dimethylformamide for dissolution, and the linear high polymer chain is dissolved out of the nano composite organic gel by utilizing the thermal dilution and the dissolubility of the nano composite organic gel, so that the linear poly (phenyl methacrylate) polymer chain dissolution liquid which is uniformly dispersed in an organic solvent is formed. And mixing the silver nanowire solution with the linear poly (phenyl methacrylate) polymer chain solution to form a precursor solution. Then the precursor solution is uniformly coated on a glass sheet, the glass sheet is placed in a vacuum drying oven at 70 ℃, the organic solvent in the organic film is removed, and then the organic film is separated from the glass substrate, so that the self-supporting and responsive nanocomposite polymer conductive film can be obtained.
The organogel used in the invention uses the dynamic coordination effect of metal and sulfur, uses the modified noble metal nano-composite as a cross-linking agent in the polymerization process, and adds a photoinitiator to enable uniform linear polymerization reaction to occur in the monomer polymerization process. And then pi-pi interaction between benzene rings on small molecules functionalized on the surface of the gold nanoparticle material and benzene rings on a poly (phenyl methacrylate) chain is utilized to generate a uniform and stable gel network structure, but the network structure of the gel has weak pi-pi interaction, so that the gel has better degradability. When the membrane is placed in acetone vapor, solvent molecules diffuse at a relatively rapid rate to the upper and lower surfaces of the porous membrane, which upper and lower surface regions experience expansion strain due to the interaction of the "solvent with the polymer chains within the membrane, and an increase in the osmotic pressure of the upper surface solvent results in more expansion than the bottom. The pore gradient produces a gradient of the action of the solvent with the polymer chains within the membrane, thereby producing a gradient of modulus, which in turn alters the curvature of the membrane. The conductive silver nanowire material and the organic gel solution are doped and mixed to endow the nano composite polymer film with conductive performance, so that the nano composite polymer conductive film has potential application in the aspects of physical sensing, detection, environmental monitoring and the like. The invention provides a simple and feasible method for preparing the responsive nano composite polymer conductive film, enriches the method for preparing the responsive conductive film, and lays a good foundation for the future application of the type of material in the fields of responders, drivers, actuators and the like.
Claims (7)
1. A preparation method of a responsive nano composite polymer conductive film is characterized in that:
firstly, compositing small molecules containing functional groups with a metal nano material in a dynamic covalent bond mode to obtain a nano composite; then, the nanocomposite is subjected to free radical polymerization reaction rapidly under the stimulation of external environment by adding an initiator in the presence of a polymerizable monomer, so that nanocomposite organogel can be obtained; after the nanocomposite organic gel is dissolved in an organic solvent, a precursor solution formed by mixing the nanocomposite organic gel and the conductive metal nanowire is coated on a substrate, and the solvent is dried, so that a responsive nanocomposite polymer conductive film is finally obtained;
the network aperture structure of the nano composite polymer conductive film has hierarchical regularity, and shows that the network aperture near the upper surface of air is small, the network aperture near the lower surface of a substrate is large, and the regularity is increased from the upper surface to the lower surface;
the preparation method comprises the following steps:
step 1: functional surface modification of gold nanoparticles
Adding a functional modifier into the metal nano material dispersion liquid, and performing ultrasonic treatment at room temperature for 30s to enable thiol small molecules to be adsorbed on the surfaces of the metal nano particles successfully, so as to obtain the surface modified functional metal nano particle dispersion liquid;
step 2: preparation of nanocomposite organogels
Under the protection of nitrogen, adding a liquid organic monomer and a photoinitiator into the surface-modified functional metal nanoparticle dispersion liquid obtained in the step 1, uniformly mixing by ultrasound, placing in a vacuum drying oven, removing oxygen dissolved in the solution, then placing in an ultraviolet lamp box for polymerization reaction for 30min, and cooling to room temperature to obtain the nanocomposite organogel;
step 3: preparation of nanocomposite polymer conductive films
Dissolving the newly prepared nano composite organic gel in an organic solvent, and dissolving the linear high polymer chains from the nano composite organic gel by utilizing the thermal dilution and the solubility of the nano composite organic gel to form a linear high polymer chain solution which is uniformly dispersed in the organic solvent; then mixing the metal nanoparticle solution with the linear high polymer chain solution to form a precursor solution; then the precursor solution is uniformly coated on a substrate, the substrate is placed in a vacuum drying oven, the organic solvent in the organic film is removed, and then the organic film is separated from the substrate, so that the self-supporting and responsive nano composite polymer conductive film can be obtained.
2. The method of manufacturing according to claim 1, characterized in that:
in the step 1, the metal nano material is a gold nano particle material with a zero-dimensional sphere; the concentration of the functional metal nanoparticle dispersion liquid is 0.1-1.0mg/mL.
3. The method of manufacturing according to claim 1, characterized in that:
in the step 1, the functional modification body is a functional micromolecule containing sulfhydryl and benzene ring, and the ratio of the added mass to the volume of the metal nano material dispersion liquid is 5mg/mL.
4. The method of manufacturing according to claim 1, characterized in that:
in the step 2, the organic monomer is phenyl methacrylate, and the added volume of the organic monomer is 80% of the volume of the mixed organic gel reaction solution.
5. The method of manufacturing according to claim 1, characterized in that:
in the step 2, the photoinitiator is 2-hydroxy-4' - (2-hydroxyethoxy) -2-methyl propiophenone, and the addition mass of the photoinitiator is 0.1% of the mass of the metal nano material dispersion liquid.
6. The method of manufacturing according to claim 1, characterized in that:
in the step 3, the organic solvent is selected from N, N-dimethylformamide or dichloromethane, and the ratio of the added volume of the organic solvent to the volume of the nanocomposite organogel is 10:1.
7. The method of manufacturing according to claim 1, characterized in that:
in the step 3, the metal nano particles are silver nano wires in a one-dimensional linear shape; the concentration of the metal nanoparticles in the precursor solution after mixing was 5mg/mL.
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