CN113758975A - Laser-induced graphene/metal oxide sensitive material and preparation method thereof - Google Patents
Laser-induced graphene/metal oxide sensitive material and preparation method thereof Download PDFInfo
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- CN113758975A CN113758975A CN202111059749.XA CN202111059749A CN113758975A CN 113758975 A CN113758975 A CN 113758975A CN 202111059749 A CN202111059749 A CN 202111059749A CN 113758975 A CN113758975 A CN 113758975A
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- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention provides a laser-induced graphene/metal oxide sensitive material and a preparation method thereof, and relates to the technical field of graphene preparation. The preparation method provided by the invention comprises three steps of preparation of a metal salt doped precursor suspension, preparation of a PI film and laser treatment, the graphene/metal oxide sensitive material is synthesized in situ by a method with simple process and low cost, and the graphene/metal oxide sensitive material prepared by the method has better conductivity; meanwhile, the hierarchical structure of the metal oxide and the three-dimensional network structure of the graphene are connected with each other, so that the specific surface area and the porosity of the material can be greatly improved, and the sensitivity to gas response is improved. The graphene/metal oxide sensitive material synthesized by the method can be patterned by laser to prepare sensitive materials with any patterns, such as electrodes with different shapes, so as to adapt to different application scenes.
Description
Technical Field
The invention relates to the technical field of graphene preparation, in particular to a laser-induced graphene/metal oxide sensitive material and a preparation method thereof.
Background
Graphene is a novel two-dimensional carbon nanomaterial with a single-layer sheet structure composed of carbon atoms, and has a larger specific surface area and higher chemical stability than Carbon Nanotubes (CNTs) and fullerenes (C60). Graphene is not only the thinnest of the known materials, but is also very strong and rigid, as a simple substance, it transports electrons faster at room temperature than known conductors. Graphene has attracted considerable attention in the field of material research by virtue of its excellent electrical, mechanical and thermal properties.
On the basis of excellent performances of graphene, researchers prepare graphene composite materials with different functions by utilizing the characteristics of graphene, so that different application requirements are met. The composite material of graphene and metal oxide is widely researched, is compounded with different metal oxides, and can realize effective functionalization of graphene while maintaining excellent performance of graphene. The metal oxide semiconductor is a common gas sensitive material, with the appearance of graphene/metal oxide sensitive materials, the addition of the graphene improves the conductivity of the original metal oxide, the sensitivity and selectivity of the compounded sensitive material to gas response are obviously improved, and meanwhile, the working temperature of the sensor can be reduced, so that the sensor can work at room temperature. Graphene/metal oxide sensitive materials exhibit non-negligible advantages, which confer new properties and functions to the materials and provide possibilities for further applications.
However, the existing method for preparing the graphene/metal oxide sensitive material has complex process and low efficiency. For example: the hydrothermal method uses a high-pressure reaction kettle as a reactor, uses a solvent (water) as a reaction medium, and synthesizes graphene/metal oxide by using hydrolytic crystallization of metal salts in a high-temperature and high-pressure environment, however, the hydrothermal method has high requirements on temperature and pressure environment, and the preparation process is complex. The electrochemical deposition method utilizes the electric field to deposit the metal oxide from the aqueous solution thereof to synthesize the graphene/metal oxide, and the result shows that the formation of oxide particles is not facilitated due to too short deposition time, and the stability of the composite is affected due to too much oxide loading caused by too long deposition time, so that the electrochemical deposition method needs to find a proper deposition time and has a complex process.
Disclosure of Invention
The invention aims to provide a laser-induced graphene/metal oxide sensitive material and a preparation method thereof.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a laser-induced graphene/metal oxide sensitive material, which comprises the following steps:
mixing polyimide, metal salt, water and an adhesive to obtain a metal salt doped precursor suspension;
coating the metal salt doped precursor suspension on a substrate, and drying to obtain a PI film;
and carrying out laser treatment on the PI film to obtain the graphene/metal oxide sensitive material.
Preferably, the metal salt comprises one or more of tin salt, iron salt, copper salt, magnesium salt, barium salt, manganese salt and zinc salt.
Preferably, the mass ratio of the polyimide to the metal salt is 25: 1-5.
Preferably, the binder is sodium carboxymethyl cellulose.
Preferably, the mass ratio of the polyimide to the adhesive is 8-12: 1.
Preferably, the drying temperature is 30-50 ℃; the drying time is 2.5-4 h.
Preferably, the thickness of the PI film is 0.15-0.3 mm.
Preferably, the temperature of the laser treatment is 500-700 ℃.
The invention provides a graphene/metal oxide sensitive material prepared by the preparation method in the technical scheme, which comprises porous graphene and metal oxide loaded on the porous graphene.
Preferably, the average pore diameter of the porous graphene is 6-12 μm.
Compared with the prior art, the method for preparing the laser-induced graphene/metal oxide sensitive material has the advantages that the graphene/metal oxide sensitive material is synthesized in situ by a method with simple process and low cost, the graphene/metal oxide sensitive material prepared by the method has better conductivity, and the diagonal resistance of a 5 mm-5 mm square at the upper right corner of a test illustration 1 is 50 ohms. Meanwhile, the hierarchical structure of the metal oxide and the three-dimensional network structure of the graphene are connected with each other, so that the specific surface area and the porosity of the material can be greatly improved, and the sensitivity to gas response is improved. The graphene/metal oxide sensitive material synthesized by the method can be patterned by laser to prepare sensitive materials with any patterns, such as electrodes with different shapes (shown in figure 2), so as to adapt to different application scenes.
Drawings
FIG. 1 is a schematic diagram of the graphene/metal oxide sensitive material prepared in examples 1-4;
FIG. 2 is the graphene/Fe prepared in example 52O3Schematic representation of the sensitive material.
Detailed Description
The invention provides a preparation method of a laser-induced graphene/metal oxide sensitive material, which comprises the following steps:
mixing polyimide, metal salt, water and an adhesive to obtain a metal salt doped precursor suspension;
coating the metal salt doped precursor suspension on a substrate, and drying to obtain a PI film;
and carrying out laser treatment on the PI film to obtain the graphene/metal oxide sensitive material.
In the present invention, unless otherwise specified, the starting materials for the preparation are all commercially available products well known to those skilled in the art.
The preparation method comprises the step of mixing polyimide, metal salt, water and an adhesive to obtain a metal salt doped precursor suspension. In the present invention, the Polyimide (PI) is preferably in a powder form; the average particle diameter of the polyimide powder is preferably 10 to 20 μm, and more preferably 15 μm. In the invention, the metal salt preferably comprises one or more of tin salt, iron salt, copper salt, magnesium salt, barium salt, manganese salt and zinc salt; the tin salt is preferably tin tetrachloride; the ferric salt is preferably ferric trichloride; the copper salt is preferably copper chloride; the magnesium salt is preferably magnesium chloride; the barium salt is preferably barium chloride; the manganese salt is preferably manganese chloride; the zinc salt is preferably zinc chloride. In the present invention, the mass ratio of the polyimide to the metal salt is preferably 25:1 to 5, and more preferably 25:3 to 4.
In the present invention, the water is preferably deionized water. In the present invention, the binder is preferably sodium carboxymethyl cellulose. In the invention, the adhesive can bond the PI powder together, so that the synthesized PI film has better film-forming property. In the invention, the mass ratio of the polyimide to the adhesive is preferably 8-12: 1, and more preferably 10: 1.
In the present invention, the polyimide, metal salt, water and binder mixture preferably includes: performing first mixing on polyimide, metal salt and part of water to obtain a PI/metal salt solution; secondly mixing the adhesive and the residual water to obtain an adhesive aqueous solution; and carrying out third mixing on the PI/metal salt solution and the adhesive aqueous solution. In the present invention, the time of the first mixing is preferably 20 min; the mass fraction of the metal salt in the PI/metal salt solution is preferably 1-5 wt%, and more preferably 2-4 wt%. In the present invention, the mass fraction of the aqueous binder solution is preferably 1 wt%. In the present invention, the time for the third mixing is preferably 3 hours.
After the metal salt doped precursor suspension is obtained, the PI film is obtained by coating the metal salt doped precursor suspension on a substrate and drying. In the present invention, the substrate is preferably filter paper. In the present invention, the method of coating is preferably droplet coating. In the invention, the drying temperature is preferably 30-50 ℃, and more preferably 40 ℃; the drying time is preferably 2.5-4 h, and more preferably 3 h.
In the present invention, the thickness of the PI film is preferably 0.15 to 0.3mm, and more preferably 0.2 mm.
After the PI film is obtained, the PI film is subjected to laser treatment to obtain the graphene/metal oxide sensitive material. In the present invention, the laser treatment is preferably performed in a laser engraving machine. In the invention, the laser power of the laser treatment is adjustable within 0-100%, and the engraving depth is adjustable within 0-100%. In the present invention, the larger the number of engraving depths, the darker the final engraved color, and the slower the engraving speed. In the invention, the laser light source can print any pattern and can ablate the PI film at any position, thereby realizing the patterning of the graphene/metal oxide sensitive material. In the specific embodiment of the invention, the PI film is placed under a laser engraving machine, and a corresponding pattern is printed by selecting proper laser power and engraving depth.
In the invention, the temperature of the laser treatment is preferably 500-700 ℃, and more preferably 600 ℃. In the laser processing process, PI is converted into graphene through laser high-temperature processing, and metal salt in a PI film is contacted with oxygen at high temperature to react to generate metal oxide, so that the graphene/metal oxide sensitive material is obtained.
The invention also provides the graphene/metal oxide sensitive material prepared by the preparation method in the technical scheme. In the invention, the graphene/metal oxide sensitive material comprises porous graphene and metal oxide loaded on the porous graphene. In the invention, the average pore diameter of the porous graphene is preferably 6-12 μm. In the present invention, the metal oxide refers to a binary compound composed of oxygen and another metal chemical element; the metal oxide preferably comprises one or more of iron oxide, ferroferric oxide, tin oxide, magnesium oxide, barium oxide, copper oxide, zinc oxide and manganese oxide.
In the invention, the specific surface area of the graphene/metal oxide sensitive material is preferably 80m2The porosity is preferably 70%/g.
The graphene/metal oxide sensitive material provided by the invention can provide more adsorption active sites for gas.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
Example 1
2.5g of PI powder and 0.5g of crystalline stannic chloride pentahydrate were added to 10mL of deionized water and stirred for 20 minutes to obtain PI/SnCl4A solution; 25g of a 1% by weight aqueous solution of sodium carboxymethylcellulose are then added to the PI/SnCl4Stirring in the solution for 3 hours continuously to obtain SnCl4Doping the PI suspension.
Adding the SnCl4Uniformly dripping the doped PI suspension on filter paper to form doped SnCl4The polyimide film was dried in a drying oven at a constant temperature of 40 ℃ for 3 hours to obtain a PI film having a thickness of 0.2 mm.
Placing the PI film under a laser engraving machine, adjusting the laser power to 35% and the engraving depth to 45%, printing a square pattern shown in figure 1, processing the PI film into graphene through laser high temperature, and processing SnCl in the PI film4Reacting to generate SnO through high temperature and oxygen contact2Thereby obtaining graphene/SnO2A sensitive material.
Example 2
2.5g of PI powder and 0.5g of iron trichloride (FeCl)3) Adding the mixture into 10mL of deionized water, and stirring for 20 minutes to obtain PI/FeCl3A solution; 25g of a 1 wt% aqueous solution of carboxymethylcellulose are then added to the PI/FeCl3Stirring in the solution for 3 hours continuously to obtain FeCl3Doping the PI suspension.
Subjecting the FeCl3The doped PI suspension is uniformly dripped on filter paper to form doped FeCl3The polyimide film was dried in a drying oven at a constant temperature of 40 ℃ for 3 hours to obtain a PI film having a thickness of 0.2 mm.
Placing the PI film under a laser engraving machine, adjusting the laser power to 35% and the engraving depth to 45%, and printing to obtain the PI film shown in figure 1The PI is changed into graphene through laser high-temperature treatment, and FeCl in the PI film3The Fe is generated by the reaction of high temperature and oxygen contact2O3Thereby obtaining graphene/Fe2O3A sensitive material.
Example 3
2.5g of PI powder and 0.5g of magnesium chloride (MgCl)2) Adding the mixture into 10mL of deionized water, and stirring for 20 minutes to obtain PI/MgCl2A solution; 25g of a 1% by weight aqueous solution of carboxymethylcellulose are then added to the PI/MgCl2Stirring the solution for 3 hours to obtain MgCl2Doping the PI suspension.
Reacting said MgCl2The doped PI suspension was uniformly drop-coated onto filter paper to form doped MgCl2The polyimide film was dried in a drying oven at a constant temperature of 40 ℃ for 3 hours to obtain a PI film having a thickness of 0.2 mm.
Placing the PI film under a laser engraving machine, adjusting the laser power to 35% and the engraving depth to 45%, printing a square pattern shown in figure 1, converting PI into graphene through laser high-temperature treatment, and MgCl in the PI film2And reacting at high temperature and under oxygen contact to generate MgO, thereby obtaining the graphene/MgO sensitive material.
Example 4
2.5g of PI powder and 0.5g of copper chloride (CuCl)2) Adding the mixture into 10mL of deionized water, and stirring for 20 minutes to obtain PI/CuCl2A solution; 25g of a 1% by weight aqueous solution of carboxymethylcellulose are then added to the PI/CuCl2Stirring in the solution for 3 hours continuously to obtain CuCl2Doping the PI suspension.
Adding the CuCl2The doped PI suspension was uniformly drop-coated onto filter paper to form doped CuCl2The polyimide film was dried in a drying oven at a constant temperature of 40 ℃ for 3 hours to obtain a PI film having a thickness of 0.2 mm.
Placing the PI film under a laser engraving machine, adjusting the laser power to 35% and the engraving depth to 45%, printing a square pattern shown in figure 1, converting PI into graphene through laser high-temperature treatment, and preparing CuCl in the PI film2By reaction at high temperature and oxygen contactCuO should be generated, thereby obtaining the graphene/CuO sensitive material.
Example 5
2.5g of PI powder and 0.5g of iron trichloride (FeCl)3) Adding the mixture into 10mL of deionized water, and stirring for 20 minutes to obtain PI/FeCl3A solution; 25g of a 1 wt% aqueous solution of carboxymethylcellulose are then added to the PI/FeCl3Stirring in the solution for 3 hours continuously to obtain FeCl3Doping the PI suspension.
Subjecting the FeCl3The doped PI suspension is uniformly dripped on filter paper to form doped FeCl3The polyimide film was dried in a drying oven at a constant temperature of 40 ℃ for 3 hours to obtain a PI film having a thickness of 0.2 mm.
Placing the PI film under a laser engraving machine, adjusting the laser power to be 35%, the engraving depth to be 45, setting a printing area to be an interdigital electrode pattern, processing the PI film into graphene through laser high temperature, and enabling FeCl in the PI film3The Fe is generated by the reaction of high temperature and oxygen contact2O3Thereby obtaining graphene/Fe2O3Electrodes as shown in fig. 2.
In the above examples 1 to 4, the gray part in fig. 1 is the synthesized PI thin film, and the black part is the metal oxide doped Laser Induced Graphene (LIG) formed after the PI thin film is subjected to laser treatment.
Example 5 in FIG. 2, the grey part is the synthesized PI film, and the black part is the graphene/Fe formed by laser processing the PI film2O3And an electrode.
The preparation method provided by the invention has low cost and is simple, the doping of the metal oxide and the formation of the porous graphene can be simultaneously realized by laser, meanwhile, the laser treatment has the advantages of imaging and the like, and the possibility is provided for realizing different application scenes.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. A preparation method of a laser-induced graphene/metal oxide sensitive material comprises the following steps:
mixing polyimide, metal salt, water and an adhesive to obtain a metal salt doped precursor suspension;
coating the metal salt doped precursor suspension on a substrate, and drying to obtain a PI film;
and carrying out laser treatment on the PI film to obtain the graphene/metal oxide sensitive material.
2. The preparation method according to claim 1, wherein the metal salt comprises one or more of tin salt, iron salt, copper salt, magnesium salt, barium salt, manganese salt and zinc salt.
3. The method according to claim 1 or 2, wherein the mass ratio of the polyimide to the metal salt is 25:1 to 5.
4. The method of claim 1, wherein the binder is sodium carboxymethyl cellulose.
5. The preparation method according to claim 1 or 4, wherein the mass ratio of the polyimide to the binder is 8-12: 1.
6. The method according to claim 1, wherein the drying temperature is 30 to 50 ℃; the drying time is 2.5-4 h.
7. The method according to claim 1, wherein the thickness of the PI film is 0.15 to 0.3 mm.
8. The method according to claim 1 or 7, wherein the temperature of the laser treatment is 500 to 700 ℃.
9. The graphene/metal oxide sensitive material prepared by the preparation method of any one of claims 1 to 8 comprises porous graphene and metal oxide loaded on the porous graphene.
10. The graphene/metal oxide sensitive material according to claim 9, wherein the average pore diameter of the porous graphene is 6-12 μm.
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| CN115161624A (en) * | 2022-07-19 | 2022-10-11 | 广东工业大学 | Coating method based on laser-induced zirconium-doped graphene |
| CN115420393A (en) * | 2022-09-06 | 2022-12-02 | 河北工业大学 | Preparation method of gas-temperature sensor |
| CN117142535A (en) * | 2023-06-28 | 2023-12-01 | 天津大学 | Universal method for synthesizing metal oxide/graphene composite material by one step through laser induction |
| CN117226806A (en) * | 2023-09-26 | 2023-12-15 | 广东工业大学 | Cluster magnetic control micro-nano robot and preparation method thereof |
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| CN115161624A (en) * | 2022-07-19 | 2022-10-11 | 广东工业大学 | Coating method based on laser-induced zirconium-doped graphene |
| CN115420393A (en) * | 2022-09-06 | 2022-12-02 | 河北工业大学 | Preparation method of gas-temperature sensor |
| CN115420393B (en) * | 2022-09-06 | 2024-03-15 | 河北工业大学 | Preparation method of gas-temperature sensor |
| CN117142535A (en) * | 2023-06-28 | 2023-12-01 | 天津大学 | Universal method for synthesizing metal oxide/graphene composite material by one step through laser induction |
| CN117226806A (en) * | 2023-09-26 | 2023-12-15 | 广东工业大学 | Cluster magnetic control micro-nano robot and preparation method thereof |
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