CN111883314A - Preparation method of oxidized cellulose-graphene nanoribbon-MXene composite conductive film - Google Patents
Preparation method of oxidized cellulose-graphene nanoribbon-MXene composite conductive film Download PDFInfo
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Abstract
The invention discloses a preparation method of a cellulose oxide-graphene nanoribbon-MXene composite conductive film, which comprises the following steps: 1) treating cellulose by a TEMPO oxidation method to obtain oxidized cellulose dispersion liquid; 2) dispersing the multi-walled carbon nano-tube in concentrated sulfuric acid, oxidizing by using potassium permanganate, and decompressing to obtain a graphene nano-belt; 3) preparing an MXene aqueous solution with a certain concentration, and dispersing by using liquid nitrogen to obtain a single-layer MXene dispersion liquid; 4) and blending the oxidized cellulose dispersion liquid, the graphene nanoribbon and the MXene dispersion liquid according to a certain proportion, and obtaining the oxidized cellulose-graphene nanoribbon-MXene composite conductive film by a vacuum filtration method. The invention has simple process, convenient operation and environmental protection; the prepared film has excellent flexibility and conductivity, good biocompatibility and mechanical property, and can be used for the fields of wearable sensor manufacturing, biological detection and the like.
Description
Technical Field
The invention relates to a preparation method of a composite conductive film material, in particular to a preparation method of a cellulose oxide-graphene nanobelt-MXene composite conductive film.
Background
With the development of wearable and portable electronic devices, many new requirements are put on the development of conductive materials, and the low thickness, low density, flexibility and high mechanical strength are very important for the application of the conductive materials in the wearable and portable electronic devices.
MXene (denoted as M)n+1XnTxWherein M represents an early transition metal, X represents C and/or N, TxIs the end group deposited on MXene during synthesis) is a novel two-dimensional (2D) transition metal carbide and/or nitride. Interest has been shown for their excellent electrochemical properties, hydrophilicity and metal conductivity, but their poor mechanical strength and flexibility limit their use in wearable and portable electronic devices.
The graphene nanoribbon is used as a quasi-one-dimensional carbon-based nanomaterial, and the good physical and chemical properties of the carbon nanoribbon, such as chemical stability, mechanical properties, conductivity and the like, are continued. Compared with graphene and carbon nanotubes, the graphene nanoribbon has the characteristics of more flexibility and adjustability due to the extremely high length-width ratio and the special edge effect. The special properties endow the graphene nanoribbon with very wide application value in the fields of energy storage, field effect transistors, electronic sensing and the like.
Cellulose has various advantages of good hydrophilicity, biodegradability, flexibility, excellent mechanical strength and the like, and is widely applied to various flexible base materials and reinforcing phase fillers at present. TEMPO oxidation is a green and environment-friendly cellulose pretreatment means, and a large amount of carboxylic acid groups with anionic charges can be generated on the surface of cellulose fibers through a carboxylation process induced by TEMPO oxidation, so that single nanofibers are fully suspended, effective contact among electroactive materials can be increased, and the method is very attractive in the field of functional composite materials. The abundant functional groups on the fiber provide interaction sites, and can be combined with MXene nano-sheets and graphene nano-ribbons through strong hydrogen bonds, so that a continuous conductive path is constructed. Therefore, the research on the preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film has important significance on the development of conductive materials.
Disclosure of Invention
The purpose of the invention is as follows: aiming at the defects of the prior art, the invention prepares the oxidized cellulose-graphene nanoribbon-MXene composite conductive film by using cellulose as a raw material through a method with simple process, convenient operation and environmental protection. The film has excellent flexibility and conductivity, good biocompatibility and mechanical property. In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
the oxidized cellulose-graphene nanoribbon-MXene composite conductive film has excellent flexibility and conductivity, good biocompatibility and mechanical properties.
1. A preparation method of a cellulose oxide-graphene nanoribbon-MXene composite conductive film comprises the following steps:
1) dispersing cellulose into deionized water, adding TEMPO and NaBr, dropwise adding a NaClO solution into a beaker, and adjusting the pH value by using a NaOH solution; and after the reaction is finished, adding ethanol, adding HCl solution for acidification to obtain oxidized cellulose, and ultrasonically dispersing the oxidized cellulose into deionized water.
The mass ratio of TEMPO to NaBr is 1: 5 to 1: 10;
the mass of the cellulose is 0.5-3 g;
the concentration of the NaClO solution is 7-14%;
the volume of the NaClO solution is 80-100 mL;
the concentration of the NaOH solution is 0.2-1M;
the pH is 10-10.5;
the reaction time is 10-16 hours;
the concentration of HCl is 0.05-0.5M;
the concentration of the oxidized cellulose suspension is 0.5-4%.
2) Dispersing multi-wall carbon nano-tube in concentrated H2SO4To which KMnO was slowly added4Heating the mixture to complete the reactionPost-addition of H-containing2O2And (4) standing the mixture in ice water. Centrifuging the graphene nano-belt dispersion liquid, and finally dispersing the graphene nano-belt dispersion liquid in ethanol to obtain the graphene nano-belt dispersion liquid.
The mass of the multi-walled carbon nano tube is 0.5-4 g;
said rich H2SO4The volume is 80-100 mL;
the KMnO4The mass is 3-5 g;
the reaction temperature is 60-80 ℃;
the reaction time is 4-8 hours;
said H2O2The volume ratio of the water to the ice water is 1: 100 to 1: 20;
the centrifugal rotating speed is 8000-12000 rpm;
the centrifugation time is 10-20 minutes;
the concentration of the graphene nanoribbon dispersion liquid is 0.5-2%.
3) And dispersing the multilayer MXene nanosheets in deionized water, placing the multilayer MXene nanosheets in liquid nitrogen, thawing at room temperature, and repeating the process to obtain the monolayer MXene nanosheet dispersion liquid.
The concentration of the single-layer MXene dispersion liquid is 0.1-0.5%;
the liquid nitrogen treatment time is 10-30 minutes;
the repetition frequency is 6-10 times.
4) Blending the prepared oxidized cellulose dispersion liquid, the graphene nanobelt dispersion liquid and the single-layer MXene dispersion liquid; and obtaining the oxidized cellulose-graphene nanoribbon-MXene composite conductive film by a vacuum filtration method.
The mass ratio of the oxidized cellulose dispersion liquid to the graphene nanoribbon dispersion liquid is 5: 1-1: 1;
the mass ratio of the oxidized cellulose dispersion liquid to the single-layer MXene dispersion liquid is 8: 1-2: 1.
The volume of the blending liquid is 20-50 mL.
The preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film comprises the step of preparing the oxidized cellulose-graphene nanoribbon-MXene composite conductive film, wherein the cellulose is cotton pulp cellulose, bamboo pulp cellulose or bacterial cellulose.
The preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film is characterized in that the oxidized cellulose is a nano-grade fiber, and the diameter of the oxidized cellulose is 10-200 nanometers.
The graphene nanoribbon in the preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite film has a width of 30-50 nanometers.
The preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite film is characterized in that the MXene nanosheet is a single layer, and the diameter of the MXene nanosheet is 2-5 microns.
The thickness of the conductive film in the preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite film is 20-100 micrometers.
According to the invention, the oxidized cellulose-graphene nanoribbon-MXene composite conductive film is obtained through a simple process design. The composite film has the obvious advantages that: the cellulose nano-fiber subjected to TEMPO oxidation treatment has very good dispersibility in water, can promote graphene nano-ribbons and MXene to be fully dispersed and contacted in a solvent, and effectively exposes the active edges of the graphene nano-ribbons and the MXene nano-sheets; the graphene nanoribbon and MXene both have excellent conductivity, the overall conductivity of the composite film can be obviously improved, the structure and the uniform distribution of the layers of the film are favorable for ion migration in the electrochemical reaction process, the graphene nanoribbon and the MXene are effectively compounded, and the novel conductive material with low thickness, low density, high biocompatibility, high flexibility and high mechanical strength can be constructed.
Has the advantages that: compared with the prior art, the preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film is simple to operate, easy to control, green, environment-friendly and easy for large-scale production; the prepared conductive composite film has the advantages of low thickness, low density, high biocompatibility, high flexibility, high mechanical strength, good electrical property and the like.
Drawings
Fig. 1 is an appearance and flexibility display of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film prepared in example 1;
fig. 2 is an effect diagram of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film prepared in example 1 for lighting an LED lamp.
Detailed Description
The present invention will be further described with reference to specific examples, but the present invention is not limited to these examples.
Example 1
Dispersing 2g of bacterial cellulose in deionized water, adding TEMPO and NaBr (the mass ratio is 1: 10), dropwise adding 80mL of NaClO solution with the mass fraction of 14% into a beaker, dropwise adding 0.5M NaOH to keep the pH of the system at 10, and reacting for 12 hours; adding ethanol to finish reaction, adding excessive 0.1M HCl for acidification to obtain oxidized cellulose, and performing ultrasonic dispersion in deionized water to obtain 1% oxidized cellulose suspension; 0.5g of multiwall carbon nanotubes dispersed in 80mL of concentrated H2SO4To this was slowly added 2.5g KMnO4Heating to 60 ℃ for reaction for 6 hours; after the reaction was complete, 500mL of 5 mLH-containing solution was added2O2And (4) standing the mixture in ice water. The graphene nano-belt dispersion liquid is centrifuged at 8000rpm for 10 minutes and finally dispersed in ethanol to obtain the graphene nano-belt dispersion liquid with the concentration of 1%. And dispersing the multiple layers of MXene nanosheets in deionized water to obtain an MXene dispersion liquid with the concentration of 0.2%. Placing the MXene dispersion liquid in liquid nitrogen for 10 minutes, then unfreezing at room temperature, and repeating the process for 6 times to obtain a monolayer MXene dispersion liquid; blending the prepared oxidized cellulose suspension, the graphene nanobelt dispersion and the single-layer MXene dispersion according to the mass ratio of 2: 1, and uniformly stirring; and finally, preparing the composite conductive film from 15mL of the blending solution by a vacuum filtration method.
Example 2
Dispersing 1.2g of cotton pulp cellulose in deionized water, adding TEMPO and NaBr (the mass ratio is 1: 5), dropwise adding 85mL of NaClO solution with the mass fraction of 7% into a beaker, dropwise adding 1M NaOH to keep the pH of the system at 10.5, and reacting for 14 hours; adding ethanol to complete the reaction, adding excessive 0.5M HCl for acidification to obtain oxidized cellulose, and dispersing in deionized water by ultrasonic wave to obtain2.5% of an oxidized cellulose suspension; 2g of multiwalled carbon nanotubes dispersed in 90mL of concentrated H2SO4To this was slowly added 5g of KMnO4Heating to 80 ℃ for reaction for 4 hours; after the reaction was complete, 200mL of 10 mLH-containing solution was added2O2And (4) standing the mixture in ice water. The graphene nanoribbon dispersion solution is centrifuged at 12000rpm for 20 minutes and finally dispersed in ethanol to obtain a graphene nanoribbon dispersion solution with the concentration of 2%. And dispersing the multiple layers of MXene nanosheets in deionized water to obtain an MXene dispersion liquid with the concentration of 0.4%. Placing the MXene dispersion liquid in liquid nitrogen for 30 minutes, then unfreezing at room temperature, and repeating the process for 8 times to obtain a monolayer MXene dispersion liquid; blending the prepared oxidized cellulose suspension, the graphene nanobelt dispersion and the single-layer MXene dispersion according to the mass ratio of 5: 1, and uniformly stirring; and finally, preparing the composite conductive film from 40mL of the blending solution by a vacuum filtration method.
Example 3
Dispersing 3g of wood pulp cellulose in deionized water, adding TEMPO and NaBr (the mass ratio is 1: 8), dropwise adding 90mL of NaClO solution with the mass fraction of 10% into a beaker, dropwise adding 0.8M NaOH to keep the pH of the system at 10.5, and reacting for 16 hours; adding ethanol to finish reaction, adding excessive 0.4M HCl for acidification to obtain oxidized cellulose, and performing ultrasonic dispersion in deionized water to obtain 4% oxidized cellulose suspension; 4g of multiwalled carbon nanotubes dispersed in 100mL of concentrated H2SO4To this was slowly added 4.5g KMnO4Heating to 75 ℃ for reaction for 7 hours; after the reaction was complete, 400mL of 15 mLH-containing solution was added2O2And (4) standing the mixture in ice water. The graphene nanoribbon dispersion liquid is centrifuged at 10000rpm for 15 minutes and finally dispersed in ethanol to obtain the graphene nanoribbon dispersion liquid with the concentration of 1.5%. And dispersing the multiple layers of MXene nanosheets in deionized water to obtain an MXene dispersion liquid with the concentration of 0.5%. Placing the MXene dispersion liquid in liquid nitrogen for 25 minutes, then unfreezing at room temperature, and repeating the process for 7 times to obtain a monolayer MXene dispersion liquid; blending the prepared oxidized cellulose suspension, the graphene nanobelt dispersion and the single-layer MXene dispersion according to the mass ratio of 8: 2: 1, and uniformly stirring; and finally, preparing the composite conductive film from 50mL of the blending solution by a vacuum filtration method.
Example 4
Dispersing 0.5g of bacterial cellulose in deionized water, adding TEMPO and NaBr (the mass ratio is 1: 6), dropwise adding 100mL of NaClO solution with the mass fraction of 12% into a beaker, dropwise adding 0.6M NaOH to keep the pH of the system at 10, and reacting for 10 hours; adding ethanol to finish reaction, adding excessive 0.2M HCl for acidification to obtain oxidized cellulose, and performing ultrasonic dispersion in deionized water to obtain 3% oxidized cellulose suspension; 3g of multiwall carbon nanotubes dispersed in 95mL of concentrated H2SO4To this was slowly added 4g KMnO4Heating to 70 ℃ for reaction for 8 hours; after the reaction was complete, 250mL of 8mLH2O2And (4) standing the mixture in ice water. The graphene nanoribbon dispersion solution was centrifuged at 12000rpm for 12 minutes and finally dispersed in ethanol to obtain a graphene nanoribbon dispersion solution with a concentration of 0.5%. And dispersing the multiple layers of MXene nanosheets in deionized water to obtain an MXene dispersion liquid with the concentration of 0.3%. Placing the MXene dispersion liquid in liquid nitrogen for 20 minutes, then unfreezing at room temperature, and repeating the process for 8 times to obtain a monolayer MXene dispersion liquid; blending the prepared oxidized cellulose suspension, the graphene nanobelt dispersion and the single-layer MXene dispersion according to the mass ratio of 8: 4: 3, and uniformly stirring; and finally, preparing the composite conductive film from 30mL of the blending solution by a vacuum filtration method.
Claims (7)
1. The preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film is characterized in that the composite conductive film has excellent flexibility and conductivity, and good biocompatibility and mechanical properties.
2. The preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film as claimed in claim 1, characterized by comprising the following steps:
1) dispersing cellulose into deionized water, adding TEMPO and NaBr, dropwise adding a NaClO solution into a beaker, and adjusting the pH value by using a NaOH solution; and after the reaction is finished, adding ethanol, adding HCl solution for acidification to obtain oxidized cellulose, and ultrasonically dispersing the oxidized cellulose into deionized water.
The mass ratio of TEMPO to NaBr is 1: 5 to 1: 10;
the mass of the cellulose is 0.5-3 g;
the concentration of the NaClO solution is 7-14%;
the volume of the NaClO solution is 80-100 mL;
the concentration of the NaOH solution is 0.2-1M;
the pH is 10-10.5;
the reaction time is 10-16 hours;
the concentration of HCl is 0.05-0.5M;
the concentration of the oxidized cellulose suspension is 0.5-4%.
2) Dispersing multi-wall carbon nano-tube in concentrated H2SO4To which KMnO was slowly added4Heating, adding H-containing solution after the reaction is finished2O2And (4) standing the mixture in ice water. Centrifuging the graphene nano-belt dispersion liquid, and finally dispersing the graphene nano-belt dispersion liquid in ethanol to obtain the graphene nano-belt dispersion liquid.
The mass of the multi-walled carbon nano tube is 0.5-4 g;
said rich H2SO4The volume is 80-100 mL;
the KMnO4The mass is 3-5 g;
the reaction temperature is 60-80 ℃;
the reaction time is 4-8 hours;
said H2O2The volume ratio of the water to the ice water is 1: 100 to 1: 20;
the centrifugal rotating speed is 8000-12000 rpm;
the centrifugation time is 10-20 minutes;
the concentration of the graphene nanoribbon dispersion liquid is 0.5-2%.
3) And dispersing the multilayer MXene nanosheets in deionized water, placing the multilayer MXene nanosheets in liquid nitrogen, thawing at room temperature, and repeating the process to obtain the monolayer MXene dispersion liquid.
The concentration of the multilayer MXene nanosheet dispersion liquid is 0.1-0.5%;
the liquid nitrogen treatment time is 10-30 minutes;
the repetition frequency is 6-10 times.
4) Blending the prepared oxidized cellulose dispersion liquid, the prepared graphene nanobelt dispersion liquid and the prepared MXene dispersion liquid; and obtaining the oxidized cellulose-graphene nanoribbon-MXene composite conductive film by a vacuum filtration method.
The mass ratio of the oxidized cellulose dispersion liquid to the graphene nanoribbon dispersion liquid is 5: 1-1: 1;
the mass ratio of the oxidized cellulose dispersion liquid to the single-layer MXene dispersion liquid is 8: 1-2: 1.
The volume of the blending liquid is 20-50 mL.
3. The preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film according to claim 2, characterized in that: the cellulose is cotton pulp cellulose, bamboo pulp cellulose or bacterial cellulose.
4. The preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite conductive film according to claim 2, characterized in that: the oxidized cellulose is a nano-grade fiber with the diameter of 10-200 nanometers.
5. The method for preparing the oxidized cellulose-graphene nanoribbon-MXene composite film according to claim 2, characterized in that; the width of the graphene nanoribbon is 30-50 nanometers.
6. The preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite film according to claim 2, characterized in that: the MXene nano-sheet is a single layer, and the sheet diameter is 2-5 microns.
7. The preparation method of the oxidized cellulose-graphene nanoribbon-MXene composite film according to claims 1-2, characterized in that: the thickness of the composite conductive film is 20-100 microns.
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| CN114213715A (en) * | 2021-11-16 | 2022-03-22 | 中科院广州化学有限公司 | High-strength bidirectional heat conduction enhanced heat management film and preparation method thereof |
| CN114605708A (en) * | 2022-03-21 | 2022-06-10 | 上海理工大学 | Preparation method of MXene nano-cellulose carbon nano-tube composite material |
| CN117180980A (en) * | 2023-08-29 | 2023-12-08 | 华北电力大学（保定） | Composite nanofiltration membrane for efficiently intercepting ammonium sulfate and ammonium nitrate and simultaneously adsorbing and removing mercury ions and preparation method thereof |
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Application publication date: 20201103 |