CN112125296A - Graphene optical drive material and preparation method thereof - Google Patents
Graphene optical drive material and preparation method thereof Download PDFInfo
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- CN112125296A CN112125296A CN202010942815.7A CN202010942815A CN112125296A CN 112125296 A CN112125296 A CN 112125296A CN 202010942815 A CN202010942815 A CN 202010942815A CN 112125296 A CN112125296 A CN 112125296A
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Abstract
The invention aims to provide a preparation method of a graphene material, which is characterized in that graphene is dispersed in water, and the graphene material with the light driving performance is finally obtained through high-temperature hydration thermal reaction, freezing, normal-temperature vacuum drying and inert gas firing.
Description
Technical Field
The invention relates to a graphene material and an improved preparation method thereof, in particular to a graphene optical drive material and a preparation method thereof.
Background
In 2015, 6 months, a research team led by professor cheng yong showplace of southern open university and professor of field building nations finds that the graphene oxide gel material generates macroscopic observable motion phenomenon under the irradiation of light sources such as laser and sunlight, and the experimental phenomenon and preliminary research result are published in Nature photosonics journal, which causes huge reverberation in academic circles. The graphene photoinduced propulsion phenomenon is a propulsion technology which is different from chemical propulsion and electric propulsion, has no working medium and no electric energy consumption, completely utilizes optical energy, has higher propulsion efficiency and is very likely to promote a new generation of aerospace propulsion technology.
Graphene photoinduced propulsion is a brand-new physical phenomenon, and although the accurate physical principle of the graphene photoinduced propulsion is yet to be researched and confirmed, the authenticity of the phenomenon is not questionable. The graphene photoinduced propulsion system is expected to have wide application prospect, and particularly has great potential to be developed into a new generation of propulsion technology which is high in efficiency, low in consumption and capable of utilizing solar energy in the field of aerospace power systems. The graphene light propulsion technology can not only promote an effective propulsion system utilizing sunlight, but also be applied to light propulsion systems in other environments, and can further develop a spacecraft light control system and a light detection system, such as attitude control of a satellite, by utilizing the response characteristic of a graphene material to light. If the technology finally moves to engineering application, a new generation of spacecraft design will be led, the aerospace cost is further reduced, and the aerospace is promoted to develop vigorously. The spacecraft can efficiently utilize sunlight, realize macroscopic propulsion depending on the sunlight, and greatly improve the service life and continuous maneuvering capability of the spacecraft such as low-orbit communication, remote sensing, scientific experiments and the like. Lays a solid foundation for the progress of the aerospace technology and is favorable for promoting the rapid development of the aerospace industry.
The prior disclosed graphene optical drive material preparation technology, a preparation method and application of an optical drive material based on graphene (CN104310386B), and a graphene material, a preparation method and application thereof as an optical drive material (CN107043100A) respectively disclose a method for preparing an optical drive material by replacing water by using an organic solvent as a dispersing agent of graphene oxide, but the preparation process is long, and the defects of high cost and poor environmental protection property are caused by the large amount of organic solvent. How to obtain the preparation method with energy conservation, environmental protection and low cost has important significance for the industrial production of the graphene photo-driving material and the popularization of the application range thereof.
Disclosure of Invention
In view of this, the invention aims to provide a preparation method of a graphene material, which has the advantages of easily available starting materials, no organic solvent, greenness and environmental friendliness, and the prepared graphene material has a light driving performance.
The invention provides a preparation method of a graphene material, which comprises the following steps:
step 1, dispersing graphene oxide in water, wherein the concentration of an aqueous solution of the graphene oxide is between 0.5 and 4mg/mL, and the pH value is between 6 and 8;
step 2: carrying out high-temperature hydration thermal reaction on the aqueous solution at the temperature of 120-180 ℃, wherein the reaction time is 8-12 hours;
and step 3: freezing at a temperature not higher than-4 deg.C;
and 4, step 4: carrying out vacuum drying treatment;
and 5: high-temperature roasting is carried out for 1-3 hours at 800-1200 ℃ in an inert atmosphere.
In the step 1, the density and the volume of the finally obtained graphene optical drive material can be adjusted by changing the concentration of the solution and the size of the reaction container.
The research shows that the graphene material with the light driving performance can be prepared by directly using water as a dispersing solvent without using an organic solvent. The method directly uses water as the dispersion solvent of the graphene, avoids the step of using an organic solvent as a dispersing agent and finally replacing water in the prior art, shortens the production procedure of the product, and simultaneously avoids high cost and environmental pollution caused by the use of the organic solvent.
Meanwhile, research finds that when water is used as a dispersing solvent, graphene is dispersed in water under the condition that the concentration of the graphene is too high or too low, and the graphene in the obtained intermediate product is dispersed in water in a powdery state through the high-temperature hydration thermal reaction in the step 2, and a spongy graphene material is not available, and is a basis for preparing a porous graphene material, and the fact that the light-driven graphene material cannot be obtained is the fact that the spongy graphene material cannot be obtained.
In addition, the research also finds that the tested pH environment is also important for preparing the light-driven graphene material. The preparation method and the post-treatment process of the graphene material have certain influence on the properties of the graphene, and different graphene raw materials have different pH values in an aqueous solution. In the test process, the pH value of the water-soluble graphene can be regulated and controlled within the range of 6-8 by adding acidic and alkaline substances. Research shows that when the pH value is too low or too high, the high-temperature hydration thermal reaction in the step 2 also has the phenomenon that the spongy graphene material cannot be obtained, so that the light-driven graphene material cannot be obtained.
Further preferably, the pH of the graphene aqueous solution in step 1 is preferably 6.5 to 7.
Further preferably, the concentration of the graphene oxide aqueous solution in the step 1 is between 1 and 3 mg/mL.
Furthermore, the graphene oxide has a single-layer thickness of less than 0.2nm, contains various functional groups such as-OH, -COOH, -O-and the like, and has an oxygen content of 10-50 wt%.
The graphene oxide is a product obtained by chemically oxidizing and stripping graphite powder, and powdery and flaky graphene oxide can be used or a commercialized aqueous solution thereof can be directly used.
Further, in step 1, in order to ensure the dispersion uniformity of the graphene oxide, stirring and ultrasonic treatment may be used to sufficiently and well disperse the graphene oxide, thereby obtaining an aqueous solution. The commercial graphite oxide aqueous solution which meets the requirement and is uniformly dispersed can also be directly used.
Further, a preferred implementation manner of step 2 is to transfer the graphene aqueous solution obtained in step 1 into a high-pressure reaction kettle, then seal the kettle, place the kettle into a preheated oven, and heat the kettle to a predetermined temperature for reaction.
It will be appreciated that the desired effect can be achieved by one skilled in the art by raising the temperature to the stated temperature by means of other reaction equipment, such as a closed reaction vessel with heating. The technical effect of the present invention can be achieved by controlling the reaction temperature and the reaction pressure in other non-closed or semi-continuous reaction equipment, and controlling the reaction pressure to be the same as or similar to the reaction pressure in the closed container, and under the corresponding reaction time.
In the prior art, freeze drying generally adopts ultra-low temperature rapid cooling at-60 ℃ to-40 ℃ to ensure that the porous structure of graphene is not damaged. Although the method is suitable for preparing the porous graphene structure, the method has the problem of high energy consumption. Researches show that the graphene dispersion system has high stability, can be frozen at the temperature below-4 ℃, and can still ensure the structural stability, thereby reducing the energy consumption.
Further, in step 3, the graphene material obtained in the reaction kettle is subjected to a freezing treatment, and a preferable mode is as follows: and (3) carrying out freeze drying at a temperature of between 30 ℃ below zero and 4 ℃ below zero to completely freeze and solidify water in pores of the graphene material.
Further preferably, the graphene material is frozen at the temperature of-4 ℃ to-15 ℃ for 2-4 hours, so that water in pores of the graphene material is completely frozen and solidified.
Further, in step 4, the frozen graphene material is placed in a vacuum tube or any device capable of vacuumizing, and vacuum drying treatment is performed. Further preferably, vacuum drying may be performed at normal temperature to reduce production cost.
The vacuum treatment of the frozen graphene material at normal temperature can also achieve the effect of full drying. Compared with the freeze drying treatment at the temperature of-60 ℃ to-40 ℃, the method has the advantages of lower requirement on equipment, lower energy consumption and benefit for popularization and application.
Further, in step 5, the graphene material after vacuum drying needs to be baked at 800-.
The inert atmosphere is preferably nitrogen or argon.
Research shows that when the technical route is adopted, only a sample after vacuum drying does not have the light driving property, and high-temperature roasting treatment under inert gas is an indispensable step for obtaining the graphene material with the light driving property.
The invention also provides a graphene material which is prepared by the preparation method. Because the preparation method does not need to use an organic solvent, the content of possible organic impurities in the prepared optical drive material is lower, and the purity is higher.
Advantageous effects
1. In the preparation process, only water is used as a solvent, and no organic solvent is used or introduced, so that the graphene optical drive material prepared in the invention has a porous spongy structure, high porosity and low density;
2. the graphene optical drive material has good light absorption performance, can absorb light from a visible light region to an ultraviolet light region, and generates a driving force;
3. the graphene material has a photoinduced driving characteristic, the graphene optical driving material is irradiated by simulated sunlight generated by laser, a short-arc xenon lamp or a long-arc xenon lamp under vacuum, and a sample of the graphene optical driving material is pushed, lifted or rotated under the irradiation of a light source;
4. the method has the advantages of easily available raw materials, no pollution in the preparation process, simple preparation process, low energy consumption, suitability for mass production and contribution to the engineering application of the graphene optical drive material.
Drawings
Fig. 1 example 1 sample diagram of graphene photo-driven materials.
Fig. 2 SEM image of example 1 graphene photo-driven material sample.
Fig. 3 is a photograph of a device for testing a photo-driven phenomenon of a graphene photo-driven material.
Fig. 4 the graphene material was obtained in comparative example 1.
Fig. 5 is a flowchart of a method for preparing a graphene optical driving material.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The optical drive performance test conditions of the graphene material prepared by the embodiment are as follows: the light driving material is placed in a vacuum environment or a vacuum device, and the vacuum degree is not more than 10 Pa. The vacuum device can be a fully transparent light-transmitting material or a light-transmitting window is locally arranged, and the light source can be required to irradiate the graphene optical drive material for the light-transmitting material or the light-transmitting window.
Light driven horizontal experiment
Placing the obtained graphene optical drive material into a horizontally placed transparent common glass tube, vacuumizing to 0.1Pa, and irradiating the graphene optical drive material by using red laser with the wavelength of 633nm and green laser with the wavelength of 532nm, wherein the graphene optical drive material can move forwards all the time; and the graphene optical drive material can still continuously advance to the other direction by irradiation in the other direction.
Light driven vertical experiment
Placing the obtained graphene optical drive material into a vertical transparent common glass tube, vacuumizing to 0.1Pa, and irradiating the graphene optical drive material by using red laser with the wavelength of 633nm and green laser with the wavelength of 532nm, so that the graphene optical drive material can be pushed up.
All reagent starting materials are commercially available in the following examples.
Example 1
Step 1, dissolving powdered graphene oxide in water, stirring, and performing ultrasonic treatment to fully and well disperse the graphene oxide to obtain a graphene oxide aqueous solution with the concentration of 1mg/ml, and adjusting the pH of the solution to 6.5;
step 2, filling 60ml of the graphene oxide aqueous solution into a 100ml of polytetrafluoroethylene lining, then filling the lining into a stainless steel reaction kettle for sealing, sealing the kettle, then putting the kettle into a preheated oven, carrying out high-temperature solvothermal reaction at the temperature of 120 ℃, wherein the reaction time is 10 hours, and after the reaction kettle is cooled to room temperature, taking out the prepared graphene material and placing the graphene material into a container;
step 3, putting the container in which the graphene material is placed into a freezing chamber of a refrigerator at the temperature of-4 ℃ and freezing for 2 hours;
step 4, putting the frozen graphene material into a vacuum tube, vacuumizing to 0.1Pa, and maintaining the vacuum degree for 6 hours;
and 5, roasting the graphene material subjected to normal-temperature vacuum drying treatment at 800 ℃ for 3h under the protection of inert atmosphere.
Example 2
Step 1, dissolving flake graphene oxide in water, stirring, and performing ultrasonic treatment to fully and well disperse the graphene oxide to obtain a graphene oxide aqueous solution with the concentration of 1mg/ml and the pH of the solution of 7;
and 2, filling the 60ml of graphene oxide aqueous solution into a 100ml of polytetrafluoroethylene lining, and then filling the lining into a stainless steel reaction kettle for sealing. Sealing the kettle, putting the kettle into a preheated oven, carrying out high-temperature solvothermal reaction at 160 ℃ for 12 hours, cooling the kettle to room temperature, taking out the prepared graphene material, and putting the graphene material into a container;
step 3, putting the container in which the graphene material is placed into a freezing chamber of a refrigerator at the temperature of-15 ℃, and freezing for 2 hours;
step 4, putting the frozen graphene material into a vacuum tube, vacuumizing to 0.1Pa, and maintaining the vacuum degree for 5 hours;
and 5, roasting the graphene material subjected to normal-temperature vacuum drying treatment for 2 hours at 1000 ℃ under the protection of inert atmosphere.
Example 3
Step 1, dissolving powder or flake graphene oxide in water, stirring, and performing ultrasonic treatment to fully and well disperse the graphene oxide to obtain a graphene oxide aqueous solution with the concentration of 4mg/ml and the pH of the solution of 8;
and 2, filling the 60ml of graphene oxide aqueous solution into a 100ml of polytetrafluoroethylene lining, and then filling the lining into a stainless steel reaction kettle for sealing. Sealing the kettle, putting the kettle into a preheated oven, carrying out high-temperature solvothermal reaction at the temperature of 180 ℃, reacting for 12 hours, cooling the reaction kettle to room temperature, taking out the prepared graphene material, and placing the graphene material in a container;
step 3, putting the container in which the graphene material is placed into a freezing chamber of a refrigerator at the temperature of-10 ℃ and freezing for 3 hours;
step 4, putting the frozen graphene material into a vacuum tube, vacuumizing to 0.1Pa, and maintaining the vacuum degree for 7 hours;
and 5, roasting the graphene material subjected to vacuum drying treatment at normal temperature for 1h at 1200 ℃ under the protection of inert atmosphere.
Comparative example 1
Step 1, dissolving powdered graphene oxide in water, stirring, and performing ultrasonic treatment to fully and well disperse the graphene oxide to obtain a graphene oxide aqueous solution with the concentration of 0.2mg/ml and the pH of the solution of 6.5;
and 2, filling the 60ml of graphene oxide aqueous solution into a 100ml of polytetrafluoroethylene lining, and then filling the lining into a stainless steel reaction kettle for sealing. The preparation method comprises the steps of sealing a kettle, putting the kettle into a preheated oven, carrying out high-temperature solvothermal reaction at 180 ℃, reacting for 12 hours, opening the kettle after the kettle is cooled to room temperature, dispersing black powder in an aqueous solution, and preparing the light driving material without a spongy graphene material.
Comparative example 2
Step 1, dissolving powdered graphene oxide in water, stirring, and performing ultrasonic treatment to fully and well disperse the graphene oxide to obtain a graphene oxide aqueous solution with the concentration of 1mg/ml, and adjusting the pH of the solution to 6.5;
step 2, filling 60ml of the graphene oxide aqueous solution into a 100ml of polytetrafluoroethylene lining, then filling the lining into a stainless steel reaction kettle for sealing, sealing the kettle, then putting the kettle into a preheated oven, carrying out high-temperature solvothermal reaction at the temperature of 120 ℃, wherein the reaction time is 10 hours, and after the reaction kettle is cooled to room temperature, taking out the prepared graphene material and placing the graphene material into a container;
step 3, putting the container in which the graphene material is placed into a freezing chamber of a refrigerator at the temperature of-4 ℃ and freezing for 2 hours;
and 4, putting the frozen graphene material into a vacuum tube, vacuumizing to 0.1Pa, and maintaining the vacuum degree for 6 hours.
And (3) carrying out a light drive test on the dried graphene material, wherein the graphene material has no light drive performance.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A preparation method of a graphene material is characterized by comprising the following steps:
step 1, dispersing graphene oxide in water, wherein the concentration of an aqueous solution of the graphene oxide is between 0.5 and 4mg/mL, and the pH value is between 6 and 8;
step 2: carrying out high-temperature hydration thermal reaction on the aqueous solution at the temperature of 120-180 ℃, wherein the reaction time is 8-12 hours;
and step 3: freezing at a temperature not higher than-4 deg.C;
and 4, step 4: vacuum drying at normal temperature;
and 5: high-temperature roasting is carried out for 1-3 hours at 800-1200 ℃ in an inert atmosphere.
2. The method for preparing a graphene material according to claim 1, wherein: the pH of the graphene aqueous solution in the step 1 is preferably 6.5 to 7.
3. The method for preparing a graphene material according to claim 1, wherein: in the step 1, the concentration of the graphene oxide aqueous solution is between 1 and 3 mg/mL.
4. The method for preparing a graphene material according to claim 1, wherein: the graphene oxide has a single-layer thickness of less than 0.2nm, contains various functional groups such as-OH, -COOH, -O-and the like, and has an oxygen content of 10-50 wt%.
5. The method for preparing a graphene material according to claim 1, wherein: stirring and ultrasonic treatment are used, so that the graphene oxide is fully and well dispersed, and an aqueous solution is obtained.
6. The method for preparing a graphene material according to claim 1, wherein: and 2, transferring the graphene aqueous solution obtained in the step 1 into a high-pressure reaction kettle, sealing the kettle, putting the kettle into a preheated oven, and heating the kettle to a preset temperature for reaction.
7. The method for preparing a graphene material according to claim 1, wherein: and 3, freezing at-30 to-4 ℃ to completely freeze and solidify water in pores of the graphene material.
8. The method of preparing graphene according to claim 1, wherein: freezing for 2-4 hours at the temperature of-4 to-15 ℃ to ensure that water in pores of the graphene material is completely frozen and solidified.
9. A graphene material, characterized in that: prepared by the process of any one of claims 1 to 8.
10. The graphene material of claim 9, wherein: the material has light driving performance.
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