CN111422858B - Method for efficiently preparing graphene - Google Patents
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- CN111422858B CN111422858B CN202010284132.7A CN202010284132A CN111422858B CN 111422858 B CN111422858 B CN 111422858B CN 202010284132 A CN202010284132 A CN 202010284132A CN 111422858 B CN111422858 B CN 111422858B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
- C01B32/19—Preparation by exfoliation
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/02—Single layer graphene
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/04—Specific amount of layers or specific thickness
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/30—Purity
Abstract
The invention relates to a method for efficiently preparing graphene, which comprises the following steps: placing graphite powder in liquid helium to enable liquid helium molecules to enter between graphene sheet layers; then placing the liquid helium containing the graphite powder under a high-temperature condition until the liquid helium is completely vaporized; repeating the steps to ensure the sufficiency of slippage between the graphene layers and the expansion of interlayer spacing, reduce the interlayer acting force and loosen the interlayers; stripping the graphite powder loosened among the layers by using a high-temperature helium gas jet mill to obtain thin-layer graphene; and putting the thin-layer graphene into the dispersion liquid to obtain a graphene suspension. The interlayer spacing of the graphene powder is increased by volume expansion thousand times in the rapid vaporization process of the used liquid helium at high temperature, and then the graphene is obtained by stripping the graphite loose between the layers by using an ultrahigh-temperature steam jet mill, so that the loss of tools is avoided, and no pollution is caused; the graphene stripped by using liquid helium, high temperature and ultrahigh temperature jet mills has the advantages of high purity and low defect, and the prepared 1-3 layers of graphene has uniform thickness and good dispersibility, and has obvious advantages in the application aspect of electronic devices.
Description
Technical Field
The invention relates to the technical field of graphene, in particular to a method for efficiently preparing graphene.
Background
Graphene is currently the thinnest and hardest nanomaterial in the world, has higher electron mobility at room temperature than carbon nanotubes or silicon crystals, has lower resistivity than copper or silver, and is the current lowest resistivity material, and therefore, development of a new generation of electronic components or transistors with thinner thickness and faster conduction speed is expected. The existing graphene preparation methods have some defects, such as time and labor waste, poor repeatability and difficulty in large-scale preparation due to a micro-mechanical stripping method; graphene produced by the orientation attachment method is uneven in thickness, and the adhesion between the graphene and a substrate influences the characteristics of the graphene; the chemical vapor deposition method has high cost, complex process and precise processing conditions, and restricts the preparation of graphene; the graphite oxide reduction method can seriously damage the electronic structure and the integrity of the crystal of the graphene, and influence the electronic property. Since graphene has a wide application range in the fields of electronics, photonics and optoelectronic devices, and has a great development prospect, quantitative production of 1-3 layers of graphene is very necessary to promote the development of graphene-related products, and an efficient and rapid preparation method is needed.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects in the prior art, and provide a method for efficiently preparing graphene, wherein the graphene can be peeled by using liquid helium, high temperature and high temperature jet mill, and the prepared 1-3 layers of graphene has uniform thickness, good dispersibility, greenness and no pollution.
Therefore, the technical scheme is a method for efficiently preparing graphene, and the method comprises the following steps:
step S1: placing graphite powder in liquid helium so that liquid helium molecules enter between graphite sheets;
step S2: placing the liquid helium containing the graphite powder obtained in the step S1 under a high-temperature condition until the liquid helium is completely vaporized;
and step S3: repeating the steps S1-S2, ensuring the sufficiency of the sliding between the graphene layers and the expansion of the interlayer spacing, reducing the interlayer acting force and loosening the interlayer;
and step S4: grinding and stripping the interlaminar loose graphite powder obtained in the step S3 by using a high-temperature helium gas flow mill to obtain thin-layer graphene;
step S5: and putting the thin-layer graphene into the dispersion liquid to obtain a graphene suspension.
Preferably, in step S1, the common multilayer graphite powder is placed in liquid helium, and ultrasonic dispersion is performed for 2 hours after the liquid helium is sealed.
Preferably, the ultrasonic dispersion power used is 500-1000W.
Preferably, the liquid helium containing graphite powder is unsealed in step S2, then placed at room temperature for 1-5 minutes, and then placed at 100 ℃ until the liquid helium is completely vaporized.
Preferably, in step S4, the graphite powder is ground and exfoliated by using a high-temperature helium gas flow mill for 1 to 5 hours, the high-temperature helium gas is ejected through a supersonic nozzle during the grinding and exfoliation process, the fineness of the thin-layer graphene powder is 0.5 to 45 micrometers, the thickness of the sheet layer of the thin-layer graphene powder is 1 to 3 layers, and the thin-layer graphene is cooled to room temperature after the grinding and exfoliation are finished.
Preferably, in step S5, the dispersion liquid is vinyl silicone oil, and the thin-layer graphene powder is placed in the vinyl silicone oil and ultrasonically dispersed for 1 to 5 hours at a power of 500 to 1000W, so as to obtain a graphene suspension.
The technical scheme of the invention has the following advantages:
1. according to the method for efficiently preparing graphene, provided by the invention, the interlayer spacing of graphite powder is increased by utilizing high-temperature vaporization of liquid helium to obtain the graphite powder with loose interlayer, and then the graphite powder with loose interlayer is ground and peeled by using an ultrahigh-temperature airflow mill to obtain the thin-layer graphene.
2. According to the method for efficiently preparing graphene, disclosed by the invention, the reason that the thin-layer graphene is put into the vinyl silicone oil dispersion liquid to prevent secondary agglomeration is that the exfoliated graphene is easy to agglomerate together due to strong interaction of sheet layers, so that the solubility of an organic solvent or water is reduced, and the application of the graphene is limited to a great extent.
3. According to the method for efficiently preparing graphene, provided by the invention, the interlayer spacing of graphite powder is increased by volume expansion thousand times in the rapid vaporization process of the used liquid helium at high temperature, and the method is simple and easy to implement, and provides sufficient preparation for grinding and stripping of 1-3 layers of graphite powder; the powder in the used ultrahigh-temperature steam jet mill is completely self-milled, so that the loss of tools is avoided, the pollution is avoided, the reached fineness limit of dry grinding stripping is successfully extended to a submicron level, and 1-3 layers of graphene can be obtained; the graphene stripped by using liquid helium, high temperature and high temperature jet mill has the advantages of high purity and low defect, and the prepared 1-3 layers of graphene has uniform thickness and good dispersibility, and has obvious advantages in the application aspect of electronic devices.
4. The method for efficiently preparing the graphene provided by the invention has the advantages that the finally prepared graphene is high in purity, good in electric conduction and heat conduction performance, safe, effective, environment-friendly and suitable for relevant application fields such as super capacitors and sensors.
Detailed Description
The technical solutions of the present invention will be described clearly and completely below, and it should be apparent that the described embodiments are some, but not all, embodiments of the present 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.
A method for efficiently preparing graphene comprises the following steps:
step S1: adding 20g of high-purity graphite powder (with the diameter of 20 mu m) into 1L of liquid helium, sealing the liquid helium, and performing ultrasonic dispersion for 2 hours (with the power of 500W) to enable liquid helium molecules to enter between graphite sheets;
step S2: placing the liquid helium containing the graphite powder in the step S1 at room temperature for 1min, and then placing the liquid helium at 100 ℃ until the liquid helium is completely vaporized;
and step S3: repeating the steps S1-S2 for three times, ensuring the sufficiency of the sliding between the graphene layers and the expansion of the interlayer spacing, reducing the interlayer acting force and loosening the interlayer;
and step S4: feeding the interlaminar loose graphite powder obtained in the step S3 into an S-JET high-temperature JET mill through high-temperature helium (at the temperature of 100 ℃) airflow, wherein the airflow speed is 25-30m/S, grinding and stripping for 2h to obtain thin-layer graphene, and separating the thin-layer graphene with different thicknesses through a grading device;
step S5: and (5) adding the thin-layer graphene obtained in the step (S4) into a dispersion liquid, and performing ultrasonic dispersion for 1 hour to obtain a graphene suspension, wherein the dispersion liquid is vinyl silicone oil with the viscosity of 100-200mPas, and the concentration of the graphene in the dispersion liquid is 10g/L.
Filling gaps among graphite powder layers with liquid helium molecules, increasing the distance between the graphite layers by utilizing volume expansion and high temperature in the process of vaporizing liquid helium, weakening the acting force between the graphite layers until the graphene layers are loosened, and repeating the processes. And (2) putting the graphite powder with the loose structure into a high-temperature helium gas jet mill, filling high-temperature helium gas into the jet mill, grinding and stripping for 1 hour to obtain thin-layer graphene powder with the particle size of 0.5-45 microns, and putting the graphene into dispersion liquid for ultrasonic dispersion to obtain the graphene suspension. The method can realize efficient batch preparation of the graphene, and the graphene with good performance can be prepared in an environment-friendly and pollution-free manner.
In order to ensure that the interlayer structure of the graphite powder is filled with liquid helium molecules, it is preferable that in step S1, the common multilayer graphite powder is placed in liquid helium, and ultrasonic dispersion is performed for 2 hours after the liquid helium is sealed.
In order to prevent liquid helium molecules from entering into the graphene interlayer structure and not sufficiently sealing the liquid helium, it is preferable that the ultrasonic dispersion power used is 500 to 1000W.
In order to prevent the liquid helium from being vaporized too violently due to sudden high temperature, the interaction force between graphene layers can be weakened due to the high temperature, and the distance between the graphene layers can be rapidly increased until the liquid helium slides due to the rapidly increased volume of the liquid helium, the preferable scheme is that in the step S2, the liquid helium containing graphite powder is sealed off, then the liquid helium is placed at room temperature for 1 minute, and then the liquid helium is placed at 100 ℃ until the liquid helium is completely vaporized.
And (3) repeating the steps S1-S2, repeatedly applying for 1-3 times according to specific conditions to ensure that the graphene layers slide, and placing the graphene layers with enough loose lamellar structures into a high-temperature airflow mill for grinding and stripping.
In order to prevent powder agglomeration, the ultrahigh Wen Haiqi is used as a medium and is accelerated to be ultrahigh-speed airflow through the supersonic nozzle to drive materials to move and collide at high speed, so that the materials are ground and stripped, tools are not wasted, and finished products are not polluted. In the preferable scheme, in the step S4, the graphite powder is ground and stripped by using an ultrahigh-temperature helium gas flow mill for 1 hour, the high-temperature helium gas is sprayed out from a supersonic nozzle in the grinding and stripping process, the fineness of the thin-layer graphene powder is 0.5-45 microns, the thickness of the sheet layer of the thin-layer graphene powder is 1-3 layers, and the thin-layer graphene is cooled to room temperature after the grinding and stripping are finished. The thickness of the prepared finished product thin-layer graphene powder can be 1-3 layers of graphene, the thickness of the graphene sheet can influence the performance of the graphene, and the heat conduction performance and the electric conduction performance of the 1-3 layers of graphene can be better than those of the multilayer graphene. The high-temperature JET mill can be S-JET high-temperature JET mill.
In order to prevent secondary agglomeration of graphene, in step S5, the dispersion liquid is vinyl silicone oil, and the finished graphene powder is placed in the vinyl silicone oil and dispersed by ultrasonic with a power of 500-1000W for 1 hour to obtain a graphene suspension.
The specific preparation method of the graphene suspension (graphene film) comprises the following steps:
(1) Placing graphite powder into enough liquid helium, sealing, and performing ultrasonic dispersion for 2 hours until liquid helium molecules fully enter the graphite powder layer;
(2) Sealing the obtained graphene liquid helium mixture, placing the graphene liquid helium mixture at normal temperature for 1 minute, and then placing the mixture at the high temperature of 100 ℃, so that liquid helium is quickly vaporized to increase the distance between graphene layers, liquid nitrogen molecules entering pores of graphene have hundreds of times or even thousands of times of volume in the vaporization process, and the expansion of the helium molecular volume causes the distance between graphene sheets to be increased, and further slippage occurs;
(3) Repeating the steps (1) and (2) for one to three times to ensure that the structure between graphene layers is loose enough;
(4) Grinding and stripping the obtained graphite powder for one hour by using an S-JET high-temperature helium gas flow mill to obtain thin graphene with the particle size of 0.5-45 micrometers, wherein the thickness of a lamella is 1-3 layers, and then cooling to room temperature;
(5) And (5) putting the graphene obtained in the step (4) into the dispersion liquid, wherein the concentration is 10g/L, and performing ultrasonic dispersion for 1 hour to obtain a graphene suspension.
The graphite powder in the step (1) is multi-layer graphene, after the liquid helium is vaporized in the step (2), slippage occurs between graphene layers, the interlayer structure becomes loose, the interaction force between the graphene layers can be weakened at high temperature, and the increase of the interlayer distance is facilitated.
When the liquid helium is used for soaking graphene, sealing and ultrasonic stirring are needed, so that the phenomenon that molecules cannot fill the inner pores of the graphene due to too fast vaporization of the liquid helium is prevented, and the ultrasonic dispersion power is 500-1000W.
The thickness of the graphene sheet layer processed by the jet mill is 1-3 layers, and high-speed helium is sprayed out through the supersonic nozzle, so that the graphene powder is prevented from agglomerating in the grinding and stripping process.
And (5) irreversible agglomeration of the successfully stripped graphene is prevented, so that the dispersibility is influenced.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications derived therefrom are intended to be within the scope of the invention.
Claims (2)
1. A method for efficiently preparing graphene is characterized by comprising the following steps:
step S1: placing high-purity graphite powder in liquid helium to enable liquid helium molecules to enter between graphite sheet layers; specifically, common multilayer graphite powder is placed in liquid helium, ultrasonic dispersion is carried out for 2 hours after the liquid helium is sealed, and the used ultrasonic dispersion power is 500-1000W;
step S2: placing the liquid helium containing graphite powder under a high-temperature condition until the liquid helium is completely vaporized; specifically, the liquid helium containing graphite powder is removed and sealed, then is placed at room temperature for 1-5 minutes, and then is placed at 100 ℃ until the liquid helium is completely vaporized;
and step S3: repeating the steps S1-S2, ensuring the sufficiency of the slippage between the graphene layers and the expansion of the interlayer spacing, reducing the interlayer acting force and loosening the interlayer;
and step S4: grinding and stripping the graphite powder loosened among the layers by using a high-temperature helium gas flow mill to obtain thin-layer graphene, wherein the fineness of the graphene powder is 0.5-45 microns, and the thickness of the sheet layer of the thin-layer graphene powder is 1-3 layers;
step S5: putting the thin-layer graphene into a dispersion liquid to obtain a graphene suspension; specifically, the dispersion liquid is vinyl silicone oil with the viscosity of 100-200mPa & s, the concentration of graphene in the dispersion liquid is 10g/L, the thin-layer graphene powder is placed in the vinyl silicone oil and is dispersed for 1~5 hours by using ultrasonic with the power of 500-1000W, and then the graphene suspension is obtained.
2. The method for efficiently preparing graphene according to claim 1, wherein in step S4, high-temperature helium gas is used for milling and stripping graphite powder for 1-5 hours, the high-temperature helium gas is sprayed out through a supersonic nozzle during milling and stripping, and the thin graphene layer is cooled to room temperature after milling and stripping.
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| CN112174160B (en) * | 2020-10-09 | 2023-07-04 | 武汉理工大学 | Method for preparing two-dimensional material by stripping high-purity bentonite through normal-temperature boiling and vaporization |
| CN113620264B (en) * | 2021-08-27 | 2023-03-17 | 昆明理工大学 | Preparation method of nano black phosphorus/graphene |
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