CN110562965A - Preparation method of graphene powder - Google Patents
Preparation method of graphene powder Download PDFInfo
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- CN110562965A CN110562965A CN201911046244.2A CN201911046244A CN110562965A CN 110562965 A CN110562965 A CN 110562965A CN 201911046244 A CN201911046244 A CN 201911046244A CN 110562965 A CN110562965 A CN 110562965A
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/184—Preparation
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- C—CHEMISTRY; METALLURGY
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- 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
Abstract
The invention relates to a preparation method of graphene powder, and belongs to the technical field of graphene preparation. The specific preparation method of the graphene powder comprises the following steps: dispersing graphene oxide in water at normal temperature to form graphene oxide aqueous dispersion, then adding reducing sugar into the dispersion according to a ratio, ultrasonically dispersing uniformly, and then placing the obtained mixed solution under a lighting condition to stir and react for 1-5 h; after the reaction is finished, cooling, centrifuging and washing the product, drying after spray drying, and grinding. The graphene powder prepared by the method has the advantages of uniform sheet layer, thin thickness (1-5 nm), regular appearance, high reduction degree, few defects and high conductivity, and can be widely applied to the fields of electronic devices such as micro-electro-mechanical systems, artificial intelligence, biomedicine and the like.
Description
Technical Field
The invention belongs to the technical field of graphene preparation, and particularly relates to a preparation method of graphene powder.
Background
Graphene is a compound represented by sp2The researchers in 2004 succeeded in separating stable graphene for the first time from a novel material with a single-layer two-dimensional honeycomb lattice structure consisting of hybridized carbon atoms. Since graphene has very high specific surface area, electron mobility, Young's modulus and thermal conductivity, graphene shows wide application prospects in various fields, such as catalyst carriers, electronic components, materials, etc,Nano functional material, energy storage material, composite material and other fields.
Graphene is also prepared by a variety of methods, which can be classified into chemical methods and physical methods. The chemical method mainly comprises a redox method, a chemical vapor deposition method, a pyrolysis reduction method and the like; the physical methods mainly include a micro-mechanical peeling method, a liquid phase peeling method, and the like. The above method usually requires the use of toxic chemical reducing agents such as hydrazine hydrate, dimethylhydrazine, phenylhydrazine and toxic organic reagents such as aldehydes and ethers, and has the disadvantages of harsh reaction conditions, complicated steps, high equipment requirements, long time consumption and uncontrollable reaction conditions. Therefore, the development process is simple and easy, and the preparation method is environment-friendly and pollution-free. Because no harmful substance is generated in the process of preparing the graphene by the photo-reduction method, compared with the traditional preparation method, the method is environment-friendly, short in preparation period and good in repeatability, and thus the method is accepted by more and more researchers.
The present application has been made for the above reasons.
Disclosure of Invention
In view of the problems or defects of the prior art, the present invention aims to provide a method for preparing graphene powder. The method is simple, rapid, safe and environment-friendly, and solves the technical problems of harsh preparation conditions, complex steps, long period and the like in the process for preparing the graphene powder in the prior art.
in order to achieve the above purpose of the present invention, the technical solution adopted by the present invention is as follows:
A preparation method of graphene powder specifically comprises the following steps:
Dispersing graphene oxide in water at normal temperature to form graphene oxide aqueous dispersion, then adding reducing sugar into the dispersion according to a ratio, ultrasonically dispersing uniformly, and then placing the obtained mixed solution under a lighting condition to stir and react for 1-5 h; and after the reaction is finished, cooling, centrifuging and washing the product, drying after spray drying, and grinding to obtain the graphene powder.
Specifically, in the above technical scheme, the normal temperature refers to a natural room temperature condition in four seasons, no additional cooling or heating treatment is performed, and the normal temperature is generally controlled to be 10-30 ℃, preferably 15-25 ℃.
Further, according to the technical scheme, the mass concentration of the graphene oxide in the graphene oxide aqueous dispersion liquid is preferably 1-5 mg/mL.
Further, according to the technical scheme, the mass ratio of the reducing sugar to the graphene oxide is 1: 1-1: 8.
further, in the above technical scheme, the reducing sugar is any one or more of glucose, fructose, sucrose, lactose and maltose.
Further, according to the above technical scheme, the illumination light source is visible light or ultraviolet light.
Further, in the technical scheme, the visible light power is preferably 1000-1500W, and the ultraviolet light power is preferably 500-800W.
Further, according to the technical scheme, the graphene oxide is prepared by oxidizing graphite, and the method specifically comprises the following steps:
Stirring and mixing graphite powder and concentrated sulfuric acid uniformly under an ice bath condition, heating the obtained mixed solution to 30-40 ℃, stirring and reacting for 1-2H, and adding hydrogen peroxide (H) into the reaction system2O2) And (3) adding deionized water until the reaction solution becomes brown yellow, continuously stirring at constant temperature for reaction for 10-60 min, centrifuging and washing the product for several times after the reaction is finished until the pH value of the washing solution is 6-7, and finally, carrying out suction filtration and drying to obtain the graphene oxide.
Further, according to the technical scheme, the usage ratio of the graphite powder to concentrated sulfuric acid, hydrogen peroxide and deionized water is 1 part by mass: 10-100 parts by volume: 1-10 parts by volume: 100-200 parts by volume, preferably 1 part by mass: 50 parts by volume: 5 parts by volume: 150 parts by volume, wherein: the mass portion and the volume portion are as follows: mL was used as a reference.
Further, according to the technical scheme, the mass percentage concentration of the concentrated sulfuric acid is 90-98%.
Further, according to the technical scheme, the mass percentage concentration of the hydrogen peroxide is 20-40%.
Compared with the prior art, the preparation method of the graphene powder has the following beneficial effects:
(1) The graphene powder prepared by the method has the advantages of uniform lamellar layer, thin thickness (1-5 nm), regular appearance, high reduction degree, few defects and high conductivity, and can be widely applied to the fields of electronic devices such as micro-electro-mechanical systems, artificial intelligence, biological medicines and the like.
(2) The method can adjust the oxygen content of the reduced graphene by changing the illumination intensity and the illumination time, and has good controllability and high repeatability.
(3) the method provided by the invention can be used for breaking the bonds of C-O and C ═ O of the graphene oxide by using the energy generated by illumination, so that the effect of removing oxygen-containing groups on the carbon layer is achieved.
(4) The preparation method provided by the invention is non-toxic and pollution-free, does not need to use a toxic and non-degradable reducing agent, uses green environment-friendly reducing sugar as the reducing agent, is environment-friendly, has a simple process, and can be used for large-scale production.
(5) The method of the invention is simple to operate and is compatible with the photoetching process.
Drawings
Fig. 1 is a transmission electron microscope image of the graphene powder prepared in example 1 of the present invention.
Fig. 2 is a transmission electron microscope image of the graphene powder prepared in example 2 of the present invention.
Fig. 3 is an atomic force microscope image of the graphene powder prepared in example 3 of the present invention.
Fig. 4 is a raman spectrum of the graphene powder prepared in embodiments 2 and 4 of the present invention.
fig. 5 is a raman spectrum of the graphene powder prepared in example 5 of the present invention.
Detailed Description
The present invention will be described in further detail below with reference to examples. The present invention is implemented on the premise of the technology of the present invention, and the detailed embodiments and specific procedures are given to illustrate the inventive aspects of the present invention, but the scope of the present invention is not limited to the following embodiments.
Various modifications to the precise description of the invention will be readily apparent to those skilled in the art from the information contained herein without departing from the spirit and scope of the appended claims. It is to be understood that the scope of the invention is not limited to the procedures, properties, or components defined, as these embodiments, as well as others described, are intended to be merely illustrative of particular aspects of the invention. Indeed, various modifications of the embodiments of the invention which are obvious to those skilled in the art or related fields are intended to be covered by the scope of the appended claims.
for a better understanding of the invention, and not as a limitation on the scope thereof, all numbers expressing quantities, percentages, and other numerical values used in this application are to be understood as being modified in all instances by the term "about". Accordingly, unless expressly indicated otherwise, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained. At the very least, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
The light source in the following embodiments of the invention is visible light or ultraviolet light, the visible light is provided by a 1000-1500W xenon lamp simulation, and the ultraviolet light is provided by a 500-800W mercury lamp simulation.
Example 1
The preparation method of the graphene powder of the embodiment specifically includes the following steps:
Step 1: preparing graphene oxide: weighing 2g of graphite powder in a glass flask, adding 100ml of concentrated sulfuric acid with the mass percent concentration of 95%, putting the beaker into a water bath kettle with ice blocks to stir for 2 hours, heating the mixed solution to 30 ℃ in the water bath kettle, continuously stirring for 1.5 hours to fully oxidize graphite, and slowly dropwise adding 10ml of hydrogen peroxide (H) with the mass percent concentration of 30% into the mixed solution while stirring2O2) Adding 300ml deionized water into the solution until the solution turns brown yellow, stirring for 30min, and centrifuging the obtained solution in a high-speed centrifugeCentrifuging at a rotation speed of 10000r/min for 20min, removing an upper layer solvent, respectively adding water and ethanol, repeatedly performing ultrasonic centrifugation washing at a rotation speed of 10000r/min until the pH value of a washing liquid is 6-7, and finally performing suction filtration and drying to obtain the graphene oxide.
step 2: preparing graphene powder: weighing 0.1g of graphene oxide obtained in the step 1 in a quartz tube, adding 50mL of deionized water into the quartz tube, performing ultrasonic dispersion to obtain 2mg/mL of graphene oxide aqueous dispersion, adding 0.1g of glucose into the dispersion, performing continuous ultrasonic dispersion at normal temperature for 30min, adding a stirrer into the quartz tube, placing the mixed solution under a 800W mercury lamp light source, stirring and illuminating for 1h, cooling the obtained product to room temperature, repeatedly centrifuging at a rotating speed of 12000r/min in a high-speed centrifuge, washing with deionized water, spray-drying the mixed solution in the centrifuge tube, transferring the mixed solution into a 100 ℃ vacuum oven, drying, and grinding to obtain graphene powder.
Fig. 1 is a morphology diagram of the graphene powder sample prepared in example 1, which is observed by a Transmission Electron Microscope (TEM), and it can be seen from the diagram that the prepared graphene powder has uniform lamella and good continuity.
Example 2
The preparation method of the graphene powder of the embodiment specifically includes the following steps:
Step 1: preparing graphene oxide: weighing 2g of graphite powder in a glass flask, adding 100ml of concentrated sulfuric acid with the mass percentage concentration of 90%, putting the beaker into a water bath kettle with ice blocks to stir for 2 hours, heating the mixed solution to 30 ℃ in the water bath kettle, continuously stirring for 1.5 hours to fully oxidize graphite, and slowly dropwise adding 10ml of hydrogen peroxide (H) with the mass percentage concentration of 30% into the mixed solution while stirring2O2) And adding 300ml of deionized water into the solution until the solution becomes brown yellow, continuously stirring for 30min, centrifuging the obtained solution in a high-speed centrifuge at the rotating speed of 10000r/min for 20min, removing the upper-layer solvent, respectively adding water and ethanol, repeatedly carrying out ultrasonic centrifugation washing at the rotating speed of 10000r/min until the pH value of the washing solution is 6-7, and finally carrying out suction filtration and drying to obtain the graphene oxide.
step 2: preparing graphene powder: weighing 0.3g of graphene oxide obtained in the step 1 in a quartz tube, adding 150mL of deionized water into the quartz tube, performing ultrasonic dispersion to obtain 2mg/mL of graphene oxide aqueous dispersion, adding 0.1g of fructose into the dispersion, performing continuous ultrasonic dispersion at normal temperature for 35min, adding a stirrer into the quartz tube, placing the mixed solution under a 500W mercury lamp, performing stirring and illumination for 2.5h, cooling the obtained product to room temperature, repeatedly centrifuging the product in a high-speed centrifuge at a rotating speed of 12000r/min, washing the product with deionized water, and finally performing spray drying on the mixed solution in the centrifuge tube, and transferring the product to a 100 ℃ vacuum oven for drying and grinding to obtain graphene powder.
Fig. 2 is a morphology diagram of a sample of example 2 observed by a Transmission Electron Microscope (TEM), and it can be seen from the diagram that the prepared graphene powder has uniform lamella and good continuity.
Example 3
The preparation method of the graphene powder of the embodiment specifically includes the following steps:
Step 1: preparing graphene oxide: weighing 2g of graphite powder in a glass flask, adding 100ml of concentrated sulfuric acid with the mass percent concentration of 98%, putting the beaker into a water bath kettle with ice blocks, stirring for 2 hours, heating the mixed solution to 30 ℃ in the water bath kettle, continuously stirring for 1.5 hours to fully oxidize graphite, and slowly dropwise adding 10ml of hydrogen peroxide (H) with the mass percent concentration of 30% into the mixed solution while stirring2O2) And adding 300ml of deionized water into the solution until the solution becomes brown yellow, continuously stirring for 30min, centrifuging the obtained solution in a high-speed centrifuge at the rotating speed of 10000r/min for 20min, removing the upper-layer solvent, respectively adding water and ethanol, repeatedly carrying out ultrasonic centrifugation washing at the rotating speed of 10000r/min until the pH value of the washing solution is 6-7, and finally carrying out suction filtration and drying to obtain the graphene oxide.
Step 2: preparing graphene powder: weighing 0.5g of graphene oxide obtained in the step 1 in a quartz tube, adding 250mL of deionized water into the quartz tube, performing ultrasonic dispersion to obtain 2mg/mL of graphene oxide aqueous dispersion, adding 0.1g of cane sugar into the dispersion, performing continuous ultrasonic dispersion for 40min at normal temperature, adding a stirrer into the quartz tube, placing the mixed solution under a 1000W xenon lamp, stirring and irradiating for 3.5h, cooling the obtained product to room temperature, repeatedly centrifuging at a rotating speed of 12000r/min in a high-speed centrifuge, washing with deionized water, and finally performing spray drying on the mixed solution in the centrifuge tube, and transferring the mixed solution into a 100 ℃ vacuum oven for drying and grinding to obtain graphene powder.
Fig. 3 is an atomic force microscope image of the graphene powder prepared in example 3 of the present invention, and it can be observed that the thickness of the graphene powder is only 1 to 5nm, and about 1 to 5 layers.
Example 4
The preparation method of the graphene powder of the embodiment specifically includes the following steps:
step 1: preparing graphene oxide: weighing 2g of graphite powder in a glass flask, adding 100ml of concentrated sulfuric acid with the mass percentage concentration of 90%, putting the beaker into a water bath kettle with ice blocks to stir for 2 hours, heating the mixed solution to 30 ℃ in the water bath kettle, continuously stirring for 1.5 hours to fully oxidize graphite, and slowly dropwise adding 10ml of hydrogen peroxide (H) with the mass percentage concentration of 30% into the mixed solution while stirring2O2) And adding 300ml of deionized water into the solution until the solution becomes brown yellow, continuously stirring for 30min, centrifuging the obtained solution in a high-speed centrifuge at the rotating speed of 10000r/min for 20min, removing the upper-layer solvent, respectively adding water and ethanol, repeatedly carrying out ultrasonic centrifugation washing at the rotating speed of 10000r/min until the pH value of the washing solution is 6-7, and finally carrying out suction filtration and drying to obtain the graphene oxide.
Step 2: preparing graphene powder: weighing 0.6g of graphene oxide obtained in the step 1 in a quartz tube, adding 300mL of deionized water into the quartz tube, performing ultrasonic dispersion to obtain 2mg/mL of graphene oxide aqueous dispersion, adding 0.1g of lactose into the dispersion, performing continuous ultrasonic dispersion for 40min at normal temperature, adding a stirrer into the quartz tube, placing the mixed solution under a 600W mercury lamp, performing stirring and illumination for 5h, cooling the obtained product to room temperature, repeatedly centrifuging the product in a high-speed centrifuge at a rotating speed of 12000r/min, washing the product with deionized water, and finally performing spray drying on the mixed solution in the centrifuge tube, and transferring the product to a 100 ℃ vacuum oven for drying and grinding to obtain graphene powder.
Fig. 4 is a raman spectrum of the graphene powder prepared in examples 2 and 4 of the present invention, and the intensities of the D peak and the G peak of the graphene powder are compared by analyzing the raman absorption spectrum bands of examples 2 and 4. When the graphene oxide is reduced, the oxygen-containing functional groups on the sheet are removed, sp2The degree of order of the carbon network structure increases, leading to ID/IGWill decrease and thus ID/IGThe lower the ratio of (a) indicates that the lower the oxygen content of the graphene oxide, the more fully the graphene oxide is reduced. Example 4 had a greater illumination intensity and illumination time than example 2, as shown by the graph, example 4ID/IGThe ratio is smaller than that of example 2, which shows that the oxygen content of example 4 is smaller than that of example 2, and graphene oxide is reduced more sufficiently.
Example 5
The preparation method of the graphene powder of the embodiment specifically includes the following steps:
Step 1: preparing graphene oxide: weighing 2g of graphite powder in a glass flask, adding 100ml of concentrated sulfuric acid with the mass percent concentration of 95%, putting the beaker into a water bath kettle with ice blocks to stir for 2 hours, heating the mixed solution to 30 ℃ in the water bath kettle, continuously stirring for 1.5 hours to fully oxidize graphite, and slowly dropwise adding 10ml of hydrogen peroxide (H) with the mass percent concentration of 30% into the mixed solution while stirring2O2) And adding 300ml of deionized water into the solution until the solution becomes brown yellow, continuously stirring for 30min, centrifuging the obtained solution in a high-speed centrifuge at the rotating speed of 10000r/min for 20min, removing the upper-layer solvent, respectively adding water and ethanol, repeatedly carrying out ultrasonic centrifugation washing at the rotating speed of 10000r/min until the pH value of the washing solution is 6-7, and finally carrying out suction filtration and drying to obtain the graphene oxide.
Step 2: preparing graphene powder: weighing 0.8g of graphene oxide obtained in the step 1 in a quartz tube, adding 400mL of deionized water into the quartz tube, performing ultrasonic dispersion to obtain 2mg/mL of graphene oxide aqueous dispersion, adding 0.1g of maltose into the dispersion, performing ultrasonic dispersion for 45min at normal temperature continuously, adding a stirrer into the quartz tube, placing the mixed solution under a 1500W xenon lamp, stirring and irradiating for 4h, cooling the obtained product to room temperature, repeatedly centrifuging at a rotating speed of 12000r/min in a high-speed centrifuge, washing with deionized water, spray-drying the mixed solution in the centrifuge tube, transferring the mixed solution into a 100 ℃ vacuum oven, drying, and grinding to obtain graphene powder.
Fig. 5 is a raman spectrum of the graphene powder prepared in example 5 of the present invention, and due to the lack of the graphene band gap, all incident waves resonate, so that the raman spectrum can effectively characterize the molecular vibration characteristics and electronic properties of the sample. The D peak is generally considered to be a defect peak of graphene, and the peak appears in the range of 1270-1450 cm-1And a weak D peak indicates high crystalline quality of the graphene sample. 1398cm from the figure-1The graphene defect peak is very weak, which indicates that the graphene defect is very few.
Claims (8)
1. A preparation method of graphene powder is characterized by comprising the following steps: the method specifically comprises the following steps:
Dispersing graphene oxide in water at normal temperature to form graphene oxide aqueous dispersion, then adding reducing sugar into the dispersion according to a ratio, ultrasonically dispersing uniformly, and then placing the obtained mixed solution under a lighting condition to stir and react for 1-5 h; and after the reaction is finished, cooling, centrifuging and washing the product, drying after spray drying, and grinding to obtain the graphene powder.
2. the method for preparing graphene powder according to claim 1, wherein: the mass concentration of the graphene oxide in the graphene oxide aqueous dispersion liquid is preferably 1-5 mg/mL.
3. the method for preparing graphene powder according to claim 1, wherein: the mass ratio of the reducing sugar to the graphene oxide is 1: 1-1: 8.
4. the method for preparing graphene powder according to claim 1, wherein: the reducing sugar is any one or more of glucose, fructose, sucrose, lactose or maltose.
5. The method for preparing graphene powder according to claim 1, wherein: the illumination light source is visible light or ultraviolet light.
6. The method for preparing graphene powder according to claim 1, wherein: the visible light power is preferably 1000-1500W, and the ultraviolet light power is preferably 500-800W.
7. The method for preparing graphene powder according to claim 1, wherein: the graphene oxide is prepared by oxidizing graphite, and comprises the following specific steps:
Stirring and mixing graphite powder and concentrated sulfuric acid uniformly under an ice bath condition, heating the obtained mixed solution to 30-40 ℃, stirring and reacting for 1-2H, and adding hydrogen peroxide (H) into the reaction system2O2) And (3) adding deionized water until the reaction solution becomes brown yellow, continuously stirring at constant temperature for reaction for 10-60 min, centrifuging and washing the product for several times after the reaction is finished until the pH value of the washing solution is 6-7, and finally, carrying out suction filtration and drying to obtain the graphene oxide.
8. The method for preparing graphene powder according to claim 7, wherein: the using amount ratio of the graphite powder to concentrated sulfuric acid, hydrogen peroxide and deionized water is 1 part by mass: 10-100 parts by volume: 1-10 parts by volume: 100-200 parts by volume, wherein: the mass portion and the volume portion are as follows: mL was used as a reference.
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Application publication date: 20191213 |