CN113443620B - Preparation method and application of few-layer graphene powder - Google Patents
Preparation method and application of few-layer graphene powder Download PDFInfo
- Publication number
- CN113443620B CN113443620B CN202110999980.0A CN202110999980A CN113443620B CN 113443620 B CN113443620 B CN 113443620B CN 202110999980 A CN202110999980 A CN 202110999980A CN 113443620 B CN113443620 B CN 113443620B
- Authority
- CN
- China
- Prior art keywords
- graphene
- few
- nano
- layer graphene
- dispersion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Classifications
-
- 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
- C01B32/19—Preparation by exfoliation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/04—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of carbon-silicon compounds, carbon or silicon
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/06—Lead-acid accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
-
- 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
-
- 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
-
- 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
- C01B2204/22—Electronic properties
-
- 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
- C01B2204/32—Size or surface area
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method of few-layer graphene powder, which comprises the following steps: stirring deionized water and an inorganic intercalation agent for pre-dispersion and high-speed shearing to obtain an inorganic intercalation solution; wherein the inorganic intercalation agent is one or more of nano fumed silica, superfine barium sulfate, nano calcium carbonate, nano titanium dioxide, nano iron oxide, nano zirconium oxide, nano zinc oxide, spherical alumina, carbon black and carbon nano tubes; adding expanded graphite and ethylene glycol into the inorganic intercalation solution, stirring for pre-dispersion, high-speed shearing and high-pressure stripping to obtain a few-layer graphene nano dispersion solution; and then centrifuging or filter-pressing for concentration, drying and crushing to obtain the few-layer graphene powder. According to the invention, the inorganic intercalation agent insoluble in water is selected as the intercalation agent for preparing graphene, so that no residue is caused in the graphene, the quality of the graphene is ensured, and meanwhile, the intercalation agent finishes intercalation and is wedged between graphene sheets, and the agglomeration of the graphene can be inhibited.
Description
Technical Field
The invention belongs to the field of graphene, and particularly relates to a preparation method and application of few-layer graphene powder.
Background
Graphene (Graphene) is the thinnest, hardest nanomaterial, and it is almost completely transparent, absorbing only 2.3% of light. Because the interatomic force is very strong, even if the surrounding carbon atoms are extruded and collided at normal temperature, the interference of electrons in the graphene is very small, and the electron mobility of the graphene exceeds 15000cm at normal temperature2V.s, the electron has a velocity of motion of 1/300 times that of light, and carbon is higher than that of nanotube or silicon crystal, and the resistivity is only about 10-6Ω · cm, lower than copper and silver.
The preparation method of the graphene mainly comprises a chemical vapor deposition method (CVD), an oxidation intercalation re-reduction method (GO-RGO), a liquid phase stripping method, a mechanical stripping method, a liquid phase mechanical stripping method and the like, wherein the chemical vapor deposition method can obtain high-quality graphene, but has low yield, high requirement on a substrate and great difficulty in transfer; the oxidation intercalation re-reduction method can realize the mass production of graphene, but the structure of the graphene is damaged in the oxidation process, so that a high-quality graphene product is difficult to obtain, a large amount of concentrated sulfuric acid is required for the oxidation intercalation, and the waste acid is huge and difficult to treat; the liquid phase exfoliation method dissociates the graphite sheet layer in a suitable solvent by using ultrasonic energy, however, the liquid phase exfoliation method for preparing graphene has the problem that the residual solvent is difficult to remove, and the solvent exfoliation yield is generally low. In contrast, the liquid-phase mechanical physical exfoliation method is a reliable and easy-to-implement method that can produce high-quality graphene at low cost. The intercalation agent is a commonly used stripping aid in a liquid-phase mechanical physical stripping method, however, most of inorganic intercalation agents in the prior art are soluble salts or surfactants, the inorganic intercalation agents mainly play a role in adjusting the surface tension of aqueous solution, and the intercalation agents are easy to remain in graphene after the preparation process of the graphene is completed and affect the quality of the graphene. For example, patent publication No. CN105967179B discloses a method for preparing a graphene powder material, in which graphene oxide is mainly used as a raw material, an organic dispersant is used to disperse and strip the graphene oxide, the organic dispersant is adsorbed in the graphene and is difficult to separate, which greatly affects the quality of the graphene, and the use of the organic dispersant affects the electrical and thermal conductivity of the graphene, which affects the application of the graphene in a lead storage battery.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the defects and shortcomings mentioned in the background technology and provide a preparation method and application of few-layer graphene powder.
In order to solve the technical problems, the technical scheme provided by the invention is as follows:
a preparation method of few-layer graphene powder comprises the following steps:
(1) stirring deionized water and an inorganic intercalation agent for pre-dispersion and high-speed shearing to obtain an inorganic intercalation solution; wherein the inorganic intercalation agent is one or more of nano fumed silica, superfine barium sulfate, nano calcium carbonate, nano titanium dioxide, nano iron oxide, nano zirconium oxide, nano zinc oxide and spherical alumina;
(2) adding expanded graphite and ethylene glycol into the inorganic intercalation solution prepared in the step (1) to perform stirring pre-dispersion, high-speed shearing and high-pressure stripping to obtain a few-layer graphene nano dispersion solution;
(3) and (3) centrifuging or filter-pressing the few-layer graphene nano dispersion liquid obtained in the step (2), concentrating, drying and crushing to obtain few-layer graphene powder.
In the preparation method, preferably, the inorganic intercalation agent is one or more of superfine barium sulfate, carbon black, carbon nano tube and spherical alumina.
In the preparation method, preferably, the particle size of the superfine barium sulfate is 2000 meshes, the diameter of the carbon nano tube is 3-30 nm, and the particle size of the spherical alumina is 0.5-5 um.
In the preparation method, preferably, in the step (1), the pre-dispersion is performed by stirring at 4000-6000rpm for 30-60 min; the shearing linear speed of the high-speed shearing is 30-60 m/s, and the high-speed shearing time is 30-60 min.
In the preparation method, preferably, in the step (2), the pre-dispersion is performed by stirring at 4000-6000rpm for 30-60 min; the shearing linear speed of the high-speed shearing is 30-60 m/s, and the high-speed shearing time is 30-180 min; the high-pressure stripping is carried out in a high-pressure homogenizer, the linear speed of the high-pressure stripping is more than 200m/s, and the time is 30-560 min.
In the preparation method, the mass ratio of the inorganic intercalation agent to the expanded graphite is preferably 1: 0.5-50.
In the preparation method, preferably, in the step (2), the mass ratio of the expanded graphite to the ethylene glycol is 1: 0.1 to 2.
In the above preparation method, preferably, the expanded graphite is high-magnification expanded graphite, and the expansion magnification is 200 times, 400 times, 600 times or 800 times.
As a general inventive concept, the invention also provides an application of the few-layer graphene powder prepared by the preparation method in a conductive material or a lead-acid storage battery.
Compared with the prior art, the invention has the advantages that:
(1) the graphene prepared by the invention has high conductivity, and particularly, the carbon nano tube and the carbon black are selected as the intercalation agent, so that the carbon nano tube and the carbon black can be used as conductive materials, the conductivity of the graphene material is not affected like the introduction of an organic intercalation agent, and the charge and discharge capacity of a battery can be better improved when the graphene is applied to a lead-acid storage battery.
(2) The invention selects the few-layer graphene prepared by using superfine barium sulfate as the intercalation agent to be applied to the lead-acid storage battery, and can inhibit lead sulfate crystallization in the process of charging and discharging, thereby prolonging the cycle life of the lead-acid storage battery, and simultaneously, the graphene as a conductive material can improve the charging capacity of the lead-acid storage battery; in addition, barium sulfate is an auxiliary material of the lead-acid battery and is applied to the lead-acid battery in a large area, so that the use of the intercalation agent not only can not bring other impurities into the lead-acid battery, but also has a positive influence on the performance of the lead-acid battery.
(3) In the preparation process of the few-layer graphene powder, high-magnification expanded graphite is selected as a main raw material of graphene, a liquid-phase mechanical stripping method is used, a water-insoluble inorganic intercalation agent is creatively selected to perform intercalation stripping on the graphene, the particles of the inorganic intercalation agent are very small, the inorganic particles are dispersed and enter between graphite sheets of the expanded graphite by using the ultrahigh linear speed of a high-pressure homogenizer, the graphite stripping efficiency is improved, then cleavage is performed to obtain a few-layer graphene dispersion liquid, and the few-layer graphene powder material is obtained after concentration, drying and crushing.
(4) The preparation method of the few-layer graphene powder has the advantages that the expanded graphite is fully stripped in the preparation process, the stripping efficiency is high, deionized water is used as a dispersing stripping medium, the production cost is greatly reduced, the graphene dispersion liquid is concentrated and then dried by using a centrifugal or filter pressing process, the energy consumption is reduced, the cost is reduced, the process is economical and reliable, the stability is high, waste acid and wastewater discharge is basically avoided, the batch low-cost green production of few-layer graphene can be realized, the prepared graphene powder is few in layers, high in purity, excellent in conductivity, large in specific surface area and complete in lamellar structure, and the preparation method is very suitable for being applied to conductive materials and lead-acid batteries.
Drawings
FIG. 1 is an SEM photograph of a few-layer graphene powder prepared in example 1 of the present invention;
FIG. 2 is an SEM photograph of a few-layer graphene powder prepared in example 3 of the present invention;
fig. 3 is an SEM photograph of the graphene powder prepared in comparative example 1 of the present invention;
fig. 4 is an SEM photograph of the graphene powder prepared in comparative example 2 of the present invention.
Detailed Description
In order to facilitate an understanding of the present invention, the present invention will be described more fully and in detail with reference to the preferred embodiments, but the scope of the present invention is not limited to the specific embodiments below.
Unless otherwise defined, all terms of art used hereinafter have the same meaning as commonly understood by one of ordinary skill in the art. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to limit the scope of the present invention.
Unless otherwise specifically stated, various raw materials, reagents, instruments, equipment and the like used in the present invention are commercially available or can be prepared by existing methods.
Example 1:
the invention discloses a preparation method of few-layer graphene powder, which comprises the following steps:
s1: stirring 85 parts of deionized water and 5 parts of 2000-mesh superfine barium sulfate at the rotating speed of 6000rpm for pre-dispersion for 60 minutes to obtain an intercalator pre-dispersion liquid;
s2: shearing the pre-dispersion liquid of S1 at a super high speed for 60 minutes at a shearing linear speed of 50m/S to obtain an intercalator dispersion liquid which is fully and uniformly dispersed;
s3: adding 9 parts of 400-time expanded graphite and 3 parts of ethylene glycol into the dispersion liquid prepared in S2, and stirring and pre-dispersing for 50 minutes at 4000rpm to obtain a pre-dispersion liquid of the expanded graphite and the intercalation agent;
s4: the pre-dispersion liquid obtained in the step S3 is sheared and peeled at a high speed, wherein the linear shearing speed is 50m/S, and the high-speed shearing is carried out for 100min, so that a preliminarily peeled graphene coarse dispersion liquid is obtained;
s5: carrying out high-pressure stripping on the graphene coarse dispersion liquid obtained in the step S4 by using a high-pressure homogenizer, wherein the high-pressure stripping linear speed is more than 200m/S, and the high-pressure stripping is carried out for 100min to obtain a fully stripped few-layer graphene dispersion liquid;
s6: centrifuging the few-layer graphene dispersion liquid obtained in the step S5 to obtain a few-layer graphene filter cake with high solid content;
s7: putting the filter cake into a high-temperature oven, and drying at 160 ℃ to obtain blocky few-layer graphene;
s8: and crushing the blocky few-layer graphene by using an airflow crusher to obtain few-layer high-purity graphene powder.
The scanning electron microscope image of the few-layer high-purity graphene powder prepared in this example is shown in fig. 1.
Example 2:
the invention discloses a preparation method of few-layer graphene powder, which comprises the following steps:
s1: stirring 88 parts of deionized water and 2 parts of carbon nano tubes at the rotating speed of 6000rpm for pre-dispersion for 60 minutes to obtain an intercalator pre-dispersion liquid;
s2: carrying out ultrahigh-speed shearing on the pre-dispersion liquid of S1 for 60 minutes at a shearing linear speed of 40m/S to obtain an intercalator dispersion liquid which is fully and uniformly dispersed;
s3: adding 9 parts of 400-time expanded graphite and 3 parts of ethylene glycol into the nano intercalation solution prepared by S2, and stirring at a high speed of 5000rpm for pre-dispersion for 30 minutes to obtain a pre-dispersion solution of the expanded graphite and the intercalation agent;
s4: shearing and stripping the pre-dispersion liquid of S3 at a super high speed, wherein the linear shearing speed is 60m/S, and the high-speed shearing is carried out for 120min to obtain a preliminarily stripped graphene coarse dispersion liquid;
s5: stripping the graphene coarse dispersion liquid obtained in the step S4 at high pressure by using a high-pressure homogenizer, wherein the high-pressure stripping linear speed is more than 200m/S, and the high-pressure stripping is carried out for 120min to obtain a fully stripped few-layer graphene dispersion liquid;
s6: centrifuging the nano graphene dispersion liquid obtained in the step S5 to obtain a few-layer graphene filter cake with high solid content;
s7: putting the filter cake into a high-temperature oven, and drying at 160 ℃ to obtain blocky few-layer graphene;
s8: and crushing the blocky few-layer graphene by using an airflow crusher to obtain few-layer high-purity graphene powder.
The scanning electron microscope image of the few-layer high-purity graphene powder prepared in this example is shown in fig. 2.
Example 3:
the invention discloses a preparation method of few-layer graphene powder, which comprises the following steps:
s1: stirring 85 parts of deionized water and 5 parts of spherical alumina at the rotating speed of 6000rpm for pre-dispersion for 50 minutes to obtain an intercalator pre-dispersion liquid;
s2: carrying out ultrahigh-speed shearing on the pre-dispersion liquid of S1 for 60 minutes at a shearing linear speed of 40m/S to obtain an intercalator dispersion liquid which is fully and uniformly dispersed;
s3: adding 9 parts of 400-time expanded graphite and 3 parts of ethylene glycol into the intercalation dispersion liquid prepared by S2, and stirring and pre-dispersing for 50 minutes at 4000rpm to obtain a pre-dispersion liquid of the expanded graphite and the intercalation agent;
s4: shearing and stripping the pre-dispersion liquid of S3 by using ultra-high-speed shearing, wherein the shearing linear speed is 60m/S, and the high-speed shearing is performed for 100min to obtain a preliminarily stripped graphene coarse dispersion liquid;
s5: stripping the graphene coarse dispersion liquid obtained in the step S4 at high pressure by using a high-pressure homogenizer, wherein the high-pressure stripping linear speed is more than 200m/S, and the high-pressure stripping is carried out for 80min to obtain a fully stripped few-layer graphene nano dispersion liquid;
s6: centrifuging the nano graphene dispersion liquid obtained in the step S5 to obtain a few-layer graphene filter cake with high solid content;
s7: putting the filter cake into a high-temperature oven, and drying at 160 ℃ to obtain blocky few-layer graphene;
s8: and crushing the blocky few-layer graphene by using an airflow crusher to obtain few-layer high-purity graphene powder.
Comparative example 1:
the preparation method of the graphene powder comprises the following steps:
s1: stirring 88 parts of deionized water at the rotating speed of 6000rpm for pre-dispersion for 60 minutes, and then shearing at an ultrahigh speed for 60 minutes at the shearing linear speed of 40m/s to obtain a dispersion liquid;
s2: adding 9 parts of 400-time expanded graphite and 3 parts of ethylene glycol into the dispersion liquid prepared in S1, and stirring at a high speed of 5000rpm for pre-dispersion for 30 minutes to obtain a pre-dispersion liquid of the expanded graphite;
s3: carrying out ultrahigh-speed shearing stripping on the pre-dispersion liquid of S2 at a shearing linear speed of 60m/S for 120min to obtain a preliminarily stripped graphene coarse dispersion liquid;
s4: stripping the graphene coarse dispersion liquid obtained in the step S3 at high pressure by using a high-pressure homogenizer, wherein the high-pressure stripping linear speed is more than 200m/S, and the high-pressure stripping is carried out for 120min to obtain a fully-stripped graphene dispersion liquid;
s5: centrifuging the graphene dispersion liquid obtained in the step S4 to obtain a few-layer graphene filter cake with high solid content;
s6: putting the filter cake into a high-temperature oven for drying, wherein the drying temperature is 160 ℃, and obtaining blocky graphene;
s7: and crushing the blocky graphene by using an airflow crusher to obtain high-purity graphene powder.
The scanning electron micrograph of the graphene powder prepared in this comparative example is shown in fig. 3.
Comparative example 2:
the preparation method of the graphene powder comprises the following steps:
s1: stirring 88 parts of deionized water and 2 parts of dispersant polyethylene oxide (PEO) at the rotating speed of 6000rpm for pre-dispersion for 60 minutes, and then shearing at a super high speed for 60 minutes at the shearing linear speed of 40m/s to obtain dispersion liquid;
s2: adding 9 parts of 400-time expanded graphite and 3 parts of ethylene glycol into the dispersion liquid prepared in S1, and stirring at a high speed of 5000rpm for pre-dispersion for 30 minutes to obtain a pre-dispersion liquid of the expanded graphite;
s3: carrying out ultrahigh-speed shearing stripping on the pre-dispersion liquid of S2 at a shearing linear speed of 60m/S for 120min to obtain a preliminarily stripped graphene coarse dispersion liquid;
s4: stripping the graphene coarse dispersion liquid obtained in the step S3 at high pressure by using a high-pressure homogenizer, wherein the high-pressure stripping linear speed is more than 200m/S, and the high-pressure stripping is carried out for 120min to obtain a fully stripped few-layer graphene dispersion liquid;
s5: centrifuging the few-layer graphene dispersion liquid obtained in the step S4 to obtain a few-layer graphene filter cake with high solid content;
s6: putting the filter cake into a high-temperature oven for drying, wherein the drying temperature is 160 ℃, and obtaining blocky few-layer graphene;
s7: and crushing the blocky few-layer graphene by using an airflow crusher to obtain the few-layer graphene powder.
The graphene powder prepared in this comparative example is shown in fig. 4.
As can be seen from comparison between fig. 1 of example 1 and fig. 2 of example 2 and fig. 3 of comparative example 1 and fig. 4 of comparative example 2, the graphene materials with fewer layers and thinner thickness can be obtained in examples 1 and 2 by using the inorganic intercalator, while the expanded graphite is not completely exfoliated in comparative example 1, and the thickness of the graphite sheet layer is thicker, which indicates that the inorganic intercalator has a significant effect on intercalation of the expanded graphite, and fig. 4 shows that the graphene powder with fewer layers can be prepared by using the organic dispersant PEO, but the graphene powder prepared by using the organic dispersant is easy to agglomerate and has a relatively smaller specific surface area, and the organic dispersant is easy to remain in the graphene powder and has a greater influence on the later-stage conductivity of the graphene.
The performance parameters of the few-layer graphene powder prepared in the embodiment and the comparative example are shown in table 1, and as can be seen from table 1, the auxiliary stripping effect of the inorganic intercalation agent selected by the invention on graphene is obvious, the nano intercalation agent disclosed by the invention is used for stripping graphite, the thickness of the prepared graphene sheet is only 3nm, the improvement is obvious compared with that of the comparative example 1 without the nano intercalation agent, the conductivity is better compared with that of the comparative example 2, the ash content is lower, and the graphene powder is relatively suitable for being applied to a lead-acid storage battery; moreover, the specific surface area of the graphene prepared by the embodiment of the invention is larger than that of the comparative example, and the loose packed density is smaller, which shows that the graphene powder prepared by the inorganic intercalation agent adopted by the invention is less agglomerated in the drying process.
TABLE 1 graphene powder Performance parameters
Claims (7)
1. The application of the few-layer graphene powder in the lead-acid storage battery is characterized in that the preparation method of the few-layer graphene powder comprises the following steps:
(1) stirring deionized water and an inorganic intercalation agent for pre-dispersion and high-speed shearing to obtain an inorganic intercalation solution; wherein the inorganic intercalation agent is superfine barium sulfate;
(2) adding expanded graphite and ethylene glycol into the inorganic intercalation solution prepared in the step (1) to perform stirring pre-dispersion, high-speed shearing and high-pressure stripping to obtain a few-layer graphene nano dispersion solution;
(3) and (3) centrifuging or filter-pressing the few-layer graphene nano dispersion liquid obtained in the step (2), concentrating, drying and crushing to obtain few-layer graphene powder.
2. The use of claim 1, wherein the ultra-fine barium sulfate has a particle size of 2000 mesh.
3. The method as claimed in claim 1, wherein in the step (1), the pre-dispersion is performed by stirring at 6000rpm for 30-60 min; the shearing linear speed of the high-speed shearing is 30-60 m/s, and the high-speed shearing time is 30-60 min.
4. The use as claimed in claim 1, wherein in step (2), the pre-dispersion is carried out by stirring at 4000-6000rpm for 30-60 min; the shearing linear speed of the high-speed shearing is 30-60 m/s, and the high-speed shearing time is 30-180 min; the high-pressure stripping is carried out in a high-pressure homogenizer, the linear speed of the high-pressure stripping is more than 200m/s, and the time is 30-560 min.
5. The use according to any one of claims 1 to 4, wherein the mass ratio of the inorganic intercalant to the expanded graphite is 1: 0.5 to 50.
6. The use according to any one of claims 1 to 4, wherein in step (2), the mass ratio of expanded graphite to ethylene glycol is 1: 0.1 to 2.
7. The use according to any one of claims 1 to 4, wherein in step (2), the expanded graphite is a high-rate expanded graphite having an expansion rate of 200 times, 400 times, 600 times or 800 times.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110999980.0A CN113443620B (en) | 2021-08-30 | 2021-08-30 | Preparation method and application of few-layer graphene powder |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110999980.0A CN113443620B (en) | 2021-08-30 | 2021-08-30 | Preparation method and application of few-layer graphene powder |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113443620A CN113443620A (en) | 2021-09-28 |
| CN113443620B true CN113443620B (en) | 2021-12-14 |
Family
ID=77818924
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110999980.0A Active CN113443620B (en) | 2021-08-30 | 2021-08-30 | Preparation method and application of few-layer graphene powder |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113443620B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114014308A (en) * | 2021-12-13 | 2022-02-08 | 中科悦达(上海)材料科技有限公司 | Preparation method of graphene composite material and graphene composite material |
| CN115465860B (en) * | 2022-07-06 | 2023-06-16 | 山东海科创新研究院有限公司 | Preparation method of low-oxygen and high-stripping graphene oxide and application of obtained product |
Family Cites Families (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101857221A (en) * | 2010-05-21 | 2010-10-13 | 哈尔滨工业大学 | Method for preparing graphene compounds and graphene oxide compounds with high efficiency |
| CN101817516A (en) * | 2010-05-21 | 2010-09-01 | 哈尔滨工业大学 | Method for preparing graphene or graphene oxide by using high-efficiency and low-cost mechanical stripping |
| CN103456520B (en) * | 2012-05-31 | 2016-12-14 | 海洋王照明科技股份有限公司 | A kind of preparation method and applications of graphene/carbon nanotube composite film |
| CN103030138B (en) * | 2012-12-17 | 2015-08-19 | 鸿纳（东莞）新材料科技有限公司 | Prevent back component and the preparation of folded few layer graphene powder and matrix material thereof |
| CN107416810A (en) * | 2017-06-19 | 2017-12-01 | 成都新柯力化工科技有限公司 | A kind of method that graphene is peeled off using alternating electric field vibro-grinding |
| CN107317034A (en) * | 2017-07-06 | 2017-11-03 | 深圳市国创珈伟石墨烯科技有限公司 | A kind of preparation, process for dispersing and the equipment of graphene/carbon nano-tube composite conducting slurry |
| CN108690346A (en) * | 2018-04-11 | 2018-10-23 | 杭州牛墨科技有限公司 | A kind of preparation method of high conversion graphene carbon nanotube heating film |
| CN108565440A (en) * | 2018-04-11 | 2018-09-21 | 杭州牛墨科技有限公司 | A kind of preparation method for the graphene carbon nanotube composite heating film covering heating region |
| CN109455707A (en) * | 2018-12-27 | 2019-03-12 | 宁波杉元石墨烯科技有限公司 | A kind of graphene slurry and preparation method thereof of the grinding aid containing dispersion |
| CN110902674B (en) * | 2019-12-17 | 2023-05-09 | 电子科技大学 | Preparation method of high-quality graphene oxide |
-
2021
- 2021-08-30 CN CN202110999980.0A patent/CN113443620B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN113443620A (en) | 2021-09-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111799464B (en) | MXene/graphene composite nanosheet, preparation method and application thereof, electrode plate and application thereof | |
| CN113443620B (en) | Preparation method and application of few-layer graphene powder | |
| CN112366301B (en) | Silicon/silicon oxide/carbon composite negative electrode material for lithium ion battery and preparation method thereof | |
| Xu et al. | Fabrication of a graphene–cuprous oxide composite | |
| CN106882796B (en) | Preparation method of three-dimensional graphene structure/high-quality graphene | |
| US20230197929A1 (en) | Method of making electrodes containing carbon sheets decorated with nanosized metal particles and electrodes made therefrom | |
| CN107978742B (en) | C-doped flower spherical titanium dioxide/molybdenum disulfide composite material formed by nanosheets and preparation method thereof | |
| KR101563585B1 (en) | Method for preparation of graphene using spontaneous process | |
| US20150158729A1 (en) | Method for Manufacturing Nano-Graphene Sheets | |
| WO2006125358A1 (en) | A composite carbon material of negative electrode in lithium ion battery and its preparation method | |
| Ye et al. | One-pot synthesis of Fe2O3/graphene and its lithium-storage performance | |
| KR101465385B1 (en) | A micron sized anode active material containing titanium dioxide nanoparticles and method for the preparation thereof | |
| CN110336003B (en) | Porous silicon-based composite material and preparation method and application thereof | |
| Guan et al. | Low-cost urchin-like silicon-based anode with superior conductivity for lithium storage applications | |
| CN111498839A (en) | Ultrathin sheet layer reduced graphene oxide and synthesis method thereof | |
| Han et al. | Facile assembly of α-Fe2O3 nanorings@ reduced graphene oxide composites with high lithium storage performance | |
| Liang et al. | Biomass based composite used as anode materials: Porous ZnO anchored on the rice husk-derived carbon substrate for Li-ion batteries | |
| Luo et al. | The optimization of porosity and particle size for micron-size porous silicon in high energy pre-lithiated silicon-graphite composite for Li-ion batteries | |
| Fu et al. | TiO2 mesoporous single crystals with controllable architectures and TiO2/graphene oxide nanocomposites for high-performance lithium ion battery anodes | |
| CN111403723A (en) | Silicon-carbon negative electrode composite material, preparation method thereof and lithium ion battery | |
| CN113130857A (en) | Nano silicon material and preparation method thereof | |
| CN110690442A (en) | Preparation method of ordered mesoporous metal oxide @ carbon lithium ion battery cathode material | |
| CN113675385B (en) | Nanoscale silicon-carbon composite negative electrode material, preparation method and lithium ion battery | |
| CN112919431B (en) | Hexagonal boron nitride nano-sheet with high yield and high crystallinity and preparation method thereof | |
| CN113659124B (en) | Germanium-doped silicon-like negative electrode material, and preparation method and application thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |