CN111155161A - Graphene-aluminum composite material and preparation method thereof - Google Patents
Graphene-aluminum composite material and preparation method thereof Download PDFInfo
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- CN111155161A CN111155161A CN201911419415.1A CN201911419415A CN111155161A CN 111155161 A CN111155161 A CN 111155161A CN 201911419415 A CN201911419415 A CN 201911419415A CN 111155161 A CN111155161 A CN 111155161A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D15/00—Electrolytic or electrophoretic production of coatings containing embedded materials, e.g. particles, whiskers, wires
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D3/00—Electroplating: Baths therefor
- C25D3/66—Electroplating: Baths therefor from melts
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- 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
- H01B1/02—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of metals or alloys
- H01B1/023—Alloys based on aluminium
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- 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
Abstract
The invention relates to a preparation method of a graphene-aluminum composite material, which comprises the following steps: providing graphene oxide containing amino groups; dispersing the graphene oxide containing the amino group in an electrolytic salt, and heating to melt the electrolytic salt to form a graphene oxide dispersion liquid; and respectively taking the two aluminum bars as a cathode and an anode, and electrolyzing by taking the graphene oxide dispersion liquid as electrolyte to form a graphene aluminum composite coating on the surface of the cathode. The invention also relates to a graphene-aluminum composite material prepared by the preparation method of the graphene-aluminum composite material. The invention further relates to a cable or wire comprising the graphene-aluminum composite material.
Description
Technical Field
The invention relates to the technical field of metal matrix composite materials, in particular to a graphene-aluminum composite material and a preparation method thereof.
Background
The graphene aluminum-based composite material has high strength, high electrical conductivity, high thermal conductivity and high wear resistance, and is a key material for the current material research, but due to the inherent wettability difference between metal and nonmetal, graphene is difficult to be uniformly distributed in an aluminum matrix, and in order to achieve a good graphene dispersion uniformity, a large amount of time is usually consumed for carrying out a mixing process; in addition, the traditional preparation method such as the powder metallurgy method can easily lead the graphene and the aluminum matrix to generate a carbon aluminum compound Al in the high-temperature process of the forming stage4C3The substance is easy to hydrolyze in air, and the generated brittle phase seriously influences the strength of the composite material.
Therefore, a method for preparing the graphene aluminum matrix composite material with high efficiency and without high-temperature molding is urgently needed to be found.
Disclosure of Invention
Based on the above, it is necessary to provide a graphene aluminum composite material, a preparation method thereof, and a cable or wire comprising the graphene aluminum composite material, aiming at the problems of long preparation time and high temperature molding.
The invention provides a preparation method of a graphene-aluminum composite material, which comprises the following steps:
providing graphene oxide containing amino groups;
dispersing the graphene oxide containing the amino group in an electrolytic salt, and heating to melt the electrolytic salt to form a graphene oxide dispersion liquid; and
and respectively taking two aluminum bars as a cathode and an anode, and taking the graphene oxide dispersion liquid as electrolyte to carry out electrolysis to form a graphene aluminum composite coating on the surface of the cathode.
In one embodiment, the content of amino groups in the graphene oxide containing amino groups is 0.2 wt% to 0.5 wt%.
In one embodiment, the number of graphene layers in the graphene oxide containing amino groups is 1 to 10, the thickness is 0.55 to 3.74nm, and the diameter is 0.5 to 3 μm.
In one embodiment, the electrolytic salt comprises one or more of sodium chloride, potassium chloride, and aluminum chloride.
In one embodiment, the electrolytic salts are sodium chloride, potassium chloride, and aluminum chloride.
In one embodiment, the mass ratio of sodium chloride, potassium chloride and aluminum chloride in the electrolytic salt is 1: (1-3): (6-10).
In one embodiment, the mass ratio of the graphene oxide containing amino groups to the electrolytic salt is (0.2-0.5): 1.
in one embodiment, the electrolysis current is 300 mA-400 mA, the electrolysis time is 40 min-60 min, and the distance between the two aluminum bars is 2 cm-5 cm.
The invention also provides a graphene-aluminum composite material prepared by the preparation method of the graphene-aluminum composite material.
The invention further provides a cable or wire containing the graphene reinforced aluminum matrix composite.
According to the preparation method of the graphene-aluminum composite material, provided by the invention, the graphene oxide containing amino groups is dispersed in molten electrolytic salt, and NH in the graphene oxide4 +The graphene oxide can rapidly move to the cathode under the action of the electric field, aluminum ions generated by the anode also move to the cathode, electrons obtained at the cathode are reduced into simple-substance aluminum, and the simple-substance aluminum and graphene oxide lamella are deposited on the cathode together to obtain the graphene-aluminum composite material.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
The embodiment of the invention provides a preparation method of a graphene-aluminum composite material, which is characterized by comprising the following steps of:
s10, providing graphene oxide containing amino groups;
s20, dispersing graphene oxide containing amino groups in electrolytic salt, and heating to melt the electrolytic salt to form a graphene oxide dispersion liquid; and
and S30, respectively taking two aluminum bars as a cathode and an anode, and taking the graphene oxide dispersion liquid formed in the step S20 as an electrolyte to carry out electrolysis, so as to form a graphene aluminum composite plating layer on the surface of the cathode.
According to the preparation method of the graphene-aluminum composite material, provided by the invention, the graphene oxide containing amino groups is dispersed in molten electrolytic salt, and NH in the graphene oxide4 +Under the action of the electric field, the graphene oxide can rapidly move to the cathode, aluminum ions generated by the anode also move to the cathode, electrons obtained at the cathode are reduced into simple substance aluminum, and the simple substance aluminum and the graphene oxide sheet layer are deposited on the cathode together to obtain the graphene aluminum composite material. Graphene in the graphene-aluminum composite material can be uniformly distributed in aluminum, and the graphene-aluminum composite material has better conductivity and mechanical strength.
In an embodiment, the content of amino groups in the amino group-containing graphene oxide is 0.2 wt% to 0.5 wt%. The content of amino groups affects the speed at which graphene oxide moves towards the cathode in an electric field.
In one embodiment, the number of graphene layers in the amino group-containing graphene oxide is 1 to 10, the thickness is 0.55 to 3.74nm, and the diameter is 0.5 to 3 μm. The number of layers, thickness, and diameter of graphene further affect the speed at which graphene oxide moves towards the cathode in an electric field.
The graphene oxide containing an amino group may be obtained by an amino group reagent addition method or an electrochemical exfoliation method.
In one embodiment, the method for preparing graphene oxide containing amino groups by using an amino group reagent method comprises the following steps:
s11, providing a graphene oxide dispersion liquid, adding an amino reagent, and uniformly mixing;
and S13, heating the mixed solution obtained in the step S11 for reaction, and then freeze-drying to obtain the graphene oxide containing amino groups.
In an embodiment, the solid content of the graphene oxide dispersion liquid in step S11 is 2mg/mL to 3 mg/mL.
In one embodiment, the amino reagents added are ethylenediamine and ammonia.
In one embodiment, the volume ratio of the amino reagent to the graphene oxide dispersion liquid is (0.002-0.003): 1.
In one embodiment, the heating temperature in step S13 is 85 to 100 ℃, preferably 95 to 100 ℃.
In one embodiment, the preparation of the graphene oxide containing amino groups by an electrochemical stripping method comprises the following steps:
and S12, providing the stripped graphene oxide as a cathode and an anode, and adding an amino-containing salt into the electrolyte for electrolysis to obtain the amino-containing graphene oxide.
In one embodiment, the salt containing amino is cyanamide sulfate, and the addition amount of the cyanamide sulfate is 0.4mol/L to 0.5 mol/L.
In one embodiment, the electrolysis current in step S12 is 0.4A to 0.5A, and the electrolysis time is 5h to 6 h.
In one embodiment, the electrolytic salt comprises one or more of sodium chloride, potassium chloride and aluminum chloride. Preferably, the electrolytic salts are sodium chloride, potassium chloride and aluminum chloride. Wherein, the mass ratio of the sodium chloride, the potassium chloride and the aluminum chloride can be 1: (1-3): (6-10), 1:2:6, 1:2:7, 1:2:8, 1:2:9, 1:3:7, 1:2:8, 1:2:9, 1:1:7, 1:1:8, 1:1:9 may also be selected. The specific composition and content of the electrolytic salt affect the moving speed of the aluminum ions.
In one embodiment, the mass ratio of the graphene oxide containing amino groups to the electrolytic salt is (0.2-0.5): 1. the graphene oxide absorption dispersion liquid with different solid contents is formed by different mass ratios of the graphene oxide containing amino and the electrolytic salt, and the different solid contents of the graphene oxide absorption dispersion liquid further influence the speed of the graphene oxide moving to the cathode in an electric field and influence the distribution condition of the graphene in the graphene aluminum composite coating.
In one embodiment, the electrolysis current is 300 mA-400 mA, the electrolysis time is 40 min-60 min, and the distance between the two aluminum bars is 2 cm-5 cm. The current magnitude directly influences the migration speed of graphene oxide and aluminum ions in electrolysis, the distance between two aluminum bars further influences the distribution condition of graphene in the graphene aluminum composite coating, and the electrolysis time determines the thickness of the graphene aluminum composite coating. In addition, when the current is large, the amino graphene is reduced.
In one embodiment, the temperature for melting the electrolytic salt is 180-220 deg.C, and may be 190 deg.C, 200 deg.C, or 210 deg.C. After the electrolytic salt is changed into a molten state, the graphene oxide containing the amino is dispersed in the molten electrolytic salt to form graphene oxide dispersion liquid, so that the viscosity of the molten electrolytic salt in a temperature range is high, the graphene cannot float upwards, and the graphene is uniformly distributed in the graphene-aluminum composite coating.
In one embodiment, the process of melting the electrolytic salt is performed under an inert atmosphere.
In one embodiment, the electrolytic salt may be previously dried.
The invention also provides a graphene-aluminum composite material prepared by the preparation method of the graphene-aluminum composite material. The graphene-aluminum composite material takes an aluminum bar as a substrate, and a graphene-aluminum composite coating is formed on the aluminum bar substrate. In one embodiment, the aluminum rod has a diameter of 3mm to 6 mm. In one embodiment, the thickness of the graphene aluminum composite coating is 100nm to 100 μm.
The following are specific examples:
example 1
(1) 500mL of graphene oxide solution with solid content of 2mg/mL is taken, 1mL of ethylenediamine and 0.2mL of ammonia water are added into the graphene oxide solution, the mixture is stirred and mixed for 2 hours by a stirrer at the rotating speed of 200rpm, then the mixture is sealed and placed into a constant-temperature water bath kettle to react for 12 hours at 95 ℃, and then the graphene oxide solution is frozen and dried to obtain the graphene oxide containing amino groups (the content of the amino groups is 0.2 wt%).
(2) 10g of sodium chloride, 10g of potassium chloride and 80g of aluminum chloride were weighed and dried at 120 ℃ for 4 hours, respectively.
(3) Taking 20g of the amino-containing graphene oxide prepared in the step (1), uniformly mixing the amino-containing graphene oxide with the sodium chloride, the potassium chloride and the aluminum chloride in the step (2), and simultaneously mixing the amino-containing graphene oxide with two diameters of
The pure aluminum rods are used as an anode and a cathode and are respectively inserted into electrolytic salt, the vacuum degree of the electrolytic cell is pumped to be below 5Pa by a vacuum pump, and then argon is introduced to the normal pressure.
(4) And heating the electrolytic bath to 200 ℃, preserving heat to enable the electrolytic salt to be molten, and dispersing the graphene oxide containing amino in the molten electrolytic salt to form a graphene oxide dispersion liquid serving as an electrolyte.
(5) And (3) introducing 300mA electrolysis current into the electrolysis device, electrolyzing for 60min, taking out the cathode after electrolysis, and washing with deionized water to obtain the graphene-aluminum composite material.
Example 2
Substantially the same as in example 1, except that in the step (1), the content of amino groups in the graphene oxide containing amino groups was 0.3 wt%.
Example 3
Substantially the same as in example 1, except that in the step (1), the content of amino groups in the graphene oxide containing amino groups was 0.5 wt%.
Example 4
Substantially the same as in example 1 except that in step (5), the electrolytic current was 350 mA.
Example 5
Substantially the same as in example 1 except that in step (5), the electrolytic current was 400 mA.
Test example
The graphene reinforced aluminum matrix composite material prepared in the embodiment 1-5 is subjected to a tensile strength test and a conductivity test. The conductivity test method comprises the steps of mechanically polishing the surface of a material, testing by using an eddy current conductivity meter, testing the tensile strength by cutting the material wire into a shape of a dog bone with a stretching interval of 18mm, polishing the surface, and testing the tensile force by using a universal experimental stretcher, wherein the stretching speed is 0.5mm/min, and the test result is shown in table 1:
tensile test a standard piece with a tensile zone of 18mm was cut by wire cutting.
TABLE 1
| Tensile strength/MPa | Conductivity/% IACS | |
| Example 1 | 105 | 65 |
| Example 2 | 104 | 62 |
| Example 3 | 104 | 60 |
| Example 4 | 102 | 60 |
| Example 5 | 100 | 58 |
| Pure aluminum of the same size | 86 | 59 |
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. The preparation method of the graphene-aluminum composite material is characterized by comprising the following steps:
providing graphene oxide containing amino groups;
dispersing the graphene oxide containing the amino group in an electrolytic salt, and heating to melt the electrolytic salt to form a graphene oxide dispersion liquid; and
and respectively taking two aluminum bars as a cathode and an anode, and taking the graphene oxide dispersion liquid as electrolyte to carry out electrolysis to form a graphene aluminum composite coating on the surface of the cathode.
2. The method for preparing the graphene aluminum composite material according to claim 1, wherein the content of the amino group in the graphene oxide containing the amino group is 0.2 wt% to 0.5 wt%.
3. The method for preparing the graphene-aluminum composite material according to claim 1, wherein the graphene oxide containing the amino group has 1 to 10 graphene layers, a thickness of 0.55 to 3.74nm, and a diameter of 0.5 to 3 μm.
4. The method for preparing the graphene aluminum composite material according to claim 1, wherein the electrolytic salt includes one or more of sodium chloride, potassium chloride and aluminum chloride.
5. The method for preparing the graphene aluminum composite material according to claim 1, wherein the electrolytic salt is sodium chloride, potassium chloride, or aluminum chloride.
6. The preparation method of the graphene-aluminum composite material according to claim 1, wherein the mass ratio of sodium chloride to potassium chloride to aluminum chloride in the electrolytic salt is 1: (1-3): (6-10).
7. The method for preparing the graphene aluminum composite material according to any one of claims 1 to 6, wherein the mass ratio of the amino group-containing graphene oxide to the electrolytic salt is (0.2 to 0.5): 1.
8. the preparation method of the graphene-aluminum composite material according to claim 1, wherein the electrolysis current is 300 mA-400 mA, the electrolysis time is 40 min-60 min, and the distance between the two aluminum bars is 2 cm-5 cm.
9. A graphene-aluminum composite material prepared by the method for preparing a graphene-aluminum composite material according to any one of claims 1 to 8.
10. A cable or wire comprising the graphene-reinforced aluminum-based composite material according to claim 9.
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