CN112071507A - Copper-coated multilayer graphene composite material and preparation method thereof - Google Patents
Copper-coated multilayer graphene composite material and preparation method thereof Download PDFInfo
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- CN112071507A CN112071507A CN202010932349.4A CN202010932349A CN112071507A CN 112071507 A CN112071507 A CN 112071507A CN 202010932349 A CN202010932349 A CN 202010932349A CN 112071507 A CN112071507 A CN 112071507A
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- H—ELECTRICITY
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- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
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- 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
- H01B1/026—Alloys based on copper
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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 belongs to the technical field of conductive fillers, and particularly relates to a preparation method of a copper-coated multilayer graphene composite material, which comprises the following steps: mixing DMF and distilled water to obtain a mixed solvent; adding expanded graphite into the mixed solvent, ultrasonically stirring and stripping the expanded graphite to strip the expanded graphite into a multilayer graphene dispersion liquid; adding copper acetate and dilute nitric acid into the multilayer graphene dispersion liquid, putting the multilayer graphene dispersion liquid into a water bath, heating the multilayer graphene dispersion liquid, taking the multilayer graphene dispersion liquid out, and cooling the multilayer graphene dispersion liquid to room temperature; cleaning by adopting a centrifugal machine, drying the cleaned sample in a drying box to obtain copper oxide/multilayer graphenePowder; placing copper oxide/multilayer graphene powder into a tube furnace in N2Heating under a protective atmosphere, and cooling to room temperature to obtain copper-coated multilayer graphene conductive powder; the formed composite material is not easy to agglomerate and is easy to combine with high polymer and rubber as a filler to form a high-quality conductive filler, so that the conductivity and the dispersibility are further improved.
Description
Technical Field
The invention belongs to the technical field of conductive fillers, and particularly relates to a copper-coated multilayer graphene composite material and a preparation method thereof.
Background
The conductive paste has the same fluidity as paint, can be coated by various coating methods, and has good conductivity, so that the conductive paste can be used for connecting joints of various electronic components to increase the conductivity. The conductive silver paste consists of conductive filler, adhesive, solvent and additive. The conductivity is mainly determined by conductive filler.
At present, silver powder and copper powder with the best conductivity are used as the conductive filler, and gold powder, graphite, carbon black, carbon fiber, nickel powder and the like are also used, and although the cost is low, the conductivity of the graphite, the carbon black and the carbon fiber is poor. After the carbon nanotubes and graphene were found, they were also used in a large amount for the research of conductive paste. However, silver powder has high performance but high cost, and copper powder has low price and excellent conductivity, and can replace silver powder in many cases. In order to improve the performance of copper powder as a conductive filler, the preparation of the nano copper powder is one of the main methods, but the preparation process and the process of the existing nano copper powder are relatively complex, and the prepared nano copper powder is easy to agglomerate. Graphite, carbon black and carbon fiber have low cost but poor conductivity. After the advent of carbon nanotubes and graphene, extensive research has also been conducted in the field of electrical conductivity. Moreover, carbon nanotubes and graphene are also expensive, and are prone to re-stacking and to disperse under van der waals forces.
In the existing preparation of graphene and copper oxide composite materials, graphene oxide is mainly used as a substrate, oxygen-containing functional groups on the surface of the graphene oxide are used for adsorbing metal copper ions, and finally, copper oxide is generated. The copper oxide obtained on the surface of the graphene has low distribution density, and a layer of copper oxide film cannot be obtained.
Disclosure of Invention
Based on the above disadvantages and shortcomings in the prior art, an object of the present invention is to solve at least one or more of the above problems in the prior art, in other words, to provide a method for preparing a copper-coated multi-layer graphene composite material that satisfies one or more of the above requirements.
The second purpose of the invention is to provide a copper-coated multilayer graphene composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a copper-coated multilayer graphene composite material comprises the following steps:
s1, mixing DMF and distilled water to obtain a mixed solvent;
s2, adding expanded graphite into the mixed solvent, and stripping the expanded graphite into a multilayer graphene dispersion liquid through ultrasonic stirring;
s3, adding copper acetate and dilute nitric acid into the multilayer graphene dispersion liquid, and heating in a water bath;
s4, cooling and cleaning, and drying the cleaned sample in a drying oven to obtain copper oxide/multilayer graphene powder;
s5, putting the copper oxide/multilayer graphene powder into a tube furnace for calcination, and adding N2And heating under a protective atmosphere to obtain the copper-coated multilayer graphene conductive powder.
Preferably, the volume ratio of the distilled water to the DMF is 1: (2-4), wherein the addition amount of the expanded graphite to the mixed solvent is 1-4 mg/mL.
Preferably, the volume ratio of the dilute nitric acid to the mixed solvent is (0.2-0.8): 1, the mass concentration of the dilute nitric acid is 10 wt%, and the addition amount of the copper acetate relative to the mixed solvent is 10-40 mg/mL.
Preferably, the time of the ultrasonic stirring is not less than 5 h.
Preferably, the temperature of the water bath heating is 85-95 ℃.
Preferably, the temperature of the drying oven is 60-80 ℃.
Preferably, N is2The heating temperature is 480-520 ℃ under the protective atmosphereThe duration is 2-4 hours.
The invention also provides the copper-coated multilayer graphene composite material prepared by the preparation method of any scheme.
According to the preferable scheme, the surface of the multilayer graphene is coated with a layer of nano copper film, the thickness of the multilayer graphene is 1-10 nm, and the thickness of the nano copper is 5-20 nm.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the method, the uniformly distributed copper oxide thin film is obtained on the surface of the unoxidized multilayer graphene, and the copper oxide thin film can be reduced to uniformly deposit on the surface of the multilayer graphene to form a layer of thin film with a nanometer thickness.
2. The preparation method disclosed by the invention can be completed at a low temperature without high temperature when preparing the copper oxide/multilayer graphene, and has the advantages of short reaction time, high production efficiency and simple preparation method.
3. The invention can be used for filling materials, is added into non-conducting materials to improve the conductivity of the materials, achieves the functions of static resistance and electric conduction, and is beneficial to keeping high conductivity because the surface of the multilayer graphene is not subjected to oxidation treatment.
4. The composite material has good wettability and bonding performance with resin, plastic and the like, has good dispersibility in slurry, easily forms a conductive grid after the conductive coating is cured due to large surface area, and has excellent conductivity.
5. The multilayer graphene can further improve the conductivity and the dispersibility under the cladding of the nano copper, and the formed composite material is not easy to agglomerate and is easy to combine with high polymers and rubber as a filler to form a high-quality conductive filler.
Drawings
Fig. 1 is a flow chart of a process for preparing a copper-coated multi-layer graphene composite material according to the present invention;
FIG. 2 is a scanning electron microscope photomicrograph of a first embodiment of the invention;
FIG. 3 is a high power scanning electron microscope photograph of a first embodiment of the present invention;
FIG. 4 is an XRD diffraction pattern of a first embodiment of the present invention;
FIG. 5 is an XRD diffraction pattern of a second example of the present invention;
FIG. 6 is an XRD diffraction pattern of example three of the present invention;
FIG. 7 is a high-power scanning electron microscope photograph of comparative example I of the present invention.
Detailed Description
The present invention is further illustrated by the following specific examples, which are intended to be merely illustrative of the principles of the present invention and not limiting thereof.
The first embodiment is as follows:
the preparation method of the copper-coated multilayer graphene composite material of the embodiment comprises the following steps:
8mL of DMF and 2mL of distilled water were measured and mixed together to form a homogeneous mixed solvent. Weighing 20mg of expanded graphite, adding the mixed solvent, performing ultrasonic treatment on an ultrasonic machine for 5 hours to perform mechanical stripping, and stripping the expanded graphite into a multilayer graphene dispersion liquid with the thickness of 1-10 nm. 200mg of copper acetate is weighed, 0.4 mu L of 10 wt% dilute nitric acid is weighed, and the copper acetate and the dilute nitric acid are poured into the graphene dispersion solution successively. And adding dilute nitric acid to enable copper oxide to be uniformly deposited on the surface of the multilayer graphene to form the nano copper oxide film. Putting the solution into a water bath kettle with the temperature of 90 ℃, reacting for 2 hours by magnetic stirring, taking out and cooling at room temperature. The samples were washed with a centrifuge, water and alcohol 3 times each. And (3) drying the cleaned sample in a drying oven at 60 ℃ to obtain copper oxide/multilayer graphene powder. Placing copper oxide/multilayer graphene powder into a tube furnace in N2Raising the temperature to 500 ℃ under protection, keeping the temperature for 2 hours, and keeping the temperature at N2And cooling to room temperature under the protective atmosphere, and taking out to obtain the copper-coated multilayer graphene conductive filler.
As shown in fig. 2 and 3, from the low-power and high-power scanning electron micrographs of the nano-copper/multilayer graphene, it can be seen that the nano-copper particles have a thickness of 5 to 20nm, are uniformly distributed on the surface of the multilayer graphene, and have a large binding force. As shown in fig. 4, a phase of the product is shown, and a diffraction peak of copper can be seen in addition to graphene.
Example two:
the preparation method of the copper-coated multilayer graphene composite material of the embodiment comprises the following steps:
8mL of DMF and 2mL of distilled water were measured and mixed together to form a homogeneous mixed solvent. Weighing 20mg of expanded graphite, adding the mixed solvent, performing ultrasonic treatment on an ultrasonic machine for 9 hours to perform mechanical stripping, and stripping the expanded graphite into a multilayer graphene dispersion liquid with the thickness of 1-10 nm. 200mg of copper acetate is weighed, 0.4 mu L of 10 wt% dilute nitric acid is weighed, and the copper acetate and the dilute nitric acid are poured into the graphene dispersion solution successively. And adding dilute nitric acid to enable copper oxide to be uniformly deposited on the surface of the multilayer graphene to form the nano copper oxide film. Putting the solution into a water bath kettle with the temperature of 95 ℃, magnetically stirring the solution for reaction for 2 hours, taking the solution out, and cooling the solution at room temperature. The samples were washed with a centrifuge, water and alcohol 3 times each. And (3) drying the cleaned sample in a drying oven at 60 ℃ to obtain copper oxide/multilayer graphene powder. Placing copper oxide/multilayer graphene powder into a tube furnace in N2Heating to 480 ℃ under protective atmosphere, keeping for 3 hours under N2And cooling to room temperature under protection, and taking out to obtain the copper-coated multilayer graphene conductive filler. The scanning electron micrographs of the nano-copper/multi-layer graphene at low power and high power can be found in example one, as shown in fig. 5, which shows the phase of the product, and the diffraction peak of copper can be observed in addition to graphene.
Example three:
the preparation method of the copper-coated multilayer graphene composite material of the embodiment comprises the following steps:
16mL of DMF and 4mL of distilled water were measured and mixed together to form a homogeneous mixed solvent. Weighing 40mg of expanded graphite, adding the mixed solvent, carrying out ultrasonic treatment on the mixed solvent for 8 hours on an ultrasonic machine for mechanical stripping, and stripping the expanded graphite into a multilayer graphene dispersion liquid with the thickness of 1-10 nm. Weighing 400mg of copper acetate, weighing 0.8 mu L of 10 wt% dilute nitric acid, and pouring the copper acetate and the dilute nitric acid into the graphene dispersion solution successively. And adding dilute nitric acid to enable copper oxide to be uniformly deposited on the surface of the multilayer graphene to form the nano copper oxide film. Putting the solution into water with the temperature of 85 DEG CIn a bath kettle, the reaction is carried out for 2 hours by magnetic stirring, and then the mixture is taken out and cooled at room temperature. The samples were washed with a centrifuge, water and alcohol 3 times each. And (3) drying the cleaned sample in a drying oven at 60 ℃ to obtain copper oxide/multilayer graphene powder. Placing copper oxide/multilayer graphene powder into a tube furnace in N2Raising the temperature to 520 ℃ under protection, keeping the temperature for 4 hours, and keeping the temperature at N2And cooling to room temperature under the protective atmosphere, and taking out to obtain the copper-coated multilayer graphene conductive filler. Referring to the first example, as shown in fig. 6, the scanning electron microscope photographs of the nano-copper/multi-layer graphene with low power and high power show the phase of the product, and besides the graphene, the diffraction peaks of the graphene and the copper can be observed.
Example four:
the preparation method of the copper-coated multilayer graphene composite material of the embodiment comprises the following steps:
4mL of DMF and 1mL of distilled water were measured and mixed together to form a homogeneous mixed solvent. Weighing 10mg of expanded graphite, adding the mixed solvent, performing ultrasonic treatment on an ultrasonic machine for 5 hours to perform mechanical stripping, and stripping the expanded graphite into a multilayer graphene dispersion liquid with the thickness of 1-10 nm. 100mg of copper acetate is weighed, 0.2 mu L of 10 wt% dilute nitric acid is weighed, and the copper acetate and the dilute nitric acid are poured into the graphene dispersion solution successively. And adding dilute nitric acid to enable copper oxide to be uniformly deposited on the surface of the multilayer graphene to form the nano copper oxide film. Putting the solution into a water bath kettle with the temperature of 85 ℃, magnetically stirring the solution for reaction for 2 hours, taking the solution out, and cooling the solution at room temperature. The samples were washed with a centrifuge, water and alcohol 3 times each. And (3) drying the cleaned sample in a drying oven at 60 ℃ to obtain copper oxide/multilayer graphene powder. Placing copper oxide/multilayer graphene powder into a tube furnace in N2Heating to 500 ℃ under protection, keeping for 3 hours, and keeping the temperature at N2And cooling to room temperature under the protective atmosphere, and taking out to obtain the copper-coated multilayer graphene conductive filler. The scanning electron micrographs of the nano-copper/multilayer graphene at low power and high power can be seen in the first example, and the phase of the product is observed, and besides the graphene, diffraction peaks of the graphene and copper can also be observed.
Comparative example one:
in this comparative example, 8mL of DMF and 2mL of distilled water were first measured and mixed together to form a homogeneous mixed solvent. Weighing 20mg of expanded graphite, adding the mixed solvent, performing ultrasonic treatment on an ultrasonic machine for 5 hours to perform mechanical stripping, and stripping the expanded graphite into a multilayer graphene dispersion liquid with the thickness of 1-10 nm. 200mg of copper acetate was weighed and poured into the graphene dispersion solution. Putting the solution into a water bath kettle with the temperature of 90 ℃, reacting for 2 hours by magnetic stirring, taking out and cooling at room temperature. The sample was washed with a centrifuge, with water and alcohol each 3 times. And drying the cleaned sample at 60 ℃ to obtain solid powder. Placing the solid powder in a tube furnace, N2Heating to 500 ℃ under protective atmosphere, keeping for 2 hours, and keeping the temperature in the presence of N2Cooling to room temperature under protection, and taking out to obtain only multilayer graphene, as shown in fig. 7, which shows that the surface is very smooth and no nano metal particles are deposited.
The preparation method of the copper-coated multilayer graphene composite material has the following mechanism:
in the mixed liquid of DMF and water, copper ions, alkaline DMF and water generate a complex, the multilayer graphene adsorbs the copper ion complex through Van der Waals force, and the copper ion complex can be uniformly precipitated on the surface of the multilayer graphite due to the existence of dilute nitric acid. The copper ion complex is decomposed at the temperature of hot water bath, and finally copper oxide nanoparticles are generated and uniformly deposited on the surface of the multilayer graphene. Also, the copper oxide nanoparticles are not able to grow to very large particles, typically less than 5 nm in diameter, due to the action of dilute nitric acid. The conversion of copper oxide/multilayer graphene into copper/multilayer graphene is based on the oxidation-reduction reaction of copper oxide with carbon atoms in multilayer graphene, the copper oxide being reduced by graphene to metallic copper in nitrogen, and part of the carbon being oxidized to carbon dioxide.
The copper-coated multilayer graphene composite material prepared by the preparation method has the following beneficial effects:
the nano copper is uniformly deposited on the surface of the multilayer graphene, and a layer of nano-thickness film is formed on the surface of the multilayer graphene. The reaction temperature is low, and high temperature is not needed when preparing the copper oxide/multilayer graphene. Short reaction time, high reaction efficiency and high yield. The composite material utilizes the advantages of light density and large specific surface area of the multilayer graphene and also utilizes the advantage of high conductivity of the nano-copper. The surface of the multilayer graphene is not subjected to oxidation treatment, so that high conductivity is maintained. The material has good wettability and bonding performance with resin, plastic and the like. The conductive coating has good dispersibility in slurry, and due to large surface area, a conductive grid is easily formed after the conductive coating is cured, so that the conductive coating has excellent conductivity.
In the above examples and alternatives, the volume ratio of distilled water to DMF may also be in the range of 1: (2-4), and the addition amount of the expanded graphite relative to the mixed solvent can be arbitrarily selected from 1-4 mg/mL.
In the above embodiment and its alternative, the volume ratio of the dilute nitric acid to the mixed solvent may also be (0.2-0.8): 1, and the addition amount of the copper acetate relative to the mixed solvent can be arbitrarily selected from 10-40 mg/mL.
In the embodiment and the alternative scheme thereof, the water bath heating temperature can be arbitrarily selected from 85-95 ℃; the temperature of the drying box can be arbitrarily selected between 60 ℃ and 80 ℃; n is a radical of2The temperature under the protective atmosphere can be optionally selected between 480 and 520 ℃, and the duration time can be optionally selected within 2 to 4 hours.
The foregoing has outlined rather broadly the preferred embodiments and principles of the present invention and it will be appreciated that those skilled in the art may devise variations of the present invention that are within the spirit and scope of the appended claims.
Claims (9)
1. A preparation method of a copper-coated multilayer graphene composite material is characterized by comprising the following steps:
s1, mixing DMF and distilled water to obtain a mixed solvent;
s2, adding expanded graphite into the mixed solvent, and stripping the expanded graphite into a multilayer graphene dispersion liquid through ultrasonic stirring;
s3, adding copper acetate and dilute nitric acid into the multilayer graphene dispersion liquid, and heating in a water bath;
s4, cooling and cleaning, and drying the cleaned sample in a drying oven to obtain copper oxide/multilayer graphene powder;
s5, putting the copper oxide/multilayer graphene powder into a tube furnace for calcination, and adding N2And heating under a protective atmosphere to obtain the copper-coated multilayer graphene conductive powder.
2. The method of claim 1, wherein the volume ratio of distilled water to DMF is 1: (2-4), wherein the addition amount of the expanded graphite to the mixed solvent is 1-4 mg/mL.
3. The preparation method of the copper-coated multilayer graphene composite material according to claim 1, wherein the volume ratio of the dilute nitric acid to the mixed solvent is (0.2-0.8): 1, the mass concentration of the dilute nitric acid is 10 wt%, and the addition amount of the copper acetate relative to the mixed solvent is 10-40 mg/mL.
4. The method of claim 1, wherein the ultrasonic agitation is performed for a period of no less than 5 hours.
5. The method for preparing the copper-coated multilayer graphene composite material according to claim 1, wherein the temperature of the water bath heating is 85-95 ℃.
6. The method for preparing the copper-coated multilayer graphene composite material according to claim 1, wherein the temperature of the drying oven is 60-80 ℃.
7. The method of claim 1, wherein the N is N2Heating temperature under protective atmosphereThe temperature is 480-520 ℃, and the duration is 2-4 hours.
8. A copper-coated multi-layer graphene composite material, characterized by being prepared by the preparation method of any one of claims 1 to 8.
9. The copper-coated multilayer graphene composite material according to claim 8, wherein the surface of the multilayer graphene is coated with a layer of nano-copper film, the thickness of the multilayer graphene is 1-10 nm, and the thickness of the nano-copper is 5-20 nm.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112982022A (en) * | 2021-02-05 | 2021-06-18 | 南京信息工程大学 | Preparation method of copper-plated reduced graphene oxide wave-absorbing paper |
| CN114477152A (en) * | 2021-12-30 | 2022-05-13 | 杭州电子科技大学 | Silver nanoparticle/multilayer graphene composite material and preparation method thereof |
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Application publication date: 20201211 |