CN108677048B - Nitrogen-doped graphene silver-based composite material and preparation method thereof - Google Patents
Nitrogen-doped graphene silver-based composite material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nitrogen-doped graphene silver-based composite material and a preparation method thereof. And mixing the nitrogen-doped graphene with the absolute ethanol solution of the silver powder, stirring and drying at the temperature of 60-80 ℃ to obtain the composite powder of the nitrogen-doped graphene and the silver powder. And performing ball milling, three-dimensional powder mixing, pressing and hot-pressing sintering on the composite powder to finally obtain the nitrogen-doped graphene silver-based composite material. By the method, nitrogen atoms are doped into the graphene, so that the conductivity of the reduced graphene oxide is improved, the distribution of the graphene in a matrix and the interface combination between the graphene and a metal matrix are improved, and the nitrogen-doped graphene silver-based bulk composite material with excellent comprehensive performance is obtained.
Description
Technical Field
The invention belongs to the technical field of silver-based composite materials, and particularly relates to a nitrogen-doped graphene silver-based composite material and a preparation method of the silver-based composite material.
Background
The material prepared from the metallic silver has low resistivity at room temperature, good ductility, small resistance and excellent oxidation resistance, is widely applied to the fields of low-voltage electrical appliances, communication electronic instruments, household electrical appliances, aerospace devices and the like, and is a noble metal material which is most widely applied and is most economical in the electronic and electrical industry. Although having many excellent properties, there are disadvantages such as low strength.
Graphene is a novel two-dimensional honeycomb nano material formed by closely arranging single-layer carbon atoms, has excellent electric and heat conducting properties and high Young modulus and hardness, and is the highest-strength and thinnest-thickness material. The excellent performance of the graphene has potential application in super capacitors, lithium ion batteries and nano composite materials, and particularly the graphene has great potential in the field of metal matrix composite materials. The graphene is introduced into the silver matrix, so that the strength of the silver matrix can be improved on the basis of keeping the good electric and thermal conductivity of the silver matrix, and the silver-based composite material of the graphene with excellent comprehensive performance is expected to be developed.
However, the common oxidation-reduction method in the preparation process of graphene causes partial damage of the graphene structure, so that the excellent performance of the graphene structure cannot be fully exerted, and the agglomeration of graphene in a matrix and poor interface bonding of graphene and the matrix also restrict the application of graphene in a silver-based composite material. Therefore, the research and development of the preparation method which can effectively regulate and control the graphene structure and can realize the dispersion of the graphene in the matrix and the close combination between the graphene and the silver matrix interface has important engineering significance and practical value for obtaining the high-performance graphene-silver-based composite material.
Disclosure of Invention
The invention aims to provide a nitrogen-doped graphene silver-based composite material, and solves the problem of poor conductivity of the existing graphene silver-based composite material.
The invention also aims to provide a preparation method of the nitrogen-doped graphene silver-based composite material.
The first technical scheme adopted by the invention is that the nitrogen-doped graphene silver-based composite material comprises the following components in percentage by mass: 99-99.9% of Ag and 0.1-1% of nitrogen-doped graphene, wherein the sum of the mass percentages of the components is 100%, and the mass percentage of nitrogen elements in the nitrogen-doped graphene is 34.13-39.33%.
The second technical scheme adopted by the invention is that the preparation method of the nitrogen-doped graphene silver-based composite material comprises the following specific operation steps:
step 1, adding graphene oxide into deionized water, and performing ultrasonic dispersion to prepare a graphene oxide dispersion liquid;
step 2, adding urea into the graphene oxide dispersion liquid to obtain a mixed solution A, performing ultrasonic dispersion treatment on the mixed solution A, and performing magnetic stirring while performing ultrasonic dispersion to obtain a mixed dispersion liquid;
step 3, preserving the temperature of the mixed dispersion liquid in a hydrothermal reaction kettle at 160 ℃ for 4-7h, taking out, naturally cooling to room temperature, adding absolute ethyl alcohol A, washing, performing centrifugal treatment, and drying the obtained precipitate to obtain nitrogen-doped graphene powder;
step 4, weighing 0.1-1% of nitrogen-doped graphene powder and 99-99.9% of Ag powder according to the mass percentage, wherein the sum of the mass percentages of the components is 100%; dispersing the nitrogen-doped graphene powder into absolute ethyl alcohol B, and performing ultrasonic treatment for 30min to obtain a nitrogen-doped graphene absolute ethyl alcohol solution; simultaneously dispersing Ag powder into other absolute ethyl alcohol C, carrying out ultrasonic treatment for 30min to obtain a silver-containing absolute ethyl alcohol solution, mixing the nitrogen-doped graphene absolute ethyl alcohol solution and the silver-containing absolute ethyl alcohol solution, continuing the ultrasonic treatment for 30min, and then carrying out magnetic stirring at 60-80 ℃ until the absolute ethyl alcohol is completely volatilized, thus obtaining composite powder;
step 5, performing ball milling treatment on the composite powder in a planetary ball mill, and then performing powder mixing treatment in a three-dimensional powder mixer to obtain mixed powder;
step 6, pressing the mixed powder into blocks, placing the blocks in a sintering furnace in a nitrogen atmosphere, heating to 800 ℃, preserving heat for 2-3h and keeping the pressure at 20-50MPa to finally obtain the nitrogen-doped graphene silver-based composite material, wherein the nitrogen-doped graphene silver-based composite material comprises the following components in percentage by mass: ag 99-99.9% and nitrogen-doped graphene 0.1-1%, wherein the sum of the mass percentages of the components is 100%, and the mass percentage of nitrogen elements in the nitrogen-doped graphene is 34.13-39.33%.
The present invention is also characterized in that,
it is characterized in that the drying environment in the step 3 is vacuum, and the vacuum degree is not less than 10-2Pa, drying temperature 60 ℃, and drying time 20-30 h.
The mass ratio of the graphene oxide to the deionized water in the step 1 is 1:0.5-1, and the ultrasonic dispersion time in the step 1 is 1-1.5 h; and 2, the mass ratio of the graphene oxide dispersion liquid to the urea is 1: 30-40.
The ball milling treatment time of the step 5 is 2-6h, and the powder mixing treatment time is 3-5 h.
And 4, the mass ratio of the nitrogen-doped graphene powder to the absolute ethyl alcohol B is 1:20, and the mass ratio of the Ag powder to the other absolute ethyl alcohol C is 1: 20.
The nitrogen-doped graphene silver-based composite material has the beneficial effects that the nitrogen is introduced into the graphene, so that the conductivity of the reduced graphene oxide is improved, the dispersion of the graphene and the wettability between the graphene and a metal matrix are improved, and the nitrogen-doped graphene silver-based bulk composite material with excellent comprehensive performance is obtained.
Drawings
FIG. 1 is a flow chart of a preparation method of a nitrogen-doped graphene silver-based composite material according to the present invention;
fig. 2 is a scanning electron microscope photograph of a silver-based composite material of nitrogen-doped graphene according to the present invention.
Detailed Description
The invention provides a nitrogen-doped graphene silver-based composite material which comprises the following components in percentage by mass: 99-99.9% of Ag and 0.1-1% of nitrogen-doped graphene, wherein the sum of the mass percentages of the components is 100%, and the mass percentage of nitrogen elements in the nitrogen-doped graphene is 34.13-39.33%.
The specific flow of the preparation method of the nitrogen-doped graphene silver-based composite material is shown in fig. 1, and the specific operation steps are as follows:
step 1, adding graphene oxide into deionized water, wherein the mass ratio of the graphene oxide to the deionized water is 1:0.5-1, and ultrasonically dispersing for 1-1.5 hours to prepare a graphene oxide dispersion liquid;
step 2, adding urea into the graphene oxide dispersion liquid to obtain a mixed solution A, performing ultrasonic dispersion treatment on the mixed solution A, performing magnetic stirring while performing ultrasonic dispersion, wherein the mass ratio of the graphene oxide dispersion liquid to the urea is 1:30-40 to obtain a mixed dispersion liquid;
step 3, keeping the temperature of the mixed dispersion liquid in a hydrothermal reaction kettle at 160 ℃ for 4-7h, taking out, naturally cooling to room temperature, washing with absolute ethyl alcohol, performing centrifugal treatment, drying the precipitate obtained after the centrifugal treatment, wherein the drying environment is vacuum, and the vacuum degree is not less than 10-2Pa, drying at 60 ℃ for 20-30h to obtain nitrogen-doped graphene powder;
step 4, weighing 0.1-1% of nitrogen-doped graphene powder and 99-99.9% of Ag powder according to the mass percentage, wherein the sum of the mass percentages of the components is 100%; dispersing nitrogen-doped graphene powder into absolute ethyl alcohol B, wherein the mass ratio of the nitrogen-doped graphene powder to the absolute ethyl alcohol B is 1:20, and performing ultrasonic treatment for 30min to obtain a nitrogen-doped graphene absolute ethyl alcohol solution; meanwhile, dispersing Ag powder into other absolute ethyl alcohol C, wherein the mass ratio of the Ag powder to the absolute ethyl alcohol C is 1:20, and performing ultrasonic treatment for 30min to obtain a silver-containing absolute ethyl alcohol solution; and mixing the nitrogen-doped graphene absolute ethyl alcohol solution and the silver-containing absolute ethyl alcohol solution, continuing to perform ultrasonic treatment for 30min, and then magnetically stirring at 60-80 ℃ until the absolute ethyl alcohol is completely volatilized, thus obtaining the composite powder of the nitrogen-doped graphene and the silver powder.
And 5, ball-milling the composite powder on a planetary ball mill for 2-6h, and then mixing the powder in a three-dimensional powder mixer for 3-5h to obtain mixed powder.
And step 6, pressing the mixed powder into blocks, placing the blocks in a sintering furnace in a nitrogen atmosphere, heating to 800 ℃, preserving heat for 2-3h and keeping the pressure at 20-50MPa to finally obtain the nitrogen-doped graphene silver-based composite material.
The present invention will be described in detail with reference to specific examples.
Example 1
Step 1, adding graphene oxide into deionized water, wherein the mass ratio of the graphene oxide to the deionized water is 1:0.5, and ultrasonically dispersing for 1h to prepare a graphene oxide dispersion liquid;
step 2, adding urea into the graphene oxide dispersion liquid to obtain a mixed solution A, performing ultrasonic dispersion treatment on the mixed solution A, performing magnetic stirring while performing ultrasonic dispersion, wherein the mass ratio of the graphene oxide dispersion liquid to the urea is 1:30 to obtain a mixed dispersion liquid;
step 3, preserving the mixed dispersion liquid in a hydrothermal reaction kettle at 160 ℃ for 4 hours, taking out, naturally cooling to room temperature, washing with absolute ethyl alcohol, performing centrifugal treatment, drying the precipitate obtained after the centrifugal treatment, wherein the drying environment is vacuum and the vacuum degree is 1 multiplied by 10-2Pa, drying temperature 60 ℃, drying time 20h, obtainingNitrogen-doped graphene powder;
step 4, weighing 0.1% of nitrogen-doped graphene powder and 99.9% of Ag powder according to mass percentage; dispersing nitrogen-doped graphene powder into absolute ethyl alcohol B, wherein the mass ratio of the nitrogen-doped graphene powder to the absolute ethyl alcohol B is 1:20, and performing ultrasonic treatment for 30min to obtain a nitrogen-doped graphene absolute ethyl alcohol solution; meanwhile, dispersing Ag powder into other absolute ethyl alcohol C, wherein the mass ratio of the Ag powder to the absolute ethyl alcohol C is 1:20, and performing ultrasonic treatment for 30min to obtain a silver-containing absolute ethyl alcohol solution; and mixing the nitrogen-doped graphene absolute ethyl alcohol solution and the silver-containing absolute ethyl alcohol solution, continuing ultrasonic treatment for 30min, and then magnetically stirring at 60 ℃ until the absolute ethyl alcohol is completely volatilized, thus obtaining the composite powder.
Step 5, ball-milling the composite powder on a planetary ball mill for 2 hours, and then carrying out powder mixing treatment in a three-dimensional powder mixer for 3 hours to obtain mixed powder;
and step 6, pressing the mixed powder into blocks, placing the blocks in a sintering furnace in a nitrogen atmosphere, heating to 500 ℃, preserving heat for 2 hours, and keeping the pressure at 20MPa to finally obtain the nitrogen-doped graphene silver-based composite material.
Example 2
Step 1, adding graphene oxide into deionized water, wherein the mass ratio of the graphene oxide to the deionized water is 1:1, and ultrasonically dispersing for 1.5 hours to prepare a graphene oxide dispersion liquid;
step 2, adding urea into the graphene oxide dispersion liquid to obtain a mixed solution A, performing ultrasonic dispersion treatment on the mixed solution A, performing magnetic stirring while performing ultrasonic dispersion, wherein the mass ratio of the graphene oxide dispersion liquid to the urea is 1:40 to obtain a mixed dispersion liquid;
step 3, preserving the mixed dispersion liquid in a hydrothermal reaction kettle at 160 ℃ for 7 hours, taking out, naturally cooling to room temperature, washing with absolute ethyl alcohol, performing centrifugal treatment, drying the precipitate obtained after the centrifugal treatment, wherein the drying environment is vacuum and the vacuum degree is 0.5 multiplied by 10-2Pa, drying at 60 ℃ for 30h to obtain nitrogen-doped graphene powder;
step 4, weighing 1% of nitrogen-doped graphene powder and 99% of Ag powder according to mass percentage; dispersing nitrogen-doped graphene powder into absolute ethyl alcohol B, wherein the mass ratio of the nitrogen-doped graphene powder to the absolute ethyl alcohol B is 1:20, and performing ultrasonic treatment for 30min to obtain a nitrogen-doped graphene absolute ethyl alcohol solution; meanwhile, dispersing Ag powder into other absolute ethyl alcohol C, wherein the mass ratio of the Ag powder to the absolute ethyl alcohol C is 1:20, and performing ultrasonic treatment for 30min to obtain a silver-containing absolute ethyl alcohol solution; and mixing the nitrogen-doped graphene absolute ethyl alcohol solution and the silver-containing absolute ethyl alcohol solution, continuing ultrasonic treatment for 30min, and then magnetically stirring at 80 ℃ until the absolute ethyl alcohol is completely volatilized, thus obtaining the composite powder.
And 5, ball-milling the composite powder on a planetary ball mill for 6 hours, and then mixing the powder in a three-dimensional powder mixer for 5 hours to obtain mixed powder.
And 6, pressing the mixed powder into blocks, placing the blocks in a sintering furnace in a nitrogen atmosphere, heating to 800 ℃, preserving heat for 3 hours, and keeping the pressure at 50MPa to finally obtain the nitrogen-doped graphene silver-based composite material.
Example 3
Step 1, adding graphene oxide into deionized water, wherein the mass ratio of the graphene oxide to the deionized water is 1:0.75, and ultrasonically dispersing for 1.25 hours to prepare a graphene oxide dispersion liquid;
step 2, adding urea into the graphene oxide dispersion liquid to obtain a mixed solution A, performing ultrasonic dispersion treatment on the mixed solution A, performing magnetic stirring while performing ultrasonic dispersion, wherein the mass ratio of the graphene oxide dispersion liquid to the urea is 1:35 to obtain a mixed dispersion liquid;
step 3, keeping the temperature of the mixed dispersion liquid in a hydrothermal reaction kettle at 160 ℃ for 4-7h, taking out, naturally cooling to room temperature, washing with absolute ethyl alcohol, performing centrifugal treatment, drying the precipitate obtained after the centrifugal treatment, wherein the drying environment is vacuum and the vacuum degree is 0.3 multiplied by 10-2Pa, drying at 60 ℃ for 25h to obtain nitrogen-doped graphene powder;
step 4, weighing 0.5% of nitrogen-doped graphene powder and 99.5% of Ag powder according to mass percentage; dispersing nitrogen-doped graphene powder into absolute ethyl alcohol B, wherein the mass ratio of the nitrogen-doped graphene powder to the absolute ethyl alcohol B is 1:20, and performing ultrasonic treatment for 30min to obtain a nitrogen-doped graphene absolute ethyl alcohol solution; meanwhile, dispersing Ag powder into other absolute ethyl alcohol C, wherein the mass ratio of the Ag powder to the absolute ethyl alcohol C is 1:20, and performing ultrasonic treatment for 30min to obtain a silver-containing absolute ethyl alcohol solution; and mixing the nitrogen-doped graphene absolute ethyl alcohol solution and the silver-containing absolute ethyl alcohol solution, continuing ultrasonic treatment for 30min, and then magnetically stirring at 70 ℃ until the absolute ethyl alcohol is completely volatilized, thus obtaining the composite powder.
Step 5, ball-milling the composite powder on a planetary ball mill for 4 hours, and then mixing the powder in a three-dimensional powder mixer for 4 hours to obtain mixed powder;
and step 6, pressing the mixed powder into blocks, placing the blocks in a sintering furnace in a nitrogen atmosphere, heating to 650 ℃, preserving heat for 2.5 hours, and keeping the pressure at 35MPa to finally obtain the nitrogen-doped graphene silver-based composite material.
Example 4
Step 1, adding graphene oxide into deionized water, wherein the mass ratio of the graphene oxide to the deionized water is 1:0.5, and ultrasonically dispersing for 1.1h to prepare a graphene oxide dispersion liquid;
step 2, adding urea into the graphene oxide dispersion liquid to obtain a mixed solution A, performing ultrasonic dispersion treatment on the mixed solution A, performing magnetic stirring while performing ultrasonic dispersion, wherein the mass ratio of the graphene oxide dispersion liquid to the urea is 1:32 to obtain a mixed dispersion liquid;
step 3, preserving the mixed dispersion liquid in a hydrothermal reaction kettle at 160 ℃ for 6 hours, taking out, naturally cooling to room temperature, washing with absolute ethyl alcohol, performing centrifugal treatment, drying the precipitate obtained by the centrifugal treatment, wherein the drying environment is vacuum and the vacuum degree is 0.6 multiplied by 10-2Pa, drying at 60 ℃ for 20h to obtain nitrogen-doped graphene powder;
step 4, weighing 0.1% of nitrogen-doped graphene powder and 99.9% of Ag powder according to mass percentage; dispersing nitrogen-doped graphene powder into absolute ethyl alcohol B, wherein the mass ratio of the nitrogen-doped graphene powder to the absolute ethyl alcohol B is 1:20, and performing ultrasonic treatment for 30min to obtain a nitrogen-doped graphene absolute ethyl alcohol solution; meanwhile, dispersing Ag powder into other absolute ethyl alcohol C, wherein the mass ratio of the Ag powder to the absolute ethyl alcohol C is 1:20, and performing ultrasonic treatment for 30min to obtain a silver-containing absolute ethyl alcohol solution; and mixing the nitrogen-doped graphene absolute ethyl alcohol solution and the silver-containing absolute ethyl alcohol solution, continuing ultrasonic treatment for 30min, and then magnetically stirring at 80 ℃ until the absolute ethyl alcohol is completely volatilized, thus obtaining the composite powder.
Step 5, ball-milling the composite powder on a planetary ball mill for 3 hours, and then mixing the powder in a three-dimensional powder mixer for 4 hours to obtain mixed powder;
and 6, pressing the mixed powder into blocks, placing the blocks in a sintering furnace in a nitrogen atmosphere, heating to 550 ℃, preserving heat for 3 hours, and keeping the pressure at 30MPa to finally obtain the nitrogen-doped graphene silver-based composite material.
Example 5
Step 1, adding graphene oxide into deionized water, wherein the mass ratio of the graphene oxide to the deionized water is 1:0.7, and ultrasonically dispersing for 1.5 hours to prepare a graphene oxide dispersion liquid;
step 2, adding urea into the graphene oxide dispersion liquid to obtain a mixed solution A, performing ultrasonic dispersion treatment on the mixed solution A, performing magnetic stirring while performing ultrasonic dispersion, wherein the mass ratio of the graphene oxide dispersion liquid to the urea is 1:35, obtaining a mixed dispersion liquid;
step 3, preserving the mixed dispersion liquid in a hydrothermal reaction kettle at 160 ℃ for 7 hours, taking out, naturally cooling to room temperature, washing with absolute ethyl alcohol, performing centrifugal treatment, drying the precipitate obtained after the centrifugal treatment, wherein the drying environment is vacuum and the vacuum degree is 1 multiplied by 10-2Pa, drying at 60 ℃ for 25h to obtain nitrogen-doped graphene powder;
step 4, weighing 0.3% of nitrogen-doped graphene powder and 99.7% of Ag powder according to mass percentage; dispersing nitrogen-doped graphene powder into absolute ethyl alcohol B, wherein the mass ratio of the nitrogen-doped graphene powder to the absolute ethyl alcohol B is 1:20, and performing ultrasonic treatment for 30min to obtain a nitrogen-doped graphene absolute ethyl alcohol solution; meanwhile, dispersing Ag powder into other absolute ethyl alcohol C, wherein the mass ratio of the Ag powder to the absolute ethyl alcohol C is 1:20, and performing ultrasonic treatment for 30min to obtain a silver-containing absolute ethyl alcohol solution; and mixing the nitrogen-doped graphene absolute ethyl alcohol solution and the silver-containing absolute ethyl alcohol solution, continuing ultrasonic treatment for 30min, and then magnetically stirring at 70 ℃ until the absolute ethyl alcohol is completely volatilized, thus obtaining the composite powder.
Step 5, performing ball milling treatment on the composite powder in a planetary ball mill for 5 hours, and then performing powder mixing treatment in a three-dimensional powder mixer for 3.5 hours to obtain mixed powder;
and step 6, pressing the mixed powder into blocks, placing the blocks in a sintering furnace in a nitrogen atmosphere, heating to 700 ℃, preserving heat for 2.5 hours, and keeping the pressure at 40MPa to finally obtain the nitrogen-doped graphene silver-based composite material.
Fig. 2 is a scanning electron micrograph of the nitrogen-doped graphene, which shows the nitrogen-doped graphene with a thinner lamellar and corrugated structure.
The performance parameters of the examples and the conventional silver-based composite material are shown in Table 1
Table 1 comparison of the examples with the performance parameters of conventional silver-based composites
| Sample name | conductivity/IACS | hardness/HV |
| Example 4 | 97.41％ | 92.3 |
| Example 5 | 93.97％ | 85.13 |
| Conventional SnO2Silver-based composite material | 67.58％ | 81.71 |
As is apparent from examples 4 and 5, the silver-based composite material of the nitrogen-doped graphene prepared by the invention has excellent conductivity and hardness. Compared with the conventional SnO2Compared with the silver-based composite material prepared in the example 4, the conductivity and the hardness of the silver-based composite material are respectively improved by 44.14 percent and 12.96 percent. The conductivity and hardness of the prepared silver-based composite material of example 5 are respectively improved by 39.05% and 4.18%. The silver-based composite material prepared by the invention can be widely applied to the electrician field of relays, contactors, low-voltage switches and the like.
Claims (5)
1. A preparation method of a nitrogen-doped graphene silver-based composite material is characterized by comprising the following specific operation steps:
step 1, adding graphene oxide into deionized water, and performing ultrasonic dispersion to prepare a graphene oxide dispersion liquid;
step 2, adding urea into the graphene oxide dispersion liquid to obtain a mixed solution A, performing ultrasonic dispersion treatment on the mixed solution A, and performing magnetic stirring while performing ultrasonic dispersion to obtain a mixed dispersion liquid;
step 3, preserving the temperature of the mixed dispersion liquid in a hydrothermal reaction kettle at 160 ℃ for 4-7h, taking out, naturally cooling to room temperature, adding absolute ethyl alcohol A, washing, performing centrifugal treatment, and drying precipitates obtained after the centrifugal treatment to obtain nitrogen-doped graphene powder;
step 4, weighing 0.1-0.3% of nitrogen-doped graphene powder and 99-99.9% of Ag powder according to the mass percentage, wherein the sum of the mass percentages of the components is 100%, dispersing the nitrogen-doped graphene powder into absolute ethyl alcohol B, performing ultrasonic treatment for 30min to obtain an absolute ethyl alcohol solution of the nitrogen-doped graphene, dispersing the Ag powder into another absolute ethyl alcohol C, performing ultrasonic treatment for 30min to obtain an absolute ethyl alcohol solution containing silver, mixing the absolute ethyl alcohol solution of the nitrogen-doped graphene and the absolute ethyl alcohol solution containing silver, continuing the ultrasonic treatment for 30min, and then magnetically stirring at 60-80 ℃ until the absolute ethyl alcohol is completely volatilized, thus obtaining a composite powder;
step 5, performing ball milling treatment on the composite powder in a planetary ball mill, and then performing powder mixing treatment in a three-dimensional powder mixer to obtain mixed powder;
step 6, pressing the mixed powder into blocks, placing the blocks in a sintering furnace in a nitrogen atmosphere, heating to 800 ℃, preserving heat for 2-3h, and keeping the pressure at 20-50MPa to finally obtain the nitrogen-doped graphene silver-based composite material, wherein the nitrogen-doped graphene silver-based composite material comprises the following components in percentage by mass: 99.7-99.9% of Ag99.9% and 0.1-0.3% of nitrogen-doped graphene, wherein the sum of the mass percentages of the components is 100%, and the mass percentage of nitrogen elements in the nitrogen-doped graphene is 34.13-39.33%.
2. The method for preparing the nitrogen-doped graphene-based silver composite material according to claim 1, wherein the drying environment in the step 3 is vacuum, and the vacuum degree is not less than 10-2Pa, drying temperature 60 ℃, and drying time 20-30 h.
3. The method for preparing the nitrogen-doped graphene-based silver composite material according to claim 1, wherein the mass ratio of the graphene oxide to the deionized water in the step 1 is 1:0.5-1, and the ultrasonic dispersion time in the step 1 is 1-1.5 h; and 2, the mass ratio of the graphene oxide dispersion liquid to the urea is 1: 30-40.
4. The method for preparing the nitrogen-doped graphene-based silver composite material according to claim 1, wherein the ball milling treatment time in the step 5 is 2-6 hours, and the three-dimensional powder mixing treatment time is 3-5 hours.
5. The method for preparing the nitrogen-doped graphene-based silver composite material according to claim 1, wherein the mass ratio of the nitrogen-doped graphene powder to the absolute ethyl alcohol B in the step 4 is 1:20, and the mass ratio of the Ag powder to the other absolute ethyl alcohol C is 1: 20.
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| CN105428097A (en) * | 2015-12-24 | 2016-03-23 | 济南大学 | Silver-based electrical contact composite material and preparation method therefor |
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