CN108677048A - A kind of silver-based composite material of nitrogen-doped graphene and preparation method thereof - Google Patents
A kind of silver-based composite material of nitrogen-doped graphene and preparation method thereof Download PDFInfo
- Publication number
- CN108677048A CN108677048A CN201810360809.3A CN201810360809A CN108677048A CN 108677048 A CN108677048 A CN 108677048A CN 201810360809 A CN201810360809 A CN 201810360809A CN 108677048 A CN108677048 A CN 108677048A
- Authority
- CN
- China
- Prior art keywords
- nitrogen
- doped graphene
- powder
- graphene
- silver
- 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.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C1/00—Making non-ferrous alloys
- C22C1/04—Making non-ferrous alloys by powder metallurgy
- C22C1/05—Mixtures of metal powder with non-metallic powder
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C5/00—Alloys based on noble metals
- C22C5/06—Alloys based on silver
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a kind of silver-based composite materials of nitrogen-doped graphene, the invention discloses a kind of silver-based composite material of nitrogen-doped graphene and preparation methods, including following preparation process, graphene oxide dispersion is configured first, urea is dissolved in graphene dispersing solution, then cooled to room temperature is taken out after keeping the temperature a few hours in hydrothermal reaction kettle, product is washed, centrifugal treating and is dried to obtain nitrogen-doped graphene powder.Nitrogen-doped graphene is mixed with the ethanol solution of silver powder, the composite granule for being dried to obtain nitrogen-doped graphene and silver powder is stirred at 60 80 DEG C.The composite granule ball milling, three-dimensional mixed powder, compacting and hot pressed sintering are finally obtained to the silver-based composite material of nitrogen-doped graphene.Pass through the above method, the electric conductivity of redox graphene will be improved in nitrogen atom doping to graphene, interface cohesion between graphene distribution in the base and graphene and metallic matrix is improved, the silver-based block composite material of the nitrogen-doped graphene of excellent combination property is obtained.
Description
Technical field
The invention belongs to silver-based composite material technical fields, and in particular to a kind of silver-based composite material of nitrogen-doped graphene,
The invention further relates to the preparation methods of the silver-based composite material.
Background technology
Material prepared by metallic silver has room temperature resistivity low, and ductility is good, resistance is small and antioxygenic property is excellent, extensively
It is general to be used for the fields such as low-voltage electrical apparatus, communication electronics instrument, household electrical appliance, aerospace device, it is to be applied in electronic apparatus industry
Most extensive while and most economical precious metal material.Although having many excellent performances, there are the deficiencies such as intensity is low.
Graphene is a kind of by the compact arranged bi-dimensional cellular shape novel nano-material of single layer of carbon atom, has excellent lead
Conductance hot property, high Young's modulus and hardness are intensity highest and the most thin material of thickness so far.The excellent performance of graphene
In ultracapacitor, lithium ion battery, nanocomposite has potential application, and especially graphene is in metal-based compound material
Material field has great potentiality.Graphene, which is introduced into silver matrix, to keep the good electrical and thermal conductivity performance of silver matrix
On the basis of improve its intensity, be expected to develop the silver-based composite material of the graphene of excellent combination property.
But graphene common oxidation-reduction method in preparation process causes the partial destruction of graphene-structured, leads
Cause its excellent properties to be not in full use, and graphene reunion in the base and graphene combined with basal body interface it is poor
Also application of the graphene in silver-based composite material is constrained.Therefore, research and develop it is a kind of can Effective Regulation graphene-structured and can be real
The preparation method combined closely between the dispersion in the base of existing graphene and graphene and silver-based body interface is to obtaining high-performance
Graphene silver-based composite material has important engineering significance and practical value.
Invention content
The object of the present invention is to provide a kind of silver-based composite materials of nitrogen-doped graphene, solve existing graphene silver-based
The problem of composite material conductive rate difference.
It is a further object to provide a kind of silver-based composite material preparation methods of nitrogen-doped graphene.
The first technical solution of the present invention is a kind of silver-based composite material of nitrogen-doped graphene, by quality hundred
Divide than composed of the following components:Ag 99-99.9%, nitrogen-doped graphene 0.1-1%, the sum of the above components mass percent are
100%, the quality accounting of nitrogen is 34.13-39.33% in nitrogen-doped graphene.
Second technical solution of the present invention is a kind of preparation side of the silver-based composite material of nitrogen-doped graphene
Method, concrete operation step are as follows:
Step 1, it adds graphene oxide into deionized water, and carries out ultrasonic disperse, graphene oxide dispersion is made
Liquid;
Step 2, urea is added in graphene oxide dispersion, obtains mixed solution A, then surpass to mixed solution A
Sound decentralized processing carries out magnetic agitation while ultrasonic disperse, obtains mixed dispersion liquid;
Step 3, it is taken out after mixed dispersion liquid being kept the temperature 4-7h in 160 DEG C of hydrothermal reaction kettles, then cooled to room temperature,
Then it is washed after absolute ethyl alcohol A being added, then carries out centrifugal treating, obtained sediment is dried to get nitrating stone
Black alkene powder;
Step 4, nitrogen-doped graphene powder 0.1-1%, Ag powder 99-99.9%, the above each group are weighed according to mass percent
It is 100% to divide the sum of mass percent;Nitrogen-doped graphene powder is distributed in absolute ethyl alcohol B, and is obtained after being ultrasonically treated 30min
To nitrogen-doped graphene ethanol solution;Ag powder is distributed in other absolute ethyl alcohol C simultaneously, and after being ultrasonically treated 30min
Obtain the ethanol solution of argentiferous, then by the ethanol solution of nitrogen-doped graphene ethanol solution and argentiferous mix and after
Continuous to be ultrasonically treated 30min, then magnetic agitation is volatilized completely to absolute ethyl alcohol at 60-80 DEG C, that is, obtains composite granule;
Step 5, composite granule is first subjected to ball-milling treatment in planetary ball mill, then again in the mixed powder machine of three-dimensional into
The mixed powder processing of row, obtains mixed-powder;
Step 6, mixed-powder briquet is placed in the sintering furnace of nitrogen atmosphere, is warming up to 500-800 DEG C, heat preservation
2-3h, pressure 20-50MPa, finally obtain the silver-based composite material of nitrogen-doped graphene, and the silver-based composite material of nitrogen-doped graphene is pressed
Mass percent is composed of the following components:Ag99-99.9%, nitrogen-doped graphene 0.1-1%, the above components mass percent it
Be 100%, in nitrogen-doped graphene the quality accounting of nitrogen be 34.13-39.33%.
The features of the present invention also characterized in that
It is characterized in that, the dry environment of step 3 is vacuum, vacuum degree is not less than 10-2Pa, 60 DEG C of drying temperature are dry
Time 20-30h.
Graphene oxide and deionized water quality ratio in step 1 are 1:The ultrasonic disperse time of 0.5-1, step 1 are 1-
1.5h;Step 2 graphene oxide dispersion is 1 with urea quality ratio:30-40.
The time of the ball-milling treatment of step 5 is 2-6h, and the time for mixing powder processing is 3-5h.
The mass ratio of step 4 nitrogen-doped graphene powder and absolute ethyl alcohol B are 1:20, Ag powder are with other absolute ethyl alcohol C's
Mass ratio is 1:20.
The invention has the advantages that a kind of silver-based composite material of nitrogen-doped graphene of the present invention, by graphene
Middle introducing nitrogen, improves the electric conductivity of redox graphene, between the dispersion and graphene and metallic matrix that improve graphene
Wetability, obtain the silver-based block composite material of the nitrogen-doped graphene of excellent combination property.
Description of the drawings
Fig. 1 is a kind of silver-based composite material preparation flow figure of nitrogen-doped graphene of the present invention;
Fig. 2 is a kind of silver-based composite material stereoscan photograph of nitrogen-doped graphene of the present invention.
Specific implementation mode
A kind of silver-based composite material of nitrogen-doped graphene provided by the invention, it is composed of the following components by mass percentage:
Ag 99-99.9%, nitrogen-doped graphene 0.1-1%, the sum of the above components mass percent are 100%, nitrogen in nitrogen-doped graphene
The quality accounting of element is 34.13-39.33%.
A kind of preparation method detailed process of the silver-based composite material of nitrogen-doped graphene is as shown in Figure 1, concrete operation step
It is as follows:
Step 1, it adds graphene oxide into deionized water, graphene oxide is 1 with deionized water quality ratio:0.5-
Graphene oxide dispersion is made in 1, ultrasonic disperse 1-1.5h;
Step 2, urea is added in graphene oxide dispersion, obtains mixed solution A, then to the mixed solution A into
The processing of row ultrasonic disperse, carries out magnetic agitation while ultrasonic disperse, and graphene oxide dispersion is 1 with urea quality ratio:
30-40 obtains mixed dispersion liquid;
Step 3, it takes out, then naturally cools to after the mixed dispersion liquid being kept the temperature 4-7h in 160 DEG C of hydrothermal reaction kettles
Then room temperature is washed with absolute ethyl alcohol, then carry out centrifugal treating, the drying precipitate that will be obtained after centrifugal treating, dry environment
For vacuum, vacuum degree is not less than 10-2Pa, 60 DEG C of drying temperature, drying time 20-30h is to get nitrogen-doped graphene powder;
Step 4, nitrogen-doped graphene powder 0.1-1%, Ag powder 99-99.9%, the above each group are weighed according to mass percent
It is 100% to divide the sum of mass percent;Nitrogen-doped graphene powder is distributed in absolute ethyl alcohol B, nitrogen-doped graphene powder and nothing
The mass ratio of water-ethanol B is 1:20, and obtain nitrogen-doped graphene ethanol solution after being ultrasonically treated 30min;Meanwhile by Ag powder
It is distributed in other absolute ethyl alcohol C, the mass ratio of Ag powder and absolute ethyl alcohol C are 1:20, and contained after being ultrasonically treated 30min
The ethanol solution of silver;The ethanol solution of nitrogen-doped graphene ethanol solution and argentiferous is mixed and continued again
It is ultrasonically treated 30min, then magnetic agitation is volatilized completely to absolute ethyl alcohol at 60-80 DEG C, that is, obtains nitrogen-doped graphene and silver
The composite granule of powder.
Step 5, by composite granule, first the ball milling on planetary ball mill, Ball-milling Time 2-6h are then mixed in three-dimensional again
Mixed powder processing is carried out in powder machine, it is 3-5h to mix the powder time, obtains mixed-powder.
Step 6, mixed-powder briquet is placed in the sintering furnace of nitrogen atmosphere, is warming up to 500-800 DEG C, heat preservation
2-3h, pressure 20-50MPa finally obtain the silver-based composite material of nitrogen-doped graphene.
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
Step 1, it adds graphene oxide into deionized water, graphene oxide is 1 with deionized water quality ratio:0.5,
Graphene oxide dispersion is made in ultrasonic disperse 1h;
Step 2, urea is added in graphene oxide dispersion, obtains mixed solution A, then to the mixed solution A into
The processing of row ultrasonic disperse, carries out magnetic agitation while ultrasonic disperse, and graphene oxide dispersion is 1 with urea quality ratio:
30, obtain mixed dispersion liquid;
Step 3, it is taken out after the mixed dispersion liquid being kept the temperature 4h in 160 DEG C of hydrothermal reaction kettles, then naturally cools to room
Then temperature is washed with absolute ethyl alcohol, then carry out centrifugal treating, the drying precipitate that will be obtained after centrifugal treating, and dry environment is
Vacuum, vacuum degree 1 × 10-2Pa, 60 DEG C of drying temperature, drying time 20h is to get nitrogen-doped graphene powder;
Step 4, nitrogen-doped graphene powder 0.1%, Ag powder 99.9% are weighed according to mass percent;By nitrogen-doped graphene powder
End is distributed in absolute ethyl alcohol B, and the mass ratio of nitrogen-doped graphene powder and absolute ethyl alcohol B are 1:20, and after being ultrasonically treated 30min
Obtain nitrogen-doped graphene ethanol solution;Meanwhile Ag powder being distributed in other absolute ethyl alcohol C, Ag powder and absolute ethyl alcohol C
Mass ratio be 1:20, and obtain the ethanol solution of argentiferous after being ultrasonically treated 30min;Again by nitrogen-doped graphene absolute ethyl alcohol
The ethanol solution of solution and argentiferous is mixed and continues to be ultrasonically treated 30min, then at 60 DEG C magnetic agitation to nothing
Water-ethanol volatilizees completely, that is, obtains composite granule.
Step 5, by composite granule, first then the ball milling on planetary ball mill, Ball-milling Time 2h mix powder in three-dimensional again
Mixed powder processing is carried out in machine, it is 3h to mix the powder time, obtains mixed-powder;
Step 6, mixed-powder briquet is placed in the sintering furnace of nitrogen atmosphere, is warming up to 500 DEG C, keep the temperature 2h,
Pressure 20MPa finally obtains the silver-based composite material of nitrogen-doped graphene.
Embodiment 2
Step 1, it adds graphene oxide into deionized water, graphene oxide is 1 with deionized water quality ratio:1, surpass
Sound disperses 1.5h, and graphene oxide dispersion is made;
Step 2, urea is added in graphene oxide dispersion, obtains mixed solution A, then to the mixed solution A into
The processing of row ultrasonic disperse, carries out magnetic agitation while ultrasonic disperse, and graphene oxide dispersion is 1 with urea quality ratio:
40, obtain mixed dispersion liquid;
Step 3, it is taken out after the mixed dispersion liquid being kept the temperature 7h in 160 DEG C of hydrothermal reaction kettles, then naturally cools to room
Then temperature is washed with absolute ethyl alcohol, then carry out centrifugal treating, the drying precipitate that will be obtained after centrifugal treating, and dry environment is
Vacuum, vacuum degree 0.5 × 10-2Pa, 60 DEG C of drying temperature, drying time 30h is to get nitrogen-doped graphene powder;
Step 4, nitrogen-doped graphene powder 1%, Ag powder 99% are weighed according to mass percent;By nitrogen-doped graphene powder point
It is scattered in absolute ethyl alcohol B, the mass ratio of nitrogen-doped graphene powder and absolute ethyl alcohol B are 1:20, and obtained after being ultrasonically treated 30min
Nitrogen-doped graphene ethanol solution;Meanwhile Ag powder being distributed in other absolute ethyl alcohol C, the matter of Ag powder and absolute ethyl alcohol C
Amount is than being 1:20, and obtain the ethanol solution of argentiferous after being ultrasonically treated 30min;Again by nitrogen-doped graphene ethanol solution
Mixed with the ethanol solution of argentiferous and continue to be ultrasonically treated 30min, then at 80 DEG C magnetic agitation to anhydrous second
Alcohol volatilizees completely, that is, obtains composite granule.
Step 5, by composite granule, first then the ball milling on planetary ball mill, Ball-milling Time 6h mix powder in three-dimensional again
Mixed powder processing is carried out in machine, it is 5h to mix the powder time, obtains mixed-powder.
Step 6, mixed-powder briquet is placed in the sintering furnace of nitrogen atmosphere, is warming up to 800 DEG C, keep the temperature 3h,
Pressure 50MPa finally obtains the silver-based composite material of nitrogen-doped graphene.
Embodiment 3
Step 1, it adds graphene oxide into deionized water, graphene oxide is 1 with deionized water quality ratio:
Graphene oxide dispersion is made in 0.75, ultrasonic disperse 1.25h;
Step 2, urea is added in graphene oxide dispersion, obtains mixed solution A, then to the mixed solution A into
The processing of row ultrasonic disperse, carries out magnetic agitation while ultrasonic disperse, and graphene oxide dispersion is 1 with urea quality ratio:
35, obtain mixed dispersion liquid;
Step 3, it takes out, then naturally cools to after the mixed dispersion liquid being kept the temperature 4-7h in 160 DEG C of hydrothermal reaction kettles
Then room temperature is washed with absolute ethyl alcohol, then carry out centrifugal treating, the drying precipitate that will be obtained after centrifugal treating, dry environment
For vacuum, vacuum degree 0.3 × 10-2Pa, 60 DEG C of drying temperature, drying time 25h is to get nitrogen-doped graphene powder;
Step 4, nitrogen-doped graphene powder 0.5%, Ag powder 99.5% are weighed according to mass percent;By nitrogen-doped graphene powder
End is distributed in absolute ethyl alcohol B, and the mass ratio of nitrogen-doped graphene powder and absolute ethyl alcohol B are 1:20, and after being ultrasonically treated 30min
Obtain nitrogen-doped graphene ethanol solution;Meanwhile Ag powder being distributed in other absolute ethyl alcohol C, Ag powder and absolute ethyl alcohol C
Mass ratio be 1:20, and obtain the ethanol solution of argentiferous after being ultrasonically treated 30min;Again by nitrogen-doped graphene absolute ethyl alcohol
The ethanol solution of solution and argentiferous is mixed and continues to be ultrasonically treated 30min, then at 70 DEG C magnetic agitation to nothing
Water-ethanol volatilizees completely, that is, obtains composite granule.
Step 5, by composite granule, first then the ball milling on planetary ball mill, Ball-milling Time 4h mix powder in three-dimensional again
Mixed powder processing is carried out in machine, it is 4h to mix the powder time, obtains mixed-powder;
Step 6, mixed-powder briquet is placed in the sintering furnace of nitrogen atmosphere, is warming up to 650 DEG C, heat preservation
2.5h, pressure 35MPa finally obtain the silver-based composite material of nitrogen-doped graphene.
Embodiment 4
Step 1, it adds graphene oxide into deionized water, graphene oxide is 1 with deionized water quality ratio:0.5,
Graphene oxide dispersion is made in ultrasonic disperse 1.1h;
Step 2, urea is added in graphene oxide dispersion, obtains mixed solution A, then to the mixed solution A into
The processing of row ultrasonic disperse, carries out magnetic agitation while ultrasonic disperse, and graphene oxide dispersion is 1 with urea quality ratio:
32, obtain mixed dispersion liquid;
Step 3, it is taken out after the mixed dispersion liquid being kept the temperature 6h in 160 DEG C of hydrothermal reaction kettles, then naturally cools to room
Then temperature is washed with absolute ethyl alcohol, then carry out centrifugal treating, and the drying precipitate that centrifugal treating is obtained, dry environment is true
Sky, vacuum degree 0.6 × 10-2Pa, 60 DEG C of drying temperature, drying time 20h is to get nitrogen-doped graphene powder;
Step 4, nitrogen-doped graphene powder 0.1%, Ag powder 99.9% are weighed according to mass percent;By nitrogen-doped graphene powder
End is distributed in absolute ethyl alcohol B, and the mass ratio of nitrogen-doped graphene powder and absolute ethyl alcohol B are 1:20, and after being ultrasonically treated 30min
Obtain nitrogen-doped graphene ethanol solution;Meanwhile Ag powder being distributed in other absolute ethyl alcohol C, Ag powder and absolute ethyl alcohol C
Mass ratio be 1:20, and obtain the ethanol solution of argentiferous after being ultrasonically treated 30min;Again by nitrogen-doped graphene absolute ethyl alcohol
The ethanol solution of solution and argentiferous is mixed and continues to be ultrasonically treated 30min, then at 80 DEG C magnetic agitation to nothing
Water-ethanol volatilizees completely, that is, obtains composite granule.
Step 5, by composite granule, first then the ball milling on planetary ball mill, Ball-milling Time 3h mix powder in three-dimensional again
Mixed powder processing is carried out in machine, it is 4h to mix the powder time, obtains mixed-powder;
Step 6, mixed-powder briquet is placed in the sintering furnace of nitrogen atmosphere, is warming up to 550 DEG C, keep the temperature 3h,
Pressure 30MPa finally obtains the silver-based composite material of nitrogen-doped graphene.
Embodiment 5
Step 1, it adds graphene oxide into deionized water, graphene oxide is 1 with deionized water quality ratio:0.7,
Graphene oxide dispersion is made in ultrasonic disperse 1.5h;
Step 2, urea is added in graphene oxide dispersion, obtains mixed solution A, then to the mixed solution A into
The processing of row ultrasonic disperse, carries out magnetic agitation while ultrasonic disperse, and graphene oxide dispersion is 1 with urea quality ratio:
35, obtain mixed dispersion liquid;
Step 3, it is taken out after the mixed dispersion liquid being kept the temperature 7h in 160 DEG C of hydrothermal reaction kettles, then naturally cools to room
Then temperature is washed with absolute ethyl alcohol, then carry out centrifugal treating, the drying precipitate that will be obtained after centrifugal treating, and dry environment is
Vacuum, vacuum degree 1 × 10-2Pa, 60 DEG C of drying temperature, drying time 25h is to get nitrogen-doped graphene powder;
Step 4, nitrogen-doped graphene powder 0.3%, Ag powder 99.7% are weighed according to mass percent;By nitrogen-doped graphene powder
End is distributed in absolute ethyl alcohol B, and the mass ratio of nitrogen-doped graphene powder and absolute ethyl alcohol B are 1:20, and after being ultrasonically treated 30min
Obtain nitrogen-doped graphene ethanol solution;Meanwhile Ag powder being distributed in other absolute ethyl alcohol C, Ag powder and absolute ethyl alcohol C
Mass ratio be 1:20, and obtain the ethanol solution of argentiferous after being ultrasonically treated 30min;Again by nitrogen-doped graphene absolute ethyl alcohol
The ethanol solution of solution and argentiferous is mixed and continues to be ultrasonically treated 30min, then at 70 DEG C magnetic agitation to nothing
Water-ethanol volatilizees completely, that is, obtains composite granule.
Step 5, composite granule is first subjected to ball-milling treatment in planetary ball mill, then Ball-milling Time 5h exists again
Mixed powder processing is carried out in the mixed powder machine of three-dimensional, it is 3.5h to mix the powder time, obtains mixed-powder;
Step 6, mixed-powder briquet is placed in the sintering furnace of nitrogen atmosphere, is warming up to 700 DEG C, heat preservation
2.5h, pressure 40MPa finally obtain the silver-based composite material of nitrogen-doped graphene.
Fig. 2 is the stereoscan photograph of nitrogen-doped graphene, it can be seen that the nitrating graphite of relatively thin lamellar and pleated structure
Alkene.
Embodiment and traditional silver-based composite material performance parameter are as shown in table 1
1 embodiment of table is compared with traditional silver-based composite material performance parameter
Sample ID | Conductivity/IACS | Hardness/HV |
Embodiment 4 | 97.41% | 92.3 |
Embodiment 5 | 93.97% | 85.13 |
Traditional SnO2Silver-based composite material | 67.58% | 81.71 |
By embodiment 4 and embodiment 5, it is apparent that the silver-based composite material tool of nitrogen-doped graphene prepared by the present invention
There are excellent conductivity and hardness.With traditional SnO2Silver-based composite material compare, embodiment 4 prepare silver-based composite material
44.14% and 12.96% has been respectively increased in conductivity and hardness.The silver-based composite material conductivity of the preparation of embodiment 5 and hard
39.05% and 4.18% has been respectively increased in degree.Silver-based composite material prepared by the present invention can be widely applied to relay, contact
Device, the electrical fields such as low tension switch.
Claims (6)
1. a kind of silver-based composite material of nitrogen-doped graphene, which is characterized in that composed of the following components by mass percentage:Ag
99-99.9%, nitrogen-doped graphene 0.1-1%, the sum of the above components mass percent are 100%, in the nitrogen-doped graphene
The quality accounting of nitrogen is 34.13-39.33%.
2. a kind of preparation method of the silver-based composite material of nitrogen-doped graphene as described in claim 1, which is characterized in that specific
Operating procedure is as follows:
Step 1, it adds graphene oxide into deionized water, and carries out ultrasonic disperse, graphene oxide dispersion is made;
Step 2, add urea in the graphene oxide dispersion, obtain mixed solution A, then to the mixed solution A into
The processing of row ultrasonic disperse, magnetic agitation is carried out while ultrasonic disperse, obtains mixed dispersion liquid;
Step 3, it is taken out after the mixed dispersion liquid being kept the temperature 4-7h in 160 DEG C of hydrothermal reaction kettles, then cooled to room temperature,
Then washed after absolute ethyl alcohol A being added, then carry out centrifugal treating, by the drying precipitate obtained after centrifugal treating to get
Nitrogen-doped graphene powder;
Step 4, nitrogen-doped graphene powder 0.1-1%, the Ag powder 99-99.9%, the above each group are weighed according to mass percent
It is 100% to divide the sum of mass percent, the nitrogen-doped graphene powder is distributed in absolute ethyl alcohol B, and be ultrasonically treated 30min
After obtain nitrogen-doped graphene ethanol solution, meanwhile, the Ag powder is distributed in other absolute ethyl alcohol C, and ultrasound at
The ethanol solution of argentiferous is obtained after reason 30min, then by the anhydrous second of the nitrogen-doped graphene ethanol solution and argentiferous
Alcoholic solution is mixed and continues to be ultrasonically treated 30min, and then magnetic agitation is volatilized completely to absolute ethyl alcohol at 60-80 DEG C,
Obtain composite granule;
Step 5, the composite granule is first subjected to ball-milling treatment in planetary ball mill, then again in the mixed powder machine of three-dimensional into
The mixed powder processing of row, obtains mixed-powder;
Step 6, the mixed-powder briquet is placed in the sintering furnace of nitrogen atmosphere, is warming up to 500-800 DEG C, heat preservation
2-3h, pressure 20-50MPa finally obtain the silver-based composite material of nitrogen-doped graphene, the silver-based composite wood of the nitrogen-doped graphene
Material is composed of the following components by mass percentage:Ag99-99.9%, nitrogen-doped graphene 0.1-1%, the above components quality percentage
Than the sum of be 100%, the quality accounting of nitrogen is 34.13-39.33% in the nitrogen-doped graphene.
3. a kind of preparation method of the silver-based composite material of nitrogen-doped graphene according to claim 2, which is characterized in that step
Dry environment described in rapid 3 is vacuum, and vacuum degree is not less than 10-2Pa, 60 DEG C of drying temperature, drying time 20-30h.
4. a kind of preparation method of the silver-based composite material of nitrogen-doped graphene according to claim 2, which is characterized in that step
Graphene oxide and deionized water quality ratio described in rapid 1 are 1:0.5-1, the ultrasonic disperse time described in step 1 are 1-
1.5h;Graphene oxide dispersion described in step 2 is 1 with urea quality ratio:30-40.
5. a kind of preparation method of the silver-based composite material of nitrogen-doped graphene according to claim 2, which is characterized in that step
The time of ball-milling treatment described in rapid 5 is 2-6h, and the time for mixing powder processing is 3-5h.
6. a kind of preparation method of the silver-based composite material of nitrogen-doped graphene according to claim 2, which is characterized in that step
The mass ratio of the rapid 4 nitrogen-doped graphene powder and absolute ethyl alcohol B are 1:20, the matter of the Ag powder and other absolute ethyl alcohol C
Amount is than being 1:20.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810360809.3A CN108677048B (en) | 2018-04-20 | 2018-04-20 | Nitrogen-doped graphene silver-based composite material and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN201810360809.3A CN108677048B (en) | 2018-04-20 | 2018-04-20 | Nitrogen-doped graphene silver-based composite material and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN108677048A true CN108677048A (en) | 2018-10-19 |
CN108677048B CN108677048B (en) | 2020-11-17 |
Family
ID=63802284
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN201810360809.3A Active CN108677048B (en) | 2018-04-20 | 2018-04-20 | Nitrogen-doped graphene silver-based composite material and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN108677048B (en) |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109811177A (en) * | 2018-11-19 | 2019-05-28 | 昆明贵金属研究所 | A kind of preparation method of highly conductive high-intensitive silver-graphene composite material |
CN112151285A (en) * | 2020-09-04 | 2020-12-29 | 安徽壹石通材料科技股份有限公司 | Two-dimensional lamellar phase enhanced silver-based electric contact material and preparation method thereof |
CN112687902A (en) * | 2020-12-28 | 2021-04-20 | 龙岩学院 | Preparation method of nitrogen-doped graphene-supported hollow nano platinum composite material |
CN113737302A (en) * | 2021-07-22 | 2021-12-03 | 常州恒利宝纳米新材料科技有限公司 | Method for modifying nylon 6 fibers by using graphene oxide |
Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20120241670A1 (en) * | 2009-12-09 | 2012-09-27 | Industry-Academic Cooperation Foundation, Yonsei University | Metal matrix composite, and preparation method thereof |
CN104032154A (en) * | 2014-06-27 | 2014-09-10 | 武汉大学 | Graphene/metal matrix composite material and preparation method thereof |
CN105428097A (en) * | 2015-12-24 | 2016-03-23 | 济南大学 | Silver-based electrical contact composite material and preparation method therefor |
CN105551861A (en) * | 2016-02-26 | 2016-05-04 | 周懿涵 | Preparation method of graphene-reinforced silver-based electric contact material |
CN105977504A (en) * | 2016-07-18 | 2016-09-28 | 郑叶芳 | Nitrogen-doped graphene loaded Pd/Co catalyst and preparation method thereof |
-
2018
- 2018-04-20 CN CN201810360809.3A patent/CN108677048B/en active Active
Patent Citations (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US20120241670A1 (en) * | 2009-12-09 | 2012-09-27 | Industry-Academic Cooperation Foundation, Yonsei University | Metal matrix composite, and preparation method thereof |
CN104032154A (en) * | 2014-06-27 | 2014-09-10 | 武汉大学 | Graphene/metal matrix composite material and preparation method thereof |
CN105428097A (en) * | 2015-12-24 | 2016-03-23 | 济南大学 | Silver-based electrical contact composite material and preparation method therefor |
CN105551861A (en) * | 2016-02-26 | 2016-05-04 | 周懿涵 | Preparation method of graphene-reinforced silver-based electric contact material |
CN105977504A (en) * | 2016-07-18 | 2016-09-28 | 郑叶芳 | Nitrogen-doped graphene loaded Pd/Co catalyst and preparation method thereof |
Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN109811177A (en) * | 2018-11-19 | 2019-05-28 | 昆明贵金属研究所 | A kind of preparation method of highly conductive high-intensitive silver-graphene composite material |
CN112151285A (en) * | 2020-09-04 | 2020-12-29 | 安徽壹石通材料科技股份有限公司 | Two-dimensional lamellar phase enhanced silver-based electric contact material and preparation method thereof |
CN112151285B (en) * | 2020-09-04 | 2023-06-20 | 安徽壹石通材料科技股份有限公司 | Silver-based electric contact material with two-dimensional lamellar phase enhancement and preparation method thereof |
CN112687902A (en) * | 2020-12-28 | 2021-04-20 | 龙岩学院 | Preparation method of nitrogen-doped graphene-supported hollow nano platinum composite material |
CN113737302A (en) * | 2021-07-22 | 2021-12-03 | 常州恒利宝纳米新材料科技有限公司 | Method for modifying nylon 6 fibers by using graphene oxide |
Also Published As
Publication number | Publication date |
---|---|
CN108677048B (en) | 2020-11-17 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
CN108677048A (en) | A kind of silver-based composite material of nitrogen-doped graphene and preparation method thereof | |
CN104711443B (en) | A kind of graphene/copper composite material and preparation method thereof | |
CN104805323B (en) | A kind of graphene/titanium composite material and preparation method thereof | |
CN103252250B (en) | Preparation method and application of nitrogen and iron modified carbon material | |
CN105206844B (en) | A kind of preparation method of the lead accumulator grid comprising lead graphene composite material | |
CN104700961A (en) | Graphene/silver composite material and preparation method thereof | |
CN108624775A (en) | A kind of the graphene enhancing Cu-base composites and preparation method of supported copper | |
CN106011521B (en) | A kind of copper-based electric contact material for adding graphene/molybdenum disulfide hetero-junctions and preparation method thereof | |
CN100400689C (en) | Method for producing nano-diamond reinforced copper-base composite material by chemical codeposition | |
CN104018019B (en) | A kind of ZrB2The preparation method of/Cu composite | |
CN104130719A (en) | Graphene oxide conductive adhesive and preparation and using method of graphene oxide conductive adhesive | |
CN106086495B (en) | Cupric oxide doped siller tin oxide composite and preparation method thereof | |
CN109852835A (en) | Preparation method of graphene/copper nanocomposite | |
CN102737863B (en) | Silver nickel graphite composite contact terminal material and processing method thereof | |
CN104480335B (en) | A kind of preparation method of silver tungsten contact material | |
CN110257662A (en) | A kind of copper-graphite alkene composite material and preparation method | |
CN107570698A (en) | A kind of graphene coated titanium composite powder material and preparation method thereof | |
CN107586988A (en) | A kind of method for preparing high conductivity titanium diboride/carbon/carbon-copper composite material | |
CN104384512B (en) | A kind of preparation method of silver-tungsten carbide contact material | |
CN106920979A (en) | One kind of proton conducts intermediate temperature solid oxide fuel cell electrolyte and its preparation | |
CN107794388A (en) | A kind of preparation method of high heat conduction graphene doped and compounded sheet material | |
CN109951902A (en) | A kind of graphene heat generating pastes and application its graphene heating film obtained and preparation method thereof | |
CN105642884A (en) | Preparation method for Bi-Te-based thermoelectric material with core-shell structure | |
CN111270171B (en) | Nano-carbon reinforced Mo-Cu-Zr composite material and preparation method thereof | |
CN116287850B (en) | Preparation method of graphene modified copper-based composite material |
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 |