CN108624775A - A kind of the graphene enhancing Cu-base composites and preparation method of supported copper - Google Patents
A kind of the graphene enhancing Cu-base composites and preparation method of supported copper Download PDFInfo
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- CN108624775A CN108624775A CN201810359568.0A CN201810359568A CN108624775A CN 108624775 A CN108624775 A CN 108624775A CN 201810359568 A CN201810359568 A CN 201810359568A CN 108624775 A CN108624775 A CN 108624775A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C9/00—Alloys based on copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/17—Metallic particles coated with metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/12—Both compacting and sintering
- B22F3/14—Both compacting and sintering simultaneously
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2998/00—Supplementary information concerning processes or compositions relating to powder metallurgy
- B22F2998/10—Processes characterised by the sequence of their steps
Abstract
The invention discloses a kind of graphene of supported copper enhancing Cu-base composites and preparation methods, including following preparation process, configure graphene oxide and copper ion solution, the two is mixed, adjust pH value, it moves into water-bath and is reacted after addition reducing agent, reaction product centrifuge washing is dried to obtain to the graphene powder of load copper particle；The graphene powder of supported copper and copper powder are dissolved in acetone and stir drying, obtains the graphene of supported copper and the composite granule of copper powder, which is subjected to powder mixing machine, compacting, hot pressed sintering finally obtains the Cu-base composites of supported copper graphene enhancing.Pass through the above method, copper particle can be introduced into graphene sheet layer by the present invention, it solves the problems, such as that graphene is easily reunited, graphene is enable to be uniformly dispersed on metallic matrix, obtain the copper-based block composite material of the graphene enhancing of excellent combination property.
Description
Technical field
The invention belongs to technical field of metal material, and in particular to a kind of copper-based composite wood of graphene enhancing of supported copper
Material, the invention further relates to the preparation methods of the Cu-base composites.
Background technology
Cu-base composites have excellent mechanical property and physical property, in switch contact, microelectronics and electrical equipment control
In various control plug connectors, resistance welding electrode, magnetic artillery rail system, microwave tube etc. have a wide range of applications in fields.To the greatest extent
The traditional particle enhancing of pipe and fiber reinforcement Cu-base composites have a good mechanical property, but conductive and heat conductivility compared with
It is low.As electric appliance is to miniaturization, multifunction and powerful development, higher performance is proposed to Cu-base composites and is wanted
It asks, such as excellent thermal conductivity and electric conductivity, the softening of good high temperature resistance, anti electric arc corrosion and antiwear property, traditional copper
Based composites cannot increasingly meet the actual needs of engineering.
Graphene is a kind of novel-section with bi-dimensional cellular shape structure accumulated and formed after sp2 hydridization by carbon atom
Material has excellent electrical and thermal conductivity performance, and high Young's modulus and hardness are to find most thin, the nanometer of maximum intensity so far
Material is the ideal reinforcement of metal-base composites.Not only Copper substrate can be kept excellent using graphene as reinforcement
Electrical and thermal conductivity performance, and the intensity of Copper substrate can be improved, it is expected to prepare the copper of the graphene enhancing of excellent combination property
Based composites.But since the specific surface area of graphene super large causes it to easy to produce reunion, it is difficult to realize in metallic matrix
It is upper evenly dispersed, so that graphene itself excellent properties is not in full use, constrains graphene in copper-based block composite material
Extensive use.Therefore, a kind of method of effective dispersed graphite alkene is researched and developed, realizes that graphene is evenly dispersed in Copper substrate,
Copper-based block composite material to preparing high performance graphene enhancing has important engineering significance and practical value.
Invention content
The object of the present invention is to provide a kind of graphenes of supported copper to enhance Cu-base composites, solves traditional Al2O3Increase
The problem of strong Cu-base composites conductivity difference.
It is a further object to provide the preparation methods that a kind of supported copper graphene enhances Cu-base composites.
The first technical solution of the present invention is a kind of supported copper graphene enhancing Cu-base composites, by matter
It is composed of the following components to measure percentage：The graphene 0.1-3% of Cu 97-99.9%, supported copper, the above components quality percentage
Than the sum of be 100%, the quality accounting of copper is 24.02%-28.22% in the graphene of supported copper.
Second technical solution of the present invention is a kind of preparation of supported copper graphene enhancing Cu-base composites
Method, concrete operation step are as follows：
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 15-30%, copper nitrate 70-85%,
The sum of above constituent mass percentage is 100%；
Step 2, graphene oxide is added in deionized water, continues ultrasonic disperse 90min after stirring 30min, is made
Graphene oxide solution；
Step 3, copper nitrate is dissolved in alcoholic solution to get to copper nitrate solution；
Step 4, copper nitrate solution is added dropwise in graphene oxide solution, dropwise addition process is carried out at the same time stirring, waits for
Continue to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, mixed solution pH value is adjusted to 9- using sodium hydroxide solution
11, then hydrazine hydrate is added dropwise in adjusting solution in adjusted solution, transfers in 90 DEG C of water-baths and keeps the temperature 2-4h,
Magnetic agitation is carried out in insulating process, is taken out after heat preservation, then cooled to room temperature sops up supernatant liquor with suction pipe,
It uses alcohol and deionized water to wash first remaining floccule, then carries out centrifugal treating, obtain solid product；
Step 6, solid product is freeze-dried to get the graphene powder of load copper particle；
Step 7, the graphene powder 0.1-3%, copper powder 97- of load copper particle are weighed respectively according to mass percent
99.9%, the sum of above constituent mass percentage is 100%；
Step 8, it is dissolved in acetone after the graphene powder of load copper particle that step 7 weighs and copper powder being mixed, ultrasound
Magnetic agitation is carried out until acetone evaporating completely, obtains composite granule at 60-80 DEG C after handling 30min；
Step 9, composite granule is subjected to powder mixing machine, powder time 2-8h is mixed, by the composite granule briquet after mixed powder
It is placed in sintering furnace afterwards and carries out hot pressed sintering, 2-3h is kept the temperature after being warming up to 600-900 DEG C, finally obtain the enhancing of supported copper graphene
Cu-base composites, supported copper graphene enhancing Cu-base composites it is composed of the following components by mass percentage：Cu
The graphene 0.1-3% of 97-99.9%, supported copper, the sum of the above components mass percent are 100%, the graphite of supported copper
The quality accounting of copper is 24.02%-28.22% in alkene.
The features of the present invention also characterized in that
The alcoholic solution mass concentration of step 3 is 99.7%, and copper nitrate is 1 with alcoholic solution mass ratio:15-35.
Hydrazine hydrate mass concentration is 85% in step 5, and hydrazine hydrate is 1 with the mass ratio for adjusting solution:10-28.
The temperature of the freeze-drying of step 6 is -55 DEG C, time 9-14h.
It is 1 that step 8, which loads the graphene powder of copper particle and the gross mass of copper powder and acetone quality ratio,:8-14.
It is 20-50MPa that step 9, which is sintered pressure,.
The invention has the advantages that the present invention a kind of supported copper graphene enhance Cu-base composites, by
Graphene film interlayer introduces the second phase copper particle, solves the problems, such as that graphene itself is easily reunited, realizes graphene copper-based
Evenly dispersed in body, having obtained the graphene of excellent combination property enhances copper-based block composite material.
Description of the drawings
Fig. 1 is a kind of supported copper graphene enhancing Cu-base composites preparation flow figure of the present invention；
Fig. 2 is a kind of graphene powder stereoscan photograph of supported copper of the present invention；
Fig. 3 is a kind of graphene powder transmission electron microscope photo of supported copper of the present invention.
Specific implementation mode
A kind of graphene of supported copper provided by the invention enhances Cu-base composites, by mass percentage by following components
Composition：The graphene 0.1-3% of Cu 97-99.9%, supported copper, the sum of the above components mass percent are 100%, load
The quality accounting of copper is 24.02%-28.22% in the graphene of copper.A kind of graphene enhancing of supported copper is copper-based compound
The preparation method flow of material is as shown in Figure 1, concrete operation step is as follows：
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 15-30%, copper nitrate 70-85%,
The sum of above constituent mass percentage is 100%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 90min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, it is the copper nitrate and alcohol quality in 99.7% alcoholic solution the copper nitrate to be dissolved in mass concentration
Than being 1:15-35 is to get to copper nitrate solution；
Step 4, the copper nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process is carried out at the same time
Stirring continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
9-11, adjusted solution, be then added dropwise in adjusting solution mass concentration be 85% hydrazine hydrate, hydrazine hydrate with mix
The mass ratio of solution is 1:10-28 is transferred in 90 DEG C of water-baths and is kept the temperature 2-4h, and magnetic agitation is carried out in insulating process, is protected
Taken out after temperature, then cooled to room temperature sops up supernatant liquor with suction pipe, to remaining floccule first use alcohol and
Deionized water is washed, then carries out centrifugal treating, obtains solid product；
Step 6, the solid product is freeze-dried, the temperature of freeze-drying is -55 DEG C, time 9-14h, i.e.,
The graphene powder of copper particle must be loaded；
Step 7, the graphene powder 0.1-3%, copper powder 97- of load copper particle are weighed respectively according to mass percent
99.9%, the sum of above constituent mass percentage is 100%；
Step 8, it is dissolved in acetone, loads after the graphene powder of load copper particle that step 7 weighs and copper powder being mixed
The graphene powder of copper particle and the gross mass of copper powder and acetone quality ratio are 1:8-14 is ultrasonically treated after 30min at 60-80 DEG C
Lower progress magnetic agitation obtains composite granule until acetone evaporating completely；
Step 9, the composite granule is subjected to powder mixing machine, mixes powder time 2-8h, the composite granule after mixed powder is suppressed
Hot pressed sintering is carried out in merging sintering furnace after blocking, 2-3h, pressure 20-50MPa are kept the temperature after being warming up to 600-900 DEG C, finally
The graphene enhancing Cu-base composites of supported copper are obtained, the Cu-base composites of the supported copper graphene enhancing press quality hundred
Divide than composed of the following components：The graphene 0.1-3% of Cu 97-99.9%, supported copper, the above components mass percent it
Be 100%, in the graphene of the supported copper quality accounting of copper be 24.02%-28.22%.
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 15%, copper nitrate 85%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 90min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, it is the copper nitrate and alcohol quality in 99.7% alcoholic solution the copper nitrate to be dissolved in mass concentration
Than being 1:15 to get to copper nitrate solution；
Step 4, the copper nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process is carried out at the same time
Stirring continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
9, adjusted solution, be then added dropwise in adjusting solution mass concentration be 85% hydrazine hydrate, hydrazine hydrate with mix it is molten
The mass ratio of liquid is 1:10, it transfers in 90 DEG C of water-baths and keeps the temperature 2h, magnetic agitation is carried out in insulating process, after heat preservation
It takes out, then cooled to room temperature sops up supernatant liquor with suction pipe, alcohol and deionized water are used first to remaining floccule
Washing, then centrifugal treating is carried out, obtain solid product；
Step 6, the solid product is freeze-dried, the temperature of freeze-drying is -55 DEG C, the time be 9h to get
Load the graphene powder of copper particle；
Step 7, according to mass percent respectively weigh load copper particle graphene powder 0.1%, copper powder 99.9%, with
The sum of upper constituent mass percentage is 100%；
Step 8, it is dissolved in acetone, loads after the graphene powder of load copper particle that step 7 weighs and copper powder being mixed
The graphene powder of copper particle and the gross mass of copper powder and acetone quality ratio are 1:8, it is carried out at 60 DEG C after being ultrasonically treated 30min
Magnetic agitation obtains composite granule until acetone evaporating completely；
Step 9, the composite granule is subjected to powder mixing machine, mixes powder time 2-8h, the composite granule after mixed powder is suppressed
Hot pressed sintering is carried out in merging sintering furnace after blocking, 2h is kept the temperature after being warming up to 600 DEG C, pressure 20MPa finally obtains supported copper
Graphene enhance Cu-base composites.
Embodiment 2
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 30%, copper nitrate 70%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 90min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, it is the copper nitrate and alcohol quality in 99.7% alcoholic solution the copper nitrate to be dissolved in mass concentration
Than being 1:35 to get to copper nitrate solution；
Step 4, the copper nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process is carried out at the same time
Stirring continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
11, adjusted solution, be then added dropwise in adjusting solution mass concentration be 85% hydrazine hydrate, hydrazine hydrate with mix it is molten
The mass ratio of liquid is 1:28, it transfers in 90 DEG C of water-baths and keeps the temperature 4h, magnetic agitation is carried out in insulating process, after heat preservation
It takes out, then cooled to room temperature sops up supernatant liquor with suction pipe, alcohol and deionized water are used first to remaining floccule
Washing, then centrifugal treating is carried out, obtain solid product；
Step 6, the solid product is freeze-dried, the temperature of freeze-drying is -55 DEG C, the time be 14h to get
Load the graphene powder of copper particle；
Step 7, the graphene powder 3% of load copper particle, copper powder 97% are weighed respectively according to mass percent；
Step 8, it is dissolved in acetone, loads after the graphene powder of load copper particle that step 7 weighs and copper powder being mixed
The graphene powder of copper particle and the gross mass of copper powder and acetone quality ratio are 1:14, be ultrasonically treated 30min after at 80 DEG C into
Row magnetic agitation obtains composite granule until acetone evaporating completely；
Step 9, the composite granule is subjected to powder mixing machine, mixes powder time 8h, the composite granule after mixed powder is pressed into
It is placed in sintering furnace after block and carries out hot pressed sintering, 3h is kept the temperature after being warming up to 900 DEG C, pressure 50MPa finally obtains supported copper
Graphene enhances Cu-base composites.
Embodiment 3
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 22.5%, copper nitrate 77.5%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 90min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, it is the copper nitrate and alcohol quality in 99.7% alcoholic solution the copper nitrate to be dissolved in mass concentration
Than being 1:25 to get to copper nitrate solution；
Step 4, the copper nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process is carried out at the same time
Stirring continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
10, adjusted solution, be then added dropwise in adjusting solution mass concentration be 85% hydrazine hydrate, hydrazine hydrate with mix it is molten
The mass ratio of liquid is 1:19, it transfers in 90 DEG C of water-baths and keeps the temperature 3h, magnetic agitation is carried out in insulating process, after heat preservation
It takes out, then cooled to room temperature sops up supernatant liquor with suction pipe, alcohol and deionized water are used first to remaining floccule
Washing, then centrifugal treating is carried out, obtain solid product；
Step 6, the solid product is freeze-dried, the temperature of freeze-drying is -55 DEG C, time 11.5h, i.e.,
The graphene powder of copper particle must be loaded；
Step 7, the graphene powder 1.5% of load copper particle, copper powder 98.5% are weighed respectively according to mass percent；
Step 8, it is dissolved in acetone, loads after the graphene powder of load copper particle that step 7 weighs and copper powder being mixed
The graphene powder of copper particle and the gross mass of copper powder and acetone quality ratio are 1:11, be ultrasonically treated 30min after at 70 DEG C into
Row magnetic agitation obtains composite granule until acetone evaporating completely；
Step 9, the composite granule is subjected to powder mixing machine, mixes powder time 5h, the composite granule after mixed powder is pressed into
It is placed in sintering furnace after block and carries out hot pressed sintering, 2.5h is kept the temperature after being warming up to 750 DEG C, pressure 35MPa finally obtains supported copper
Graphene enhance Cu-base composites.
Embodiment 4
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 18%, copper nitrate 82%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 90min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, it is the copper nitrate and alcohol quality in 99.7% alcoholic solution the copper nitrate to be dissolved in mass concentration
Than being 1:20 to get to copper nitrate solution；
Step 4, the copper nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process is carried out at the same time
Stirring continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
9, adjusted solution, be then added dropwise in adjusting solution mass concentration be 85% hydrazine hydrate, hydrazine hydrate with mix it is molten
The mass ratio of liquid is 1:15, it transfers in 90 DEG C of water-baths and keeps the temperature 2h, magnetic agitation is carried out in insulating process, after heat preservation
It takes out, then cooled to room temperature sops up supernatant liquor with suction pipe, alcohol and deionized water are used first to remaining floccule
Washing, then centrifugal treating is carried out, obtain solid product；
Step 6, the solid product is freeze-dried, the temperature of freeze-drying is -55 DEG C, the time be 13h to get
Load the graphene powder of copper particle；
Step 7, the graphene powder 0.1% of load copper particle, copper powder 99.9% are weighed respectively according to mass percent；
Step 8, it is dissolved in acetone, loads after the graphene powder of load copper particle that step 7 weighs and copper powder being mixed
The graphene powder of copper particle and the gross mass of copper powder and acetone quality ratio are 1:10, be ultrasonically treated 30min after at 80 DEG C into
Row magnetic agitation obtains composite granule until acetone evaporating completely；
Step 9, the composite granule is subjected to powder mixing machine, mixes powder time 6h, the composite granule after mixed powder is pressed into
It is placed in sintering furnace after block and carries out hot pressed sintering, 2h is kept the temperature after being warming up to 900 DEG C, pressure 30MPa finally obtains supported copper
Graphene enhances Cu-base composites.
Embodiment 5
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 29%, copper nitrate 71%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 90min systems after stirring 30min
Obtain graphene oxide solution；
Step 3, it is the copper nitrate and alcohol quality in 99.7% alcoholic solution the copper nitrate to be dissolved in mass concentration
Than being 1:30 to get to copper nitrate solution；
Step 4, the copper nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process is carried out at the same time
Stirring continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, are adjusted to the mixed solution pH value using sodium hydroxide solution
11, adjusted solution, be then added dropwise in adjusting solution mass concentration be 85% hydrazine hydrate, hydrazine hydrate with mix it is molten
The mass ratio of liquid is 1:18, it transfers in 90 DEG C of water-baths and keeps the temperature 2h, magnetic agitation is carried out in insulating process, after heat preservation
It takes out, then cooled to room temperature sops up supernatant liquor with suction pipe, alcohol and deionized water are used first to remaining floccule
Washing, then centrifugal treating is carried out, obtain solid product；
Step 6, the solid product is freeze-dried, the temperature of freeze-drying is -55 DEG C, the time be 10h to get
Load the graphene powder of copper particle；
Step 7, the graphene powder 0.5% of load copper particle, copper powder 99.5% are weighed respectively according to mass percent；
Step 8, it is dissolved in acetone, loads after the graphene powder of load copper particle that step 7 weighs and copper powder being mixed
The graphene powder of copper particle and the gross mass of copper powder and acetone quality ratio are 1:12, be ultrasonically treated 30min after at 80 DEG C into
Row magnetic agitation obtains composite granule until acetone evaporating completely；
Step 9, the composite granule is subjected to powder mixing machine, mixes powder time 6h, the composite granule after mixed powder is pressed into
It is placed in sintering furnace after block and carries out hot pressed sintering, 2h is kept the temperature after being warming up to 800 DEG C, pressure 40MPa finally obtains supported copper
Graphene enhances Cu-base composites.
Fig. 2 is a kind of supported copper graphene powder stereoscan photograph of the present invention, it can be seen that copper particle is dispersed in graphite
On alkene.Fig. 3 is a kind of supported copper graphene powder transmission electron microscope photo of the present invention, and load can be seen more clearly under high power
Copper particle is evenly dispersed on graphene.
1 embodiment of table is compared with traditional Cu-base composites performance parameter
| Sample ID | Conductivity/%IACS | Hardness/HV |
| Embodiment 4 | 89.6% | 65.2 |
| Embodiment 5 | 87.9% | 135 |
| Traditional Al2O3Enhance Cu-base composites | 41% | 58 |
With traditional Al2O3The Cu-base composites of enhancing are compared, and embodiment 4 and conductivity in embodiment 5 and hardness are aobvious
Write and improve, the wherein conductivity of embodiment 4 and hardness has been respectively increased 118.54%, 12.41%, the conductivity of embodiment 5 and
Hardness has been respectively increased 114.39%, 132.75%.
Claims (7)
1. a kind of graphene of supported copper enhances Cu-base composites, which is characterized in that by mass percentage by following components group
At：The graphene 0.1-3% of Cu 97-99.9%, supported copper, the sum of the above components mass percent are 100%, described negative
The quality accounting of copper is 24.02%-28.22% in copper-loaded graphene.
2. a kind of preparation method of the Cu-base composites of supported copper graphene enhancing as described in claim 1, feature exist
In concrete operation step is as follows：
Step 1, following material is weighed respectively according to mass percent：Graphene oxide 15-30%, copper nitrate 70-85%, it is above
The sum of constituent mass percentage is 100%；
Step 2, the graphene oxide is added in deionized water, continues ultrasonic disperse 90min after stirring 30min, is made
Graphene oxide solution；
Step 3, the copper nitrate is dissolved in alcoholic solution to get to copper nitrate solution；
Step 4, the copper nitrate solution is added dropwise in the graphene oxide solution, dropwise addition process, which is carried out at the same time, to be stirred
It mixes, continues to stir 30min after completion of dropwise addition, then be ultrasonically treated 60min to get mixed solution；
Step 5,2mol/L sodium hydroxide solutions are prepared, the mixed solution pH value is adjusted to 9- using sodium hydroxide solution
11, then hydrazine hydrate is added dropwise in adjusting solution in adjusted solution, transfers in 90 DEG C of water-baths and keeps the temperature 2-4h,
Magnetic agitation is carried out in insulating process, is taken out after heat preservation, then cooled to room temperature sops up supernatant liquor with suction pipe,
It uses alcohol and deionized water to wash first remaining floccule, then carries out centrifugal treating, obtain solid product；
Step 6, the solid product is freeze-dried to get the graphene powder of load copper particle；
Step 7, graphene powder 0.1-3%, the copper powder 97-99.9% of load copper particle are weighed respectively according to mass percent,
The sum of above constituent mass percentage is 100%；
Step 8, it is dissolved in acetone, is ultrasonically treated after the graphene powder of load copper particle that step 7 weighs and copper powder being mixed
Magnetic agitation is carried out until acetone evaporating completely, obtains composite granule at 60-80 DEG C after 30min；
Step 9, the composite granule is subjected to powder mixing machine, powder time 2-8h is mixed, by the composite granule briquet after mixed powder
It is placed in sintering furnace afterwards and carries out hot pressed sintering, 2-3h is kept the temperature after being warming up to 600-900 DEG C, finally obtain the enhancing of supported copper graphene
Cu-base composites, the Cu-base composites of supported copper graphene enhancing are composed of the following components by mass percentage：
The graphene 0.1-3% of Cu 97-99.9%, supported copper, the sum of the above components mass percent are 100%, the supported copper
Graphene in copper quality accounting be 24.02%-28.22%.
3. a kind of preparation method of the graphene enhancing Cu-base composites of supported copper according to claim 1, feature
It is, the alcoholic solution mass concentration described in step 3 is 99.7%, and the copper nitrate is 1 with alcoholic solution mass ratio:15-35.
4. a kind of preparation method of the graphene enhancing Cu-base composites of supported copper according to claim 1, feature
It is, hydrazine hydrate mass concentration described in step 5 is 85%, and the hydrazine hydrate is 1 with the mass ratio for adjusting solution:10-28.
5. a kind of preparation method of the graphene enhancing Cu-base composites of supported copper according to claim 1, feature
It is, the temperature of the freeze-drying described in step 6 is -55 DEG C, time 9-14h.
6. a kind of preparation method of the graphene enhancing Cu-base composites of supported copper according to claim 1, feature
It is, it is 1 that the graphene powder of copper particle and the gross mass of copper powder and acetone quality ratio are loaded described in step 8:8-14.
7. a kind of preparation method of the graphene enhancing Cu-base composites of supported copper according to claim 1, feature
It is, it is 20-50MPa that pressure is sintered described in step 9.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111560533A (en) * | 2020-05-23 | 2020-08-21 | 湖南大学 | High-thermal-conductivity boron nitride/copper composite material and preparation method thereof |
| CN111961903A (en) * | 2020-08-19 | 2020-11-20 | 西安理工大学 | Preparation method of nanoparticle-doped graphene oxide reinforced copper-based composite material |
| CN112176217A (en) * | 2020-10-28 | 2021-01-05 | 江西勇骏实业有限公司 | High-strength copper alloy and preparation method thereof |
| CN112359244A (en) * | 2020-10-21 | 2021-02-12 | 有研工程技术研究院有限公司 | High-strength high-conductivity graphene copper composite wire and preparation method thereof |
| CN112593108A (en) * | 2020-11-28 | 2021-04-02 | 江西森通新材料科技有限公司 | Preparation method of graphene-copper composite material |
| CN113249633A (en) * | 2021-06-10 | 2021-08-13 | 北京石墨烯技术研究院有限公司 | Dispersion strengthening alloy and preparation method and application thereof |
| CN113355146A (en) * | 2021-06-18 | 2021-09-07 | 西安工业大学 | Preparation method of graphene-loaded copper nanoparticles for lubricating oil additive |
| CN113512662A (en) * | 2021-07-16 | 2021-10-19 | 陕西科技大学 | Silver-loaded graphene/copper self-lubricating material and preparation method thereof |
| CN114131036A (en) * | 2021-12-03 | 2022-03-04 | 安徽工业大学 | Low-cost preparation method of functionalized micro-nano particle reinforcement |
| CN117198585A (en) * | 2023-09-06 | 2023-12-08 | 广东日鸿电缆有限公司 | Flexible graphene cable and preparation method thereof |
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| CN111560533A (en) * | 2020-05-23 | 2020-08-21 | 湖南大学 | High-thermal-conductivity boron nitride/copper composite material and preparation method thereof |
| CN111560533B (en) * | 2020-05-23 | 2021-05-04 | 湖南大学 | High-thermal-conductivity boron nitride/copper composite material and preparation method thereof |
| CN111961903A (en) * | 2020-08-19 | 2020-11-20 | 西安理工大学 | Preparation method of nanoparticle-doped graphene oxide reinforced copper-based composite material |
| CN111961903B (en) * | 2020-08-19 | 2021-11-16 | 西安理工大学 | Preparation method of nanoparticle-doped graphene oxide reinforced copper-based composite material |
| CN112359244A (en) * | 2020-10-21 | 2021-02-12 | 有研工程技术研究院有限公司 | High-strength high-conductivity graphene copper composite wire and preparation method thereof |
| CN112176217A (en) * | 2020-10-28 | 2021-01-05 | 江西勇骏实业有限公司 | High-strength copper alloy and preparation method thereof |
| CN112593108A (en) * | 2020-11-28 | 2021-04-02 | 江西森通新材料科技有限公司 | Preparation method of graphene-copper composite material |
| CN113249633A (en) * | 2021-06-10 | 2021-08-13 | 北京石墨烯技术研究院有限公司 | Dispersion strengthening alloy and preparation method and application thereof |
| CN113355146A (en) * | 2021-06-18 | 2021-09-07 | 西安工业大学 | Preparation method of graphene-loaded copper nanoparticles for lubricating oil additive |
| CN113512662A (en) * | 2021-07-16 | 2021-10-19 | 陕西科技大学 | Silver-loaded graphene/copper self-lubricating material and preparation method thereof |
| CN114131036A (en) * | 2021-12-03 | 2022-03-04 | 安徽工业大学 | Low-cost preparation method of functionalized micro-nano particle reinforcement |
| CN117198585A (en) * | 2023-09-06 | 2023-12-08 | 广东日鸿电缆有限公司 | Flexible graphene cable and preparation method thereof |
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Application publication date: 20181009 |