CN109585187A - Graphene coated copper raw powder's production technology, copper-graphite alkene electrical contact and preparation method thereof - Google Patents
Graphene coated copper raw powder's production technology, copper-graphite alkene electrical contact and preparation method thereof Download PDFInfo
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 156
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 135
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 129
- 229910002804 graphite Inorganic materials 0.000 title claims abstract description 58
- 239000010439 graphite Substances 0.000 title claims abstract description 58
- 239000010949 copper Substances 0.000 title claims abstract description 57
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 55
- 239000000843 powder Substances 0.000 title claims abstract description 45
- 238000002360 preparation method Methods 0.000 title claims abstract description 33
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000005516 engineering process Methods 0.000 title claims abstract description 15
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 95
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 48
- 239000011812 mixed powder Substances 0.000 claims abstract description 43
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000010703 silicon Substances 0.000 claims abstract description 25
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 25
- 238000000034 method Methods 0.000 claims abstract description 21
- 230000008569 process Effects 0.000 claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 9
- 238000000151 deposition Methods 0.000 claims abstract description 5
- 230000008021 deposition Effects 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 5
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 52
- 239000007789 gas Substances 0.000 claims description 39
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 32
- 238000005229 chemical vapour deposition Methods 0.000 claims description 30
- 239000001257 hydrogen Substances 0.000 claims description 26
- 229910052739 hydrogen Inorganic materials 0.000 claims description 26
- 229910052786 argon Inorganic materials 0.000 claims description 16
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 15
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 15
- 239000006185 dispersion Substances 0.000 claims description 11
- 150000002431 hydrogen Chemical class 0.000 claims description 11
- 239000007788 liquid Substances 0.000 claims description 11
- 238000010438 heat treatment Methods 0.000 claims description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 235000019441 ethanol Nutrition 0.000 claims description 6
- 230000001681 protective effect Effects 0.000 claims description 5
- 150000001336 alkenes Chemical class 0.000 claims description 4
- 239000004575 stone Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 239000007791 liquid phase Substances 0.000 claims description 3
- 239000000320 mechanical mixture Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000012071 phase Substances 0.000 claims description 3
- 238000005191 phase separation Methods 0.000 claims description 3
- 238000007740 vapor deposition Methods 0.000 claims 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 11
- 239000001301 oxygen Substances 0.000 abstract description 11
- 229910052760 oxygen Inorganic materials 0.000 abstract description 11
- 230000003197 catalytic effect Effects 0.000 abstract description 6
- 239000007792 gaseous phase Substances 0.000 abstract description 6
- 230000004927 fusion Effects 0.000 abstract description 5
- 238000003466 welding Methods 0.000 abstract description 5
- 239000000463 material Substances 0.000 description 20
- 239000008188 pellet Substances 0.000 description 12
- 229910052814 silicon oxide Inorganic materials 0.000 description 12
- 230000005611 electricity Effects 0.000 description 8
- 230000012010 growth Effects 0.000 description 8
- 229910003978 SiClx Inorganic materials 0.000 description 5
- 239000002131 composite material Substances 0.000 description 5
- 238000004080 punching Methods 0.000 description 5
- 238000001291 vacuum drying Methods 0.000 description 5
- 238000010792 warming Methods 0.000 description 5
- 238000005137 deposition process Methods 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 4
- 239000002184 metal Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- 238000001069 Raman spectroscopy Methods 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- -1 Transition Metal Sulfur selenides Chemical class 0.000 description 3
- 238000010907 mechanical stirring Methods 0.000 description 3
- 238000004321 preservation Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 229910001316 Ag alloy Inorganic materials 0.000 description 2
- 230000003026 anti-oxygenic effect Effects 0.000 description 2
- 239000011324 bead Substances 0.000 description 2
- 230000008901 benefit Effects 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000005260 corrosion Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- CWQXQMHSOZUFJS-UHFFFAOYSA-N molybdenum disulfide Chemical compound S=[Mo]=S CWQXQMHSOZUFJS-UHFFFAOYSA-N 0.000 description 2
- 229910052982 molybdenum disulfide Inorganic materials 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- VDGJOQCBCPGFFD-UHFFFAOYSA-N oxygen(2-) silicon(4+) titanium(4+) Chemical compound [Si+4].[O-2].[O-2].[Ti+4] VDGJOQCBCPGFFD-UHFFFAOYSA-N 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 1
- 239000005751 Copper oxide Substances 0.000 description 1
- 206010037660 Pyrexia Diseases 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000011889 copper foil Substances 0.000 description 1
- 229910000431 copper oxide Inorganic materials 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 239000011133 lead Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 238000005461 lubrication Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- ITRNXVSDJBHYNJ-UHFFFAOYSA-N tungsten disulfide Chemical compound S=[W]=S ITRNXVSDJBHYNJ-UHFFFAOYSA-N 0.000 description 1
- 238000005019 vapor deposition process Methods 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H1/00—Contacts
- H01H1/02—Contacts characterised by the material thereof
- H01H1/021—Composite material
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01H—ELECTRIC SWITCHES; RELAYS; SELECTORS; EMERGENCY PROTECTIVE DEVICES
- H01H11/00—Apparatus or processes specially adapted for the manufacture of electric switches
- H01H11/04—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts
- H01H11/048—Apparatus or processes specially adapted for the manufacture of electric switches of switch contacts by powder-metallurgical processes
Abstract
A kind of graphene coated copper raw powder's production technology, comprising the following steps: step a: copper powder is uniformly mixed with silica, obtains copper-silica mixed powder；Step b: copper-silica mixed powder carries out oxygen catalytic chemical gaseous phase deposition, obtains copper/graphene and silica or silicon mixed powder；Step c: copper removal/graphene and silica or silica or silicon in silicon mixed powder are removed, graphene coated copper powder body is obtained.Invention additionally discloses the graphene coated copper powder bodies that will be obtained as obtained copper-graphite alkene electrical contact of raw material and preparation method thereof.Graphene coated copper powder preparation is able to achieve graphene high-effect high-quality on copper powder body and grows in the present invention.Copper-graphite alkene electrical contact preparation method can be applicable on the process equipment of conventional electrical contacts, conventional production lines are facilitated to convert, obtained copper-graphite alkene electrical contact electrical and thermal conductivity is high, contact resistance is low, wear-resistant strength is high, and has anti-dielectric etch, fusion welding resisting ability.
Description
Technical field
The present invention relates to electrical contact material and its technical fields of preparation, and in particular to a kind of graphene coated copper powder body
Preparation method, copper-graphite alkene electrical contact and preparation method thereof.
Background technique
Electrical contact is electric current transmission and one of important materials in conversion process, be prepare electric power, switching control in appliance circuit
The contact element of system and load current electric appliance (such as electric switch, relay, instrument and meter and starter), is widely used in electricity
Power, telecommunication system.
Modern electrical contact material is broadly divided into: copper-based electrical contact material, Ag-based electrical contact material and expensive/cheap metal close
Golden class electrical contact material, such as using Cu as substrate, Ag is the Ag alloy electrical contact materials of composite layer, or using Cu as substrate,
AgSnO2For the Ag alloy electrical contact materials of composite layer.Wherein silver is used as a kind of noble metal, and it is expensive and stock number is limited,
Using silver as raw material be electrical contact price it is prohibitively expensive, be unfavorable for large-scale utilization and extention.And that metallic copper has is excellent
Electrical and thermal conductivity performance, and it is cheap, plasticity is high, this is easily promoted in contact material field.But metallic copper is as electrical contact
The strength of materials is low, oxidizable, and in practical work process, the contact resistance of contact element can constantly increase, and is easy fever, wear-resisting
Property is poor, and the service life of electrical contact and reliability is caused to substantially reduce.
Copper-based electrical contact mainly uses middle high-pressure environment at present, mainly based on Cu-base composites, such as addition lead, oxygen
Change lead, graphite, tungsten disulfide, molybdenum disulfide etc., the intrinsic mechanical performance of holding copper-based electrical contact, good electrical and thermal conductivity
Can, while also tool has certain effect in terms of antifriction and lubrication.But with the raising of environmental consciousness, lead-free copper-based electricity touching
Head becomes hot spot, and graphite, molybdenum disulfide and other Transition Metal Sulfur selenides are increasingly becoming the main of copper-based electrical contact material
Lubricant component.In general, Copper substrate content increases, and the mechanical strength of electrical contact, conduction, heating conduction are promoted, but wear-resistant
Performance weakens；And addition element content increases, when mechanical property is promoted, electrical and thermal conductivity performance reduces electrical contact.So this
Serial added material improves the intensity of electrical contact, reduces costs for silver-based, but also affects electrical contact simultaneously
The conductivity of material, while the shortcomings that there is also itself, for example, it is toxic, oxidizable, wear no resistance.
With the development of modern industry, noble metal is substituted with cheap metal, extends cheap metal answering in electrical contact field
It is inevitable with becoming.Therefore, there is excellent conductive, heating conduction and corrosion-resistant, oxidation resistant copper-based electrical contact to become urgently for research and development
Problem to be solved.A kind of two-dimensional material of the graphene as high strength and high conductivity, the specific surface area with super large, carrier move
Shifting rate reaches 15000cm2/ (Vs), and thermal conductivity is up to 5150W/ (mK), it is considered to be the strengthening material of ideal copper-based electrical contact
Material.Currently, the research of Metal Substrate graphene composite material is increasing, the performance of composite material is also played certain excellent
Gesture.
Therefore the special construction and superior function for combining graphene, are prepared with excellent conductive heating conduction, low contact
The high-performance copper-base graphite alkene electricity touching of resistance, anti-dielectric etch, fusion welding resisting ability, excellent wear, high rigidity, obdurability
Head has very big market application prospect.
Summary of the invention
It is an object of the invention to overcome the deficiencies of existing technologies, a kind of preparation side of graphene coated copper powder body is provided
Method.
To achieve the above object, present invention employs following technical solutions:
A kind of graphene coated copper raw powder's production technology, comprising the following steps:
Step a: copper powder is uniformly mixed with silica, obtains copper-silica mixed powder；
Step b: copper-silica mixed powder that step a is obtained is placed in chemical vapor deposition vacuum chamber, is being restored
It under the atmosphere of gas and protective gas, is maintained at 600~1050 DEG C of temperature and normal pressure state, is passed through carbon-source gas, carry out
Chemical vapor deposition obtains copper/graphene and silica or silicon mixed powder；
Step c: it disperses copper/graphene and silica or silicon mixed powder in dispersion liquid, is gone using liquid phase separation
Except silica or silicon, graphene coated copper powder body is obtained.
Preferably, in the step a, copper powder is one or both of electrolytic copper powder, atomized copper powder, the partial size of copper powder
50nm~300 μm；The partial size of silica is 10nm~20 μm, and copper powder and silica quality ratio are 2: 1~5: 8.
Preferably, in the step b, chemical gas-phase deposition system is first evacuated to 10-3KPa, then be passed through as protection
To 600~1050 DEG C, then the argon gas of gas until being in normal pressure state in chemical vapor deposition vacuum chamber, then increases temperature
It is passed through the hydrogen as reducing gas, keeps the temperature, the methane gas as carbon-source gas is finally passed through, in 600~1050 DEG C of constant temperature
For a period of time, after to chemical vapor deposition processes, stopping be passed through methane and hydrogen, be down to room temperature, obtain copper/graphene with
Silica or silicon mixed powder.
Preferably, in the step b, argon flow is 100~500sccm, and the flow of hydrogen is 2~50sccm, methane
Gas flow is 3~10sccm, and heating rate is 10~20 DEG C/min, and cooling rate is 5~15 DEG C/min.
Preferably, in the step c, dispersion liquid is one or both of water and ethyl alcohol.
Graphene coated copper powder preparation of the invention, silicon oxide pellets are mixed with copper powder, utilize titanium dioxide
Silicon bead discharges oxygen under the high temperature conditions, realizes that graphene is efficiently high on copper powder body by oxygen catalytic chemical gaseous phase deposition process
Mass growth.
Another object of the present invention is to provide a kind of low cost, electric-conductivity heat-conductivity high, low contact resistance, anti-dielectric are rotten
Copper-graphite alkene electrical contact of corrosion, fusion welding resisting ability and wear-resisting high-strength degree and preparation method thereof.
To achieve the above object, present invention employs following technical solutions:
A kind of preparation method of copper-graphite alkene electrical contact, comprising the following steps:
Step d: the graphene coated copper raw powder's production technology by graphene powder and according to the above technical scheme
Graphene coated copper powder body mechanical mixture obtained, obtains copper-graphite alkene mixed powder；
Step e: copper-graphite alkene electrical contact is made in the copper-graphite alkene mixed powder that step d is obtained.
Preferably, in the step d, graphene powder used is to pass through electrochemical stripping using crystalline flake graphite as raw material
Method obtains.
Preferably, in the step d, the partial size of graphene coated copper powder body is 50nm~300 μm.
A kind of copper-graphite alkene electrical contact, by graphene powder and the graphene coated copper according to the above technical scheme
Graphene coated copper powder body made from raw powder's production technology composition, wherein the content of graphene coated copper powder body be 95wt%~
100wt%, the content of graphene powder are 0wt%~5wt%.
Copper-graphite alkene electrical contact of the invention and preparation method thereof realizes stone by oxygen catalytic chemical gaseous phase deposition process
Fast and high quality growth of the black alkene on copper powder body, using graphene as the reinforcement of copper-based electrical contact material, comprehensive raising
The conduction of copper-based electrical contact, heating conduction and mechanical performance, reduce the contact resistance of electrical contact.Meanwhile with graphene
Coated copper powder can effectively enhance anti-dielectric etch, the antioxygenic property, fusion welding resisting ability of electrical contact, extend electrical contact
Actual life.The present invention focuses on material building innovation, can be realized on a large scale using traditional electrical contact process equipment
Production, at low cost, wide market.
Detailed description of the invention
Fig. 1 is the field emission scanning electron microscope figure of graphene coated copper powder body in the embodiment of the present invention one；
Fig. 2 is the Raman spectrogram of copper graphene powder in the embodiment of the present invention one；
Fig. 3 is the field emission scanning electron microscope figure of graphene coated copper powder body in the embodiment of the present invention four；
Fig. 4 is the Raman spectrogram of copper graphene powder in the embodiment of the present invention four.
Specific embodiment
Below in conjunction with the embodiment that attached drawing 1 to 4 provides, the preparation of graphene coated copper powder body of the invention is further illustrated
The specific embodiment of method, copper-graphite alkene electrical contact and preparation method thereof.The preparation of graphene coated copper powder body of the invention
Method, copper-graphite alkene electrical contact and preparation method thereof are not limited to the following description.
The present invention prepares graphene coated copper powder body as steps described below, specific as follows:
Step a: copper powder is uniformly mixed with silica, obtains copper-silica mixed powder；
In this step, used copper powder is one or both of electrolytic copper powder, atomized copper powder, the partial size 50nm of copper powder
~300 μm；The partial size of silica is 10nm~20 μm, and copper powder and silica quality ratio are 2: 1~5: 8.
Step b: copper-silica mixed powder that step a is obtained is placed in chemical vapor deposition vacuum chamber, is being restored
It under the atmosphere of gas and protective gas, is maintained at 600~1050 DEG C of temperature and normal pressure state, is passed through carbon-source gas, carry out
Chemical vapor deposition obtains copper/graphene and silica or silicon mixed powder；
Specifically, chemical gas-phase deposition system is first evacuated to 10-3KPa, then it is passed through the argon gas as protective gas, directly
It is in normal pressure state in chemical vapor deposition vacuum chamber, then increases temperature to 600~1050 DEG C, then passes to as also Primordial Qi
The hydrogen of body, heat preservation, be finally passed through the methane gas as carbon-source gas, 600~1050 DEG C of constant temperature for a period of time, to chemistry
After vapor deposition processes, stopping is passed through methane and hydrogen, is down to room temperature, obtains copper/graphene and silica or silicon is mixed
Close powder.
In this step, argon flow is 100~500sccm, and the flow of hydrogen is 2~50sccm, and methane gas flow is 3
~10sccm, heating rate are 10~20 DEG C/min, and cooling rate is 5~15 DEG C/min.
Step c: it disperses copper/graphene and silica or silicon mixed powder in dispersion liquid, is gone using liquid phase separation
Except silica or silicon, graphene coated copper powder body is obtained.
In this step, used dispersion liquid is one or both of water and ethyl alcohol, and separate mode is vibration separation.
Graphene coated copper powder preparation of the invention, silicon oxide pellets are mixed with copper powder, utilize titanium dioxide
Silicon bead discharges oxygen under the high temperature conditions, realizes that graphene is efficiently high on copper powder body by oxygen catalytic chemical gaseous phase deposition process
Mass growth.The technical principle of oxygen catalytic chemical gaseous phase deposition: the processing by oxygen to Copper Powder Surface, it is possible to reduce copper powder table
The impurity and defect in face obtain the graphene film of larger size domain so as to reduce the nucleation density of graphene；Copper powder
After being oxidized, in graphene growth stage being passed through due to hydrogen, copper oxide surface can be restored, in this hot environment
Under, the Copper Powder Surface being reduced can occur to reconstruct (single crystallization), form the crystal face of more suitable graphene growths, in the process copper foil
Surface can also become more flat and smooth, be conducive to the fast-growth of graphene, lifting process efficiency；It has proven to certain density
Oxygen can reduce the energy barrier of methane gas decomposition, and methane gas is accelerated to decomposite more carbon atoms, accelerate carbon source in copper powder
Surface deposits the speed to form graphene, so that the speed of growth of graphene be made to accelerate
The present invention prepares copper-graphite alkene electrical contact as steps described below, specific as follows:
Step d: it by graphene powder and by graphene coated copper powder body mechanical mixture made from step a~c, obtains
Copper-graphite alkene mixed powder；
In this step, the partial size of used graphene coated copper powder body is 50nm~300 μm；Graphene powder used
It is to be obtained using crystalline flake graphite as raw material by electrochemical stripping method.
Step e: the copper-graphite alkene mixed powder that step d is obtained is obtained into copper-stone by traditional electrical contact processing technology
Black alkene electrical contact.
Via in copper-graphite alkene electrical contact made from above-mentioned steps, each composition is as follows: graphene coated copper powder body, content
For 95wt%~100wt%；Graphene powder, content are 0wt%~5wt%.
Copper-graphite alkene electrical contact of the invention and preparation method thereof realizes stone by oxygen catalytic chemical gaseous phase deposition process
Fast and high quality growth of the black alkene on copper powder body, using graphene as the reinforcement of copper-based electrical contact material, comprehensive raising
The conduction of copper-based electrical contact, heating conduction and mechanical performance, reduce the contact resistance of electrical contact.Meanwhile with graphene
Coated copper powder can effectively enhance anti-dielectric etch, the antioxygenic property, fusion welding resisting ability of electrical contact, extend electrical contact
Actual life.The present invention focuses on material building innovation, can be realized on a large scale using traditional electrical contact process equipment
Production, at low cost, wide market.
Make more below by the copper-graphite alkene electrical contact and preparation method thereof in one~embodiment of embodiment, five couples of present invention
Specific description.
Embodiment one
A kind of copper-graphite alkene electrical contact, by graphene coated copper powder system at content 100wt%.
The graphene coated copper powder body specifically sequentially includes the following steps:
10min is mixed firstly, copper powder and silicon oxide pellets are placed in batch mixer in the ratio of 5:4, obtains copper-dioxy
SiClx mixed powder；For the copper powder used for electrolytic copper powder, partial size is 70~75 μm, and the partial size of silicon oxide pellets is 10 μm.
Then, obtained copper-silica mixed powder is placed in chemical vapor deposition vacuum chamber, by chemical vapor deposition
Product system is evacuated to 10-3KPa vacuum degree is that 500sccm is passed through argon gas with throughput, until at chemical vapor deposition vacuum chamber
In normal pressure state, the throughput of argon gas is adjusted to 300sccm；1000 DEG C are warming up to the heating rate of 10 DEG C/min again, with
Throughput is that 50sccm is passed through hydrogen, keeps the temperature 30min；Finally be passed through methane, by the throughput of hydrogen and methane adjust separately for
20sccm and 20sccm keeps the temperature 10min；After chemical vapor deposition processes, stopping be passed through hydrogen and methane, with 8 DEG C/
The speed of min is down to room temperature to get copper/graphene and silica or silicon mixed powder is arrived.
Then, using water as dispersion liquid, vibration separation removal silica or silicon, vacuum drying obtain graphene coated copper
Powder.
The appearance of the graphene coated copper powder body that the present embodiment is prepared is as shown in Figure 1, the wherein graphene of growth in situ
Clad ratio is high on copper powder body, substantially not exposed copper surface topography；The Raman map for the copper graphene powder that Fig. 2 is shown
It shows that the fault of construction of graphene is few, and the peak 2D with higher and lesser peak width, calculates it is found that few layer graphene
It is coated on copper powder surface.
Continue the graphene coated copper powder body of above-mentioned preparation to be sintered by pressure-like, roll, squeeze, punching press it is traditional
Electric contact preparation process obtains copper-graphite alkene electrical contact.Its density is 8.31g/cm3, conductivity 94%IACS, contact resistance
For 1.31m Ω, and its density of traditional copper-based electrical contact is 8.3~8.9g/cm3, conductivity is 70~90%IACS, contact electricity
1.2~1.7m Ω is hindered, in comparison, effect of the copper-graphite alkene electrical contact because of graphene film in the present invention, mass density drop
It is low, but graphene has superpower effective electronic conductivity energy, reveals the conductivity meter of copper-graphite alkene electrical contact apparent excellent
Gesture, while contact resistance is also below traditional copper-based electrical contact.
Embodiment two
A kind of copper-graphite alkene electrical contact, is made, wherein graphene coated of graphene coated copper powder body and graphene powder
Copper powder content is 95wt%, and graphene powder content is 5wt%.
The graphene coated copper powder body of the present embodiment specifically sequentially includes the following steps:
10min is mixed firstly, copper powder and silicon oxide pellets are placed in batch mixer in the ratio of 5:5, obtains copper-dioxy
SiClx mixed powder；For the copper powder used for electrolytic copper powder, partial size is 20~25 μm, and the partial size of silicon oxide pellets is 5 μm.
Then, obtained copper-silica mixed powder is placed in chemical vapor deposition vacuum chamber, by chemical vapor deposition
Product system is evacuated to 10-3KPa is that 500sccm is passed through argon gas with throughput, until chemical vapor deposition vacuum chamber is in normal pressure
The throughput of argon gas is adjusted to 400sccm by state；1050 DEG C are warming up to 15 DEG C/min speed again, is with throughput
20sccm is passed through hydrogen, constant temperature 30min；It is finally passed through methane, and the throughput of hydrogen and methane is adjusted separately as 10sccm
And 10sccm, keep the temperature 10min；After chemical vapor deposition processes, stopping is passed through methane and hydrogen, with 5 DEG C/min speed
It is down to room temperature, obtains copper/graphene and silica or silicon mixed powder.
Finally, isolating silica or silicon using ethanol/water as dispersion liquid, after vacuum drying, graphene coated copper is obtained
Powder.
The copper-graphite alkene electrical contact of the present embodiment specifically sequentially includes the following steps:
Firstly, graphene powder is mixed with graphene coated copper powder body, mechanical stirring 2h, the mixing of copper-graphite alkene is obtained
Powder.
Finally, the copper-graphite alkene mixed powder of above-mentioned preparation is sintered according to pressure-like, roll, squeezes, the tradition of punching press
Electric contact preparation process obtain copper-graphite alkene electrical contact.
The present embodiment copper-graphite alkene electricity obtained containing graphene coated copper powder body 95wt%, graphene powder 5wt%
Contact carries out dependence test, density 8.20g/cm3, conductivity 95%IACS, contact resistance is 1.23m Ω, same to have
There is biggish advantage, it is prominent in terms of conductivity and contact resistance.
Embodiment three
A kind of copper-graphite alkene electrical contact, is made, wherein graphene coated of graphene coated copper powder body and graphene powder
Copper powder content is 98wt%, and graphene powder content is 2wt%.
The graphene coated copper powder body of the present embodiment specifically sequentially includes the following steps:
10min is mixed firstly, copper powder and silicon oxide pellets are placed in batch mixer in 2: 1 ratio, obtains copper-dioxy
SiClx mixed powder；The copper powder used is electrolytic copper powder, partial size 50nm, and silicon oxide pellets partial size is 10nm.
Then, obtained copper-silica mixed powder is placed in chemical vapor deposition vacuum chamber, by chemical vapor deposition
Product system is evacuated to 10-3KPa is that 500sccm is passed through argon gas with throughput, until chemical vapor deposition vacuum chamber is in normal pressure
The throughput of argon gas is adjusted to 100sccm by state；950 DEG C are warming up to 20 DEG C/min speed again, is passed through hydrogen 20sccm simultaneously
Constant temperature 30min；It is finally passed through hydrogen and methane, the throughput of hydrogen and methane is adjusted separately as 10sccm and 5sccm, heat preservation
30min；After chemical vapor deposition processes, stopping is passed through methane and hydrogen, is down to room temperature with 5 DEG C/min speed, obtains
Copper/graphene and silica or silicon mixed powder.
Finally, isolating silica or silicon using ethanol/water as dispersion liquid, graphene coated copper being obtained after vacuum drying
Powder.
The copper-graphite alkene electrical contact of the present embodiment specifically sequentially includes the following steps:
Firstly, graphene powder is mixed with graphene coated copper powder body, mechanical stirring 3h obtains copper-graphite alkene mixed powder
Body.
Finally, the copper-graphite alkene mixed powder of above-mentioned preparation is sintered according to pressure-like, roll, squeezes, the tradition of punching press
Electric contact preparation process obtain copper-graphite alkene electrical contact.
The present embodiment copper-graphite alkene electricity obtained containing graphene coated copper powder body 98wt%, graphene powder 2wt%
Contact carries out dependence test, density 8.36g/cm3, conductivity 98%IACS, contact resistance be 1.16m Ω, comparison with
Traditional copper-based electrical contact, conductivity is high, and contact resistance is low, has apparent advantage in actual product application.
Example IV
A kind of copper-graphite alkene electrical contact, is made, wherein graphene coated of graphene coated copper powder body and graphene powder
Copper powder content is 97wt%, and graphene powder content is 3wt%.
The graphene coated copper powder body of the present embodiment specifically sequentially includes the following steps:
10min is mixed firstly, copper powder and silicon oxide pellets are placed in batch mixer in 5: 8 ratio, obtains copper-dioxy
SiClx mixed powder；The copper powder used is is atomized spherical copper powder, and partial size is 100 μm, and silicon oxide pellets partial size is 20 μm.
Then, obtained copper-silica mixed powder is placed in chemical vapor deposition vacuum chamber, by chemical vapor deposition
Product system is evacuated to 10-3KPa is that 500sccm is passed through argon gas with throughput, until chemical vapor deposition vacuum chamber is in normal pressure
The throughput of argon gas is adjusted to 100sccm by state, is warming up to 650 DEG C with 10 DEG C/min speed, open plasma radio frequency electrical
Source, power 150W.Finally it is passed through methane and hydrogen, the throughput of methane and hydrogen is respectively 5sccm and 2sccm, heat preservation
20min.After chemical vapor deposition processes, plasma rf power supply is closed, stopping is passed through methane and hydrogen, with 10
DEG C/min speed is down to room temperature, obtain copper/graphene and silica or silicon mixed powder.
Finally, isolating silica or silicon using ethanol/water as dispersion liquid, graphene coated copper being obtained after vacuum drying
Powder.
The copper-graphite alkene electrical contact of the present embodiment specifically sequentially includes the following steps:
Firstly, graphene powder is mixed with graphene coated copper powder body, mechanical stirring 3h, the mixing of copper-graphite alkene is obtained
Powder.
Finally, the copper-graphite alkene mixed powder of above-mentioned preparation is sintered according to pressure-like, roll, squeezes, the tradition of punching press
Electric contact preparation process obtain copper-graphite alkene electrical contact.
The present embodiment copper-graphite alkene electricity obtained containing graphene coated copper powder body 97wt%, graphene powder 3wt%
Contact carries out dependence test, density 8.31g/cm3, conductivity 96%IACS, contact resistance is 1.21m Ω, with tradition
Copper-based electrical contact compare, conductivity improve, contact resistance reduce, have very big practical application value.
Embodiment five
A kind of copper-graphite alkene electrical contact, by graphene coated copper powder system at content 100wt%.
The graphene coated copper powder body specifically sequentially includes the following steps:
10min is mixed firstly, copper powder and silicon oxide pellets are placed in batch mixer in 5: 4 ratio, obtains copper-dioxy
SiClx mixed powder；For the copper powder used for electrolytic copper powder, partial size is 300 μm, and the partial size of silicon oxide pellets is 1 μm.
Then, obtained copper-silica mixed powder is placed in chemical vapor deposition vacuum chamber, by chemical vapor deposition
Product system is evacuated to 10-3KPa vacuum degree is that 500sccm is passed through argon gas with throughput, until at chemical vapor deposition vacuum chamber
In normal pressure state, the throughput of argon gas is adjusted to 500sccm；600 DEG C are warming up to the heating rate of 10 DEG C/min again, with gas
Flow is that 50sccm is passed through hydrogen, keeps the temperature 30min；Finally be passed through methane, by the throughput of hydrogen and methane adjust separately for
10sccm and 3sccm keeps the temperature 10min；After chemical vapor deposition processes, stopping be passed through hydrogen and methane, with 15 DEG C/
The speed of min is down to room temperature to get copper/graphene and silica or silicon mixed powder is arrived.
Then, using water as dispersion liquid, vibration separation removal silica or silicon, vacuum drying obtain graphene coated copper
Powder.
Continue the graphene coated copper powder body of above-mentioned preparation to be sintered by pressure-like, roll, squeeze, punching press it is traditional
Electric contact preparation process obtains copper-graphite alkene electrical contact.Its density is 8.42g/cm3, conductivity 99.8%IACS, contact electricity
Resistance is 0.81m Ω, and compared with traditional copper-based electrical contact, conductivity is improved, and contact resistance reduces.
The above content is a further detailed description of the present invention in conjunction with specific preferred embodiments, and it cannot be said that
Specific implementation of the invention is only limited to these instructions.For those of ordinary skill in the art to which the present invention belongs, exist
Under the premise of not departing from present inventive concept, a number of simple deductions or replacements can also be made, all shall be regarded as belonging to of the invention
Protection scope.
Claims (9)
1. a kind of graphene coated copper raw powder's production technology, it is characterised in that: the following steps are included:
Step a: copper powder is uniformly mixed with silica, obtains copper-silica mixed powder；
Step b: copper-silica mixed powder that step a is obtained is placed in chemical vapor deposition vacuum chamber, in reducing gas
It under the atmosphere of protective gas, is maintained at 600~1050 DEG C of temperature and normal pressure state, is passed through carbon-source gas, carry out chemistry
Vapor deposition, obtains copper/graphene and silica or silicon mixed powder；
Step c: dispersing copper/graphene and silica or silicon mixed powder in dispersion liquid, using liquid phase separation removal two
Silica or silicon obtain graphene coated copper powder body.
2. graphene coated copper raw powder's production technology according to claim 1, it is characterised in that: in the step a, copper
Powder is one or both of electrolytic copper powder, atomized copper powder, partial size 50nm~300 μm of copper powder；The partial size of silica is
10nm~20 μm, copper powder and silica quality ratio are 2: 1~5: 8.
3. graphene coated copper raw powder's production technology according to claim 1, it is characterised in that: in the step b, first
Chemical gas-phase deposition system is evacuated to 10-3KPa, then it is passed through the argon gas as protective gas, until chemical vapor deposition is true
It is in normal pressure state in empty room, then increases temperature to 600~1050 DEG C, then passes to the hydrogen as reducing gas, keeps the temperature, most
Be passed through the methane gas as carbon-source gas afterwards, 600~1050 DEG C of constant temperature for a period of time, to the end of chemical vapor deposition processes
Afterwards, stop being passed through methane and hydrogen, be down to room temperature, obtain copper/graphene and silica or silicon mixed powder.
4. graphene coated copper raw powder's production technology according to claim 3, it is characterised in that: in the step b, argon
Throughput is 100~500sccm, and the flow of hydrogen is 2~50sccm, and methane gas flow is 3~10sccm, and heating rate is
10~20 DEG C/min, cooling rate is 5~15 DEG C/min.
5. graphene coated copper raw powder's production technology according to claim 1, it is characterised in that: in the step c, point
Dispersion liquid is one or both of water and ethyl alcohol.
6. a kind of preparation method of copper-graphite alkene electrical contact, it is characterised in that: the following steps are included:
Step d: by graphene powder and according to claim 1-5 any graphene coated copper raw powder's production technology systems
The graphene coated copper powder body mechanical mixture obtained, obtains copper-graphite alkene mixed powder；
Step e: copper-graphite alkene electrical contact is made in the copper-graphite alkene mixed powder that step d is obtained.
7. the preparation method of copper-graphite alkene electrical contact according to claim 6, it is characterised in that: in the step d, institute
Graphene powder is to be obtained using crystalline flake graphite as raw material by electrochemical stripping method.
8. the preparation method of copper-graphite alkene electrical contact according to claim 6, it is characterised in that: in the step d, stone
The partial size of black alkene coated copper powder is 50nm~300 μm.
9. a kind of copper-graphite alkene electrical contact, it is characterised in that: any described with according to claim 1-5 by graphene powder
The composition of graphene coated copper powder body made from graphene coated copper raw powder's production technology, wherein graphene coated copper powder body contains
Amount is 95wt%~100wt%, and the content of graphene powder is 0wt%~5wt%.
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