CN108716114A - Preparation method of novel copper/graphene/polymer composite fiber - Google Patents
Preparation method of novel copper/graphene/polymer composite fiber Download PDFInfo
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- CN108716114A CN108716114A CN201810581263.4A CN201810581263A CN108716114A CN 108716114 A CN108716114 A CN 108716114A CN 201810581263 A CN201810581263 A CN 201810581263A CN 108716114 A CN108716114 A CN 108716114A
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- 239000000835 fiber Substances 0.000 title claims abstract description 94
- 239000010949 copper Substances 0.000 title claims abstract description 92
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 90
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 89
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 81
- 229910021389 graphene Inorganic materials 0.000 title claims abstract description 78
- 239000002131 composite material Substances 0.000 title claims abstract description 67
- 229920000642 polymer Polymers 0.000 title claims abstract description 39
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 25
- 238000005229 chemical vapour deposition Methods 0.000 claims abstract description 17
- 238000005498 polishing Methods 0.000 claims abstract description 12
- 230000003746 surface roughness Effects 0.000 claims abstract description 6
- -1 polypropylene Polymers 0.000 claims description 21
- 230000008595 infiltration Effects 0.000 claims description 8
- 238000001764 infiltration Methods 0.000 claims description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000007789 gas Substances 0.000 claims description 7
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 6
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 6
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 5
- 239000001257 hydrogen Substances 0.000 claims description 5
- 229910052739 hydrogen Inorganic materials 0.000 claims description 5
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 5
- 239000004698 Polyethylene Substances 0.000 claims description 4
- 239000004743 Polypropylene Substances 0.000 claims description 4
- 229910052799 carbon Inorganic materials 0.000 claims description 4
- 229910052751 metal Inorganic materials 0.000 claims description 4
- 239000002184 metal Substances 0.000 claims description 4
- 229920000573 polyethylene Polymers 0.000 claims description 4
- 229920001155 polypropylene Polymers 0.000 claims description 4
- 239000004425 Makrolon Substances 0.000 claims description 3
- 239000004952 Polyamide Substances 0.000 claims description 3
- 239000004642 Polyimide Substances 0.000 claims description 3
- 239000004734 Polyphenylene sulfide Substances 0.000 claims description 3
- 239000004793 Polystyrene Substances 0.000 claims description 3
- 229910052786 argon Inorganic materials 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 229920002492 poly(sulfone) Polymers 0.000 claims description 3
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- 229920000069 polyphenylene sulfide Polymers 0.000 claims description 3
- 229920002223 polystyrene Polymers 0.000 claims description 3
- 229920001169 thermoplastic Polymers 0.000 claims description 3
- 238000004804 winding Methods 0.000 claims description 3
- XECAHXYUAAWDEL-UHFFFAOYSA-N acrylonitrile butadiene styrene Chemical compound C=CC=C.C=CC#N.C=CC1=CC=CC=C1 XECAHXYUAAWDEL-UHFFFAOYSA-N 0.000 claims description 2
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims 2
- 239000002253 acid Substances 0.000 claims 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 claims 1
- 239000004676 acrylonitrile butadiene styrene Substances 0.000 claims 1
- 150000005690 diesters Chemical class 0.000 claims 1
- 150000004702 methyl esters Chemical class 0.000 claims 1
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- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000000956 alloy Substances 0.000 description 1
- 229910045601 alloy Inorganic materials 0.000 description 1
- 239000003708 ampul Substances 0.000 description 1
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- 150000001721 carbon Chemical group 0.000 description 1
- 125000004432 carbon atom Chemical group C* 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
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- 229920001596 poly (chlorostyrenes) Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 1
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000002210 silicon-based material Substances 0.000 description 1
- 239000002356 single layer Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000011232 storage material Substances 0.000 description 1
- 229920003048 styrene butadiene rubber Polymers 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000010936 titanium Substances 0.000 description 1
- 229910052719 titanium Inorganic materials 0.000 description 1
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- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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Abstract
The invention discloses a preparation method of a novel copper/graphene/polymer composite fiber, which comprises the following steps: firstly, processing the surface of a high-purity copper fiber by using a polishing method to prepare a copper fiber with low surface roughness; secondly, placing the high-purity copper fiber in a chemical vapor deposition tube furnace, and growing graphene on the surface of the copper fiber by a chemical vapor deposition method to obtain a copper/graphene composite fiber; thirdly, preparing copper/graphene/polymer multilayer composite fibers; the preparation method of the novel copper/graphene/polymer composite fiber has the advantages of simple process conditions, easily controlled flow, uniform distribution of the obtained composite conductive fiber material, tight combination, higher quality of the composite fiber and high yield.
Description
Technical field
The present invention relates to a kind of preparation methods of new copper/graphene/polymer composite fibrous, belong to conductive material preparation
Technical field.
Background technology
Copper and its alloy conductive and thermal conductivity are preferable, but hardness and strength are relatively low, poor heat resistance, and easily softening becomes under high temperature
Shape, therefore application range is very restricted;To obtain high-strength material, the method generally used is to be added to increase into Copper substrate
Strong body forms composite material, and common reinforcement type has particle, fiber, graphite etc., novel reinforcement also have carbon nanotubes,
Graphene etc.;Electric conductivity is to weigh the important indicator of Cu-base composites, when developing high-strength copper based composites, the head that faces
It is that the electric conductivity of material and intensity are difficult to take into account to want problem, i.e. the raising of intensity is using the loss of conductivity as cost, intensity Gao Ze
Conductivity is low;Therefore, when improving the intensity of Cu-base composites, ensure that its conductivity is still maintained at higher level, become mesh
One of the hot spot of preceding Cu-base composites research;Copper fiber electric conductivity is fine, is largely used to manufacture electric wire, cable, brush etc.;For
The comprehensive performance of copper fiber is promoted, many researchs make it have good for manufacturing regeneration copper fiber and compound copper fiber
Electric conductivity and mechanical property;With the development of science and technology, it develops multiple by the various new type functionals of matrix of copper fiber
Copper fiber is closed, application field and the market of copper fiber have been further expanded.
Graphene has perfect two dimensional crystal structure, its lattice is the hexagon surrounded by six carbon atoms, thickness
For an atomic layer;It is keyed with σ between carbon atom, combination sp2Hydridization, it is extremely excellent that these σ keys assign graphene
Mechanical property and structural rigidity;Its feature is frivolous, high-strength, electric conductivity is excellent, is once called " king of new material ", these
Special physical property makes it in numerous necks such as semi-conducting material, energy storage material, polymer composite, electronic device and sensor
Domain has a wide range of applications;Graphene is as a kind of New Two Dimensional material of monoatomic layer thickness, compared with other carbon materials, tool
There are more excellent physical and chemical properties;Graphene theoretical specific surface area is 2630 m2g-1, Young's modulus reaches 1000
GPa, tensile strength are 130 GPa, are more than 100 times of steel;The carrier mobility of graphene at room temperature is about
15000cm2/ (V s), this numeric ratio have exceeded 10 times of silicon materials;Meanwhile graphene has superelevation thermal conductivity(~5000
Wm-1K-1), play an important roll for the transmission of energy;There is graphene quantum hall effect, ambipolar field to imitate in terms of electricity
Properties should be waited, therefore the fields such as scene effect transistor, ultracapacitor have a good application prospect;In various graphenes
In preparation method, for chemical vapour deposition technique because it can realize large-scale production, the number of plies is controllable, suitable growth high quality, big face
The advantages that long-pending graphene, increasingly favored by researcher;In chemical vapour deposition technique preparation process, the choosing of base material
It selects particularly important;The result shows that, copper is selected to be obtained extensively as the base material of chemical vapor deposition method by years of researches
Approve.
Copper is both growth substrate during the CVD growth of graphene, while being also used as catalyst, has certain catalysis
Activity;The graphene that CVD method obtains is utilized on Cu foils surface, due to its special growth mechanism, i.e. surface self termination effect
Absolute monolayer growth may be implemented, simultaneously because the Van der Waals interaction of interlayer can lead to the growth of bilayer graphene;Cause
This, the graphene grown on Cu foils has become the important materials in related Fundamental Aspects research;In the base of this technology
On plinth, by graphene growth in the surface of copper fiber, copper/graphene composite material of high-quality graphene cladding is also can get,
However such research is less at present;Method that at present can be by graphene coated in copper fiber mainly has:CVD method, hydro-thermal method, spray
Coating etc., however graphene and copper fiber interface obtained by hydro-thermal method are loose, generate larger gap, interface connection is insecure, spraying
Method is simple for process, but is difficult to coat uniformly;CVD method obtains the best in quality and very high with copper surface compatability of graphene, can
Give full play to the advantage and performance of composite construction.
Insulating material of polymer not only has many advantages, such as light weight, easy processing, at low cost, also has environment wide adaptation range
The characteristics of, it has been widely used in electrical, electronics industry;Currently, power equipment and electronic device etc. are just towards high-power, small-sized
Change and the directions such as lightweight are developed, requirements at the higher level are proposed to Insulation Problems;Conductive fiber surfaces coated polymer can rise
To insulating effect, simultaneously as the mechanical property that polymer is excellent, can effectively promote the flexibility of fiber, avoid internal junction
Structure is destroyed;Polymer for conductive fiber insulation usually has excellent electric property and mechanical property, simultaneously also
Should have good high temperature resistance, such as polyethylene, modified polypropene.The present invention by graphene and is gathered using copper as base material
It closes object and is wrapped in copper material surface successively and copper/graphene/polymer composite fibrous is made so that the electric conductivity and power of composite fibre
It learns performance to improve a lot compared with copper/graphene composite material, and infiltrating can be further in the polymeric layer of fiber surface
The flexibility and fatigue resistance of composite fibre are improved, while assigning the insulating properties of fiber surface, and internal structure can be protected
Do not corroded by the external world, improve corrosion resistance, extends working life.
Invention content
To solve the above problems, the present invention proposes a kind of preparation side of new copper/graphene/polymer composite fibrous
Method, composite conducting fiber material made from this method are evenly distributed, are tightly combined.
New copper/graphene of the present invention/polymer composite fibrous preparation method, includes the following steps:
The first step prepares the copper fiber of low surface roughness, handles high purity copper fiber surface using polishing method, prepares low surface
The copper fiber of roughness;
Second step prepares copper/graphene composite fibre, high-purity copper fiber is placed in chemical vapor deposition tube furnace, is passed through
Chemical vapor deposition grows graphene, to obtain copper/graphene composite fibre on copper fiber surface;
Third walks, and prepares copper/graphene/polymer multi-layer composite fibre, takes infiltrated with molten metal method, utilizes traction machine travel second
Copper/graphene bundle of composite fibers obtained makes composite fibre by the mold of the thermoplastic polymer materials containing melting in step
Beam is extracted out after obtaining good infiltration, prepares copper/graphene/polymer multi-layer composite fibre.
Further, for high-purity copper fiber in the first step after the polishing treatment of surface, surface roughness reduces by 10
Times or more.
Still further, the polishing method in the first step is electrochemical polishing method.
As preferred embodiment, graphene is grown on copper fiber surface using chemical vapor deposition in the second step
During, using methane gas as carbon source, hydrogen is during which passed through into tube furnace;And in copper/graphene composite fibre cooling
When, argon gas and hydrogen are passed through into tube furnace.
Further, the graphene growth time in the second step is 40min, growth pressure 80Pa.
Further, the high polymer is polypropylene, polyethylene, polystyrene, makrolon, acrylonitrile-styrene-fourth
Diene copolymers, polyamide, polybutylene terephthalate, polyethylene terephthalate, polyphenylene oxide, polyphenylene sulfide, hard are poly-
Vinyl chloride, polymethyl methacrylate, polyformaldehyde, polysulfones, polyimides, polytetrafluoroethylene (PTFE), polytrifluorochloroethylene, perfluoroethylene
The modified product of propylene, polybutylene terephthalate, chlorinated polyether or above-mentioned high polymer.
Further, the bundle of composite fibers for the package high polymer extracted out after infiltration is immersed in the third step cold in sink
But, composite fibre after cooling is at the uniform velocity wound on reel;By 60 ~ 120 DEG C in an oven of the composite fibre of winding after coiling
Dry 8 hours or more, it is put into the dry container of guarantor and preserves.
The present invention compared with prior art, the preparation side of new copper/graphene of the invention/polymer composite fibrous
Method, process conditions are simple, and flow is easy to control, and gained composite fibre quality is higher, high yield rate;Graphene is on copper fiber surface
Be not in the agglomeration of graphene, therefore graphene is evenly distributed on copper fiber surface during growth;It is coated on copper
The graphene number of plies of fiber surface is few, and defect is few, can give full play to graphene excellent electricity and mechanical property, therefore compound
The electric conductivity and mechanical property of fiber improve a lot, including conductivity, intensity, elasticity, fatigue resistance, the property such as corrosion-resistant
Energy;Infiltration can further increase the flexibility and fatigue resistance of composite fibre in the polymeric layer of fiber surface, assign simultaneously
The insulating properties of fiber surface is given, and not corroded by the external world for internal structure can be protected, improves corrosion resistance, extends working life;
The structure of MULTILAYER COMPOSITE has given full play to the characteristics of layers of material performance, ensure that conductive fiber can normal work in the presence of a harsh environment
Make, special equipment higher especially suitable for performance requirement and complicated working environment can be widely applied to electronic product, electricity
Device, Communication Equipment, safety equipment, information are transmitted and the civil and militaries product scopes such as safety.
Description of the drawings
Fig. 1 is the process flow chart of the present invention.
Fig. 2 is copper/graphene/polymer composite fibrous microstructure schematic diagram of the present invention.
Each component is labeled as in attached drawing:1- copper fibers, 2- graphene layers, 3- polymeric layers.
Specific implementation mode
The preparation method of new copper/graphene as shown in Figure 1/polymer composite fibrous, includes the following steps:
The first step prepares the copper fiber of low surface roughness, handles high purity copper fiber surface using polishing method, prepares low surface
The copper fiber of roughness;
High-purity copper fiber is polished in electrobrightening equipment, 5 μm of copper fiber diameter, electrobrightening power supply two-phase
220V selects silicon controlled rectifier (SCR), and quartz ampoule heating, titanium hanger, high-purity copper fiber is after the polishing treatment of surface, rough surface
Degree reduces by 10 times or more;
Second step, prepares copper/graphene composite fibre, and high-purity copper fiber is placed in chemical vapor deposition(CVD)In tube furnace,
By chemical vapor deposition, graphene is grown on copper fiber surface, to obtain copper/graphene composite fibre;
(1)Copper fiber after polishing is positioned in CVD tube furnaces, graphene layer is grown on copper fiber surface using CVD method,
Wherein 1000 DEG C of growth temperature, carbon source is methane(CH4)Gas, argon gas(Ar)As current-carrying gas, hydrogen(H2)For protecting
With raising graphene quality, intrinsic standoff ratio p (CH4):p(H2)=1:10,80 Pa of graphene growth pressure, growth time 40 minutes;
(2)The composite fibre that surface is grown to graphene is cooled to room temperature in CVD tube furnaces, during which keeps being passed through Ar and H2;
Third walks, and prepares copper/graphene/polymer multi-layer composite fibre, takes infiltrated with molten metal method, utilizes traction machine travel second
Copper/graphene bundle of composite fibers obtained makes composite fibre by the mold of the thermoplastic polymer materials containing melting in step
Beam is extracted out after obtaining good infiltration, prepares copper/graphene/polymer multi-layer composite fibre, as shown in Figure 2;
(1)It is pure high poly- by containing molten with copper/graphene fiber beam prepared by traction machine travel using infiltrated with molten metal method
Object material or its polymer-modified impregnation mold, 120 ~ 300 DEG C of mould temperature make bundle of composite fibers obtain good infiltration;
(2)The composite fibre of package high polymer that will be after infiltration immerse it is cooling in sink, by fiber after cooling at the uniform velocity winding
It places;
(3)The composite fibre of preparation is dried 8 hours or more for 60 ~ 120 DEG C in an oven, is put into protect in dry container and preserves.
Wherein, the high polymer is polypropylene, polyethylene, polystyrene, makrolon, acrylonitrile-styrene-butadiene
Copolymer, polyamide, polybutylene terephthalate, polyethylene terephthalate, polyphenylene oxide, polyphenylene sulfide, hard polychlorostyrene second
Alkene, polymethyl methacrylate, polyformaldehyde, polysulfones, polyimides, polytetrafluoroethylene (PTFE), polytrifluorochloroethylene, perfluoroethylene third
The modified product of alkene, polybutylene terephthalate, chlorinated polyether or above-mentioned high polymer.
Above-described embodiment is only the better embodiment of the present invention, therefore all structures according to described in present patent application range
It makes, the equivalent change or modification that feature and principle are done, is included within the scope of present patent application.
Claims (7)
1. a kind of new copper/graphene/polymer composite fibrous preparation method, which is characterized in that include the following steps:
The first step prepares the copper fiber of low surface roughness, handles high purity copper fiber surface using polishing method, prepares low surface
The copper fiber of roughness;
Second step prepares copper/graphene composite fibre, high-purity copper fiber is placed in chemical vapor deposition tube furnace, is passed through
Chemical vapor deposition grows graphene, to obtain copper/graphene composite fibre on copper fiber surface;
Third walks, and prepares copper/graphene/polymer multi-layer composite fibre, takes infiltrated with molten metal method, utilizes traction machine travel second
Copper/graphene bundle of composite fibers obtained makes composite fibre by the mold of the thermoplastic polymer materials containing melting in step
Beam is extracted out after obtaining good infiltration, prepares copper/graphene/polymer multi-layer composite fibre.
2. new copper/graphene according to claim 1/polymer composite fibrous preparation method, it is characterised in that:Institute
High-purity copper fiber in the first step is stated after the polishing treatment of surface, surface roughness reduces by 10 times or more.
3. new copper/graphene according to claim 1/polymer composite fibrous preparation method, it is characterised in that:Institute
It is electrochemical polishing method to state the polishing method in the first step.
4. new copper/graphene according to claim 1/polymer composite fibrous preparation method, it is characterised in that:Institute
It states in second step using chemical vapor deposition during copper fiber surface grows graphene, using methane gas as carbon source,
Period is passed through hydrogen into tube furnace;And in copper/graphene composite fibre cooling, argon gas and hydrogen are passed through into tube furnace.
5. new copper/graphene according to claim 1 or 4/polymer composite fibrous preparation method, feature exists
In:The graphene growth time in the second step is 40min, growth pressure 80Pa.
6. new copper/graphene according to claim 1/polymer composite fibrous preparation method, it is characterised in that:Institute
State high polymer be polypropylene, polyethylene, polystyrene, makrolon, acrylonitrile-butadiene-styrene copolymer, polyamide,
Polybutylene terephthalate, polyethylene terephthalate, polyphenylene oxide, polyphenylene sulfide, Hard PVC, polymethylacrylic acid
Methyl esters, polyformaldehyde, polysulfones, polyimides, polytetrafluoroethylene (PTFE), polytrifluorochloroethylene, perfluoroethylene-propylene, poly terephthalic acid fourth
The modified product of diester, chlorinated polyether or above-mentioned high polymer.
7. new copper/graphene according to claim 1/polymer composite fibrous preparation method, it is characterised in that:Institute
It states and the bundle of composite fibers for the package high polymer extracted out after infiltration is immersed to cooling in sink, composite fibre after cooling in third step
At the uniform velocity it is wound on reel;The composite fibre of winding is dried 8 hours or more for 60 ~ 120 DEG C in an oven after coiling, it is dry to be put into guarantor
It is preserved in container.
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