CN106702732A - Graphene-copper composite fiber and preparation method thereof - Google Patents
Graphene-copper composite fiber and preparation method thereof Download PDFInfo
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- CN106702732A CN106702732A CN201611220124.6A CN201611220124A CN106702732A CN 106702732 A CN106702732 A CN 106702732A CN 201611220124 A CN201611220124 A CN 201611220124A CN 106702732 A CN106702732 A CN 106702732A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—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
- D06M11/83—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 metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D7/00—Electroplating characterised by the article coated
- C25D7/06—Wires; Strips; Foils
- C25D7/0607—Wires
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/40—Fibres of carbon
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- Inorganic Fibers (AREA)
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Abstract
The invention discloses a graphene-copper composite fiber and a preparation method thereof. The method comprises the steps of firstly preparing a graphene oxide fiber of which the diameter is 1-50 microns by adopting a wet spinning method, and then putting the graphene oxide fiber into a high-temperature furnace for heating and reducing to obtain a continuous pure graphene fiber. Due to a special treatment mode, the fiber surface is provided with multi-stage wrinkles, the pure graphene fiber is fixed on a negative electrode of a plating bath for electroplating, and a copper layer has an extension structure embedded into the wrinkles. Graphene is tightly combined with copper crystals, a hole defect is avoided, the electrical properties of the material are greatly improved, the fiber is stable in structure and constant in electric conductivity after being bent for 100 times.
Description
Technical field
The present invention relates to a kind of novel graphite alkene metallic composite, particularly a kind of Graphene-copper composite fibre and its
Preparation method.
Background technology
Metallic copper is very proper with our daily life, possesses widely in the field such as new industry and electric power energy
Application potential, relative to other metal materials, it shows more excellent electric conductivity, thermal conductivity and ductility.In order to improve copper
Application value, the method for generally using at present is that its carbon material good with more tough and electric conductivity is made into composite
Make the reduction of its specific conductivity, carbon material such as graphite and CNT have preferable pliability, so the composite made
Its processing characteristics and performance will not be significantly affected while reduces cost.
Relative to graphite and CNT, Graphene has more excellent electric conductivity and more preferably pliability, therefore more
It is adapted to make composite with copper.Copper facing mainly has two kinds of paths of chemical plating and plating, relative to chemical plating, electroplates more environmentally-friendly
Clean and easy to operate, therefore realize that electro-coppering is a kind of ideal method on Graphene in the way of electroplating.
However, being different from other carbon materials, there is super lubrication, adhesive force therebetween between Graphene and metal
Very weak, this brings huge challenge to grapheme material directly electroplating on surface copper.
The content of the invention
For problem above, the invention provides a kind of economical and effective, and a kind of Graphene-copper of energy large-scale application is multiple
Condensating fiber and preparation method thereof, composite fibre good stability obtained in the method, density is low, and conductance is high, and pliability is good.
The purpose of the present invention is achieved through the following technical solutions：A kind of Graphene-copper composite fibre, the compound fibre
Tie up and be made up of the layers of copper of pure graphene fiber and the pure graphene fiber of cladding；The pure graphene fiber surface has fold,
Layers of copper has the extended structure for being embedded in fold.
Further, the width of the fold is 20 nanometers to 5 microns.
A kind of preparation method of Graphene-copper composite fibre, its preparation process is as follows：
(1) graphene oxide fiber (a diameter of 1-50 microns) is prepared using the method for wet spinning；
(2) graphene oxide fiber is placed on again and reduction is heated in high temperature furnace, temperature is 800-3000 DEG C, and the recovery time is
1-24 hours, obtain pure graphene fiber.
(3) negative pole that pure graphene fiber is fixed on electroplating bath is electroplated, electroplating bath just extremely copper rod applies with electricity
Pressure value is the DC voltage of 0.1-20V, after being electroplated 2-120 seconds in electroplate liquid, takes out fiber, and fiber table is washed with deionized water
The electroplate liquid in face, dries in vacuum drying oven, obtains Graphene-copper composite fibre.The electroplate liquid composition is as follows：Copper sulphate
Concentration is 50-160g/L, and the volumetric concentration of the sulfuric acid of 98wt% is 3-10mL/L, and it is 0.5-2mL/L that surfactant Qula is led to.
Further, in the step 1, the spinning solution of wet spinning is：Piece diameter is 1-50 microns of oxidation stone
Dispersion liquid of the black alkene in dimethylformamide, the concentration of graphene oxide is 1~10mg/mL；The internal diameter of spinning pipeline is 60-
500 microns；Coagulating bath is that (the two volume ratio is 1 for the mixed solution of ethyl acetate and dichloromethane：1-50：1) it is, outer during receipts silk
Boundary's heating-up temperature is 80-200 DEG C.
Further, in the step 3, when voltage is 20V, required electroplating time is 2s.
Further, in the step 3, when voltage is 1V, required electroplating time is 13s.
The beneficial effects of the present invention are：Preparation process of the present invention is simple and safe controllable, and time consumption and energy consumption is few, raw material sources
Extensively.Because graphenic surface has many folds, metal copper layer can be made closely to be combined with graphene fiber surface, obtained
Complex structure of filament is fine and close, functional.
Brief description of the drawings
Fig. 1 is the structural representation of Graphene-copper composite fibre；
Fig. 2 is the graphenic surface multistage pleated structure figure under different multiplying；
Fig. 3 is the distribution of copper particle and growth conditions when Graphene-copper composite fibre is electroplated；
Fig. 4 is the XRD of Graphene-copper composite fibre；
Fig. 5 a, b, c are respectively the state that smooth graphenic surface plates metal.
Specific embodiment
As shown in figure 1, a kind of Graphene-copper composite fibre, the composite fibre is by a diameter of 1-50 microns pure graphite
The layers of copper composition of alkene fiber and the pure graphene fiber of cladding；The pure graphene fiber surface has fold, and layers of copper has embedding
Enter the extended structure of fold.The good physical property of fiber is combined closely from layers of copper and graphene fiber surface, solution
Determine and the problem of plating modification has been difficult between Graphene and metallic particles.On the one hand the fibre structure stabilization for obtaining, such as can be with
Bend 100 conductances constant；On the other hand, two kinds of material tights are combined, and are not in hole defect, substantially increase material
The electric property of material.
As shown in Fig. 2 the width of the fold is 20 nanometers to 5 microns.After tested, obtained copper-plated graphite alkene cebollite
Black alkene bulk density is 1.8-5.8g/cm3, Graphene mass fraction is 10-80%, and the mass fraction of copper is 20-90%, fiber
Conductance be 1.1 × 105S/m–3.5×107S/m。
As shown in figure 3, in the plating starting stage, due to graphene fiber surface irregularity, electronics is in radius of curvature ratio
Larger plication region aggregation, the crystal grain of copper preferentially in nucleation herein and apposition growth, with the carrying out of plating, gradually give birth to by particle
Long, particle becomes big, and the crack being crimped is fixed, and further, copper crystal grain is along fold homoepitaxial and mutually fusion is until paving
Full whole fiber surface, this growth pattern from inside to outside ensures final coating energy uniform fold in fiber surface and stabilization
Attachment.On the one hand the fibre structure stabilization for obtaining, such as can bend 100 conductances constant；On the other hand, two kinds of materials
Combine closely, be not in hole defect, substantially increase the electric property of material.With reference to embodiment the present invention is made into
One step explanation.
Embodiment 1
A kind of method that galvanoplastic prepare Graphene and copper composite fibre, including procedure below：
(1) a diameter of 5 microns of graphene oxide fiber is prepared using the method for wet spinning, specially：Wet spinning
Spinning solution be：Piece diameter is the dispersion liquid of 5 microns of graphene oxide (on carbon paddy wish) in dimethylformamide, oxygen
The concentration of graphite alkene is 10mg/mL；The internal diameter of spinneret is 100 microns；Coagulating bath is the mixed of ethyl acetate and dichloromethane
(the two volume ratio is 1 to close solution：1) extraneous heating-up temperature when, receiving silk is 200 DEG C.
(2) graphene oxide fiber is placed on and reduction is heated in high temperature furnace, temperature is 800 DEG C, after heating 1.5 hours, is obtained
To a diameter of 5 microns of graphene fiber.
(3) negative pole that graphene fiber is fixed on electroplating bath is electroplated, electroplating bath just extremely high purity copper rod, apply with
Magnitude of voltage is the DC voltage of 0.1V, and electroplate liquid is copper sulphate (160g/L), and the concentrated sulfuric acid (3mL/L) and Qula of 98wt% lead to
The mixed aqueous solution of (0.5mL/L), after electroplating 10 seconds, washes the electroplate liquid of fiber surface with water, 1 is dried in vacuum drying oven small
When.Because voltage is relatively low, the time is shorter, obtains coating and is about 3 microns.As shown in figure 4, XRD results show final compound fibre
There is the peak of obvious copper crystal in dimension table face.Initial collection of illustrative plates has the signal of cuprous ion, but is gone back completely by after hydrogen reducing
Original, and remain to keep good stability after the two weeks.After tested, its conductance is 7.3 × 105S/m。
Embodiment 2
A kind of method that galvanoplastic prepare Graphene and copper composite fibre, including procedure below,
(1) a diameter of 10 microns of graphene oxide fiber is prepared using the method for wet spinning, specially：Wet spinning
Spinning solution be：Piece diameter is the dispersion liquid of 5 microns of graphene oxide (on carbon paddy wish) in dimethylformamide, oxygen
The concentration of graphite alkene is 8mg/mL；The internal diameter of spinneret is 250 microns；Coagulating bath is the mixing of ethyl acetate and dichloromethane
(the two volume ratio is 10 to solution：1) extraneous heating-up temperature when, receiving silk is 80 DEG C.
(2) graphene oxide fiber is placed on again and reduction is heated in high temperature furnace, temperature is 2200 DEG C, after heating 3 hours, is obtained
To a diameter of 10 microns of graphene fiber；
(3) negative pole that graphene fiber is fixed on electroplating bath is electroplated, electroplating bath just extremely high purity copper rod, apply with
Magnitude of voltage is the DC voltage of 1V, and electroplate liquid is copper sulphate (100g/L), and the concentrated sulfuric acid (4mL/L) and Qula of 98wt% lead to
The mixed aqueous solution of (0.7mL/L), after electroplating 120 seconds, washes the electroplate liquid of fiber surface with water, and 9 are dried in vacuum drying oven
Hour.Obtain coating and be about 5 microns.After tested, its conductance is 1.5 × 107S/m。
Embodiment 3
A kind of method that galvanoplastic prepare Graphene and copper composite fibre, including procedure below：
(1) a diameter of 30 microns of graphene oxide fiber is prepared using the method for wet spinning, specially：Wet spinning
Spinning solution be：Piece diameter is the dispersion liquid of 50 microns of graphene oxide (on carbon paddy wish) in dimethylformamide,
The concentration of graphene oxide is 11mg/mL；The internal diameter of spinneret is 500 microns；Coagulating bath is ethyl acetate and dichloromethane
(the two volume ratio is 200 to mixed solution：1) extraneous heating-up temperature when, receiving silk is 100 DEG C.
(2) graphene oxide fiber is placed on again and reduction is heated in high temperature furnace, temperature is 3000 DEG C, after heating 1 hour, is obtained
To a diameter of 30 microns of graphene fiber.
(3) negative pole that graphene fiber is fixed on electroplating bath is electroplated, the just extremely pure copper rod of electroplating bath, apply with
Magnitude of voltage is the DC voltage of 20V, and electroplate liquid is copper sulphate (50g/L), and the concentrated sulfuric acid (10mL/L) and Qula of 98wt% lead to
The mixed aqueous solution of (2mL/L), after electroplating 2 seconds, washes the electroplate liquid of fiber surface with water, is dried 5 hours in vacuum drying oven.
Improve after supply voltage, the potential of fiber is raised, and is obtained coating and is about 8 microns.After tested, its conductance is 3.1 × 107S/
m。
Embodiment 4
The importance of the fold for metal plating of graphenic surface is verified using smooth graphenic surface, including it is following
Process：
(1) as shown in Figure 5 a, smooth graphene film is taken, is conventionally electroplated, the metal for obtaining is answered
Close film as shown in Figure 5 b, coating is relatively thin and very uneven.
(2) metallic graphite carbon alkene composite membrane is slightly rinsed in water, the result for obtaining as shown in Figure 5 c, shell completely by coating
Fall, show the adhesion and stability of extreme difference.
Claims (6)
1. a kind of Graphene-copper composite fibre, it is characterised in that the composite fibre is by pure graphene fiber and coats pure stone
The layers of copper composition of black alkene fiber；The pure graphene fiber surface has fold, and layers of copper has the extended structure for being embedded in fold.
2. Graphene according to claim 1-copper composite fibre, it is characterised in that the width of the fold is 20 nanometers
To 5 microns.
3. a kind of preparation method of the Graphene described in claim 1-copper composite fibre, it is characterised in that its preparation process
It is as follows：
(1) graphene oxide fiber (a diameter of 1-50 microns) is prepared using the method for wet spinning；
(2) graphene oxide fiber is placed on again and reduction is heated in high temperature furnace, obtain pure graphene fiber.
(3) negative pole that pure graphene fiber is fixed on electroplating bath is electroplated, electroplating bath just extremely copper rod applies with magnitude of voltage
It is the DC voltage of 0.1-20V, after being electroplated 2-120 seconds in electroplate liquid, takes out fiber, fiber surface is washed with deionized water
Electroplate liquid, dries in vacuum drying oven, obtains Graphene-copper composite fibre.The electroplate liquid composition is as follows：The concentration of copper sulphate
It is 50-160g/L, the volumetric concentration of the sulfuric acid of 98wt% is 3-10mL/L, and it is 0.5-2mL/L that surfactant Qula is led to.
4. method according to claim 3, it is characterised in that in the step 1, the spinning solution of wet spinning is：Piece is straight
The dispersion liquid that footpath size is 1-50 micron of graphene oxide in dimethylformamide, the concentration of graphene oxide is 1~
10mg/mL；The internal diameter of spinning pipeline is 60-500 microns；Coagulating bath is mixed solution (the two of ethyl acetate and dichloromethane
Volume ratio is 1：1-50：1) extraneous heating-up temperature when, receiving silk is 80-200 DEG C.
5. method according to claim 3, it is characterised in that in the step 3, when voltage is 20V, required electroplating time
It is 2s.
6. method according to claim 3, it is characterised in that in the step 3, when voltage is 1V, required electroplating time
It is 13s.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108707998A (en) * | 2018-04-11 | 2018-10-26 | 杭州牛墨科技有限公司 | Graphene fiber and graphene fiber non-woven fabrics of a kind of fold and preparation method thereof |
| CN109321951A (en) * | 2018-11-13 | 2019-02-12 | 辽宁工程技术大学 | A kind of preparation method of the high-strength high-conductivity copper based nano composite material based on plating |
| DE102018200236A1 (en) | 2018-01-09 | 2019-07-11 | Robert Bosch Gmbh | Process for producing graphene fibers, graphene fiber, yarn, electrical component and electrical conductor |
| CN110777411A (en) * | 2019-11-13 | 2020-02-11 | 中国科学院高能物理研究所 | Preparation method of graphene paper-metal composite material |
| WO2021004692A1 (en) * | 2019-07-10 | 2021-01-14 | Robert Bosch Gmbh | Method for producing graphene fibres |
| CN116377714A (en) * | 2023-05-23 | 2023-07-04 | 江苏欣晨雅新材料有限公司 | Composite graphene non-woven fabric, preparation method and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN109321951B (en) * | 2018-11-13 | 2019-10-29 | 辽宁工程技术大学 | A kind of preparation method of the high-strength high-conductivity copper based nano composite material based on plating |
| WO2021004692A1 (en) * | 2019-07-10 | 2021-01-14 | Robert Bosch Gmbh | Method for producing graphene fibres |
| US11939703B2 (en) | 2019-07-10 | 2024-03-26 | Robert Bosch Gmbh | Method for producing graphene fibres |
| CN110777411A (en) * | 2019-11-13 | 2020-02-11 | 中国科学院高能物理研究所 | Preparation method of graphene paper-metal composite material |
| CN116377714A (en) * | 2023-05-23 | 2023-07-04 | 江苏欣晨雅新材料有限公司 | Composite graphene non-woven fabric, preparation method and application thereof |
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Effective date of registration: 20190902 Address after: 313199 Room 830, 8th Floor, Changxing World Trade Building, 1278 Mingzhu Road, Changxing Economic Development Zone, Huzhou City, Zhejiang Province Patentee after: Changxin de Technology Co., Ltd. Address before: 310058 Xihu District, Zhejiang, Yuhang Tong Road, No. 866, No. Patentee before: Zhejiang University |