CN105908493A - Metal modified carbon fiber, preparation method and application thereof - Google Patents
Metal modified carbon fiber, preparation method and application thereof Download PDFInfo
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- CN105908493A CN105908493A CN201610248248.9A CN201610248248A CN105908493A CN 105908493 A CN105908493 A CN 105908493A CN 201610248248 A CN201610248248 A CN 201610248248A CN 105908493 A CN105908493 A CN 105908493A
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/20—Electroplating: Baths therefor from solutions of iron
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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
- C25D3/00—Electroplating: Baths therefor
- C25D3/02—Electroplating: Baths therefor from solutions
- C25D3/56—Electroplating: Baths therefor from solutions of alloys
- C25D3/562—Electroplating: Baths therefor from solutions of alloys containing more than 50% by weight of iron or nickel or cobalt
-
- 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
- C25D5/10—Electroplating with more than one layer of the same or of different metals
- C25D5/12—Electroplating with more than one layer of the same or of different metals at least one layer being of nickel or chromium
-
- 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
Abstract
The invention discloses a metal modified carbon fiber, a preparation method and an application thereof and belongs to the technical fields of electromagnetic shielding and electroplating. The surface of the metal modified carbon fiber is provided with a double magnetic layer comprising an iron layer and an iron-cobalt-nickel layer, wherein the double magnetic layer is high in iron content, so that the metal modified carbon fiber is high in magnetic permeability and is strong in electromagnetic interference absorption capability. An electromagnetic shield material prepared from the metal modified carbon fiber has excellent magnetic permeability and electric conductivity and is suitable for a wide-frequency-band electromagnetic shield material. The material is also improved in anti-oxidizing and anti-chemical-corrosion properties and is durable. Through a two-step electroplating process, the iron metal layer and the iron-cobalt-nickel alloy layer are plated onto the surface of the carbon fiber. The preparation method is simple and is easy to carry out, and can achieve continuous production of the modified carbon fiber. The content of magnetic component in the plated layer is easy to control. The bonding force of the plated layer and the carbon fiber substrate is increased. The modified carbon fiber is suitable for being promoted in the field of wide-frequency-band electromagnetic shielding.
Description
Technical field
The present invention relates to a kind of metal-modified carbon fiber, also relate to the preparation method and application of this metal-modified carbon fiber,
Belong to electromagnetic shielding and electroplating technology field.
Background technology
In electronics, the epoch of microelectronics high speed development, Contamination of Electromagnetic Wave make electromagnetic shielding material become indispensable in life,
The material that can not be substituted.Comparing traditional metal shield materials, carbon fiber has light weight, high ratio modulus, endurance, high-strength
The advantages such as degree, high conductivity, will be combined with resin matrix after carbon fiber surface metalized modified, the composite proportion made
Little, shield effectiveness good, have broad application prospects in electromagnetic shielding field.
At present, the method for material surface metalized modified includes galvanoplastic, electroless plating method, ion sputtering process, vacuum vapour deposition
Deng, wherein galvanoplastic, electroless plating method are used equally to carbon fiber surface modification, especially galvanoplastic, and production efficiency is high, technique
Stable and little to carrying capacity of environment.Studies have reported that, can obviously improve the electric conductivity of material in carbon fiber surface nickel plating, and
Strengthen the electromagnetic wave shielding of composite.
The patent of invention of publication No. CN103806042A discloses a kind of method at carbon fiber surface electroplating iron-nickel alloy, bag
Include: electroplate liquid (is included the component of following mass fraction: NiSO4·6H2O 60～90 parts, NiCl2·6H2O 10～30 parts,
FeSO4·7H2O 60～80 parts, C6H5Na3O7·2H2O 15～20 parts, C7H5NO3S 1～3 parts, H3BO310～30 parts,
PH 3～4.5) it is warming up to 50～70 DEG C and is incubated, carbon fiber bundle removes photoresist after aoxidizing and is connected into circuit as negative electrode, and nickel plate is as sun
Pole, adjusting cathode and anode distance is 5～15cm, regulation D.C. regulated power supply, holding voltage 0.5～3V, electric current 50～300mA,
At carbon fiber bundle electroplating surface iron-nickel alloy 5～60min, carbon fiber surface 2～3 times are cleaned in plating after terminating, then at 30～80 DEG C
It is dried 4～10h under vacuum, to obtain final product.The method technique is simple, workable, can realize production continuously, and ferrum nickel closes
Gold is strong with the adhesion of matrix, and thickness of coating, composition, magnetic etc. are the most adjustable, but the electromagnetic shielding of gained modified carbon fiber
Performance still has much room for improvement.
Summary of the invention
It is an object of the invention to provide a kind of metal-modified carbon fiber, by being coated with ferrous metal layer and ferrum continuously at carbon fiber surface
Cobalt-nickel alloy layer, can obtain the magnetosphere of high Fe content, on the one hand improves permeability and the electric conductivity of material, on the other hand carries
The non-oxidizability of high material and resistance to chemical corrosion.
Meanwhile, the present invention also provides for the preparation method of a kind of metal-modified carbon fiber.
Finally, the present invention reoffers the application of a kind of metal-modified carbon fiber.
In order to realize object above, the technical solution adopted in the present invention is:
Metal-modified carbon fiber, is sequentially provided with ferrous metal layer and iron cobalt nickel alloy layer at carbon fiber surface.
The thickness of described ferrous metal layer is 2～5nm, and the thickness of iron cobalt nickel alloy layer is 5～15nm, ferrum in alloy-layer, cobalt,
The mass ratio of nickel is 10～30:6～15:50～70.
The preparation method of metal-modified carbon fiber, comprises the following steps: carbon fiber bundle removes photoresist and is connected into as negative electrode after oxidation processes
Circuit, nickel plate, as anode, is first coated with ferrous metal layer in iron content electroplate liquid A, then in iron content, cobalt, nickel plating solution B
It is coated with iron cobalt nickel alloy layer, electroplates complete cleaning, be dried, to obtain final product.
Described oxidation processes of removing photoresist is: in air atmosphere, carbon fiber bundle is calcination 30～90min at temperature 400～550 DEG C, cold
But.
Described electroplate liquid A is made up of the component of following mass fraction: FeCl290～110 parts, C6H5Na3O7·2H2O 15～20
Part, C7H5NO3S 1～3 parts, H3BO310～30 parts, KCl 10～20 parts, water 500～1000 parts；Natural pH under room temperature
Value 3～4.5.
Described electroplate liquid B is made up of the component of following mass fraction: FeCl290～110 parts, NiSO4·6H2O 60～80 parts,
CoSO4·7H2O 15～30 parts, C6H5Na3O7·2H2O 10～15 parts, C7H5NO3S 1～3 parts, H3BO315～25 parts,
KCl 10～20 parts, water 500～1000 parts；Natural ph 3.5～4.7 under room temperature.
The condition of described plating is: cathode and anode distance 5～12cm, DC voltage 1～3V, electric current 50～200mA, plating
Time 5～30min.
Described dry condition is: be vacuum dried 4～8h at temperature 60～100 DEG C.
The application of metal-modified carbon fiber, the application in electromagnetic shielding material of the most metal-modified carbon fiber.
Beneficial effects of the present invention:
In the present invention, metal-modified carbon fiber surface has the ferrum of high Fe content, ferrum-cobalt-nickel two-layer magnetic layer, and permeability is high,
Absorption electromagnetic interference capability is strong, and the electromagnetic shielding material thus prepared has good permeability and electric conductivity, it is adaptable to wideband
Section electromagnetic shielding material, and the non-oxidizability of material and resistance to chemical corrosion improve, durable in use.
The present invention uses two step electroplating technologies to be coated with ferrous metal layer and iron cobalt nickel alloy layer at carbon fiber surface, and technique is simple, behaviour
Make simplicity, the continuous prodution of modified carbon fiber can be realized, and in coating, magnetic components content is easily controllable, coating and carbon
The adhesion of fibrous matrix increases, and is conducive to being widely popularized in wide-band electromagnetic shielding field.
Accompanying drawing explanation
Fig. 1 is electroplanting device structural representation in embodiment；
Fig. 2 is the scanning electron microscope (SEM) photograph of metal-modified carbon fiber surface coating in embodiment 1；
Fig. 3 is the scanning electron microscope (SEM) photograph of metal-modified carbon fiber surface coating in embodiment 2；
Fig. 4 is the scanning electron microscope (SEM) photograph of metal-modified carbon fiber surface coating in embodiment 3.
Detailed description of the invention
The present invention is only described in further detail by following embodiment, but does not constitute any limitation of the invention.
Embodiment 1
In the present embodiment, the preparation process of metal-modified carbon fiber is as follows:
1) remove photoresist oxidation processes
Carbon fiber bundle is placed in Muffle furnace, in air atmosphere, controls 8 DEG C/min of heating rate, treat that temperature rises to 450 DEG C of guarantors
Temperature 60min, insulation terminates, and is down to room temperature with stove, standby；
2) preparation electroplate liquid A, B
In terms of mass fraction, by 90 parts of FeCl2, 15 parts of C6H5Na3O7·2H2O, 1 part of C7H5NO3S, 10 parts of H3BO3
Being dissolved in 500 parts of ultra-pure waters with 10 parts of KCl, stir under room temperature, solution natural ph is 3, obtains electroplate liquid
A；
In terms of mass fraction, by 90 parts of FeCl2, 10 parts of C6H5Na3O7·2H2O, 1 part of C7H5NO3S, 15 parts of H3BO3、
10 parts of KCl, 60 parts of NiSO4·6H2O and 15 parts of CoSO4·7H2O is dissolved in 500 parts of ultra-pure waters, stirs under room temperature
Uniformly, solution natural ph is 4.2, obtains electroplate liquid B；
3) ferrous metal layer and iron-cobalt-nickel metal level it are coated with
Electroplate liquid A is placed in 65 DEG C of water-baths (electroplanting device structural representation is shown in Fig. 1, in figure 1～6 be followed successively by electroplate liquid,
Water, coating bath, by plating object, temperature controlled water bath pot and D.C. regulated power supply), cross 30min after temperature stabilization, after processing
Carbon fiber bundle be connected into circuit as negative electrode, nickel plate is as anode, and even after good circuit, adjusting cathode and anode distance is 5cm,
Regulation D.C. regulated power supply, keeps voltage 1.0V, electric current 100mA, cleans carbon fiber with deionized water after plating 15min
3 times, surface, standby；
Being placed in by electroplate liquid B in 65 DEG C of water-baths, 30min excessively, after temperature stabilization, will be coated with the carbon fiber of ferrous metal layer
Shu Zuowei negative electrode is connected into circuit, and nickel plate is as anode, and even after good circuit, adjusting cathode and anode distance is 10cm, regulates direct current
Regulated power supply, keeps voltage 2.0V, electric current 100mA, cleans carbon fiber surface 3 times with deionized water after plating 15min,
It is placed in again in 80 DEG C of vacuum drying ovens and is dried 6h, to obtain final product.
In the present embodiment, the thickness of metal-modified carbon fiber surface ferrous metal layer is 3.0nm, and the thickness of iron cobalt nickel alloy layer is
6.0nm.Coating scanning electron microscope (SEM) photograph is shown in Fig. 2.
Embodiment 2
In the present embodiment, the preparation process of metal-modified carbon fiber is as follows:
1) remove photoresist oxidation processes
Carbon fiber bundle is placed in Muffle furnace, in air atmosphere, controls 8 DEG C/min of heating rate, treat that temperature rises to 400 DEG C of guarantors
Temperature 60min, insulation terminates, and is down to room temperature with stove, standby；
2) preparation electroplate liquid A, B
In terms of mass fraction, by 100 parts of FeCl2, 18 parts of C6H5Na3O7·2H2O, 2 parts of C7H5NO3S, 20 parts of H3BO3
Being dissolved in 500 parts of ultra-pure waters with 18 parts of KCl, stir under room temperature, solution natural ph is 3.5, is electroplated
Liquid A；
In terms of mass fraction, by 100 parts of FeCl2, 12 parts of C6H5Na3O7·2H2O, 2 parts of C7H5NO3S, 20 parts of H3BO3、
18 parts of KCl, 70 parts of NiSO4·6H2O and 20 parts of CoSO4·7H2O is dissolved in 500 parts of ultra-pure waters, stirs under room temperature
Uniformly, solution natural ph is 4.0, obtains electroplate liquid B；
3) ferrous metal layer and iron-cobalt-nickel metal level it are coated with
Being placed in by electroplate liquid A (electroplanting device is with embodiment 1) in 65 DEG C of water-baths, 30min excessively, will after temperature stabilization
Carbon fiber bundle after process is connected into circuit as negative electrode, and nickel plate is as anode, and even after good circuit, adjusting cathode and anode distance is
10cm, regulates D.C. regulated power supply, keeps voltage 2.2V, electric current 180mA, cleans with deionized water after plating 10min
Carbon fiber surface 5 times, standby；
Being placed in by electroplate liquid B in 65 DEG C of water-baths, 30min excessively, after temperature stabilization, will be coated with the carbon fiber of ferrous metal layer
Shu Zuowei negative electrode is connected into circuit, and nickel plate is as anode, and even after good circuit, adjusting cathode and anode distance is 10cm, regulates direct current
Regulated power supply, keeps voltage 2.2V, electric current 180mA, cleans carbon fiber surface 5 times with deionized water after plating 10min,
It is placed in again in 80 DEG C of vacuum drying ovens and is dried 6h, to obtain final product.
In the present embodiment, the thickness of metal-modified carbon fiber surface ferrous metal layer is 3.5nm, and the thickness of iron cobalt nickel alloy layer is
6.0nm.Coating scanning electron microscope (SEM) photograph is shown in Fig. 3.
Embodiment 3
In the present embodiment, the preparation process of metal-modified carbon fiber is as follows:
1) remove photoresist oxidation processes
Carbon fiber bundle is placed in Muffle furnace, in air atmosphere, controls 10 DEG C/min of heating rate, treat that temperature rises to 450 DEG C
Insulation 60min, insulation terminates, and is down to room temperature with stove, standby；
2) preparation electroplate liquid A, B
In terms of mass fraction, by 110 parts of FeCl2, 20 parts of C6H5Na3O7·2H2O, 3 parts of C7H5NO3S, 30 parts of H3BO3
Being dissolved in 500 parts of ultra-pure waters with 20 parts of KCl, stir under room temperature, solution natural ph is 4.2, is electroplated
Liquid A；
In terms of mass fraction, by 110 parts of FeCl2, 15 parts of C6H5Na3O7·2H2O, 3 parts of C7H5NO3S, 25 parts of H3BO3、
20 parts of KCl, 80 parts of NiSO4·6H2O and 30 parts of CoSO4·7H2O is dissolved in 500 parts of ultra-pure waters, stirs under room temperature
Uniformly, controlling solution ph is 3.5, obtains electroplate liquid B；
3) ferrous metal layer and iron-cobalt-nickel metal level it are coated with
Being placed in by electroplate liquid A (electroplanting device is with embodiment 1) in 65 DEG C of water-baths, 30min excessively, will after temperature stabilization
Carbon fiber bundle after process is connected into circuit as negative electrode, and nickel plate is as anode, and even after good circuit, adjusting cathode and anode distance is
10cm, regulates D.C. regulated power supply, keeps voltage 2.2V, electric current 180mA, cleans with deionized water after plating 15min
Carbon fiber surface 3 times, standby；
Being placed in by electroplate liquid B in 65 DEG C of water-baths, 30min excessively, after temperature stabilization, will be coated with the carbon fiber of ferrous metal layer
Shu Zuowei negative electrode is connected into circuit, and nickel plate is as anode, and after perfecting circuit, adjusting cathode and anode distance is 10cm, regulates direct current
Regulated power supply, keeps voltage 2.2V, electric current 180mA, cleans carbon fiber surface 3 times with deionized water after plating 15min,
It is placed in again in 80 DEG C of vacuum drying ovens and is dried 6h, to obtain final product.
In the present embodiment, the thickness of metal-modified carbon fiber surface ferrous metal layer is 3.5nm, and the thickness of iron cobalt nickel alloy layer is
7.5nm.Coating scanning electron microscope (SEM) photograph is shown in Fig. 4.
Comparative example
In this comparative example, the preparation process of ferro-nickel modified carbon fiber is with embodiment 2 in patent CN103806042A.
Test example
1, each metal element content analysis in coating
Metal-modified carbon fiber in Example 1～3, analyzes ferrum, cobalt, the content of nickel element in coating, and result see table 1.
The content of each metallic element in table 1 coating
2, the soft magnetic characteristic of carbon fiber surface coating measures
Metal-modified carbon fiber in Example 1～3, measures the saturation magnetization of material and maximum coercivity, and result sees below
Table 2.
The soft magnetic characteristic measurement result of table 2 carbon fiber surface coating
Claims (10)
- The most metal-modified carbon fiber, it is characterised in that: it is sequentially provided with ferrous metal layer and iron cobalt nickel alloy layer at carbon fiber surface.
- Metal-modified carbon fiber the most according to claim 1, it is characterised in that: ferrum in described iron cobalt nickel alloy layer, Cobalt, the mass ratio of nickel are 10～30:6～15:50～70.
- Metal-modified carbon fiber the most according to claim 1 and 2, it is characterised in that: the thickness of described ferrous metal layer Being 2～5nm, the thickness of iron cobalt nickel alloy layer is 5～15nm.
- 4. the preparation method of metal-modified carbon fiber as according to any one of claims 1 to 3, it is characterised in that: include with Lower step: carbon fiber bundle removes photoresist and is connected into circuit as negative electrode after oxidation processes, nickel plate is as anode, first at iron content electroplate liquid A In be coated with ferrous metal layer, then be coated with iron cobalt nickel alloy layer in iron content, cobalt, nickel plating solution B, electroplate complete cleaning, be dried, Obtain.
- Preparation method the most according to claim 4, it is characterised in that oxidation processes of removing photoresist described in: is: air atmosphere In, carbon fiber bundle is calcination 30～90min at temperature 400～550 DEG C, cooling.
- Preparation method the most according to claim 4, it is characterised in that: described electroplate liquid A is by following mass fraction Component forms: FeCl290～110 parts, C6H5Na3O7·2H2O 15～20 parts, C7H5NO3S 1～3 parts, H3BO310～30 Part, KCl 10～20 parts, water 500～1000 parts.
- Preparation method the most according to claim 4, it is characterised in that: described electroplate liquid B is by following mass fraction Component forms: FeCl290～110 parts, NiSO4·6H2O 60～80 parts, CoSO4·7H2O 15～30 parts, C6H5Na3O7·2H2O 10～15 parts, C7H5NO3S 1～3 parts, H3BO315～25 parts, KCl 10～20 parts, water 500～1000 parts.
- Preparation method the most according to claim 4, it is characterised in that: the condition of described plating is: gap between cathode and anode From 5～12cm, DC voltage 1～3V, electric current 50～200mA, electroplating time 5～30min.
- Preparation method the most according to claim 4, it is characterised in that: described dry condition is: temperature 60～100 DEG C Lower vacuum drying 4～8h.
- 10. metal-modified carbon fiber application in electromagnetic shielding material as according to any one of claims 1 to 3.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114622400A (en) * | 2022-04-12 | 2022-06-14 | 武汉纺织大学 | Surface modification method for enhancing oxidation resistance and electric heating performance of carbon fiber |
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Application publication date: 20160831 |