CN106521931A - Method for plating carbon nanotube fibers with nickel - Google Patents
Method for plating carbon nanotube fibers with nickel Download PDFInfo
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- CN106521931A CN106521931A CN201610716561.0A CN201610716561A CN106521931A CN 106521931 A CN106521931 A CN 106521931A CN 201610716561 A CN201610716561 A CN 201610716561A CN 106521931 A CN106521931 A CN 106521931A
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- tube fibre
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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
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/14—Metallic material, boron or silicon
- C23C14/18—Metallic material, boron or silicon on other inorganic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The invention provides a method for plating carbon nanotube fibers with nickel. The method comprises the following steps: S1, performing cleaning treatment on carbon nanotube fibers by using an acid solution; S2, preheating the carbon nanotube fibers at least cleaned in the step S1; S3, winding a wire winding frame with the carbon nanotube fibers preheated in the step S2, and placing the wire winding frame in a sputtering chamber, wherein the wire winding frame comprises a plurality of wire winding rods which are arranged at intervals, and gaps are formed between two adjacent turns of the carbon nanotube fibers; S4, sputtering and plating the carbon nanotube fibers which is wound on the wire winding frame by taking metal nickel as a target material at a predetermined temperature, wherein relative rotation exists between the target material and the wire winding frame. In the method, nickel particles deposit on the surfaces of the carbon nanotube fibers in a physical vapor deposition way, so that harmful gas or harmful liquid is prevented. Thus, the method provided by the invention is more environmentally-friendly.
Description
Technical field
The present invention relates to the preparation field of composite, in particular it relates to a kind of carry out nickel plating to carbon nano-tube fibre
Method.
Background technology
In the prior art, it is generally required that using the method for electrochemistry nickel plating on carbon nano-tube fibre plated nickel film.But,
During this method nickel plating, pollution is easily caused, also, nickel film is not very fine and close.
Therefore, how to carry out nickel plating in environmentally friendly manner and become present invention technology urgently to be resolved hurrily asking to carbon nano-tube fibre
Topic.
The content of the invention
It is an object of the invention to provide a kind of method to carbon nano-tube fibre plated film, the method can be in CNT
The surface of fiber forms the metal film of densification, and will not be to environment during plated film.
To achieve these goals, the present invention provides a kind of method to carbon nano-tube fibre nickel plating, including：
S1, cleaning treatment is carried out to the carbon nano-tube fibre using acid solution；
S2, the pre-heat treatment is carried out to the carbon nano-tube fibre at least through step S1；
S3, will be arranged on after the carbon nano-tube fibre of step S2 is wrapped on lacing stand in sputtering chamber, the wrapping wire
Frame includes multiple spaced wire winding rods, there is interval between adjacent two circles carbon nano-tube fibre；
S4, the carbon nano-tube fibre with metallic nickel as target at a predetermined temperature to being wrapped on the lacing stand splash
Plated film is penetrated, wherein, is existed between the target and the lacing stand and is relatively rotated.
Preferably, in step S4, the target is arranged on outside the lacing stand, and the lacing stand is around itself axle
Line is rotated, and arranges multiple targets, and multiple targets are arranged around the lacing stand.
Preferably, in step s 2, between 100 DEG C to 200 DEG C, preheating time is in 0.5h to 3h for the temperature of the pre-heat treatment
Between.
Preferably, methods described is additionally included in what is carried out between step S1 and step S2：
The carbon nano-tube fibre through step S1 is cleaned using sonic oscillation method, cleaning fluid includes ethanol.
Preferably, in step s 4, between 1h to 3h, the predetermined temperature is at 200 DEG C for magnetron sputtering duration
To between 400 DEG C.
Preferably, step S4 includes：
S41, respectively by the target and be wound with carbon nano-tube fibre lacing stand be arranged in the sputtering chamber after, it is right
The sputtering chamber carries out vacuumizing until the first preset air pressure；
S42, the sputtering chamber is carried out being heated to the predetermined temperature；
S43, unlatching radio-frequency power supply, and the unlatching duration of the radio-frequency power supply is between 1h to 2h.
Preferably, first preset air pressure is 10-2Pa to 10-1Between Pa.
Preferably, in step S42, the sputtering chamber is heated using the mode of sensing heating.
Preferably, the acid solution includes nitric acid of the concentration between 1mol/L to 5mol/L.
Preferably, the process time of step S1 is between 10min to 30min.
In method provided by the present invention, after step S1, the catalyst particles of the interior remaining of carbon nano-tube fibre
Grain is removed, and after step S2, the amorphous carbon in carbon nano-tube fibre is decomposed, so as to be conducive to nickel shot in step S4
Son is deposited on the surface of carbon nano-tube fibre.When carbon nano-tube fibre is arranged on lacing stand, as adjacent two circles carbon is received
There is gap between mitron fiber, therefore, being bombarded the nickel particles for producing by magnetron can be fine through adjacent two circles CNT
Gap between dimension reaches carbon nano-tube fibre not towards on the surface of target.Also, in step s 4, target and lacing stand it
Between exist and relatively rotate, such that it is able to guarantee that the carbon nano-tube fibre being wrapped on lacing stand can equably plated film.At this
In bright, nickel particles are deposited on the surface of carbon nano-tube fibre in the way of physical vapour deposition (PVD), will not produce pernicious gas or have
Evil liquid, therefore, method provided by the present invention is more environmentally-friendly.
Description of the drawings
Fig. 1 is the schematic diagram of lacing stand；
Fig. 2 is wound around the relative position schematic diagram between the lacing stand of carbon nano-tube fibre and target；
Fig. 3 is the top view of Fig. 2；
Fig. 4 is the scanned picture of the nanotube fibers that the present invention is used, and multiplication factor is 150 times；
Fig. 5 is the scanned picture of the nickel-plating carbon nanotube fiber that embodiment 1 is obtained, and multiplication factor is 500 times；
Fig. 6 is the scanned picture of the nickel-plating carbon nanotube fiber that embodiment 1 is obtained, and multiplication factor is 3500 times；
Fig. 7 is the scanned picture of the nickel-plating carbon nanotube fiber that embodiment 2 is obtained, and multiplication factor is 125 times；
Fig. 8 is the scanned picture of the nickel-plating carbon nanotube fiber that embodiment 2 is obtained, and multiplication factor is 472 times.
Description of reference numerals
100：Lacing stand 110：Wire winding rod
120：Rotating shaft 200：Carbon nano-tube fibre
300：Target
Specific embodiment
The specific embodiment of the present invention is described in detail below in conjunction with accompanying drawing.It should be appreciated that this place is retouched
The specific embodiment stated is merely to illustrate and explains the present invention, is not limited to the present invention.
The present invention provides a kind of method to carbon nano-tube fibre plated film, and wherein, methods described includes：
S1, cleaning treatment is carried out to the carbon nano-tube fibre using acid solution；
S2, the pre-heat treatment is carried out to the carbon nano-tube fibre at least through step S1；
S3, will be arranged on after the carbon nano-tube fibre 200 of step S2 is wrapped on lacing stand 100 in sputtering chamber, around
Guide frame 100 includes multiple spaced wire winding rods 110, there is interval between adjacent two circles carbon nano-tube fibre 200；
S4, with metallic nickel as target 300, the carbon nano-tube fibre 200 to being wrapped on lacing stand 100 at a predetermined temperature
Sputter coating is carried out, wherein, is existed between target 300 and lacing stand 100 and is relatively rotated.
In the present invention, the method to obtaining carbon nano-tube fibre does not do special restriction.For example, it is possible to use array
Spin processes prepare carbon nano-tube fibre.When carbon nano-tube fibre is prepared, catalyst iron can be used, catalyst is remained in fiber
Portion can affect the quality of fiber, in step sl, fine to CNT using acid solution (for example, the strong acid such as nitric acid or watery hydrochloric acid)
Dimension carries out the catalyst remained during process can remove carbon nano-tube fibre, such that it is able to improve the quality of carbon nano-tube fibre.
After step S2, the amorphous carbon in carbon nano-tube fibre is decomposed, so as to be conducive to metal in step S4
It is deposited on the surface of carbon nano-tube fibre.It is pointed out that step S4 is carried out in the sputtering chamber of magnetron sputtering apparatus.
Shown in Fig. 1 is the concrete structure of lacing stand 100, as illustrated, the lacing stand 100 include it is spaced around
Screw mandrel 110, therefore, carbon nano-tube fibre is smaller with the contact area of wire winding rod.Due to adjacent two circles carbon nano-tube fibre it
Between there is gap, therefore, being bombarded the nickel particles for producing by magnetron can be through between adjacent two circles carbon nano-tube fibre
Gap is reached on surface of the carbon nano-tube fibre not towards target 300.
Also, in step s3, exist between target 300 and lacing stand 100 and relatively rotate, such that it is able to guarantee to be wrapped in
Carbon nano-tube fibre on lacing stand can equably plated film.In the present invention, nickel particles are sunk in the way of physical vapour deposition (PVD)
Product will not produce pernicious gas or harmful liquid on the surface of carbon nano-tube fibre, therefore, method provided by the present invention is more
Environmental protection.Also, after step S1 and step S2, in carbon nano-tube fibre, there is no amorphous carbon and catalyst, Ke Yiti
The electric conductivity of high final nickel-plating carbon nanotube fiber living.
For the ease of arranging, it is preferable that target 300 can be arranged on the outside of lacing stand 100, also, lacing stand 100
Around own axis.Used as a kind of preferred embodiment of the present invention, target 300 can be fixedly installed in sputtering chamber.
As shown in Figures 1 and 2, lacing stand 100 can also include rotating shaft 120, can set rotating shaft 120 installed in sputtering
On standby rotating mechanism, rotated with band lacing stand 100.Lacing stand 100 rotate speed preferably 2r/min to 10r/min it
Between.
In step sl, the acid solution for using can include concentration between 1mol/L to 5mol/L.
It is further preferred that in step sl, carbon nano-tube fibre can be immersed in nitric acid, time of immersion can be with
Between 10min to 30min.
Described " at least through step S1 " is referred in step s 2, after step S1, directly can be walked
Rapid S2, it is also possible to after step S1, then the step of carry out other, after other steps, then carry out step S2.
For instance, it is preferred that methods described is additionally included in what is carried out between step S1 and step S2：
The carbon nano-tube fibre through step S1 is cleaned using sonic oscillation method, cleaning fluid includes ethanol.
Cleaning fluid can be absolute ethyl alcohol, or ethanol water.
Sonic oscillation method is referred to be put into carbon nano-tube fibre and is provided with the container of cleaning fluid, then using ultrasound
Wave apparatus are vibrated to cleaning fluid, such that it is able to the impurity adhered on carbon nano-tube fibre is removed.Specifically, using ultrasound
Succusion is to including the step of the carbon nano-tube fibre of step S1 is cleaned：
Carbon nano-fiber pipe fiber through step S1 is put into and is contained with the container of cleaning fluid；
Said vesse is placed on supersonic oscillations equipment, carbon nano-tube fibre is carried out clearly using supersonic oscillations method
Wash, scavenging period is between 2min-10min.
In the present invention, the quantity of target is not particularly limited.The particular number of target depends primarily on carbon and receives
The thickness of the nickel film of mitron fiber surface.If it is desired to the relatively large nickel film of thickness is obtained on the surface of carbon nano-tube fibre,
The relatively large number of target of quantity can be so set；If it is desired to it is relatively thin to obtain thickness on the surface of carbon nano-tube fibre
Nickel film, then can arrange the relatively small number of target of quantity.
Also, in order to the nickel film thickness to be formed be sputtered uniformly on the surface of carbon nano-tube fibre, and improve sputtering yield,
Preferably, in step S4, multiple targets 300 can be set, the plurality of target 300 is arranged around lacing stand 100.It is preferred that
Ground, each one magnetic control means of correspondence of target 300, so that multiple targets 300 can be controlled independently of one another.Operator can
To select the quantity of the target for playing a role according to specific technological requirement.
As a kind of preferred embodiment of the present invention, 6 targets can be set, each target is along lacing stand 100
Axially the other end of lacing stand 100 is extended to from one end of lacing stand 100.Preferably, it should be ensured that on lacing stand, be wound with carbon
The length of of length no more than target in the region of nanotube fibers.
As mentioned above it is possible, in the present invention, carry out the purpose preheated by carbon nano-tube fibre and be that decomposition carbon is received
Amorphous carbon in mitron fiber, it is preferable that in step s 2, between the temperature of the pre-heat treatment is between 100 DEG C to 200 DEG C,
The pre-heat treatment duration between 0.5h to 3h, so as to the amorphous carbon that both may insure in carbon nano-tube fibre can be with thorough
Bottom is decomposed and is volatilized, and can prevent from again carbon nano-tube fibre being caused to damage because preheating temperature is too high.It is pointed out that step
Rapid S2 is not to carry out in sputtering chamber, but is carried out in vacuum heat treatment furnace.
In sputtering, the radio-frequency power supply frequency of magnetron sputtering apparatus depends primarily on the composition of target.In the present invention, institute
It is nickel target to state target, it is preferable that the power of the radio-frequency power supply is preferably between 0.5KW to 1KW.
As nickel has good ductility and good electric conductivity, therefore, in the plating nickel on surface of carbon nano-tube fibre
After film, it is possible to obtain electric conductivity is good, the uniform composite of film forming, it is many that the composite is applied to wire, electrode etc.
Plant in application.
When radio-frequency power supply power setting within the above range when, both can form densification on the surface of carbon nano-tube fibre
Nickel film, the energy consumption in whole sputter procedure can be reduced again, also, can also be improved in carbon nano-tube fibre plating nickel on surface
Efficiency.
For the nickel film of thickness uniformity lived on the surface of carbon nano-tube fibre, it is preferable that in step s 4, magnetic control
Sputtering duration is between 1h to 3h.It is easily understood that magnetron sputtering duration is longer, obtain nickel film thickness more
Greatly.Preferably, in step s3, magnetron sputtering duration is less than 3 hours, such that it is able to prevent carbon nano-tube fibre
The nickel film of upper formation is blocked up to come off.
In the present invention, do not have special regulation to sputter temperature, for example, in step s 4, the predetermined temperature exists
Between 200 DEG C to 400 DEG C.When temperature within this range to the plating nickel on surface of carbon nano-tube fibre when, temperature is higher, deposit film forming
Speed it is faster.Similarly, preferably more than 400 DEG C of the predetermined temperature, such that it is able to guarantee carbon nano-tube fibre in sputtering
During be not damaged.
In the present invention, in order to prevent the nickel film for sputtering formation to be oxidized, sputtering technology can be carried out under vacuum conditions.
Specifically, step S4 can include：
S41, by the target and be wound with carbon nano-tube fibre lacing stand be arranged in the sputtering chamber after, to described
Sputtering chamber carries out vacuumizing until the first preset air pressure；
S42, the sputtering chamber is carried out being heated to the predetermined temperature；
S43, unlatching radio-frequency power supply, the duration is between 1h to 3h.
Preferably, first preset air pressure is 10-2Pa to 10-1Between Pa.
After the completion of sputtering technology, shielding power supply is closed, close heater, closed less than 30 DEG C later in sputtering cavity temperature
Vacuum system is closed, air is put into into sputtering chamber to cavity pressure is sputtered and is reached atmospheric pressure, open sputtering chamber, obtain nickel-plated carbon and receive
Mitron fiber.
As another kind of preferred embodiment of the present invention, protective gas can be passed through into sputtering chamber.The protective gas
Do not react with carbon nano-tube fibre, also do not react with target.For example, protective gas can be argon gas or nitrogen, or, shielding gas
Body can also be other should not CNT and target reaction inert gas.In the present embodiment, step S4 includes：
S41, by the target and be wound with carbon nano-tube fibre lacing stand be arranged in the sputtering chamber after, to described
Sputtering chamber carries out vacuumizing up to the second preset air pressure, and into the sputtering chamber is passed through inert gas, is passed through inert gas and holds
The continuous time is between 0.5h to 3h；
S42, the sputtering chamber is carried out being heated to the predetermined temperature；
S43, the sputtering chamber is vacuumized, until second preset air pressure
S44, unlatching radio-frequency power supply, the duration is between 1h to 3h.
It is to be understood that inert gas refers to the gas not reacted with the material for making target.For example, when target is nickel
When, inert gas can be argon gas.
Due to being passed through inert gas into sputtering chamber in step S41, therefore, it can for the second preset air pressure to be set to ratio
The slightly higher air pressure of first preset air pressure.For example, second preset air pressure is 3 × 10-1Pa to 5 × 10-1Between Pa.
After sputtering technology terminates, shielding power supply is closed, close heater, temperature is opened less than 30 DEG C later and splashed in the cabin
The chamber door in chamber is penetrated, air is passed through, nickel-plating carbon nanotube fiber is obtained.
Preferably, in execution step S42, it is possible to use the mode of sensing heating is heated to the sputtering chamber.From
And the horizontal proliferation of metallic atom can be promoted, advantageously form densification, continuous nickel film.Certainly, the present invention is not limited to this.
Using method provided by the present invention to carbon nano-tube fibre plated film, can be in the surface shape of carbon nano-tube fibre
Into the nickel film that surface is smooth and fine and close.The carbon nano-tube fibre for being coated with nickel film has preferable electric conductivity, can serve as electrode,
Wire etc..
Embodiment
In embodiment provided by the present invention, it is Shenyang Scientists Friend Vacuum Technology Co., Ltd. to sputter the sputtering equipment used
The magnetron sputtering apparatus of the MS560D models that company provides, the target used is that Beijing Guan Jinli new materials Science and Technology Ltd. carries
For high-purity anaerobic nickel matter target.Carbon nano-tube fibre is the carbon nano-tube fibre obtained in above-mentioned preparation example.Heat-treatment furnace is
The VHA-446 model heat-treatment furnaces that Shenyang Scientists Friend Vacuum Technology Co., Ltd. provides.
The carbon nano-tube fibre used in following examples is as shown in figure 4, conductance is 2 × 104S/m。
Embodiment 1
S1, carbon nano-tube fibre is immersed in concentration be 1mol/L nitric acid in, soak time is 30min；
Carbon nano-tube fibre through step S1 is inserted in the container for filling absolute ethyl alcohol, and the container is placed on
On ultrasonic equipment, ultrasonic equipment, duration 3min is opened；
S2, the pre-heat treatment is carried out in heat-treatment furnace to carbon nano-tube fibre, heating-up temperature is 100 DEG C, preheating time is
3h；
S3, will be arranged on after the carbon nano-tube fibre 200 of step S2 is wrapped on lacing stand 100 in sputtering chamber, around
Guide frame 100 includes multiple spaced wire winding rods 110, there is the interval of 20mm between adjacent two circles carbon nano-tube fibre 200；
S4, the carbon nano-tube fibre 200 being wrapped on lacing stand 100 is arranged in sputtering chamber, with metallic nickel as target
300, wherein, 6 targets in sputtering chamber, are provided with, 6 targets are uniformly arranged around lacing stand, close sputtering chamber, to sputtering chamber
Vacuumized, until 10-1Pa, 100 velocity of rotation of lacing stand are 5r/min, and sputtering chamber is heated to 300 DEG C, and mode of heating is
Sensing heating, opens radio-frequency power supply, and power is 0.5KW, and sputtering continues 1h；
S5, closing shielding power supply, close heater, when sputtering cavity temperature closes vacuum system less than 30 DEG C later,
Air is put into into sputtering chamber, atmospheric pressure is reached to sputtering cavity pressure, is opened sputtering chamber, is taken out lacing stand, obtain nickel-plated carbon
Nanotube fibers.
Shown in Fig. 5 be in the present embodiment 1 obtained by nickel-plating carbon nanotube fiber scanned picture, Fig. 6 is Fig. 5
Enlarged drawing.It will be seen from figures 5 and 6 that nickel film is fine and close and continuous.Jing is tested, and the nickel-plating carbon nanotube that the present embodiment is obtained is fine
The resistivity of dimension is 1 × 106S/m。
Embodiment 2
Nickel-plating carbon nanotube is prepared using the method provided in embodiment 1, difference is, in step sl, nitre
Acid concentration is 5mol/L, and soak time is 10min, and in step s 4, sputtering chamber is heated to 350 DEG C, and radio-frequency power supply power is
1.0KW, sputtering time are 2h.
Shown in Fig. 7 be in the present embodiment 2 obtained by nickel-plating carbon nanotube fiber scanned picture, Fig. 8 is Fig. 7
Enlarged drawing.Can see from Fig. 7 and Fig. 8, nickel film is fine and close and continuous.Jing is tested, and the nickel-plating carbon nanotube that the present embodiment is obtained is fine
The resistivity of dimension is 3 × 106S/m。
It is understood that the embodiment of above principle being intended to be merely illustrative of the present and the exemplary enforcement for adopting
Mode, but the invention is not limited in this.For those skilled in the art, in the essence without departing from the present invention
In the case of god and essence, various modifications and improvement can be made, these modifications and improvement are also considered as protection scope of the present invention.
Claims (10)
1. a kind of method to carbon nano-tube fibre nickel plating, it is characterised in that methods described includes：
S1, cleaning treatment is carried out to the carbon nano-tube fibre using acid solution；
S2, the pre-heat treatment is carried out to the carbon nano-tube fibre at least through step S1；
S3, will be arranged on after the carbon nano-tube fibre of step S2 is wrapped on lacing stand in sputtering chamber, the lacing stand bag
Multiple spaced wire winding rods are included, between adjacent two circles carbon nano-tube fibre, there is interval；
S4, the carbon nano-tube fibre with metallic nickel as target at a predetermined temperature to being wrapped on the lacing stand carry out sputtering plating
Film, wherein, exists between the target and the lacing stand and relatively rotates.
2. method according to claim 1, it is characterised in that in step S4, the target be arranged on it is described around
Outside guide frame, the lacing stand is around own axis, and arranges multiple targets, and multiple targets are around the wrapping wire
Frame is arranged.
3. method according to claim 1 and 2, it is characterised in that in step s 2, the temperature of the pre-heat treatment is at 100 DEG C
To between 200 DEG C, preheating time is between 0.5h to 3h.
4. method according to claim 1 and 2, it is characterised in that methods described be additionally included in step S1 and step S2 it
Between carry out：
The carbon nano-tube fibre through step S1 is cleaned using sonic oscillation method, cleaning fluid includes ethanol.
5. method according to claim 1 and 2, it is characterised in that in step s 4, magnetron sputtering duration is in 1h
To between 3h, the predetermined temperature is between 200 DEG C to 400 DEG C.
6. method according to claim 4, it is characterised in that step S4 includes：
S41, respectively by the target and be wound with carbon nano-tube fibre lacing stand be arranged in the sputtering chamber after, to described
Sputtering chamber carries out vacuumizing until the first preset air pressure；
S42, the sputtering chamber is carried out being heated to the predetermined temperature；
S43, unlatching radio-frequency power supply, and the unlatching duration of the radio-frequency power supply is between 1h to 2h.
7. method according to claim 6, it is characterised in that first preset air pressure is 10-2Pa to 10-1Between Pa.
8. method according to claim 6, it is characterised in that in step S42, using the mode of sensing heating to described
Sputtering chamber is heated.
9. the method according to claim 1 and 2, it is characterised in that the acid solution includes concentration in 1mol/L to 5mol/
Nitric acid between L.
10. method according to claim 9, it is characterised in that the process time of step S1 is in 10min to 30min
Between.
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| CN109957963A (en) * | 2019-04-04 | 2019-07-02 | 江苏金秋弹性织物有限公司 | A kind of preparation method of conductive fiber |
| CN109972250A (en) * | 2019-04-04 | 2019-07-05 | 江苏金秋弹性织物有限公司 | A kind of preparation method of more conductive conductive fibers |
| CN110950321A (en) * | 2019-12-17 | 2020-04-03 | 哈尔滨金纳科技有限公司 | High-specific-surface-area and high-conductivity carbon nanotube material and preparation method thereof |
| CN114032513A (en) * | 2021-12-14 | 2022-02-11 | 湘潭大学 | Method for preparing welding wire coating based on magnetic filtration cathode vacuum arc method |
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| CN108948529A (en) * | 2018-07-06 | 2018-12-07 | 佛山市高明区爪和新材料科技有限公司 | A kind of preparation method of composite conductive plastic |
| CN109957963A (en) * | 2019-04-04 | 2019-07-02 | 江苏金秋弹性织物有限公司 | A kind of preparation method of conductive fiber |
| CN109972250A (en) * | 2019-04-04 | 2019-07-05 | 江苏金秋弹性织物有限公司 | A kind of preparation method of more conductive conductive fibers |
| CN109957963B (en) * | 2019-04-04 | 2021-06-04 | 江苏金秋绳带科技有限公司 | Preparation method of conductive fiber |
| CN109972250B (en) * | 2019-04-04 | 2021-09-10 | 江苏金秋弹性织物有限公司 | Preparation method of multi-metal conductive fiber |
| CN110950321A (en) * | 2019-12-17 | 2020-04-03 | 哈尔滨金纳科技有限公司 | High-specific-surface-area and high-conductivity carbon nanotube material and preparation method thereof |
| CN114032513A (en) * | 2021-12-14 | 2022-02-11 | 湘潭大学 | Method for preparing welding wire coating based on magnetic filtration cathode vacuum arc method |
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