CN105970155A - Method for coating carbon nanotube fibers - Google Patents
Method for coating carbon nanotube fibers Download PDFInfo
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- CN105970155A CN105970155A CN201510974782.3A CN201510974782A CN105970155A CN 105970155 A CN105970155 A CN 105970155A CN 201510974782 A CN201510974782 A CN 201510974782A CN 105970155 A CN105970155 A CN 105970155A
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- Prior art keywords
- carbon nano
- sputtering chamber
- tube fibre
- target
- lacing stand
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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
- C23C14/185—Metallic material, boron or silicon on other inorganic substrates by cathodic sputtering
-
- 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
- C23C14/352—Sputtering by application of a magnetic field, e.g. magnetron sputtering using more than one target
-
- 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
- C23C14/50—Substrate holders
- C23C14/505—Substrate holders for rotation of the substrates
Abstract
The invention provides a method for coating carbon nanotube fibers. The method comprises the following steps: S1) the carbon nanotube fibers are preheated; S2) the carbon nanotube fibers obtained in the step 1) are wound on a wire wrapping rack and then are arranged in a sputtering chamber, the wire wrapping rack comprises several wire wrapping rods which are arranged at intervals, a space is provided between the adjacent carbon nanotube fibers; and S3) under preset temperature, by tasking metal as a target material, the carbon nanotube fibers on the wire wrapping rack are subjected to sputter coating, wherein, the target material and the wire wrapping rack enables relative rotation. According to the invention, the metal particles are deposited on the surface of the carbon nanotube fibers by a physical vapor deposition method, harmful gas or harmful liquid is not generated, so that the method is environmentally friendly.
Description
Technical field
The present invention relates to sputter copper facing field, in particular it relates to one carries out copper facing to carbon nano-tube fibre
Method.
Background technology
In the prior art, it is generally required that utilize the method for electrochemical filming gold-plated on carbon nano-tube fibre
Belong to film.But, during this method metal-coated membrane, easily cause pollution, and, metal film is not very
Fine and close.
Therefore, the most in environmentally friendly manner carbon nano-tube fibre is carried out metal-coated membrane and become the present invention urgently
Solve the technical problem that.
Summary 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
The surface of carbon nano-tube fibre forms the metal film of densification, and will not cause environment during plated film
Pollute.
To achieve these goals, the present invention provides a kind of method to carbon nano-tube fibre plated film, wherein,
Described method includes:
S1, described carbon nano-tube fibre is carried out the pre-heat treatment;
S2, will be arranged in sputtering chamber after the carbon nano-tube fibre of step S1 is wrapped on lacing stand,
Described lacing stand includes multiple spaced wire winding rod, between existing between adjacent two circle carbon nano-tube fibres
Every;
S3, with metal for target at a predetermined temperature to the carbon nano-tube fibre being wrapped on described lacing stand
Carry out sputter coating, wherein, exist between described target and described lacing stand and relatively rotate.
Preferably, in described step S3, described target is arranged on outside described lacing stand, described around
Guide frame is around own axis.
Preferably, in described step S3, arranging multiple described target, multiple described targets are around institute
State lacing stand to arrange.
Preferably, in step sl, the temperature of the pre-heat treatment is between 200 DEG C to 400 DEG C, during preheating
Between between 0.5h to 3h.
Preferably, described target is metallic copper, and in step s3, the power of radio-frequency power supply is at 0.5KW
Between 1.0KW.
Preferably, in step s3, magnetron sputtering duration is between 1h to 3h, described pre-
Fixed temperature is between 200 DEG C to 400 DEG C.
Preferably, step S3 includes:
S31, respectively by described target be wound with the lacing stand of carbon nano-tube fibre and be arranged on described sputtering
After intracavity, described sputtering chamber is carried out evacuation until the first preset air pressure;
S32, described sputtering chamber is heated to described predetermined temperature;
S33, open radio-frequency power supply, and the unlatching of described radio-frequency power supply persistently put into practice 1h to 3h it
Between.
Preferably, described first preset air pressure is 10-2Pa to 10-1Between Pa.
Preferably, step S3 includes:
S31, by described target be wound with the lacing stand of carbon nano-tube fibre and be arranged in described sputtering chamber
After, described sputtering chamber is carried out evacuation until the second preset air pressure, and be passed through lazy in described sputtering chamber
Property gas;
S32, described sputtering chamber is heated to described predetermined temperature;
S33, described sputtering chamber is carried out evacuation until described second preset air pressure;
S34, open radio-frequency power supply, and the unlatching persistent period of described radio-frequency power supply 1h to 3h it
Between.
Preferably, described second preset air pressure is 3 × 10-1Pa to 5 × 10-1Between Pa.
Preferably, in step s 32, described sputtering chamber is heated by the mode utilizing sensing heating.
In method provided by the present invention, after step S1, the nothing in carbon nano-tube fibre is fixed
Shape carbon is decomposed, thus beneficially in step S3 metal deposit on the surface of carbon nano-tube fibre.To
When carbon nano-tube fibre is arranged on lacing stand, between existing between adjacent two circle carbon nano-tube fibres
Gap, therefore, by magnetron bombardment produce metallic can through adjacent two circle carbon nano-tube fibres it
Between gap arrive carbon nano-tube fibre not towards on the surface of target.Further, in step s3, target
Exist between material and lacing stand and relatively rotate, such that it is able to guarantee that the CNT being wrapped on lacing stand is fine
Dimension can plated film equably.In the present invention, metallic is deposited on carbon in the way of physical vapour deposition (PVD)
The surface of nanotube fibers, will not produce harmful gas or harmful liquid, therefore, provided by the present invention
Method is more environmentally-friendly.
Accompanying drawing explanation
Fig. 1 is the schematic diagram of lacing stand;
The relative position view that Fig. 2 is wound around 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 that the present invention prepares the copper nanotube fibers of profit acquisition, and amplification is 1500
Times;
Fig. 5 is the scanned picture of the coppered carbon nanotube fibers that embodiment 1 obtains, and amplification is 195
Times;
Fig. 6 is the scanned picture of the coppered carbon nanotube fibers that embodiment 1 obtains, and amplification is 2500
Times;
Fig. 7 is the scanned picture of the coppered carbon nanotube fibers that embodiment 2 obtains, and amplification is 500
Times;
Fig. 8 is the scanned picture of the coppered carbon nanotube fibers that embodiment 2 obtains, and amplification is 2000
Times;
Fig. 9 is the scanned picture of the coppered carbon nanotube fibers that embodiment 3 obtains, and amplification is 1000
Times;
Figure 10 is the scanned picture of the coppered carbon nanotube fibers that embodiment 3 obtains, and amplification is 4500
Times.
Description of reference numerals
100: lacing stand 110: wire winding rod
120: rotating shaft 200: carbon nano-tube fibre
300: target
Detailed description of the invention
Below in conjunction with accompanying drawing, the detailed description of the invention of the present invention is described in detail.It should be appreciated that
Detailed description of the invention described herein is merely to illustrate and explains the present invention, is not limited to this
Bright.
The present invention provides a kind of method to carbon nano-tube fibre plated film, and wherein, described method includes:
S1, described carbon nano-tube fibre is carried out the pre-heat treatment;
S2, will be arranged on after the carbon nano-tube fibre 200 of step S1 is wrapped on lacing stand 100
In sputtering chamber, lacing stand 100 includes multiple spaced wire winding rod 110, adjacent two circle CNTs
Interval is there is between fiber 200;
S3, with metal for target 300, at a predetermined temperature to the carbon nanometer being wrapped on lacing stand 100
Pipe fiber 200 carries out sputter coating, wherein, exists and relatively rotate between target 300 and lacing stand 100.
In method provided by the present invention, after step S1, the nothing in carbon nano-tube fibre is fixed
Shape carbon is decomposed, thus beneficially in step S3 metal deposit on the surface of carbon nano-tube fibre.Step
S3 is to carry out in the sputtering chamber of magnetron sputtering apparatus.
Shown in Fig. 1 is the concrete structure of lacing stand 100, as it can be seen, this lacing stand 100 includes
Spaced wire winding rod 110, therefore, carbon nano-tube fibre is less with the contact area of wire winding rod.
Owing to there is gap between adjacent two circle carbon nano-tube fibres, therefore, magnetron bombardment the metal produced
Particle can through adjacent two circle carbon nano-tube fibres gap arrive carbon nano-tube fibre not towards
On the surface of target 300.
Further, in step s3, exist between target 300 and lacing stand 100 and relatively rotate, thus
May insure that the carbon nano-tube fibre that is wrapped on lacing stand can plated film equably.In the present invention, gold
Belong to particle in the way of physical vapour deposition (PVD), be deposited on the surface of carbon nano-tube fibre, harmful gas will not be produced
Body or harmful liquid, therefore, method provided by the present invention is more environmentally-friendly.
In the present invention, the method obtaining carbon nano-tube fibre is not done special restriction.Such as, may be used
To utilize array spin processes to prepare carbon nano-tube fibre.Array spin processes how is utilized to prepare CNT fine
Dimension is known in those skilled in the art, repeats no more here.
For the ease of arranging, it is preferable that target 300 can be arranged on the outside of lacing stand 100, and
And, lacing stand 100 is around own axis.As a kind of preferred implementation 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 be by rotating shaft 120
It is arranged on the rotating mechanism of sputtering equipment, rotates with band lacing stand 100.The speed that lacing stand 100 rotates
Degree is preferably between 2r/min to 10r/min.
In the present invention, the quantity of target is not particularly limited.The particular number of target mainly takes
The certainly thickness of the metal film in carbon nano-tube fibre surface.It is it desired to obtain on the surface of carbon nano-tube fibre
Obtain the metal film that thickness is relatively large, then the relatively large number of target of quantity can be set;It is it desired to
The surface of carbon nano-tube fibre obtains the metal film that thickness is relatively thin, then can arrange quantity relatively fewer
Target.
Further, in order to the thickness of metal film formed in the sputtering of the surface of carbon nano-tube fibre is uniform, and carry
High sputtering yield, it is preferable that in described step S3, can arrange multiple target 300, the plurality of
Target 300 is arranged around lacing stand 100.Preferably, the corresponding magnetic control means of each target 300,
So that multiple targets 300 can control independently of one another.Operator can want according to concrete technique
Seek the quantity of target selecting to play a role.
As a kind of preferred implementation of the present invention, 6 targets can be set, each target along around
Axial one end from lacing stand 100 of guide frame 100 extends to the other end of lacing stand 100.Preferably,
It should be ensured that be wound with the length length less than target in the region of carbon nano-tube fibre on lacing stand.
As mentioned above it is possible, in the present invention, carry out the purpose that carbon nano-tube fibre carries out preheating and be that
Amorphous carbon in decomposing carbon nano-tube fiber, it is preferable that in step sl, the temperature of the pre-heat treatment
Between between 200 DEG C to 400 DEG C, the pre-heat treatment duration is between 0.5h to 3h, thus both
May insure that the amorphous carbon in carbon nano-tube fibre can thoroughly decompose and volatilize, be possible to prevent again because of pre-
Hot temperature is too high and carbon nano-tube fibre is caused damage.It is pointed out that step S1 be not
Carry out in sputtering chamber, but carry out in vacuum heat treatment furnace.
When sputtering, the radio-frequency power supply frequency of magnetron sputtering apparatus depends primarily on the composition of target.Described
Target can be copper target material, it is possible to use method provided by the present invention copper facing on carbon nano-tube fibre
Film.In this case, the power of described radio-frequency power supply is preferably at 0.5KW to 1.0KW.
Owing to copper has good ductility and good electric conductivity, therefore, at carbon nano-tube fibre
After plated surface copper film, it is possible to obtain electric conductivity is good, the uniform composite of film forming, this composite wood
Material is be applicable to the multiple application such as wire, electrode.
When radio-frequency power supply power setting within the above range time, both can be on the surface of carbon nano-tube fibre
Form fine and close copper film, the energy consumption in whole sputter procedure can be reduced again, and, it is also possible to improve
The efficiency of carbon nano-tube fibre copper coating.
The uniform copper film the most always of thickness in order to live on the surface of carbon nano-tube fibre, it is preferable that in step
In S3, magnetron sputtering duration is between 1h to 3h.It is easily understood that magnetron sputtering is held
The continuous time is the longest, it is the biggest to obtain copper film thickness.Preferably, in step s3, magnetron sputtering is lasting
Time less than 3 hours, such that it is able to prevent that the copper film formed on carbon nano-tube fibre is blocked up to come off.
In the present invention, sputter temperature is not had special regulation, such as, in step s3, institute
State predetermined temperature between 200 DEG C to 400 DEG C.The table to carbon nano-tube fibre in this range when temperature
During the copper facing of face, temperature is the highest, and the speed of deposition film forming is the fastest.Similarly, described predetermined temperature is the most not
More than 400 DEG C, such that it is able to guarantee that carbon nano-tube fibre is not damaged during sputtering.
In the present invention, for the metal membrane-coating oxidation preventing sputtering from being formed, can enter under vacuum conditions
Row sputtering technology.Specifically, step S3 may include that
S31, by described target be wound with the lacing stand of carbon nano-tube fibre and be arranged in described sputtering chamber
After, described sputtering chamber is carried out evacuation until the first preset air pressure;
S32, described sputtering chamber is heated to described predetermined temperature;
S33, unlatching radio-frequency power supply, the persistent period is between 1h to 3h.
Preferably, described first preset air pressure is 10-2Pa to 10-1Between Pa.
After sputtering technology completes, close shielding power supply, close heater, be less than at sputtering cavity temperature
Close vacuum system after 30 DEG C, in sputtering chamber, put into air reach atmospheric pressure to sputtering cavity pressure,
Open sputtering chamber, obtain coppered carbon nanotube fibers.
As the another kind of preferred implementation of the present invention, protective gas can be passed through in sputtering chamber.Should
Protective gas does not reacts with carbon nano-tube fibre, does not reacts with target.Such as, protective gas can be
Argon or nitrogen, or, protective gas can also is that other do not want CNT and target reaction lazy
Property gas.In the present embodiment, step S3 includes:
S31, by described target be wound with the lacing stand of carbon nano-tube fibre and be arranged in described sputtering chamber
After, described sputtering chamber is carried out evacuation until the second preset air pressure, and be passed through lazy in described sputtering chamber
Property gas, is passed through noble gas duration between 0.5h to 3h;
S32, described sputtering chamber is heated to described predetermined temperature;
S33, described sputtering chamber is carried out evacuation, until described second preset air pressure
S34, unlatching radio-frequency power supply, the persistent period is between 1h to 3h.
It is to be understood that noble gas refers to the gas not reacted with the material making target.Such as,
When target is copper, noble gas can be argon.
Owing to step S31 being passed through in sputtering chamber noble gas, therefore, it can the second predetermined gas
Pressure is set to the air pressure more slightly higher than the first preset air pressure.Such as, described second preset air pressure is 3 × 10-1Pa
To 5 × 10-1Between Pa.
After sputtering technology terminates, closing shielding power supply, close heater, in cabin, temperature is less than 30 DEG C
Open the chamber door of sputtering chamber later, be passed through air, obtain coppered carbon nanotube fibers.
Preferably, when performing step S32, it is possible to use described sputtering chamber is entered by the mode of sensing heating
Row heating.Such that it is able to promote the horizontal proliferation of metallic atom, advantageously form densification, continuous print metal
Film.Certainly, the present invention is not limited to this.
Utilize method provided by the present invention to carbon nano-tube fibre plated film, can be at carbon nano-tube fibre
Surface form smooth surface and the metal film of densification.The carbon nano-tube fibre of metal-plated membrane has preferably
Electric conductivity, can serve as electrode, wire etc..
Embodiment
In embodiment provided by the present invention, the sputtering equipment that sputtering is used is Shenyang section friend's vacuum technique
The magnetron sputtering apparatus of the MS560D model that company of company limited provides, the target used is Beijing hat gold
The high-purity oxygen-free copper matter target that profit new material Science and Technology Ltd. provides.Carbon nano-tube fibre is above-mentioned preparation
The carbon nano-tube fibre obtained in example.Heat-treatment furnace provides for Shenyang Scientists Friend Vacuum Technology Co., Ltd.
VHA-446 model heat-treatment furnace.Carrying out the method to carbon nano-tube fibre plated film provided by the present invention
Before, first carbon nano-tube fibre is carried out pre-clean processes, comprises the following steps:
Stp1, carbon nano-fiber pipe fiber is put in the container being contained with dehydrated alcohol;
Stp2, said vesse is prevented on supersonic oscillations equipment, utilize supersonic oscillations method that carbon is received
Mitron fiber is carried out, and scavenging period is between 2min-10min.
The carbon nano-tube fibre used in following example is the carbon Nanowire after pre-clean processes
Dimension pipe, the carbon nano-tube fibre obtained after pre-clean processes is as shown in Figure 4.
Embodiment 1
S1, in heat-treatment furnace, carbon nano-tube fibre being carried out the pre-heat treatment, heating-up temperature is 200 DEG C,
Preheating time is 3h;
S2, the carbon nano-tube fibre after the pre-heat treatment is wrapped on lacing stand, adjacent two circle CNTs
Gap between fiber is 20mm;
S31, carbon nano-tube fibre is arranged in sputtering chamber, 6 targets are set in sputtering chamber, 6
Individual target is uniformly arranged around lacing stand, closes sputtering chamber, sputtering chamber is carried out evacuation, until 10-1Pa;
S32, sputtering chamber being heated to 300 DEG C, mode of heating is sensing heating;
S33, unlatching radio-frequency power supply, power is 0.5KW, and sputtering continues 1h;
S4, closedown shielding power supply, close heater, pass after sputtering cavity temperature is less than 30 DEG C
Close vacuum system, in sputtering chamber, put into air, reach atmospheric pressure to sputtering cavity pressure, open sputtering
Chamber, takes out lacing stand, obtains coppered carbon nanotube fibers.
Shown in Fig. 5 is the scanned picture of coppered carbon nanotube fibers obtained in the present embodiment 1, Fig. 6
It it is the enlarged drawing of Fig. 5.It will be seen that copper film smooth surface, densification and continuously from Fig. 5 and Fig. 6.
After tested, the resistance of the coppered carbon nanotube fibers that the present embodiment obtains is 0.24 Ω/cm.
Embodiment 2
According to the method in embodiment 1, carbon nano-tube fibre being carried out copper facing, difference is: in step
In rapid S1, preheating temperature is 200 DEG C, and preheating time is 3h, in step S31, sets in sputtering chamber
Putting 4 targets, the air pressure in sputtering chamber is 10-1Pa, in step s 32, is heated to sputtering chamber
200 DEG C, in step S33, shielding power supply frequency is 0.75kw, and the sputtering persistent period is 2h.
Shown in Fig. 7 is the scanned picture of coppered carbon nanotube fibers obtained in the present embodiment 2,
Fig. 8 is the enlarged drawing of Fig. 7.It will be seen that copper film smooth surface, densification and even from Fig. 7 and Fig. 8
Continuous.After tested, the resistance of the coppered carbon nanotube fibers that the present embodiment obtains is 0.19 Ω/cm.
Embodiment 3
According to the method in embodiment 1, carbon nano-tube fibre being carried out copper facing, difference is: in step
In rapid S1, preheating temperature is 300 DEG C, and preheating time is 1h,
Step S3 includes:
S31, by described target be wound with the lacing stand of carbon nano-tube fibre and be arranged in described sputtering chamber
After, described sputtering chamber is carried out evacuation until 5 × 10-1Pa, and it is passed through argon in described sputtering chamber,
The persistent period being passed through argon is 3h;
S32, described sputtering chamber being heated to 300 DEG C, mode of heating is sensing heating;
S33, described sputtering chamber is carried out evacuation until 3 × 10-1Pa;
S34, unlatching radio-frequency power supply, the frequency of radio-frequency power supply is 0.75kw, and the sputtering persistent period is 2h.
Shown in Fig. 9 is the scanned picture of coppered carbon nanotube fibers obtained in the present embodiment 3,
Figure 10 is the enlarged drawing of Fig. 9.From Fig. 9 and Figure 10 it will be seen that copper film smooth surface, densification and
Continuously.After tested, the resistance of the coppered carbon nanotube fibers that the present embodiment obtains is 0.21 Ω/cm.
Embodiment 4
According to the method in embodiment 3, carbon nano-tube fibre being carried out copper facing, difference is, in step
In rapid S31, described sputtering chamber is carried out evacuation until 3 × 10-1Pa, and logical in described sputtering chamber
Entering argon, the persistent period being passed through argon is 20min, in step s 32, carries out described sputtering chamber
Being heated to 400 DEG C, in step S34, rf frequency is 1KW, and the persistent period is 1h.After tested,
The resistance of the coppered carbon nanotube fibers that the present embodiment obtains is 0.26 Ω/cm.
It is understood that the principle that is intended to be merely illustrative of the present of embodiment of above and showing of using
Example embodiment, but the invention is not limited in this.For one of ordinary skilled in the art
Speech, without departing from the spirit and substance in the present invention, can make various modification and improvement, this
A little modification and improvement are also considered as protection scope of the present invention.
Claims (10)
1. the method to carbon nano-tube fibre plated film, it is characterised in that described method includes:
S1, described carbon nano-tube fibre is carried out the pre-heat treatment;
S2, will be arranged in sputtering chamber after the carbon nano-tube fibre of step S1 is wrapped on lacing stand,
Described lacing stand includes multiple spaced wire winding rod, between existing between adjacent two circle carbon nano-tube fibres
Every;
S3, with metal for target at a predetermined temperature to the carbon nano-tube fibre being wrapped on described lacing stand
Carry out sputter coating, wherein, exist between described target and described lacing stand and relatively rotate.
Method the most according to claim 1, it is characterised in that in described step S3, described
Target is arranged on outside described lacing stand, and described lacing stand is around own axis, and arranges multiple described
Target, multiple described targets are arranged around described lacing stand.
Method the most according to claim 1 and 2, it is characterised in that in step sl, preheating
The temperature processed is between 200 DEG C to 400 DEG C, and preheating time is between 0.5h to 3h.
Method the most according to claim 1, it is characterised in that described target is metallic copper,
In step S3, the power of radio-frequency power supply is between 0.5KW to 1.0KW.
Method the most according to claim 4, it is characterised in that in step s3, magnetron sputtering
Duration is between 1h to 3h, and described predetermined temperature is between 200 DEG C to 400 DEG C.
Method the most according to claim 4, it is characterised in that step S3 includes:
S31, respectively by described target be wound with the lacing stand of carbon nano-tube fibre and be arranged on described sputtering
After intracavity, described sputtering chamber is carried out evacuation until the first preset air pressure;
S32, described sputtering chamber is heated to described predetermined temperature;
S33, open radio-frequency power supply, and the unlatching persistent period of described radio-frequency power supply 1h to 3h it
Between.
Method the most according to claim 6, it is characterised in that described first preset air pressure is 10-2Pa
To 10-1Between Pa.
Method the most according to claim 4, it is characterised in that step S3 includes:
S31, by described target be wound with the lacing stand of carbon nano-tube fibre and be arranged in described sputtering chamber
After, described sputtering chamber is carried out evacuation until the second preset air pressure, and be passed through lazy in described sputtering chamber
Property gas;
S32, described sputtering chamber is heated to described predetermined temperature;
S33, described sputtering chamber is carried out evacuation until described second preset air pressure;
S34, open radio-frequency power supply, and the unlatching persistent period of described radio-frequency power supply 1h to 3h it
Between.
Method the most according to claim 8, it is characterised in that described second preset air pressure is 3
×10-1Pa to 5 × 10-1Between Pa.
10. according to the method described in any one in claim 6 to 9, it is characterised in that in step
In S32, utilize the mode of sensing heating that described sputtering chamber is heated.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113088913A (en) * | 2021-04-13 | 2021-07-09 | 安徽工程大学 | Carbon fiber modification method and product thereof |
CN115142008A (en) * | 2022-07-11 | 2022-10-04 | 吉林大学 | Continuous carbon nanotube fiber reinforced copper-based composite material and preparation method and application thereof |
Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH08253861A (en) * | 1995-03-16 | 1996-10-01 | Kawasaki Steel Corp | C/c composite material having high oxidation resistance |
CN102251224A (en) * | 2011-07-11 | 2011-11-23 | 中国科学院金属研究所 | Device and method for depositing film on SiC fiber surface |
CN102534535A (en) * | 2012-02-29 | 2012-07-04 | 中国科学院金属研究所 | Device and method for uniformly and fast depositing metal/compound thin film on surface of continuous fiber/strip |
CN104878357A (en) * | 2015-06-11 | 2015-09-02 | 桂林理工大学 | Method for preparing SiC coating layers on surfaces of carbon fibers by radio-frequency (RF) magnetron sputtering |
-
2015
- 2015-12-24 CN CN201510974782.3A patent/CN105970155A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
JPH08253861A (en) * | 1995-03-16 | 1996-10-01 | Kawasaki Steel Corp | C/c composite material having high oxidation resistance |
CN102251224A (en) * | 2011-07-11 | 2011-11-23 | 中国科学院金属研究所 | Device and method for depositing film on SiC fiber surface |
CN102534535A (en) * | 2012-02-29 | 2012-07-04 | 中国科学院金属研究所 | Device and method for uniformly and fast depositing metal/compound thin film on surface of continuous fiber/strip |
CN104878357A (en) * | 2015-06-11 | 2015-09-02 | 桂林理工大学 | Method for preparing SiC coating layers on surfaces of carbon fibers by radio-frequency (RF) magnetron sputtering |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN113088913A (en) * | 2021-04-13 | 2021-07-09 | 安徽工程大学 | Carbon fiber modification method and product thereof |
CN113088913B (en) * | 2021-04-13 | 2022-03-29 | 安徽工程大学 | Carbon fiber modification method and product thereof |
WO2022217679A1 (en) * | 2021-04-13 | 2022-10-20 | 安徽工程大学 | Carbon fiber modification method and product thereof |
CN115142008A (en) * | 2022-07-11 | 2022-10-04 | 吉林大学 | Continuous carbon nanotube fiber reinforced copper-based composite material and preparation method and application thereof |
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