CN106702729A - Method for aluminizing carbon nano tube fibers - Google Patents
Method for aluminizing carbon nano tube fibers Download PDFInfo
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- CN106702729A CN106702729A CN201610716565.9A CN201610716565A CN106702729A CN 106702729 A CN106702729 A CN 106702729A CN 201610716565 A CN201610716565 A CN 201610716565A CN 106702729 A CN106702729 A CN 106702729A
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- carbon nano
- tube fibre
- nano tube
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- sputtering
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Abstract
The invention provides a method for aluminizing carbon nano tube fibers. The method comprises the steps that S1, cleanout fluid with oxidability is utilized for carrying out pretreatment on the carbon nano tube fibers so that the surfaces of the carbon nano tube fibers can have oxygen-containing functional groups; S2, the carbon nano tube fibers at least treated in S1 are preheated; S3, the carbon nano tube fibers treated in S2 are wound around a wire winding frame and then arranged in a sputtering cavity, the wire winding frame comprises a plurality of wire winding rods arranged at intervals, and an interval exists between every two turns of sputtering carbon nano tube fibers; S4, the carbon nano tube fibers wound around the wire winding frame are subjected to sputter coating with metal as a target material at preset temperature, wherein the target material and the wire winding frame have relative rotation. According to the method, aluminum particles are deposited on the surfaces of the carbon nano tube fibers in a physical vapor deposition mode, no harmful gas or harmful liquid is generated, and therefore the method is more environmentally friendly.
Description
Technical field
The present invention relates to the preparation field of composite, carbon nano-tube fibre is aluminized in particular it relates to a kind of
Method.
Background technology
In the prior art, it is generally required that the method aluminized using electrochemistry aluminizer on carbon nano-tube fibre.But,
When this method is aluminized, pollution is easily caused, also, aluminium film is not very fine and close.
Therefore, how in environmentally friendly manner carbon nano-tube fibre aluminize and asked as present invention technology urgently to be resolved hurrily
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 environment will not be polluted during plated film.
To achieve these goals, the present invention provides a kind of method aluminized to carbon nano-tube fibre, wherein, methods described
Including：
S1, the carbon nano-tube fibre is pre-processed using the cleaning fluid of oxidisability, to cause the CNT
The surface of fiber has oxygen-containing functional group；
S2, the pre-heat treatment is carried out to the carbon nano-tube fibre at least through step S1；
S3, will be arranged in sputtering chamber after the carbon nano-tube fibre of step S2 is wrapped on lacing stand, 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 aluminium as target at a predetermined temperature to being wrapped on the lacing stand splash
Plated film is penetrated, wherein, exist between the target and the lacing stand and relatively rotate.
Preferably, in the step S4, the target is arranged on outside the lacing stand, and the lacing stand is around itself axle
Line is rotated, and sets multiple targets, and multiple targets are set 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 by 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 100 DEG C for magnetron sputtering duration
To between 300 DEG C.
Preferably, step S4 includes：
S41, by the target and it is wound with after the lacing stand of carbon nano-tube fibre is arranged in the sputtering chamber respectively, it is right
The sputtering chamber vacuumize until the first preset air pressure；
S42, the sputtering chamber is carried out to be heated to the predetermined temperature；
S43, open radio-frequency power supply, and the radio-frequency power supply the unlatching duration between 1h to 3h.
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 cleaning fluid of the oxidisability includes hydrogen peroxide, and the concentration of the hydrogen peroxide is 10~30%.
Preferably, the process time of the step S1 is between 10min to 30min.
In method provided by the present invention, after step S1, the surface of carbon nano-tube fibre introduces oxygen-containing official
Can group, by step S2 after, the amorphous carbon in carbon nano-tube fibre is decomposed, so as to be conducive to aluminum particulate in step S4 to sink
Product is on the surface of carbon nano-tube fibre.When carbon nano-tube fibre is arranged on lacing stand, due to adjacent two circles CNT
There is gap between fiber, therefore, by magnetron bombardment produce aluminum particulate can through adjacent two circles carbon nano-tube fibre it
Between gap reach carbon nano-tube fibre not towards on the surface of target.Also, in step s 4, deposited between target and lacing stand
Relatively rotating, can equably plated film such that it is able to ensure to be wrapped in carbon nano-tube fibre on lacing stand.In the present invention,
Aluminum particulate is deposited on the surface of carbon nano-tube fibre in the way of physical vapour deposition (PVD), will not produce pernicious gas or harmful liquid
Body, therefore, method provided by the present invention is more environmentally-friendly.
Brief 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 that the present invention prepares the nanotube fibers of aluminizing that profit is obtained, and multiplication factor is 200 times；
Fig. 5 is the scanned picture of the carbon nano-tube fibre of aluminizing that embodiment 1 is obtained, and multiplication factor is 100 times；
Fig. 6 is the scanned picture of the carbon nano-tube fibre of aluminizing that embodiment 1 is obtained, and multiplication factor is 500 times；
Fig. 7 is the scanned picture of the copper facing carbon nano-tube fibre that embodiment 1 is obtained, and multiplication factor is 2000 times.
Description of reference numerals
100：Lacing stand 110：Wire winding rod
120：Rotating shaft 200：Carbon nano-tube fibre
300：Target
Specific embodiment
Specific embodiment of the 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 explain the present invention, and is not intended to limit the invention.
The present invention provides a kind of method to carbon nano-tube fibre plated film, wherein, methods described includes：
S1, the carbon nano-tube fibre is pre-processed using the cleaning fluid of oxidisability, to cause the CNT
The surface of fiber has oxygen-containing functional group；
S2, the pre-heat treatment is carried out to the carbon nano-tube fibre at least through step S1；
S3, will be arranged in sputtering chamber after the carbon nano-tube fibre 200 of step S2 is wrapped on lacing stand 100, around
Guide frame 100 includes multiple spaced wire winding rods 110, there is interval between adjacent two circles carbon nano-tube fibre 200；
S4, it is target 300 with metallic aluminium, the carbon nano-tube fibre 200 to being wrapped on lacing stand 100 at a predetermined temperature
Sputter coating is carried out, wherein, exist between target 300 and lacing stand 100 and relatively rotate.
In method provided by the present invention, after step S1, the surface of carbon nano-tube fibre introduces oxygen-containing official
Can group.In step s 4, metallic aluminium is deposited on when on the surface of carbon nano-tube fibre, can be reacted with oxygen-containing functional group,
Such that it is able to strengthen the adhesion between the aluminium film and carbon nano-tube fibre that ultimately form.
After by 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.Step S4 is carried out in the sputtering chamber of magnetron sputtering apparatus.
Shown in Fig. 1 be lacing stand 100 concrete structure, 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, the aluminum particulate produced by magnetron bombardment can be through between adjacent two circles carbon nano-tube fibre
Gap reaches carbon nano-tube fibre not towards on the surface of target 300.
Also, in step s3, exist between target 300 and lacing stand 100 and relatively rotate, such that it is able to ensure to be wrapped in
Carbon nano-tube fibre on lacing stand can equably plated film.In the present invention, aluminum particulate is 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.
In the present invention, special restriction is not done to the method for obtaining carbon nano-tube fibre.For example, it is possible to use array
Spin processes prepare carbon nano-tube fibre.How to prepare carbon nano-tube fibre using array spin processes is that those skilled in the art institute is public
Know, repeat no more here.
For the ease of setting, 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 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, rotating shaft 120 can be set 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.
Described " at least through step S1 " refers to and after by step S1, can directly be walked in step s 2
Rapid S2, it is also possible to after by step S1, then the step of carry out other, by other steps after, 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 by 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 refers to and carbon nano-tube fibre is put into the container for being provided with cleaning fluid, then using ultrasound
Wave apparatus are vibrated to cleaning fluid, and the impurity such that it is able to will adhere on carbon nano-tube fibre is removed.Specifically, using ultrasound
The step of succusion is cleaned to the carbon nano-tube fibre by step S1 includes：
To be put into the container for being contained with cleaning fluid by the carbon nano-fiber pipe fiber of step S1；
Said vesse is placed in 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 to target is not particularly limited.The particular number of target depends primarily on carbon and receives
The thickness of the aluminium film of mitron fiber surface.If it is desired to the relatively large aluminium 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
Aluminium film, then can set the relatively small number of target of quantity.
Also, in order to sputter the aluminium film thickness to be formed uniformly on the surface of carbon nano-tube fibre, and sputtering yield is improved,
Preferably, in the step S4, multiple targets 300 can be set, the plurality of target 300 is set around lacing stand 100.It is preferred that
Ground, each target 300 one magnetic control means of correspondence, so that multiple targets 300 can be controlled independently of one another.Operator can
The quantity of the target to be played a role according to the selection of specific technological requirement.
As a kind of preferred embodiment of the invention, 6 targets can be set, each target is along lacing stand 100
The other end of lacing stand 100 is axially extended to from one end of lacing stand 100.Preferably, it should be ensured that carbon is wound with lacing stand
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 that carbon nano-tube fibre preheated 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 is between 0.5h to 3h, so as to both may insure that the amorphous carbon in carbon nano-tube fibre can be with thorough
Bottom is decomposed and is volatilized, can prevent again because preheating temperature is too high and to carbon nano-tube fibre caused by damage.It is pointed out that step
Rapid S2 is not to be carried 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 aluminium target to state target, it is preferable that the power of the radio-frequency power supply is preferably between 0.1KW to 0.2KW.
Because aluminium has good ductility and good electric conductivity, therefore, aluminized on the surface of carbon nano-tube fibre
After film, can obtain that electric conductivity is good, the uniform composite of film forming, it is many that the composite is applied to wire, electrode etc.
Plant in applying.
When radio-frequency power supply power setting within the above range when, both can form densification on the surface of carbon nano-tube fibre
Aluminium film, the energy consumption in whole sputter procedure can be reduced again, also, can also improve what is aluminized on carbon nano-tube fibre surface
Efficiency.
For the aluminium 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 more long, obtain aluminium film thickness more
Greatly.Preferably, in step s3, magnetron sputtering duration is no more than 3 hours, such that it is able to prevent carbon nano-tube fibre
The aluminium 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 100 DEG C to 300 DEG C.When surface of the temperature within this range to carbon nano-tube fibre is aluminized, temperature is higher, deposits film forming
Speed it is faster.Similarly, the predetermined temperature is preferably more than 300 DEG C, such that it is able to ensure carbon nano-tube fibre in sputtering
During be not damaged.
In the present invention, in order to the aluminium film for preventing sputtering from being formed is oxidized, sputtering technology can under vacuum conditions be carried out.
Specifically, step S4 can include：
S41, by the target and it is wound with after the lacing stand of carbon nano-tube fibre is arranged in the sputtering chamber, to described
Sputtering chamber vacuumize until the first preset air pressure；
S42, the sputtering chamber is carried out to be 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 later less than 30 DEG C in sputtering cavity temperature
Vacuum system is closed, atmospheric pressure is reached to cavity pressure is sputtered to air is put into sputtering chamber, open sputtering chamber, the carbon that obtains aluminizing is received
Mitron fiber.
As another preferred embodiment of the invention, can be to being passed through protective gas in sputtering chamber.The protective gas
Do not reacted with carbon nano-tube fibre, also do not reacted with target.For example, protective gas can be argon gas or nitrogen, or, protect 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 it is wound with after the lacing stand of carbon nano-tube fibre is arranged in the sputtering chamber, to described
Sputtering chamber vacuumize up to the second preset air pressure, and to inert gas is passed through in the sputtering chamber, is passed through inert gas and holds
The continuous time is between 0.5h to 3h；
S42, the sputtering chamber is carried out to be 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 being made target.For example, when target is aluminium
When, inert gas can be argon gas.
Due to inert gas has been passed through in sputtering chamber, therefore, it can for the second preset air pressure be set to ratio in step S41
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 and splashed later less than 30 DEG C in cabin
The chamber door in chamber is penetrated, air is passed through, carbon nano-tube fibre of aluminizing is obtained.
Preferably, when step S42 is performed, 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 fine and close, continuous aluminium film.Certainly, the present invention is not limited thereto.
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 aluminium film that surface is smooth and fine and close.Being coated with the carbon nano-tube fibre of aluminium film has preferable 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 Scientists Friend Vacuum Technology Co., Ltd.
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
The high-purity anaerobic aluminum target for supplying.Carbon nano-tube fibre is the carbon nano-tube fibre of acquisition 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, by carbon nano-tube fibre immersion during concentration is 20% hydrogen peroxide again, soak time is 30min；
To be inserted in the container for filling absolute ethyl alcohol by the carbon nano-tube fibre of step S1, and the container is placed again
On ultrasonic equipment, ultrasonic equipment, duration 3min are opened；
S2, the pre-heat treatment is carried out to carbon nano-tube fibre in heat-treatment furnace, heating-up temperature is 100 DEG C, preheating time is
3h；
S3, will be arranged in sputtering chamber after the carbon nano-tube fibre 200 of step S2 is wrapped on lacing stand 100, 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 that will be wrapped on lacing stand 100 are arranged in sputtering chamber, with metallic aluminium as target
300, wherein, 6 targets are provided with sputtering chamber, 6 targets are uniformly arranged around lacing stand, sputtering chamber are closed, to sputtering chamber
Vacuumized, until 10-1Pa, the velocity of rotation of lacing stand 100 is 5r/min, and sputtering chamber is heated into 200 DEG C, and mode of heating is
Sensing heating, opens radio-frequency power supply, and power is 0.2KW, and sputtering continues 1h；
S5, closing shielding power supply, close heater, when later sputtering cavity temperature closes vacuum system less than 30 DEG C,
To air is put into sputtering chamber, atmospheric pressure is reached to sputtering cavity pressure, open sputtering chamber, take out lacing stand, obtain carbon of aluminizing
Nanotube fibers.
Shown in Fig. 5 be resulting carbon nano-tube fibre of aluminizing in the present embodiment 1 scanned picture, Fig. 6 and Fig. 7 institutes
What is shown is the enlarged drawing of Fig. 5.Be can see in from Fig. 5 to Fig. 7, aluminium film is fine and close and continuous.After tested, the plating that the present embodiment is obtained
The resistivity of aluminium carbon nano-tube fibre 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 implementation for using
Mode, but the invention is not limited in this.For those skilled in the art, essence of the invention is not being departed from
In the case of god and essence, various changes and modifications can be made therein, and these variations and modifications are also considered as protection scope of the present invention.
Claims (10)
1. a kind of method aluminized to carbon nano-tube fibre, it is characterised in that methods described includes：
S1, the carbon nano-tube fibre is pre-processed using the cleaning fluid of oxidisability, to cause the carbon nano-tube fibre
Surface there is oxygen-containing functional group；
S2, the pre-heat treatment is carried out to the carbon nano-tube fibre at least through step S1；
S3, will be arranged in sputtering chamber after the carbon nano-tube fibre of step S2 is wrapped on lacing stand, the lacing stand bag
Multiple spaced wire winding rods are included, there is interval between adjacent two circles carbon nano-tube fibre；
S4, the carbon nano-tube fibre with metallic aluminium as target at a predetermined temperature to being wrapped on the lacing stand carry out sputtering plating
Film, wherein, exist between the target and the lacing stand and relatively rotate.
2. method according to claim 1, it is characterised in that in the step S4, the target be arranged on it is described around
Outside guide frame, the lacing stand sets multiple targets around own axis, and multiple targets are around the wrapping wire
Frame is set.
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 by 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 100 DEG C to 300 DEG C.
6. method according to claim 4, it is characterised in that step S4 includes：
S41, by the target and it is wound with after the lacing stand of carbon nano-tube fibre is arranged in the sputtering chamber respectively, to described
Sputtering chamber vacuumize until the first preset air pressure；
S42, the sputtering chamber is carried out to be heated to the predetermined temperature；
S43, open radio-frequency power supply, and the radio-frequency power supply the unlatching duration between 1h to 3h.
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 cleaning fluid of the oxidisability includes hydrogen peroxide, described
The concentration of hydrogen peroxide is 10~30%.
10. method according to claim 9, it is characterised in that the process time of the step S1 is in 10min to 30min
Between.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610716565.9A CN106702729A (en) | 2016-08-25 | 2016-08-25 | Method for aluminizing carbon nano tube fibers |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610716565.9A CN106702729A (en) | 2016-08-25 | 2016-08-25 | Method for aluminizing carbon nano tube fibers |
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| CN201610716565.9A Pending CN106702729A (en) | 2016-08-25 | 2016-08-25 | Method for aluminizing carbon nano tube fibers |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109836130A (en) * | 2019-03-01 | 2019-06-04 | 姚晓东 | A kind of preparation method of safe high thermal conductivity floor heating material |
| WO2022217679A1 (en) * | 2021-04-13 | 2022-10-20 | 安徽工程大学 | Carbon fiber modification method and product thereof |
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| 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 |
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- 2016-08-25 CN CN201610716565.9A patent/CN106702729A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
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| YINGJIU ZHANG AT AL: ""Coating of carbon nanotubes with tungsten by physical vapor depositon"", 《SOLID STATE COMMUNICATION》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109836130A (en) * | 2019-03-01 | 2019-06-04 | 姚晓东 | A kind of preparation method of safe high thermal conductivity floor heating material |
| WO2022217679A1 (en) * | 2021-04-13 | 2022-10-20 | 安徽工程大学 | Carbon fiber modification method and product thereof |
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