CN106758171A - Composite carbon nanometer tube fiber and preparation method thereof - Google Patents
Composite carbon nanometer tube fiber and preparation method thereof Download PDFInfo
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- CN106758171A CN106758171A CN201610716562.5A CN201610716562A CN106758171A CN 106758171 A CN106758171 A CN 106758171A CN 201610716562 A CN201610716562 A CN 201610716562A CN 106758171 A CN106758171 A CN 106758171A
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Abstract
The present invention provides a kind of composite carbon nanometer tube fiber, wherein, the composite carbon nanometer tube fiber includes carbon nano-tube fibre core and coats the copper film of the core, and the carbon nano-tube fibre core includes the intermolecular copper molecule of carbon nano-tube fibre and infiltration in the carbon nano-tube fibre.The present invention also provides the preparation method of above-mentioned composite carbon nanometer tube fiber.The composite carbon nanometer tube fiber has more preferable electric conductivity.
Description
Technical field
The present invention relates to the preparation field of composite, in particular it relates to a kind of composite carbon nanometer tube fiber is combined with this
The preparation method of carbon nano-tube fibre.
Background technology
Carbon nano-tube fibre is a kind of emerging conductive material, and conductive good, density is low a little, in structural material
And field of functional materials has fabulous application prospect.But, the conductance of current carbon nano-tube fibre also differs from 1 compared with copper
To 2 orders of magnitude.
Therefore, the electric conductivity for how further improving carbon nano-tube fibre is asked as this area technology urgently to be resolved hurrily
Topic.
The content of the invention
It is an object of the invention to provide a kind of composite carbon nanometer tube fiber and the preparation side of the composite carbon nanometer tube fiber
Method, the composite carbon nanometer tube fiber obtained using the preparation method has electric conductivity higher.
To achieve these goals, the present invention provides a kind of composite carbon nanometer tube fiber, wherein, the composite carbon nanometer tube
Fiber includes carbon nano-tube fibre core and coats the copper film of the core, and the carbon nano-tube fibre core includes that CNT is fine
The intermolecular copper molecule in the carbon nano-tube fibre is permeated in peacekeeping.
Preferably, a diameter of 20-100 μm of the carbon nano-tube fibre core, the thickness of the copper film is 2-20 μm.
As another aspect of the present invention, there is provided a kind of preparation method of composite carbon nanometer tube fiber, wherein, the system
Preparation Method includes：
Infiltration treatment is carried out to carbon nano-tube fibre using the solution containing copper ion；
Mantoquita powder is arranged on the carbon nano-tube fibre surface after infiltration treatment；
The carbon nano-tube fibre that mantoquita powder will be provided with is put into reduction treatment is carried out in process cavity, is received with will be attached to carbon
The copper ion permeated in the carbon nano-tube fibre is reduced into copper point by the mantoquita powder reduction on mitron fiber into copper film
Son is obtaining composite carbon nanometer tube fiber.
Preferably, the step of infiltration treatment being carried out to carbon nano-tube fibre using the solution containing copper ion includes：
Carbon nano-tube fibre is immersed in the solution containing copper ion；
Ultrasonic oscillation is carried out to the solution containing copper ion immersed with carbon nano-tube fibre.
Preferably, the step of ultrasonic oscillation is carried out to the solution containing copper ion immersed with carbon nano-tube fibre
In, between 200Hz to 300Hz, the time of ultrasonic oscillation is between 20 minutes to 40 minutes for the frequency of ultrasonic oscillation.
Preferably, the solution containing copper ion includes copper sulphate supersaturated solution.
Preferably, the mantoquita powder includes anhydrous slufuric acid copper powders.
Preferably, the carbon nano-tube fibre that will be provided with mantoquita powder is put into process cavity the step of carrying out reduction treatment bag
Include：
The process cavity is vacuumized；
The process cavity that the carbon nano-tube fibre of mantoquita powder will be provided with is heated to first object temperature, and it is pre- to be incubated first
Fix time, to cause that copper sulphate resolves into cupric oxide；
To hydrogen is passed through in the process cavity of vacuum, cupric oxide is reduced into copper.
Preferably, the first object temperature is between 600 DEG C to 700 DEG C, first scheduled time at 20 minutes extremely
Between 40 minutes.
Preferably, the gas that will be produced in the step of being heated to target temperature to the carbon nano-tube fibre for being provided with mantoquita powder
Body be passed through can with the liquid of the gas reaction in.
Preferably, the carbon nano-tube fibre that will be provided with mantoquita powder is put into process cavity the step of carrying out reduction treatment bag
Including also includes：
Will be provided with the step of the process cavity of carbon nano-tube fibre of mantoquita powder is heated to first object temperature with to
Carried out between the step of being passed through hydrogen in the process cavity of vacuum the step of the process cavity is cooled into the second target temperature；With
And
After hydrogen is passed through in the process cavity of vacuum, the process cavity is kept into for second scheduled time in the second target temperature
The step of.
Preferably, second target temperature is between 200 DEG C to 300 DEG C, second scheduled time in 20min extremely
Between 40min.
Preferably, the preparation method is additionally included in and will be provided with the carbon nano-tube fibre of mantoquita powder and be put into process cavity
Carried out after the step of carrying out reduction treatment：
Process cavity is vacuumized；
Protective gas is passed through, untill air pressure in the process cavity is consistent with the process cavity external pressure.
In the carbon nano-tube fibre, it is coated on the copper film of carbon nano-tube fibre core surfaces and permeates in carbon nanometer
The intermolecular copper molecule of pipe fiber is respectively provided with preferable electric conductivity, therefore, composite carbon nanometer tube provided by the present invention is fine
Dimension also has preferable electric conductivity.
And, in composite carbon nanometer tube fiber provided by the present invention, carbon nano-tube fibre remains as main component, because
This, the composite carbon nanometer tube fiber still remains that carbon nano-tube fibre intensity is high, the low advantage of density.
Brief description of the drawings
Fig. 1 is the schematic diagram of the system for performing preparation method provided by the present invention；
Fig. 2 is the surface topography map of the composite carbon nanometer tube fiber that the embodiment of the present invention 1 is obtained, and multiplication factor is 250 times；
Fig. 3 is the internal morphology figure of the composite carbon nanometer tube fiber that the embodiment of the present invention 1 is obtained, and multiplication factor is 600 times；
Fig. 4 is the internal morphology figure of the composite carbon nanometer tube fiber that the embodiment of the present invention 1 is obtained, and multiplication factor is 3000
Times；
Fig. 5 is the inside microcell EDS figures of the composite carbon nanometer tube that the embodiment of the present invention 1 is obtained.
Description of reference numerals
100：Process cavity 200：Heating mantles
300：Hydrogen feeding pipe 400：Defeated argon pipe
500：Pumped vacuum systems 600：Tank
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.
As one aspect of the present invention, there is provided a kind of composite carbon nanometer tube fiber, wherein, the composite carbon nanometer tube is fine
Dimension includes carbon nano-tube fibre core and coats the copper film of the core, and the carbon nano-tube fibre core includes carbon nano-tube fibre
With infiltration the carbon nano-tube fibre intermolecular copper molecule.
The copper film and infiltration for being coated on carbon nano-tube fibre core surfaces divide in the intermolecular copper of carbon nano-tube fibre
Son is respectively provided with preferable electric conductivity, therefore, composite carbon nanometer tube fiber provided by the present invention also has preferable electric conductivity
Energy.
And, in composite carbon nanometer tube fiber provided by the present invention, carbon nano-tube fibre remains as main component, because
This, the composite carbon nanometer tube fiber still remains that carbon nano-tube fibre intensity is high, the low advantage of density.
Preferably, a diameter of 20-100 μm of the carbon nano-tube fibre core, the thickness of the copper film is 2-20 μm.
As another aspect of the present invention, there is provided the preparation method of above-mentioned composite carbon nanometer tube fiber, wherein, the system
Preparation Method includes：
S1, infiltration treatment is carried out to carbon nano-tube fibre using the solution containing copper ion；
S2, the carbon nano-tube fibre surface being arranged on mantoquita powder after infiltration treatment；
S3, the carbon nano-tube fibre that will be provided with mantoquita powder are put into reduction treatment are carried out in process cavity, will be attached to
Be reduced into for the copper ion permeated in the carbon nano-tube fibre into copper film by the mantoquita powder reduction on carbon nano-tube fibre
Copper molecule is obtaining composite carbon nanometer tube fiber.
In step sl, copper ion penetrates into the intermolecular of carbon nano-tube fibre.In step s 2, mantoquita powder is formed
On the surface of carbon nano-tube fibre.After step S3, copper ion and infiltration in the mantoquita on carbon nano-tube fibre surface
It is reduced in the intermolecular copper ion of carbon nano-tube fibre, obtains metallic copper.Positioned at the mantoquita quilt on carbon nano-tube fibre surface
Copper film is formed after reduction, the copper ion permeated in the carbon nano-tube fibre is reduced into copper molecule, it is hereby achieved that this hair
Bright provided above-mentioned composite carbon nanometer tube.
Preferably, upon step s 2, drying and processing can be carried out to the carbon nano-tube fibre for being provided with mantoquita powder.Should
Drying and processing can be carried out in vacuum drying chamber, and between 60 DEG C to 100 DEG C, the duration is 1h to 3h to drying temperature.
In the present invention, do not have not special requirement in carbon nano-tube fibre to how penetrating into copper ion, as
A kind of preferred embodiment of the invention, the step of permeating treatment is carried out using the solution containing copper ion to carbon nano-tube fibre
(that is, step S1) includes：
S11, carbon nano-tube fibre is immersed in the solution containing copper ion；
S12, ultrasonic oscillation is carried out to the solution containing copper ion immersed with carbon nano-tube fibre.
Ultrasonic oscillation can accelerate the movement velocity of copper ion, such that it is able to ensure that copper ion penetrates into CNT
In the molecular gap of fiber.
In the molecular gap of carbon nano-tube fibre being penetrated into order to ensure copper ion, it is preferable that to being received immersed with carbon
In the step of solution containing copper ion of mitron fiber carries out ultrasonic oscillation (that is, in step S12), the frequency of ultrasonic oscillation
Between 200Hz to 300Hz, the time of ultrasonic oscillation is between 20 minutes to 40 minutes for rate.
In the present invention, the solution containing copper ion is not required specifically, as long as being received with copper ion and not with carbon
Mitron fiber-reactive.Preferably, the solution containing copper ion includes copper sulphate supersaturated solution.Copper sulphate supersaturated solution
In sulfate ion and copper ion penetrate into the molecular gap of carbon nano-tube fibre together, copper sulphate is carried out at heating
Cupric oxide and SO that reason can live3Gas, SO3Gas is easily drained, and will not remain in composite carbon nanometer tube fibrous inside.
In order to reduce the impurity in composite carbon nanometer tube fiber, it is preferable that the mantoquita powder includes anhydrous slufuric acid copper powder
End.
As mentioned above it is possible, in remaining in composite carbon nanometer tube fiber in order to avoid sulfate ion, mantoquita will be provided with
The carbon nano-tube fibre of powder is put into process cavity the step of carrying out reduction treatment (that is, step S3) to be included：
S31, the process cavity is vacuumized；
S32, the process cavity of the carbon nano-tube fibre that will be provided with mantoquita powder are heated to first object temperature, and are incubated the
One scheduled time, to cause that copper sulphate resolves into cupric oxide；
S33, to hydrogen is passed through in the process cavity of vacuum, cupric oxide is reduced into copper.
In step S31, when air pressure reaches 10 in process cavity-3During below Pa, stop step S31.
In step s 32, the chemical mode of the reaction of generation is as follows：
CuSO4=CuO+SO3↑。
As mentioned above it is possible, SO3It is gas, is escaped after heating, in will not remaining in carbon nano-tube fibre, such that it is able to true
Protecting the final composite carbon nanometer tube fiber for obtaining has good electric conductivity.
In order to ensure copper sulphate can be decomposed thoroughly, it is preferable that the first object temperature between 600 DEG C to 700 DEG C,
First scheduled time is between 20 minutes to 40 minutes.
In order to avoid decomposing the SO for producing3Gas is polluted to air, it is preferable that can be by being provided with mantoquita powder
Gas for being produced in (that is, step S31) the step of be heated to first object temperature of carbon nano-tube fibre be passed through can with it is described
In the liquid of gas reaction.SO3Product after being reacted with liquid can also be recycled.
For example, can be by SO3Gas is passed through in water, SO3Gas and water reaction generation sulfuric acid, are shown below：
SO3+H2O=H2SO4。
Preferably, the carbon nano-tube fibre that will be provided with mantoquita powder is put into process cavity the step of carrying out reduction treatment bag
Include：
The process cavity is cooled to the second target temperature；And
After hydrogen is passed through in the process cavity of vacuum, the process cavity is kept into the second pre- timing in the second target temperature
Between.
Wherein, it is described to enter between step S32 and step S33 the step of the process cavity is cooled into the second target temperature
OK, after to hydrogen is passed through in the process cavity of vacuum, the process cavity is kept the step of second scheduled time in the second target temperature
Suddenly carried out after step S33.
In the present invention, the occurrence to second target temperature does not have special restriction, it is preferable that described
Under two target temperatures, reduction reaction both can rapidly occur, will not cause that the copper film excessive grain for obtaining is grown up again, so that can
To ensure that copper film can securely be fitted in the surface of carbon nano-tube fibre.Preferably, second target temperature at 200 DEG C extremely
Between 300 DEG C, second scheduled time is between 20min to 40min.
In order to obtain the more preferable composite carbon nanometer tube fiber of performance, it is preferable that the preparation method is additionally included in step S3
Carry out afterwards：
S4, process cavity is vacuumized；
S5, protective gas is passed through, untill air pressure in the process cavity is consistent with the process cavity external pressure.
By step S4, the water vapour in process cavity can be taken away.
After by step S5, the copper film of composite carbon nanometer tube fiber surface can be prevented to be oxidized.
Shown in Fig. 1 is the system for performing preparation method provided by the present invention.As shown in figure 1, the system includes
Tubular type hydrogen treatment furnace, the tubular type hydrogen treatment furnace includes process cavity 100 and the heating mantles 200 being set in outside the process cavity 100.
Hydrogen feeding pipe 300 for being passed through hydrogen is connected with the inside of process cavity 100, defeated argon pipe 400 and process cavity 100 for being passed through argon gas
Inside connection, inside of the pumped vacuum systems 500 also with process cavity 100 connects.The delivery outlet of pumped vacuum systems 500 also with tank
600 connections, the gas of generation is passed through in tank.
In the present invention, switch valve is provided with hydrogen feeding pipe 300, controls to be passed through the flow of hydrogen by controlling switch valve
Be passed through the time.Preferably, can with the speed of 1L/min to hydrogen is passed through in the tubular type hydrogen treatment furnace, be passed through hydrogen when
Between to continue 90s be the concentration needed for the density of hydrogen that may be such that in the tubular type hydrogen treatment furnace reaches reaction.It is then turned off described
Switch valve, is incubated second scheduled time.
Similarly, switch valve is also equipped with defeated argon pipe 400, can controls to be passed through the moment of argon gas by controlling switch valve
And the duration.
Embodiment 1
Profit prepares composite carbon nanometer tube fiber with the following method：
S11,10cm is long, diameter is about 100 μm of CNT and is put into the beaker for filling supersaturated copper-bath；
S12, will be equipped with supersaturated copper-bath and carbon nano-tube fibre beaker be placed on supersonic wave cleaning machine in surpass
30min is swung in acoustic shock, and frequency is 280Hz；
S2, carbon nano-tube fibre after immersion is chosen from supersaturated copper-bath with tweezers are careful, and at it
Its surface is set to be stained with anhydrous slufuric acid copper powders by way of sprinkling before surface is unseasoned；
S21, will be stained with copper sulphate powder carbon nano-tube fibre be placed in vacuum drying chamber dry, drying temperature is 80
DEG C, the time is 2h；
S31, dried carbon nano-tube fibre is put into during tubular type puts hydrogen stove, is taken out very using mechanical pump and molecular pump camera
Sky, vacuum reaches 10-3Below Pa；
S32 and then 650 DEG C of first object temperature is warming up in 60min, is incubated the first scheduled time 30min, and will
The gas of discharge is passed through tank；
Stove is cooled to the 250 DEG C of insulations of the second predetermined temperature, closes pumped vacuum systems；
S33 and with the speed of 1L/min to put in hydrogen stove lead to H2, lead to H2Time is 90s, closes logical H2Valve；
It is incubated the second scheduled time 30min；
S4, opening pumped vacuum systems, take vapor in stove away, are then shut off pumped vacuum systems；
S5 and to being passed through Ar in stove2, when air pressure in stove is equal with atmospheric pressure, close Ar2, fire door is opened, take out compound
Carbon nano-tube fibre sample.
The surface of composite carbon nanometer tube fiber and internal morphology using scanning electron microscopic observation, and analyzed using EDS multiple
The surface of compound/carbon nano pipe fiber and the material of inside.
Analyzed by the surface of composite carbon nanometer tube fiber described in scanning electron microscopic observation and internal morphology and power spectrum EDS.
As shown in Figure 2, carbon nano-tube fibre surface uniform fold has copper film, and copper film is completely continuously coated on fiber table
Face.By the way that in Fig. 3, copper film comes into fibrous inside, continuous copper compound structure is formed.As shown in Figure 4, copper atom with
The form of crystal is deposited on fiber surface, contacts tight between crystal grain, and imporosity is present, it was demonstrated that copper film compactness is good.
As shown in Figure 5, the corresponding peak value of copper is significantly larger than carbon correspondence peak value, and this explanation composite fiber surface is mainly copper, basic card
Bright copper film completely covers fiber surface.After tested, the electrical conductivity of the composite carbon nanometer tube fiber that embodiment 1 is obtained can be with
Reach 4.5 × 107S/m, already close to the electrical conductivity of copper.
Implement 2
Composite carbon nanometer tube fiber is prepared using the method described in embodiment 1, difference is：
In step s 12, the ultrasonic vibration time is 40min, and frequency is 300Hz；
In the step s 21, drying temperature is 90 DEG C, and the time is 1h；
In step s 32, first object temperature is 700 DEG C, is incubated the first scheduled time 20min；
Subsequent stove is cooled to 200 DEG C of the second predetermined temperature；
40min is incubated after being passed through hydrogen.
The conductance for implementing the 2 composite carbon nanometer tube fibers for obtaining is 5.2 × 107S/m。
Embodiment 3
Composite carbon nanometer tube fiber is prepared using the method described in embodiment 1, difference is：
In step s 12, the ultrasonic vibration time is 20min, and frequency is 200Hz；
In the step s 21, drying temperature is 60 DEG C, and the time is 3h；
In step s 32, first object temperature is 600 DEG C, is incubated the first scheduled time 40min；
Subsequent stove is cooled to 300 DEG C of the second predetermined temperature；
20min is incubated after being passed through hydrogen.
The conductance for implementing the 3 composite carbon nanometer tube fibers for obtaining is 4.1 × 107S/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 (13)
1. a kind of composite carbon nanometer tube fiber, it is characterised in that the composite carbon nanometer tube fiber includes carbon nano-tube fibre core
Material and the copper film for coating the core, the carbon nano-tube fibre core include carbon nano-tube fibre and infiltration in CNT fibre
The intermolecular copper molecule of dimension.
2. composite carbon nanometer tube fiber according to claim 1, it is characterised in that the carbon nano-tube fibre core it is straight
Footpath is 20-100 μm, and the thickness of the copper film is 2-20 μm.
3. a kind of preparation method of composite carbon nanometer tube fiber, it is characterised in that the preparation method includes：
Infiltration treatment is carried out to carbon nano-tube fibre using the solution containing copper ion；
Mantoquita powder is arranged on the carbon nano-tube fibre surface after infiltration treatment；
The carbon nano-tube fibre that mantoquita powder will be provided with is put into reduction treatment is carried out in process cavity, will be attached to CNT
Mantoquita powder reduction on fiber into copper film, and will permeate copper ion in the carbon nano-tube fibre be reduced into copper molecule with
Obtain composite carbon nanometer tube fiber.
4. preparation method according to claim 3, it is characterised in that fine to CNT using the solution containing copper ion
The step of dimension carries out infiltration treatment includes：
Carbon nano-tube fibre is immersed in the solution containing copper ion；
Ultrasonic oscillation is carried out to the solution containing copper ion immersed with carbon nano-tube fibre.
5. preparation method according to claim 4, it is characterised in that to immersed with carbon nano-tube fibre containing copper from
During the solution of son is the step of carry out ultrasonic oscillation, the frequency of ultrasonic oscillation between 200Hz to 300Hz, ultrasonic oscillation
Time between 20 minutes to 40 minutes.
6. the preparation method according to any one in claim 3 to 5, it is characterised in that the solution bag containing copper ion
Include copper sulphate supersaturated solution.
7. preparation method according to claim 6, it is characterised in that the mantoquita powder includes anhydrous slufuric acid copper powders.
8. preparation method according to claim 7, it is characterised in that the carbon nano-tube fibre that will be provided with mantoquita powder is put
The step of entering carried out in process cavity reduction treatment includes：
The process cavity is vacuumized；
The process cavity that the carbon nano-tube fibre of mantoquita powder will be provided with is heated to first object temperature, and is incubated the first pre- timing
Between, to cause that copper sulphate resolves into cupric oxide；
To hydrogen is passed through in the process cavity of vacuum, cupric oxide is reduced into copper.
9. preparation method according to claim 8, it is characterised in that the first object temperature 600 DEG C to 700 DEG C it
Between, first scheduled time is between 20 minutes to 40 minutes.
10. preparation method according to claim 8, it is characterised in that will be fine to being provided with the CNT of mantoquita powder
Dimension the step of be heated to target temperature in the gas that produces be passed through can with the liquid of the gas reaction in.
11. preparation methods according to claim 8, it is characterised in that the carbon nano-tube fibre of mantoquita powder will be provided with
Being put into process cavity the step of carrying out reduction treatment includes also including：
To be provided with the step of the process cavity of carbon nano-tube fibre of mantoquita powder is heated to first object temperature and to vacuum
Process cavity in the step of be passed through hydrogen between carry out the step of the process cavity is cooled into the second target temperature；And to
After being passed through hydrogen in the process cavity of vacuum, by the process cavity the step of the second target temperature is kept for second scheduled time.
12. preparation methods according to claim 11, it is characterised in that second target temperature is at 200 DEG C to 300 DEG C
Between, second scheduled time is between 20min to 40min.
13. preparation methods according to claim 8, it is characterised in that the preparation method is additionally included in will be provided with copper
The carbon nano-tube fibre of salt powder is put into process cavity after the step of carrying out reduction treatment what is carried out：
Process cavity is vacuumized；
Protective gas is passed through, untill air pressure in the process cavity is consistent with the process cavity external pressure.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110871270A (en) * | 2018-09-04 | 2020-03-10 | 天津大学 | Preparation method of high-elasticity high-heat-conductivity three-dimensional carbon nanotube composite material |
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Application publication date: 20170531 |