CN107381538B - A kind of preparation method of carbon nanotube - Google Patents
A kind of preparation method of carbon nanotube Download PDFInfo
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- CN107381538B CN107381538B CN201610326216.6A CN201610326216A CN107381538B CN 107381538 B CN107381538 B CN 107381538B CN 201610326216 A CN201610326216 A CN 201610326216A CN 107381538 B CN107381538 B CN 107381538B
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- C01B2202/00—Structure or properties of carbon nanotubes
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- C01P2004/00—Particle morphology
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
Abstract
The present invention provides a kind of preparation methods of carbon nanotube, comprising the following steps: metal net mask is placed in the cavity of PECVD device on negative plate, two blocks of catalyst metals plates of superposition are placed above the metal net mask；The cavity of the PEVCD equipment is heated and is passed through reaction gas thereto, powers on, catalyst granules is obtained after reaction；It is passed through carbon source and carrier gas after the cavity of PEVCD equipment is heated, powers on, carbon nanotube is obtained after reaction.The application catalyst metal particles and carbon nanotube are completed in same PECVD cavity, and can be realized continuous preparation, improve the efficiency of carbon nanotube preparation；On the other hand, low temperature preparation makes carbon nanotube can be applied to the fields of many non-refractories.
Description
Technical field
The present invention relates to carbon nanotube technology field more particularly to a kind of low temperature preparing methods of carbon nanotube.
Background technique
Carbon nanotube has the performances such as excellent mechanics, electricity, optics and Flied emission, therefore carbon nanotube since 1991
Since being found, preparation, performance and the application of carbon nanotube are all had received widespread attention.At present about the system of carbon nanotube
Preparation Method mainly has arc discharge method, laser evaporization method and chemical vapour deposition technique.Wherein arc discharge method is in hot conditions
Under, it is ionized using reaction gas, the method for making graphite electrode surface evaporation obtain carbon nanotube, reaction is violent, it is difficult to control
The structure of the carbon nanotube of generation；Laser evaporization method be focused under the high temperature conditions using high energy laser beam metallic catalyst and
On the target of graphite mixing, the process of carbon nanotube is generated with catalytic action by evaporating；Chemical vapor deposition method is to utilize
Metal catalyst particles are as template, and under conditions of 600~1200 DEG C, pyrolysis gaseous hydrocarbon generates carbon nanotube.Chemical gaseous phase
The reaction process of deposition method preparation carbon nanotube is easy to control and at low cost, is suitable for a large amount of synthesis.
However, traditional thermal chemical vapor deposition reaction temperature is excessively high, condition is harsh, limits carbon nanotube in microelectronics
The application of the temperature sensitive Material Field such as material and high molecular material.In addition to this, currently, in the process for preparing carbon nanotube
In, thermal chemical vapor deposition method use catalyst fines be usually it is well prepared in advance, due to Van der Waals between nanometer powder
The effect of power can usually generate reunion, and then influence the preparation efficiency and appearance structure of carbon nanotube.How carbon nanotube is reduced
The cost of preparation simplifies the critical issue that preparation process is current carbon nanotube preparation, research and application.
Summary of the invention
Present invention solves the technical problem that being to provide a kind of low temperature preparation method of carbon nanotube.
In view of this, this application provides a kind of preparation methods of carbon nanotube, comprising the following steps:
A), metal net mask is placed in the cavity of PECVD device on negative plate, superposition is placed above the metal net mask
Two blocks of catalyst metals plates；
B), the cavity of the PEVCD equipment is heated and is passed through reaction gas thereto, powered on, obtained after reaction
Catalyst metal particles；
C), it is passed through carbon source and carrier gas after the cavity of the PEVCD equipment being heated, powers on, carbon is obtained after reaction and is received
Mitron.
Preferably, the distance between described two blocks of catalyst metals plates are 1~5cm, the material of the catalyst metals plate
For iron, cobalt, nickel or composite material, the catalyst metals plate surface is provided with pierced pattern.
Preferably, step A) described in reaction gas be selected from one or both of hydrogen and argon gas, the reaction gas
Flow be 50~100sccm, the power of the power supply is 500~1000W.
Preferably, the partial size of the catalyst metal particles is 1~50nm.
Preferably, step C) described in carbon source include one of methane, ethyl alcohol, acetylene and normal butane or a variety of, it is described
The flow of carbon source is 5~50sccm.
Preferably, the carrier gas is selected from one of hydrogen, nitrogen and argon gas or a variety of, and the flow of the carrier gas is 100
~150sccm.
Preferably, step C) described in the temperature of reaction be 350~500 DEG C, the power of the power supply is 10~100W, institute
The time for stating reaction is 10~100min.
Preferably, the metal net mask is cylindric stainless steel mesh enclosure or cylindric copper mesh cover.
This application provides a kind of preparation methods of array carbon nano tube, and metal net mask is placed in PEVCD equipment first
On negative plate in cavity, place two blocks of catalyst metals plates of superposition above metal net mask, then by cavity heat and to its
In be passed through reaction gas, power on, the intracorporal reaction gas of electric field excitation cavity, so that it becomes plasma, passes through control chamber
Internal air pressure makes to generate hollow cathode effect between metal plate, utilizes the high energy high-density plasma in hollow cathode effect region
Bombard sheet metal, sputter nanocatalyst metallic particles, continue heating reach reaction temperature after, carbon source is passed through into cavity
With carrier gas, power on, decomposes the nanoparticle growth generated using catalyst metal particles and go out carbon nanotube.The application carbon is received
During mitron free growth, using the metal net mask of auxiliary, the effective activity for improving plasma is more effectively decomposed
Carbon-source gas realizes low temperature preparation of the carbon nanotube at 350~500 DEG C, so that in the electronic device surface in situ of non-refractory
Preparing array carbon nano tube film becomes feasible, has widened its application prospect.
Detailed description of the invention
Fig. 1 is the schematic diagram of the PECVD device that the present invention uses and metal net mask device；
Fig. 2 is the stereoscan photograph of carbon nanotube prepared by the embodiment of the present invention 1；
Fig. 3 is the transmission electron microscope photo of carbon nanotube prepared by the embodiment of the present invention 1；
Fig. 4 is the stereoscan photograph of carbon nanotube prepared by the embodiment of the present invention 2；
Fig. 5 is the transmission electron microscope photo of carbon nanotube prepared by the embodiment of the present invention 2；
Fig. 6 is the stereoscan photograph of carbon nanotube prepared by the embodiment of the present invention 3；
Fig. 7 is the transmission electron microscope photo of carbon nanotube prepared by the embodiment of the present invention 3.
Specific embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described below with reference to embodiment, still
It should be appreciated that these descriptions are only further explanation the features and advantages of the present invention, rather than to the claims in the present invention
Limitation.
The embodiment of the invention discloses a kind of preparation methods of array carbon nano tube film, comprising the following steps:
A), metal net mask is placed in the cavity of PECVD device on negative plate, superposition is placed above the metal net mask
Two blocks of catalyst metals plates；
B), the cavity of the PEVCD equipment is heated and is passed through reaction gas thereto, powered on, obtained after reaction
Catalyst granules；
C), it is passed through carbon source and carrier gas after the cavity of PEVCD equipment being heated, powers on, carbon nanotube is obtained after reaction.
This application provides a kind of preparation method of carbon nanotube, the carbon nanotube of the application preparation is really a kind of no base
The free growing carbon nanotube in bottom.The catalyst metal particles that the application sputters fall in cathode plate, it is difficult to generate with the surface
It effectively combines, therefore the carbon nanotube of the application is into existing for particle.This method utilizes the booster action of metal net mask, realizes
The low temperature preparation of nano-tube film.
The preparation method of the application carbon nanotube includes the preparation and low temperature carbon nanotube of nanocatalyst metallic particles
Two steps are prepared, and two steps are continuously finished in the same PECVD reaction cavity.
The application carries out the preparation of nanocatalyst metallic particles first.As shown in FIG. 1, FIG. 1 is carbon nanotubes of the present invention
The schematic device of the PECVD device of preparation.Metal net mask is placed in negative plate in the cavity of PECVD device first by the application
On, two blocks of catalyst metals plates for being sequentially overlapped placement are placed above metal net mask.Herein described PECVD cavity is
The reaction cavity of PECVD device, the PECVD device is equipment well known to those skilled in the art, to this application without spy
Other limitation, the PECVD device that the application uses is preferably as shown in Figure 1, metal net mask is urged with two pieces in PECVD reaction cavity
The setting of agent metal plate specifically: the metal net mask is placed on bottom crown, the top of the metal net mask and and metal
What mesh enclosure directly contacted is provided with two blocks of catalyst metals plates being sequentially overlapped, and the metal net mask is respectively provided with catalyst sheet
Between top crown and bottom crown.Herein described metal net mask can be cylindric stainless steel mesh enclosure or cylindric copper mesh cover.
Herein described catalyst sheet surface is provided with pierced pattern, to increase the quantity for being splashed to catalyst granules on cathode plate,
The pierced pattern can be round or other shapes, be not particularly limited to this application.Herein described two
The spacing of block catalyst metals plate is preferably 1~5cm.The catalyst metals plate is preferably iron, cobalt, nickel or composition metal material
Material, herein described catalyst metals plate is preferably same metal material.
During preparing catalyst nano-particles, the cavity of PECVD device is heated first and is led into PECVD cavity
Enter reaction gas, powers on after reaching predetermined temperature, the intracorporal reaction gas of electric field excitation cavity, so that it becomes plasma,
By controlling the intracorporal gas pressure of PECVD chamber, so that generating hollow cathode effect between two plate of catalyst.Utilize the sky of generation
The high energy high-density plasma in the heart-yin polar effect region bombards sheet metal, sputters nano-metal particle.Two pieces of catalyst
The distance between thin plate is to control the plasma density generated between metal plate, under certain reaction pressure and power,
It obtains the very high plasma of density to be used to bombard metal surface, sputters nano-metal particle.In the process, metal net mask
For the effect of cathode plate and catalytic metal plate to be connected, so that hollow cathode effect can be generated between metal plate.In above-mentioned mistake
Cheng Zhong, the reaction gas are preferably one or both of argon gas and hydrogen, by control electric field power and are selected properly
Reaction gas, the catalyst granules of different-grain diameter can be obtained, size range is 1~50nm.The stream of the reaction gas
Amount is preferably 50~100sccm, and in embodiment, the reaction gas is preferably hydrogen and argon gas, and the flow of the argon gas is excellent
It is selected as 50~80sccm, the flow of the hydrogen is preferably 20~50sccm.Power is preferably 500~1000W, example
, the power is preferably 600~800W.The temperature powered on is preferably 300~400 DEG C.According to the present invention,
The PECVD device is preferably evacuated to 10- before by the heating of the cavity of the PECVD device4Pa。
The application makes nanocatalyst by exciting sputtering to generate nano-catalyst particles in PECVD vacuum cavity
The size of grain is relatively uniform, and the sputtering along different directions reduces the reunion of nano particle, while avoiding oxidation and urging nanometer
The influence of agent metallic particles performance.
After catalyst metal particles are prepared, the application then continues to carry out carbon nanotube in PECVD cavity
Preparation.This process realizes the low temperature preparation of carbon nanotube using metal net mask device.Detailed process are as follows: by PECVD device
Cavity is passed through carbon-source gas and carrier gas after continuing heating, powers on, carbon nanotube is obtained after reaction.During this, metal mesh
On the one hand cover improves the temperature of conversion zone, on the other hand can adsorb high energy particle, reduces corrasion, and is conducive to freely
Grow carbon nanotube.The application is not particularly limited the carbon source with carrier gas, is carbon well known to those skilled in the art
Source and carrier gas, the carbon source is preferably selected from one of methane, ethyl alcohol, acetylene and normal butane or a variety of, described exemplary, described
Carbon source is preferably selected from acetylene, and the carrier gas is preferably selected from one of argon gas, nitrogen and hydrogen or a variety of, exemplary, the load
Gas is preferably selected from the mixed gas or argon gas of argon gas and hydrogen, the mixed gas of hydrogen and nitrogen.Argon gas and hydrogen are as carrier gas
Mainly play two aspects, on the one hand, by being passed through for carrier gas, the intracorporal air pressure of reaction chamber is controlled, so that plasma field holds
Easily it is excited；On the other hand, it is passed through the growth that carrier gas effectively dilutes carbon-source gas and is conducive to carbon nanotube, this is because working as carbon
When ratio of the source gas in reaction cavity is higher, prepared by reaction tends to generate amorphous carbon, rather than carbon nanotube.It is preparing
During carbon nanotube, the ratio of carbon-source gas is controlled preferably 5%-20%.
The carbon-source gas that the PECVD device used in the application is passed through during the preparation process is preferably 5sccm~50sccm,
In embodiment, the flow of the carbon source is preferably 10~20sccm.The flow of the carrier gas is preferably 100~150sccm, is shown
Example, the flow of the argon gas in the carrier gas is preferably 50~80sccm, and the flow of hydrogen is preferably 60~70sccm, the nitrogen
The flow of gas is preferably 5~10sccm.The time of the reaction is preferably 10~100min, exemplary, and the reaction time is excellent
It is selected as 30~60min；The temperature of the reaction is preferably 350~500 DEG C, and power is preferably 10~100W, exemplary, institute
Stating power is preferably 30~60W.
The application can be by adjusting corresponding response parameter, such as reaction temperature, power, gas flow and reaction time
Deng can control the morphology and size for the catalyst being prepared, and then pattern, structure and the ruler of carbon nanotube can be influenced
It is very little.The present invention can realize the preparation of carbon nanotube, while the carbon nanotube being prepared is equal under conditions of being lower than 500 DEG C
For multi-walled carbon nanotube.
As the common sense of this field, although Preparation equipment used by this example is radio frequency PECVD, the preparation method institute
The device of use is equally applicable to the similar equipment such as direct current PECVD.It the present invention and traditional thermal chemical vapor deposition and waits
The method of gas ions enhancing chemical vapor deposition preparation carbon nanotube is compared, and advantage is the electric field preparation catalysis using PECVD
Agent particle, without being additionally provided catalyst；The ingredient of catalyst granules can be controlled by selecting the metal plate of different materials
System.By the power for controlling electric field, moreover it is possible to the effectively size of control catalyst granules.At the same time, due to entire catalyst system
The problems such as during standby, all completing in a vacuum, avoiding the oxidation encountered in traditional handicraft catalyst transfer process, pollution,
The reunion of catalyst granules can also be avoided to a certain extent.
Metal net mask technology of the present invention can effectively reduce the temperature that reaction generates carbon nanotube, 350
Under conditions of~500 DEG C, the preparation of carbon nanotube is realized.Present approach reduces energy consumed by preparation carbon nanotube.With this
Meanwhile realize the low temperature preparation of carbon nanotube, can aid in and the combination of other technologies, such as realize carbon nanotube with it is some low
Temperature alloy or high molecular material it is compound etc., expanded the application field of carbon nanotube significantly.
For a further understanding of the present invention, below with reference to embodiment to the system of array carbon nano tube film provided by the invention
Preparation Method is described in detail, and protection scope of the present invention is not limited by the following examples.
Embodiment 1
A method of preparing carbon nanotube at 400 DEG C, method includes the following steps:
Step 1: two pieces of catalyst metals thin plates are placed at the metal net mask made using 316 stainless steels, metal net mask top,
For the thin plate used in the present embodiment for 316 stainless steel substrates, the spacing between two plates is 1cm, and metal net mask is placed under PECVD
On pole plate.
Step 2: reaction cavity is evacuated to 10-4After Pa, argon gas and hydrogen are passed through into cavity, flow is respectively
60sccm and 30sccm；After being heated to 350 DEG C, startup power supply, power setting 600W, sputtering time 10min；Electric field excitation
The intracorporal argon gas of chamber and hydrogen generate plasma；By the intracorporal gas pressure of control chamber, so that between catalyst metals plate
Hollow cathode effect is generated, a plasma enrichment region is generated between sheet metal, the highdensity plasma of high energy is held
Continuous bombardment sheet metal, so that nanocatalyst metallic particles is sputtered out from metal sheet surface；
Step 3: on the basis of step 2, continuing to heat, bottom crown temperature is made to reach 400 DEG C；At the same time, to cavity
It is inside passed through carbon-source gas (acetylene) and carrier gas (argon gas and hydrogen), gas flow is respectively 10sccm, 60sccm, 30sccm, electricity
The power adjustment in source is 50W, reaction time 30min；
Step 4: after reaction, closing power supply, stop heating, continue to be passed through argon gas and hydrogen, carbon source is closed, with furnace
It is cooled to room temperature, obtains carbon nanotube.
By the length in control reaction time in the present embodiment, the carbon nanotube of different length can be obtained.It is urged in metal
In agent preparation process, argon ion and hydrionic main function are bombardment metal plates, generate catalyst granules；Carbon nanotube is raw
In growth process, argon ion and hydrogen ion can effectively inhibit the generation of amorphous carbon, promote carbon nanotube continued propagation.The present embodiment system
SEM the and TEM photo difference of standby carbon nanotube is as shown in Figures 2 and 3.
Embodiment 2
A method of preparing carbon nanotube under the conditions of 500 DEG C, method includes the following steps:
Step 1: using Ni plate and 316 stainless steel plates as catalyst plates in the present embodiment, two plate spacings are 1cm, remaining
It is arranged with the step 1 in embodiment 1.
Step 2: reaction cavity is evacuated to 10-4After Pa, argon gas and hydrogen are passed through into cavity, flow is respectively
50sccm and 20sccm；After being heated to 300 DEG C, startup power supply, power setting 500W；The argon ion and hydrogen ion of electric field excitation
Constant bombardment catalyst metals plate, to sputter catalyst granules；The present embodiment improves catalyst particles by using Ni plate
The content of Ni element in grain.
Step 3: heating makes bottom crown temperature reach 500 DEG C；At the same time, be passed through into cavity carbon-source gas (acetylene) and
Carrier gas (argon gas and hydrogen), gas flow is respectively 5sccm, 50sccm, 20sccm；The power adjustment of power supply is 30W, when reaction
Between be 30min.
Step 4: with 1 step 4 of embodiment.
Embodiment 2 has the variation of three aspects with respect to embodiment 1: first is that using Ni metal plate, it is therefore intended that improve catalysis
The content of Ni element in agent particle promotes the growth of carbon nanotube using its activity；Two are reduction of in sputtering reaction process
Gas flow, while temperature and power when sputtering are reduced, and then reduce preparation cost, raising efficiency；Third is that changing carbon
The growth temperature of nanotube reduces the flow and reaction power of carbon-source gas, by adjusting parameter, it is intended to obtain impurity more
It is few, the faster carbon nanotube of growth rate.SEM the and TEM photo of carbon nanotube manufactured in the present embodiment is respectively such as Fig. 4 and Fig. 5
It is shown.
Embodiment 3
A method of nitrogen-doping carbon nanotube is prepared under the conditions of 500 DEG C.The preparation method the following steps are included:
Step 1: preparing the condition of the process of catalyst granules with step 1 in embodiment 2；
Step 2: with step 2 in embodiment 2；
Step 3: heating makes bottom crown temperature reach 500 DEG C；At the same time, be passed through into cavity acetylene, argon gas, hydrogen and
Nitrogen, gas flow are respectively 5sccm, 50sccm, 20sccm, 5sccm；The power adjustment of power supply is 30W, and the reaction time is
30min。
Step 4: with 1 step 4 of embodiment.
The main distinction of this example and embodiment 1 is to be passed through N during growing carbon nanotube2As auxiliary gas,
To investigate influence of the N element doping for carbon nano tube growth.SEM the and TEM photo of carbon nanotube manufactured in the present embodiment point
Not not as shown in Figure 6 and Figure 7.
The above description of the embodiment is only used to help understand the method for the present invention and its core ideas.It should be pointed out that pair
For those skilled in the art, without departing from the principle of the present invention, the present invention can also be carried out
Some improvements and modifications, these improvements and modifications also fall within the scope of protection of the claims of the present invention.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention.
Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein
General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention
It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one
The widest scope of cause.
Claims (7)
1. a kind of preparation method of carbon nanotube, comprising the following steps:
A), metal net mask is placed in the cavity of PECVD device on negative plate, the two of superposition is placed above the metal net mask
Block catalyst metals plate；
B), the cavity of the PEVCD equipment is heated and is passed through reaction gas thereto, powered on, using between metal plate
Hollow cathode effect sputtering generates catalyst metal particles；
C), it is passed through carbon source and carrier gas after the cavity of the PEVCD equipment being heated, powers on, carbon nanotube is obtained after reaction；
Step A) described in reaction gas be selected from one or both of hydrogen and argon gas, the flow of the reaction gas is 50~
100sccm, the power of the power supply are 500~1000W.
2. preparation method according to claim 1, which is characterized in that the distance between described two blocks of catalyst metals plates are
The material of 1~5cm, the catalyst metals plate are iron, cobalt, nickel or composite material, and the catalyst metals plate surface is set
It is equipped with pierced pattern.
3. preparation method according to claim 1, which is characterized in that the partial size of the catalyst metal particles be 1~
50nm。
4. preparation method according to claim 1, which is characterized in that step C) described in carbon source include methane, ethyl alcohol, second
One of alkynes and normal butane are a variety of, and the flow of the carbon source is 5~50sccm.
5. preparation method according to claim 1, which is characterized in that the carrier gas is in hydrogen, nitrogen and argon gas
One or more, the flow of the carrier gas is 100~150sccm.
6. preparation method according to claim 1, which is characterized in that step C) described in reaction temperature be 350~500
DEG C, the power of the power supply is 10~100W, and the time of the reaction is 10~100min.
7. preparation method according to claim 1, which is characterized in that the metal net mask be cylindric stainless steel mesh enclosure or
Cylindric copper mesh cover.
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