CN107381538A - A kind of preparation method of CNT - Google Patents
A kind of preparation method of CNT Download PDFInfo
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- CN107381538A CN107381538A CN201610326216.6A CN201610326216A CN107381538A CN 107381538 A CN107381538 A CN 107381538A CN 201610326216 A CN201610326216 A CN 201610326216A CN 107381538 A CN107381538 A CN 107381538A
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- C01B2202/00—Structure or properties of carbon nanotubes
- C01B2202/06—Multi-walled nanotubes
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/01—Crystal-structural characteristics depicted by a TEM-image
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- 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 invention provides a kind of preparation method of CNT, comprise 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 reacting gas thereto, switches on power, catalyst granules is obtained after reaction；Carbon source and carrier gas will be passed through after the cavity heating of PEVCD equipment, switch on power, CNT is obtained after reaction.The application catalyst metal particles and CNT are completed in same PECVD cavitys, and can realize continuous preparation, improve the efficiency of CNT preparation；On the other hand, low temperature preparation enable CNT be applied to many non-refractories field.
Description
Technical field
The present invention relates to carbon nanotube technology field, more particularly to a kind of low temperature preparation method of CNT.
Background technology
Since CNT has the performances such as excellent mechanics, electricity, optics and Flied emission, therefore CNT is found since 1991, the preparation of CNT, performance and application are all of great interest.The preparation method on CNT mainly has arc discharge method, laser evaporization method and chemical vapour deposition technique at present.Wherein arc discharge method is under the high temperature conditions, to be ionized using reacting gas, the method for making graphite electrode surface evaporation obtain CNT, and it reacts violent, it is difficult to controls the structure of the CNT of generation；Laser evaporization method is focused under the high temperature conditions using high energy laser beam on metallic catalyst and the target of graphite mixing, generates the process of CNT with catalytic action by evaporating；Chemical gaseous phase depositing process is to be used as template, under conditions of 600~1200 DEG C, pyrolysis gaseous hydrocarbon generation CNT by the use of metal catalyst particles.The course of reaction that chemical gaseous phase depositing process prepares CNT is easily controlled and cost is low, suitable for a large amount of synthesis.
However, traditional thermal chemical vapor deposition reaction temperature is too high, condition is harsh, limits application of the CNT in the temperature sensitive Material Field such as microelectronic material and high polymer material.In addition, at present, during CNT is prepared; the catalyst fines that thermal chemical vapor deposition method uses is usually well prepared in advance; due to the effect of Van der Waals force between nanometer powder, reunion can be usually produced, and then influence the preparation efficiency and appearance structure of CNT.How the cost of CNT preparation is reduced, and it is the key issue that current CNT is prepared, studies and applied to simplify preparation technology.
The content of the invention
Present invention solves the technical problem that it is to provide a kind of low temperature preparation method of CNT.
In view of this, this application provides a kind of preparation method of CNT, comprise the following steps：
A), metal net mask is placed in the cavity of PECVD device on negative plate, two blocks of catalyst metals plates of superposition is placed above the metal net mask；
B), the cavity of the PEVCD equipment is heated and is passed through reacting gas thereto, switched on power, catalyst metal particles are obtained after reaction；
C), carbon source and carrier gas will be passed through after the cavity heating of the PEVCD equipment, switch on power, CNT is obtained after reaction.
Preferably, the distance between described two blocks of catalyst metals plates are 1~5cm, and the material of the catalyst metals plate is iron, cobalt, nickel or composite material, and the catalyst metals plate surface is provided with pierced pattern.
Preferably, step A) described in reacting gas be selected from one or both of hydrogen and argon gas, the flow of the reacting gas is 50~100sccm, and the power of the power supply is 500~1000W.
Preferably, the particle diameter of the catalyst metal particles is 1~50nm.
Preferably, step C) described in carbon source include methane, ethanol, acetylene and normal butane in one or more, the flow of the carbon source is 5~50sccm.
Preferably, one or more of the carrier gas in hydrogen, nitrogen and argon gas, the flow of the carrier gas is 100~150sccm.
Preferably, step C) described in the temperature reacted be 350~500 DEG C, the power of the power supply is 10~100W, and the time of the reaction is 10~100min.
Preferably, the metal net mask is cylindric stainless steel guard or cylindric copper mesh cover.
This application provides a kind of preparation method of array carbon nano tube, metal net mask is placed on the negative plate in the cavity of PEVCD equipment first, two blocks of catalyst metals plates of superposition are placed above metal net mask, cavity is heated again and is passed through reacting gas thereto, switch on power, reacting gas in electric field excitation cavity body, so that it becomes plasma, pass through air pressure in control chamber body, make to produce hollow cathode effect between metallic plate, sheet metal is bombarded using the high energy high-density plasma in hollow cathode effect region, sputter nanocatalyst metallic particles, continue after heating reaches reaction temperature, carbon source and carrier gas are passed through into cavity, switch on power, using catalyst metal particles decompose caused by nanoparticle growth go out CNT.During the application CNT free growth, using the metal net mask of auxiliary, the effective activity for improving plasma, more effectively decompose carbon-source gas, realize low temperature preparation of the CNT at 350~500 DEG C, so that the electronic device surface in situ in non-refractory prepares array carbon nano tube film and becomes feasible, its application prospect has been widened.
Brief description of the drawings
Fig. 1 is the PECVD device and the schematic diagram of metal net mask device that the present invention uses；
Fig. 2 is the stereoscan photograph of CNT prepared by the embodiment of the present invention 1；
Fig. 3 is the transmission electron microscope photo of CNT prepared by the embodiment of the present invention 1；
Fig. 4 is the stereoscan photograph of CNT prepared by the embodiment of the present invention 2；
Fig. 5 is the transmission electron microscope photo of CNT prepared by the embodiment of the present invention 2；
Fig. 6 is the stereoscan photograph of CNT prepared by the embodiment of the present invention 3；
Fig. 7 is the transmission electron microscope photo of CNT prepared by the embodiment of the present invention 3.
Embodiment
For a further understanding of the present invention, the preferred embodiment of the invention is described with reference to embodiment, but it is to be understood that these descriptions are simply further explanation the features and advantages of the present invention, rather than limiting to the claimed invention.
The embodiment of the invention discloses a kind of preparation method of array carbon nano tube film, comprise the following steps：
A), metal net mask is placed in the cavity of PECVD device on negative plate, two blocks of catalyst metals plates of superposition is placed above the metal net mask；
B), the cavity of the PEVCD equipment is heated and is passed through reacting gas thereto, switched on power, catalyst granules is obtained after reaction；
C), carbon source and carrier gas will be passed through after the cavity heating of PEVCD equipment, switch on power, CNT is obtained after reaction.
This application provides a kind of preparation method of CNT, CNT prepared by the application is really one kind without the free growing CNT of substrate.The catalyst metal particles that the application sputters fall in minus plate, it is difficult to produce with the surface and effectively combine, therefore the CNT 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 CNT includes the preparation of nanocatalyst metallic particles and two steps of preparation of low temperature CNT, and two steps are continuously finished in same PECVD reaction cavities.
The application carries out the preparation of nanocatalyst metallic particles first.As shown in figure 1, Fig. 1 is the schematic device of PECVD device prepared by CNT of the present invention.Metal net mask is placed in the cavity of PECVD device on negative plate by the application first, and two blocks of catalyst metals plates for being sequentially overlapped placement are placed above metal net mask.Herein described PECVD cavitys are the reaction cavity of PECVD device, the PECVD device is equipment well known to those skilled in the art, this the application is had no particular limits, the application use PECVD device preferably as shown in figure 1, in PECVD reaction cavities the setting of metal net mask and two blocks of catalyst metals plates be specially：The metal net mask is positioned on bottom crown, the top of the metal net mask and is provided be sequentially overlapped two blocks of catalyst metals plates with what metal net mask directly contacted, and the metal net mask and catalyst sheet may be contained between top crown and bottom crown.Herein described metal net mask can be cylindric stainless steel guard or cylindric copper mesh cover.Herein described catalyst sheet surface is provided with pierced pattern, the quantity of catalyst granules on minus plate is splashed to increase, the pierced pattern can be circular, can also be other shapes, and this application is had no particular limits.The spacing of herein described two blocks of catalyst metals plates is preferably 1~5cm.The catalyst metals plate is preferably iron, cobalt, nickel or composite material, and herein described catalyst metals plate is preferably same metal material.
During catalyst nano-particles are prepared, the cavity of PECVD device is heated first and is passed through reacting gas into PECVD cavitys, switch on power after reaching predetermined temperature, reacting gas in electric field excitation cavity body, so that it becomes plasma, by controlling the gas pressure in PECVD cavitys so that produce hollow cathode effect between the plate of catalyst two.Sheet metal is bombarded using the high energy high-density plasma in caused hollow cathode effect region, sputters nano-metal particle.The distance between two pieces of catalyst sheets produce the plasma density between metallic plate with control, under certain reaction pressure and power, obtain the very high plasma of density and are used for bombarding metal surface, sputter nano-metal particle.In the process, metal net mask is used for the effect for turning on minus plate and catalytic metal plate so that hollow cathode effect can be produced between metallic plate.In above process, the reacting gas is preferably one or both of argon gas and hydrogen, by controlling electric field power and the suitable reacting gas of selection, can obtain the catalyst granules of different-grain diameter, its size range is 1~50nm.The flow of the reacting gas is preferably 50~100sccm, and in embodiment, the reacting gas is preferably hydrogen and argon gas, and the flow of the argon gas is preferably 50~80sccm, and the flow of the hydrogen is preferably 20~50sccm.Power is preferably 500~1000W, example, and the power is preferably 600~800W.The temperature to switch on power is preferably 300~400 DEG C.According to the present invention, the PECVD device is preferably evacuated to 10- before the cavity of the PECVD device is heated4Pa。
The application in PECVD vacuum cavities by exciting sputtering generation nano-catalyst particles, make the size of nano-catalyst particles relatively uniform, reduce the reunion of nano particle along the sputtering of different directions, while avoid influence of the oxidation to nanocatalyst metallic particles performance.
After catalyst metal particles are prepared, the application then continues to carry out the preparation of CNT in PECVD cavitys.This process realizes the low temperature preparation of CNT using metal net mask device.Detailed process is：Carbon-source gas and carrier gas are passed through after the cavity of PECVD device is continued into heating, switches on power, CNT is obtained after reaction.During this, on the one hand metal net mask improves the temperature of conversion zone, on the other hand can adsorb high energy particle, reduces corrasion, and goes out CNT beneficial to free growth.The application has no particular limits to the carbon source with carrier gas, for carbon source well known to those skilled in the art and carrier gas, the carbon source is preferably selected from the one or more in methane, ethanol, acetylene and normal butane, the example, the carbon source is preferably selected from acetylene, the carrier gas is preferably selected from the one or more in argon gas, nitrogen and hydrogen, example, and the carrier 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 mainly play two aspects as carrier gas, on the one hand, by being passed through for carrier gas, control the air pressure in reaction cavity so that plasma field is easily excited；On the other hand, the growth that carrier gas effectively dilutes carbon-source gas and is advantageous to CNT is passed through, when this is due to that ratio when carbon-source gas in reaction cavity is higher, reaction preparation is tended to generate amorphous carbon, rather than CNT.During CNT is prepared, 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 in preparation process are preferably 5sccm~50sccm, and in embodiment, the flow of the carbon source is preferably 10~20sccm.The flow of the carrier gas is preferably 100~150sccm, example, and the flow of the argon gas in the carrier gas is preferably 50~80sccm, and the flow of hydrogen is preferably 60~70sccm, and the flow of the nitrogen is preferably 5~10sccm.The time of the reaction is preferably 10~100min, example, and the reaction time is preferably 30~60min；The temperature of the reaction is preferably 350~500 DEG C, and power is preferably 10~100W, example, and the power is preferably 30~60W.
The application can control the pattern and size of the catalyst being prepared, and then can influence the pattern of CNT, structure snd size by adjusting corresponding response parameter, such as reaction temperature, power, gas flow and reaction time.The present invention can realize the preparation of CNT under conditions of less than 500 DEG C, while the CNT being prepared is multi-walled carbon nanotube.
As the general knowledge of this area, although Preparation equipment is radio frequency PECVD used by this example, device is equally applicable to the similar equipment such as direct current PECVD used by the preparation method.It is of the invention compared with traditional thermal chemical vapor deposition and plasma enhanced chemical vapor deposition prepare the method for CNT, advantage is to prepare catalyst granules using PECVD electric field, without being additionally provided catalyst；The composition of catalyst granules can be controlled by the metallic plate from different materials.By the power for controlling electric field, moreover it is possible to the effectively size of control catalyst granules.At the same time, due in whole catalyst preparation process, all completing in a vacuum, the problems such as avoiding the oxidation run into traditional handicraft catalyst transfer process, pollute, additionally it is possible to avoid the reunion of catalyst granules to a certain extent.
Metal net mask technology of the present invention, the temperature of reaction generation CNT can be effectively reduced, under conditions of 350~500 DEG C, realizes the preparation of CNT.Present approach reduces the energy for preparing CNT and being consumed.At the same time, the low temperature preparation of CNT is realized, can aid in and the combination of other technologies, the compound of CNT and some low-temperature alloys or high polymer material is such as realized, has expanded the application field of CNT significantly.
For a further understanding of the present invention, the preparation method of array carbon nano tube film provided by the invention is described in detail with reference to embodiment, protection scope of the present invention is not limited by the following examples.
Embodiment 1
A kind of method that CNT is prepared at 400 DEG C, this method comprise 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, and 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 positioned on PECVD bottom crowns.
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；Argon gas and hydrogen in electric field excitation cavity body, produce plasma；Pass through the gas pressure in control chamber body, so that produce hollow cathode effect between catalyst metals plate, a plasma enrichment region is produced between sheet metal, the highdensity plasma constant bombardment sheet metal of high energy so that nanocatalyst metallic particles sputters out from metal sheet surface；
Step 3：On the basis of step 2, continue to heat, bottom crown temperature is reached 400 DEG C；At the same time, carbon-source gas (acetylene) and carrier gas (argon gas and hydrogen) are passed through into cavity, gas flow is respectively 10sccm, 60sccm, 30sccm, and the power of power supply is adjusted to 50W, reaction time 30min；
Step 4：After reaction terminates, close power supply, stop heating, continue to be passed through argon gas and hydrogen, close carbon source, cool to room temperature with the furnace, obtain CNT.
By controlling the length in reaction time in the present embodiment, the CNT of different length can be obtained.In metallic catalyst preparation process, argon ion and hydrionic main function are bombardment metallic plates, generate catalyst granules；In carbon nanotube growth process, argon ion and hydrogen ion can effectively suppress the generation of amorphous carbon, promote CNT continued propagation.SEM the and TEM photos difference of CNT manufactured in the present embodiment is as shown in Figures 2 and 3.
Embodiment 2
A kind of method that CNT is prepared under the conditions of 500 DEG C, this method comprise the following steps：
Step 1：Using Ni plates and 316 stainless steel plates as catalyst plates in the present embodiment, two plate spacing are 1cm, and remaining is set 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 constant bombardment catalyst metals plate that electric field excites, so as to sputter catalyst granules；The present embodiment improves the content of Ni elements in catalyst granules by using Ni plates.
Step 3：Heating makes bottom crown temperature reach 500 DEG C；At the same time, carbon-source gas (acetylene) and carrier gas (argon gas and hydrogen) are passed through into cavity, gas flow is respectively 5sccm, 50sccm, 20sccm；The power of power supply is adjusted to 30W, reaction time 30min.
Step 4：With the step 4 of embodiment 1.
Embodiment 2 has the change of three aspects with respect to embodiment 1：First, employ Ni metallic plates, it is therefore intended that improve the content of Ni elements in catalyst granules, promote the growth of CNT using its activity；Two are reduction of the gas flow in sputtering course of reaction, while temperature and power when reducing sputtering, and then reduce and prepare cost, raising efficiency；Third, changing the growth temperature of CNT, the flow and reaction power of carbon-source gas are reduced, passes through adjusting parameter, it is intended to which it is less to obtain impurity, the faster CNT of growth rate.SEM the and TEM photos difference of CNT manufactured in the present embodiment is as shown in Figure 4 and Figure 5.
Embodiment 3
A kind of method that nitrogen-doping CNT is prepared under the conditions of 500 DEG C.The preparation method comprises the following steps：
Step 1：The condition of the process of catalyst granules is prepared 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, acetylene, argon gas, hydrogen and nitrogen are passed through into cavity, gas flow is respectively 5sccm, 50sccm, 20sccm, 5sccm；The power of power supply is adjusted to 30W, reaction time 30min.
Step 4：With the step 4 of embodiment 1.
The main distinction of this example and embodiment 1 is to be passed through N during growing CNT2As auxiliary gas, to investigate influence of the N element doping for carbon nano tube growth.SEM the and TEM photos difference of CNT manufactured in the present embodiment is as shown in Figure 6 and Figure 7.
The explanation of above example is only intended to help the method and its core concept for understanding the present invention.It should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention, some improvement and modification can also be carried out to the present invention, these are improved and modification is also fallen into the protection domain of the claims in the present invention.
The foregoing description of the disclosed embodiments, professional and technical personnel in the field are enable to realize or using the present invention.A variety of modifications to these embodiments be will be apparent for those skilled in the art, and generic principles defined herein can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, the present invention is not intended to be limited to the embodiments shown herein, and is to fit to the most wide scope consistent with principles disclosed herein and features of novelty.
Claims (8)
1. a kind of preparation method of CNT, comprises the following steps：
A), metal net mask is placed in the cavity of PECVD device on negative plate, in the gold
Belong to two blocks of catalyst metals plates that superposition is placed above guard；
B), the cavity of the PEVCD equipment is heated and is passed through reacting gas thereto, connect
Energization source, catalyst metal particles are obtained after reaction；
C), carbon source and carrier gas will be passed through after the cavity heating of the PEVCD equipment, connect electricity
Source, CNT is obtained after reaction.
2. preparation method according to claim 1, it is characterised in that described two pieces are urged
The distance between agent metallic plate is 1~5cm, the material of the catalyst metals plate is iron, cobalt,
Nickel or composite material, the catalyst metals plate surface are provided with pierced pattern.
3. preparation method according to claim 1, it is characterised in that step A) in institute
State reacting gas and be selected from one or both of hydrogen and argon gas, the flow of the reacting gas is
50~100sccm, the power of the power supply is 500~1000W.
4. preparation method according to claim 1, it is characterised in that the catalyst
The particle diameter of metallic particles is 1~50nm.
5. preparation method according to claim 1, it is characterised in that step C) in institute
Stating carbon source includes the one or more in methane, ethanol, acetylene and normal butane, the carbon source
Flow is 5~50sccm.
6. preparation method according to claim 1, it is characterised in that the carrier gas choosing
One or more from hydrogen, nitrogen and argon gas, the flow of the carrier gas are
100~150sccm.
7. preparation method according to claim 1, it is characterised in that step C) in institute
The temperature for stating reaction is 350~500 DEG C, and the power of the power supply is 10~100W, the reaction
Time be 10~100min.
8. preparation method according to claim 1, it is characterised in that the wire netting
Cover for cylindric stainless steel guard or cylindric copper mesh cover.
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