CN114057184B - Density regulation and control method and preparation device of self-supporting carbon nanotube film target - Google Patents
Density regulation and control method and preparation device of self-supporting carbon nanotube film target Download PDFInfo
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- CN114057184B CN114057184B CN202010763009.3A CN202010763009A CN114057184B CN 114057184 B CN114057184 B CN 114057184B CN 202010763009 A CN202010763009 A CN 202010763009A CN 114057184 B CN114057184 B CN 114057184B
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- C01B32/00—Carbon; Compounds thereof
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Abstract
The invention discloses a self-supporting carbon nanotube film and a self-supporting carbon nanotube film target, a preparation method and a density regulation method thereof, and a preparation device adopted correspondingly. The device and/or the method provided by the invention can prepare the microscopically uniform low-density carbon tube film by the floating catalytic chemical vapor deposition method, then compress and transfer the film by using a high-precision film pressing machine to obtain the self-supporting film target with specified density, realize self-supporting and large-scale specified density regulation and control at the target hole, and can be used for laser targeting experiments or application.
Description
Technical Field
The invention relates to a self-supporting carbon nano tube film target with adjustable density, a density regulating and controlling method or a preparation method of the film target, and a device adopted by the film target, and belongs to the technical field of novel nano material manufacturing and application.
Background
The interaction of ultrashort and ultrastrong laser pulses and a self-supporting film target material can realize ion acceleration, and the ion acceleration has the advantages of high acceleration gradient, low manufacturing cost, no breakdown threshold limit and the like, and has attracted wide attention in the fields of proton imaging, nuclear fusion rapid ignition and the like. Experimental research shows that the quality of the film target material has key influence on the quality of the cut-off energy, the flow intensity, the energy dispersion and the like of the accelerated ion beam. The self-supporting carbon nano tube film is microscopically uniform and porous, and can generate high-temperature and high-energy-density uniform plasmas when being acted with super-strong laser pulses. When the carbon tube films with different densities interact with the ultra-strong laser pulse, a new acceleration mechanism can be induced to form, and the proton/carbon ion beam with high average energy and small energy dispersion is obtained. The energy deposition effect of the protons/carbon ions obtained by acceleration in the method has Bragg peaks, and has unique advantages in radiotherapy for cancer treatment.
At present, the preparation method of the self-supporting carbon nano tube film mainly comprises a solution method and a chemical vapor deposition method. The carbon tube prepared by the solution method is difficult to prepare a homogeneous carbon tube film which is uniformly dispersed unless complicated carbon tube functionalization treatment is carried out due to the property of large pi-bond oleophobic and hydrophobic surface. In order to realize a peelable self-supporting film independent of a substrate, most of carbon nanotubes prepared by chemical vapor deposition have high density and thickness, and it is difficult to realize a self-supporting film with low density. Patent CN105271163a discloses a continuous preparation and film forming method of a macroscopic body of a carbon nanotube, and the success rate of self-supporting of the prepared carbon nanotube film by mechanical stripping or dissolution stripping is low. Considering the problem that the self-supporting film is easy to damage, the self-supporting carbon tube film prepared by the method is high in general density, the density of the carbon tube film can be changed within a certain range only by controlling reaction conditions, the carbon tube film is difficult to carry out large-range designated density adjustment, and the density requirement of a laser acceleration experiment on a self-supporting carbon tube film target is difficult to meet.
Therefore, it is desirable to provide a self-supporting thin film with low density, which is easy to peel, and can adjust the density conveniently and flexibly, so as to obtain the self-supporting carbon tube thin film target meeting the requirement of laser acceleration experiments.
Disclosure of Invention
The invention aims to solve the problems, and provides a self-supporting carbon nano tube film, a self-supporting carbon nano tube film target, a preparation method and a density regulation method thereof and a correspondingly adopted preparation device aiming at the application requirements of the self-supporting carbon tube film in the field of laser acceleration. The device and/or the method provided by the invention can prepare the microscopically uniform low-density carbon tube film by the floating catalytic chemical vapor deposition method, then compress and transfer the film by using a high-precision film pressing machine to obtain the self-supporting film target with specified density, realize self-supporting and large-scale specified density regulation and control at the target hole, and can be used for laser targeting experiments or application, thereby completing the invention.
Thus, according to a first aspect of the present invention, there is provided a method for preparing a self-supporting carbon nanotube film target, comprising the steps of preparing a carbon nanotube film first, then pressing the carbon nanotube film into a high-density carbon nanotube film, and finally transferring the carbon nanotube film to prepare a self-supporting carbon nanotube film target with adjustable density.
In the present invention, the preparation of the carbon nanotubes or carbon nanotube films is carried out in a preparation apparatus comprising a tube furnace, preferably a high temperature tube furnace, such as a quartz tube.
According to the present invention, the preparation of the carbon nanotube or carbon nanotube film comprises the steps of:
step 1, preparing a carbon source and a catalyst,
and step 3, forming a carbon nano tube film on the substrate.
In step 1, the carbon source is a carbohydrate, particularly a hydrocarbon compound, and preferably a mixed gas containing a carbon source, in which a gas inert to the reaction (such as nitrogen or a rare gas such as argon) is mixed as a carrier gas, for example, methane is added at a flow rate of 5 to 15sccm, and argon is added at a flow rate of 800 to 1200 sccm. Ferrocene is used as a catalyst, preferably a mixed catalyst of ferrocene and a sulfur-containing compound, which may be sulfur powder, the catalyst being used in the form of a mixed powder, wherein ferrocene is mixed with sulfur powder in a weight ratio of 90-95:1, preferably 91-94:1, more preferably 92-93:1.
In step 2, the cracking reaction is carried out in a preparation device comprising a tube furnace, wherein the temperature of a central high-temperature zone of the tube furnace can reach more than 1000 ℃, preferably 1100-1200 ℃, the tube furnace is preferably a quartz tube, the tube length of the tube furnace is 100-300cm, preferably 120-200cm, such as 150cm, and the diameter of the tube furnace is 30-90mm, preferably 40-80mm, such as 60mm. The mixed gas containing carbon source is contacted with catalyst, and the catalyst is heated to above 100 deg.c, for example 120-150 deg.c, preferably 130-140 deg.c, in heating zone, and the mixed gas carries the sublimated catalyst into the furnace tube center for reaction, and the sublimated catalyst is cracked to form carbon nanotube, which is floated in carrier gas and moves together with the gas flow toward the tail of the furnace tube.
In step 3, the substrate is a conductive monocrystalline silicon wafer, which is horizontally inserted into the tail of the furnace tubeThe carbon nanotubes floating on the carrier gas and moving together with the carrier gas overlap each other in the deposition boat, and form a carbon nanotube film on the substrate with the temperature at the tail of the furnace tube falling, the thickness of the carbon nanotube film is in the range of 0.05-1000 mu m, preferably 0.1-800 mu m, and the density is lower than 10mg/cm 3 Preferably less than 5mg/cm 3 Even as low as 1mg/cm 3 。
In the preparation method, a low-density carbon nano tube film is pressed into a high-density carbon nano tube film, and then the high-density carbon nano tube film is transferred, so that a self-supporting carbon nano tube film target with adjustable density is obtained, preferably, a substrate (or a deposited silicon wafer and a conductive silicon wafer) covered with the carbon nano tube film is taken out of a tube furnace, and is reversely buckled, so that the substrate is placed on a coupling/nesting target frame comprising a base and a target piece, and is compressed by a film pressing machine until the specified height is reached, the silicon wafer is removed, and the base is pulled out, so that the self-supporting carbon nano tube film target is obtained.
According to a second aspect of the present invention, there is provided a method for controlling the density of a self-supporting carbon nanotube film target, which is realized by mechanical compression and adhesive transfer, preferably, a conductive silicon wafer is placed on a coupling target frame in an aligned manner on one side, and then is transferred to a film pressing machine for compression, wherein the compression height (i.e. thickness) is set according to the required density, i.e. the compression height is set to meet the specified density requirement.
According to a third aspect of the present invention, there is provided a device for preparing a self-supporting carbon nanotube film target, comprising a device for preparing a carbon nanotube or a carbon nanotube film, and a coupling target frame, wherein the coupling target frame is composed of a base and a target piece coupled and nested/complementary with the base, the base of the coupling target frame comprises an aluminum alloy flat plate and a cylindrical bump array on the surface of the aluminum alloy flat plate, preferably only the two parts, the cylindrical height is the thickness of the target piece, the diameter of the cross section is the inner diameter of a target hole on the target piece, preferably, the upper surface of the cylindrical bump is subjected to precision polishing treatment. The spatial arrangement is consistent with the arrangement of the target holes on the target piece.
In the invention, the sizes of the target piece and the base of the coupling target frame can be adjusted according to actual requirements, and the inner diameter of the target hole, namely the diameter of the columnar bulge, d, can be 1-3mm; the thickness of the target, i.e. the height of the stud bump, h, may be 0.5-1mm, the target and the base may be of equal size, and may be square, e.g. 25-50mm, more preferably 35-40mm, on a side.
Compared with the prior art, the invention has the following advantages:
1) The prepared carbon nano tube film has uniform and disordered carbon tubes, good microcosmic uniformity and low film density (as low as 1 mg/cm) 3 )。
2) The method is matched with the subsequent mechanical compression and self-supporting transfer processes, so that the successful preparation of the self-supporting carbon nanotube film target in the low-density region is realized, and the problems of easiness in breakage and low success rate when the self-supporting of the low-density carbon nanotube film target is realized are solved.
3) The density regulation and control method provided by the invention is independent of the regulation of preparation parameters, can carry out large-scale designated density regulation and control on the carbon nanotube film target at a low-density starting point, prepares the self-supporting carbon nanotube film target with specific density, and well meets the requirements of laser acceleration experiments and application
Drawings
FIG. 1 is a schematic diagram of an apparatus for preparing a carbon nanotube film;
FIG. 2 is a schematic diagram of a compression and transfer process for controlling the density of a carbon tube film target;
FIG. 3 is a photograph of a base of a coupling target holder and a target plate coupled and nested therewith;
FIG. 4 is an SEM image of a carbon tube thin film target prepared in example 1.
Detailed Description
The invention is further described in detail below by means of the figures and examples. The features and advantages of the present invention will become more apparent from the description.
The word "exemplary" is used herein to mean "serving as an example, embodiment, or illustration. Any embodiment described herein as "exemplary" is not necessarily to be construed as preferred or advantageous over other embodiments. Although various aspects of the embodiments are illustrated in the accompanying drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The invention is described in further detail below with reference to the drawings and the preferred embodiments. The features and advantages of the present invention will become more apparent from the description.
According to the invention, a preparation method or a density regulation method of a self-supporting carbon nanotube film target is provided, wherein a carbon nanotube film is prepared first, then a high-density carbon nanotube film is pressed, and finally transfer is carried out, so that the self-supporting carbon nanotube film target with adjustable density is prepared.
In the invention, the preparation of the carbon nano tube or the carbon nano tube film is carried out in a preparation device comprising a tube furnace, wherein the tube furnace is preferably a high-temperature tube furnace, such as a quartz tube, a high-temperature zone can be formed in the middle part of the tube furnace, namely the center of the tube furnace, one side of the preparation device is provided with a catalyst heating zone, the other side of the tube furnace opposite to the catalyst heating zone is provided with a deposition zone, a deposition boat is placed in the deposition zone, and a substrate can be inserted into the deposition boat.
The device for preparing the carbon nano tube film is shown in figure 1, wherein an air inlet 1 carries a catalyst 2 heated by a heater 3 into a tube furnace, a high temperature zone 4 in the furnace reacts, the generated carbon nano tube moves towards the tail of the furnace tube, and a carbon nano tube film is formed on a deposited silicon wafer 5.
According to the invention, the device can be used for preparing the carbon nano tube or the carbon nano tube film, and the preparation method specifically comprises the following steps:
step 1, preparing a carbon source and a catalyst.
In the present invention, the carbon source is a carbon-containing compound that can be catalytically cracked to form carbon nanotubes, and preferably, a carbohydrate, particularly a hydrocarbon compound such as an alkane such as methane, ethane, propane, butane, and the like, and an aromatic hydrocarbon such as benzene, toluene, xylene, and the like, and methane is preferably used as the carbon source.
In the present invention, the catalyst is capable of catalyzing the cracking of a carbon source, ferrocene can be used as a catalyst, preferably a mixed catalyst of ferrocene and a sulfur-containing compound, which may be sulfur powder, the catalyst being used in the form of a mixed powder, wherein ferrocene and sulfur powder are mixed in a weight ratio of 90-95:1, preferably 91-94:1, more preferably 92-93:1, and optionally milled in an agate mortar, for example, for several minutes to several hours, preferably 10 minutes to 2 hours, more preferably 15 minutes to 1 hour, for example, for half an hour, to be thoroughly mixed.
According to a preferred embodiment of the present invention, a mixed gas containing a carbon source is used, in which a gas inert to the reaction (such as nitrogen or a rare gas) is mixed as a carrier gas in addition to a hydrocarbon compound as a carbon source, preferably a rare gas such as helium, neon, argon, more preferably argon.
According to the invention, the mixing of the mixture is effected in a gas mixing box, wherein methane is added at a flow rate of 2 to 20sccm, preferably 5 to 15sccm, and an inert gas, such as argon, is added at a flow rate of 500 to 2000sccm, preferably 800 to 1200sccm, and after mixing is introduced into the preparation device as inlet gas 1.
And 2, performing catalytic cracking reaction to form the carbon nano tube.
In the invention, the cracking reaction is carried out in the preparation device comprising the tube furnace, the temperature of the central high-temperature area of the tube furnace can reach more than 1000 ℃, preferably 1100-1200 ℃, and the tube furnace is easy to break above the temperature. The tube furnace is preferably a quartz tube having a tube length of between 100 and 300cm, preferably 120 to 200cm, for example 150cm, and a diameter of between 30 and 90mm, preferably 40 to 80mm, for example 60mm.
According to the invention, the air in the quartz tube is evacuated before the reaction, for example by purging with a gas, preferably with the said mixed gas or one of the gases, for example by introducing argon (preferably at a flow rate of 800-1200 sccm) for a few seconds to a few minutes, for example for 5 seconds to 2 minutes, preferably for 10 seconds, before the reaction, and then the gas is discharged from the furnace tube via the exhaust gas 6.
According to the invention, after being uniformly mixed by a gas mixing box, the mixed gas containing carbon source is introduced into a quartz tube with air exhausted by an air inlet 1, and is firstly contacted with a catalyst 2 positioned on one side of the quartz tube, the catalyst is heated to more than 100 ℃ in a heating zone by a heater 3, for example, 120-150 ℃, preferably 130-140 ℃, the catalyst is sublimated by heating, and the mixed gas carries the sublimated catalyst heated by heating into a high-temperature reaction zone 4 in the center of a furnace tube for reaction, and the carbon nano tube is formed by high-temperature catalytic pyrolysis.
In the invention, hydrocarbon compounds such as methane serving as a carbon source are reaction gases, are catalytically cracked, are reformed into carbon nanotubes, float in carrier gas, and are beneficial to movement of the carbon nanotubes in a quartz tube, for example, the carbon nanotubes can move towards the tail of a furnace tube along with air flow.
And step 3, forming a carbon nano tube film on the substrate.
In the invention, the substrate is a conductive monocrystalline silicon wafer, and the monocrystalline silicon wafer is horizontally inserted into a deposition boat positioned at the tail part of a quartz furnace tube to form a deposition area of the quartz tube.
And the carbon nanotubes floating on the carrier gas and moving together with the carrier gas overlap with each other along with the temperature decrease of the tail part of the furnace tube, so that a carbon nanotube film is formed on the substrate.
Therefore, by using the preparation device provided by the invention, the carbon nano tube and/or the carbon nano tube film is obtained according to the method provided by the invention, the carbon nano tube is uniformly and randomly distributed, the microcosmic uniformity is good, and the deposited silicon wafer 5 provides a certain support for the carbon nano tube film. The carbon tubes are uniformly and randomly distributed.
In the present invention, the density and thickness of the carbon tube film on the substrate can be measured, and the inventors have found that the thickness of the formed film can be controlled, for example, in the range of 0.05 μm to 1000 μm, preferably 0.1 μm to 800 μm, and the thickness can be controlled, for example, by the deposition time. In addition, the carbon nano tubes of the film are in unordered and uniform distribution in microcosmic mode, and have lower density, and are generally smaller than 10mg/cm 3 Preferably less than 5mg/cm 3 Even as low as 1mg/cm 3 。
According to the method provided by the invention, the prepared carbon nanotube film is pressed into a high-density carbon nanotube film, and then the high-density carbon nanotube film is transferred, so that the self-supporting carbon nanotube film target with adjustable density is obtained.
According to a preferred embodiment of the present invention, a substrate (or a deposited silicon wafer, a conductive silicon wafer) covered or attached with a carbon nanotube film is taken out of a tube furnace, inverted, placed on a coupling/nesting target frame including a base and a target, compressed by a film press until reaching a specified height, removed, and the base is withdrawn to obtain a self-supporting carbon nanotube film target.
In the invention, the density regulation and the self-supporting of the carbon tube film are realized by mechanical compression, bonding and transferring, and the specific realization modes are as follows:
the surface of the conductive silicon chip covered with the carbon tube is aligned and laid on the coupling target frame, and then the conductive silicon chip is transferred to the film pressing machine for compression, and the compression height (i.e. thickness) is set according to the required density, namely, the conductive silicon chip is compressed to the specified height to meet the specified density requirement.
According to the invention, after the carbon nanotube film is reversely buckled and pressed, the thickness of the carbon film is reduced relative to the initial thickness, the density is correspondingly increased, meanwhile, the viscosity of the carbon tube and the difference of the surface roughness of the target sheet and the substrate are utilized, namely, the surface of the target sheet is far rougher than the surface of the silicon wafer, the carbon tube is tightly adhered to the target sheet while being compressed, so that the nondestructive transfer of the film and the self-support at the target hole are realized, and the self-support carbon nanotube film attached to the target sheet with the designated density is obtained, and can be directly installed for laser targeting experiments or practical application.
The compression and transfer processes of the carbon tube film target density regulation are shown in figure 2, the base of the coupling/nesting target frame is shown in the left figure of figure 3, and the coupling/nesting target frame is formed by covering target pieces on the base, as shown in the right figure of figure 3.
In the invention, the coupling target frame consists of a base and a target piece which is coupled with the base and nested/complemented with the base. The base comprises a flat plate of aluminum alloy and an array of cylindrical projections on its surface, preferably consisting of only the two parts. The height of the cylinder is the thickness of the target piece, the diameter of the cross section is the inner diameter of a target hole on the target piece, and the upper surface of the columnar bulge is subjected to precise polishing treatment. The space arrangement is consistent with the arrangement of the target holes on the target pieces, so that the target pieces can be tightly buckled on the base to form a target frame with a flat upper surface.
According to the preferred embodiment of the invention, the sizes of the target and the base can be adjusted according to actual requirements. The inner diameter of the target hole, i.e., the diameter of the columnar protrusion, d, may be 0,5-5mm, preferably 1-3mm, and most preferably 2mm; the thickness of the target, i.e. the height of the stud bumps, h, may be 0.1-3mm, preferably 0.5-1mm, most preferably 0.7mm, and the target and the base may be of equal size, square, e.g. 10-100mm, preferably 25-50mm, more preferably 35-40mm, e.g. 38mm x 38mm.
The invention is further illustrated below with reference to examples.
Example 1
And (3) placing the silicon wafer to be deposited with the carbon tube into a film pressing machine for zeroing, then inserting a deposition boat, and placing the silicon wafer into a deposition area of a tube furnace. As shown in FIG. 1, a quartz boat filled with a catalyst (mixed powder of ferrocene and sulfur powder in a weight ratio of 92:1) is placed on the air inlet side of a tube furnace and is positioned above a heater, and is heated to 130 ℃, 1000sccm of argon is introduced at the moment, and air in the tube furnace is discharged to form an inert atmosphere. After 10 seconds, methane is introduced together with argon at a flow of 10sccm, and the methane and the argon carry a heating sublimation catalyst to enter the center of a furnace tube at 1100 ℃, the methane is catalytically cracked and reformed into carbon nanotubes, and the carbon nanotubes are deposited on a silicon wafer along with carrier gas to form a film. After 30 minutes, all air valves are closed, deposition is finished, and the precipitator silicon wafer and the carbon nano tube film on the precipitator silicon wafer are taken out.
And measuring the thickness and density of the carbon tube film on the silicon wafer, and determining the compression height according to the density requirement of the experiment. The coated silicon wafer is carefully and reversely buckled on a coupling target frame shown in the right diagram of fig. 3, placed on a compression table which is calibrated, and accurately compressed according to the set compression height. After compression, the silicon wafer on the upper surface of the carbon nanotube film was slightly removed with tweezers while carefully removing the base of the coupling target frame to obtain a self-supporting carbon nanotube film target. Through visual observation, the film target is intact, has no rupture and is even and smooth.
The initial thickness of the prepared carbon nano tube film is 188 mu m, and the corresponding initial density is 1.24mg/cm 3 The compressed height was 17 μm and the corresponding density was 13.71mg/cm 3 。
From the scanning electron microscope image of the prepared carbon tube film shown in fig. 4, it can be seen that the carbon nanotubes in the film are uniformly distributed in disorder and in micron scale, the surface is clean, the granular impurities are few, and the requirement of a laser acceleration experiment is well met.
Example 2
And (3) placing the silicon wafer to be deposited with the carbon tube into a film pressing machine for zeroing, then inserting a deposition boat, and placing the silicon wafer into a deposition area of a tube furnace. As shown in FIG. 1, a quartz boat filled with a catalyst (mixed powder of ferrocene and sulfur powder in a weight ratio of 93:1) was placed on the air inlet side of a tube furnace and above a heater, heated to 140 ℃, and 800sccm argon was introduced at this time to remove air in the furnace tube and form an inert atmosphere. After 10 seconds, methane is introduced together with argon at a flow of 12sccm, and the methane and the argon carry a heating sublimation catalyst to enter the center of a furnace tube at 1100 ℃, the methane is catalytically cracked and reformed into carbon nanotubes, and the carbon nanotubes are deposited on a silicon wafer along with carrier gas to form a film. And closing all air valves after 20 minutes, ending deposition, and taking out the precipitator silicon wafer and the carbon nanotube film thereon.
And measuring the thickness and density of the carbon tube film on the silicon wafer, and determining the compression height according to the density requirement of the experiment. The coated silicon wafer is carefully and reversely buckled on a designed coupling target frame as shown in the right diagram of fig. 3, is placed on a compression table which is calibrated to zero, and is accurately compressed according to the set compression height. After compression, the silicon wafer on the upper surface of the carbon nanotube film was slightly removed with tweezers while carefully removing the base of the coupling target frame to obtain a self-supporting carbon nanotube film target.
The initial thickness of the prepared carbon nano tube film is 127 mu m, and the corresponding initial density is 2.68mg/cm 3 The compressed height was 26 μm and the corresponding density was 13.10mg/cm 3 。
The invention has been described above in connection with preferred embodiments, which are, however, exemplary only and for illustrative purposes. On this basis, the invention can be subjected to various substitutions and improvements, and all fall within the protection scope of the invention.
Claims (13)
1. The preparation method of the self-supporting carbon nanotube film target is characterized in that firstly, a carbon nanotube film is prepared, then the carbon nanotube film is pressed into a high-density carbon nanotube film, finally, the transfer is carried out, and a self-supporting carbon nanotube film target with adjustable density is prepared by utilizing a preparation device of the self-supporting carbon nanotube film target;
the preparation of the carbon nanotubes or carbon nanotube films is carried out in a preparation device comprising a tube furnace, comprising the steps of:
step 1, preparing a carbon source and a catalyst, wherein the carbon source is a hydrocarbon compound, a mixed gas containing the carbon source is used, a gas inert to the reaction is mixed in the mixed gas as a carrier gas, a mixed catalyst of ferrocene and sulfur powder is used,
step 2, carrying out catalytic cracking reaction to form carbon nanotubes, wherein the cracking reaction is carried out in a preparation device comprising a tube furnace, the temperature of a central high-temperature area of the tube furnace is 1100-1200 ℃,
step 3, forming a carbon nano tube film on a substrate, wherein the substrate is a conductive monocrystalline silicon wafer, is horizontally inserted into a deposition boat at the tail part of a furnace tube, floats on a carrier gas and is mutually overlapped with carbon nano tubes moving together with the carrier gas, and forms the carbon nano tube film on the substrate along with the reduction of the temperature at the tail part of the furnace tube;
the preparation device of the self-supporting carbon nanotube film target comprises a preparation device of a carbon nanotube or a carbon nanotube film and a coupling target frame, wherein the coupling target frame is composed of a base and a target piece which is coupled with the base in a nesting/complementary manner, the base comprises an aluminum alloy flat plate and a cylindrical bulge array on the surface of the aluminum alloy flat plate, the cylindrical height is the thickness of the target piece, and the diameter of the cross section is the inner diameter of a target hole on the target piece.
2. The method of manufacturing according to claim 1, wherein the tube furnace is a quartz tube.
3. The method according to claim 1, wherein in step 1,
the inert gas for reaction is argon, in the mixed gas, methane is added at the flow rate of 5-15 sccm, argon is added at the flow rate of 800-1200 sccm,
the catalyst is used in the form of a mixed powder in which ferrocene is mixed with sulfur powder in a weight ratio of 90-95:1.
4. The method according to claim 1, wherein in step 2,
the tube furnace is a quartz tube, the tube length is 100-300cm, the diameter is 30-90mm,
the mixed gas containing carbon source is contacted with a catalyst, the catalyst is heated to 120-150 ℃ in a heating zone, the mixed gas carries the sublimated catalyst to enter the center of a furnace tube for reaction, and the carbon nano tube is formed by pyrolysis.
5. The method according to claim 4, wherein in step 2,
the length of the quartz tube is 120-200cm, the diameter is 40-80mm,
the catalyst is heated to 130-140 ℃ in a heating zone, and the carbon nano tube floats in carrier gas and moves towards the tail of the furnace tube along with air flow.
6. The method according to any one of claims 1 to 5, wherein in step 3, the carbon nanotube film has a thickness in the range of 0.05 μm to 1000 μm and a density of less than 10mg/cm 3 。
7. The method according to claim 6, wherein in step 3, the carbon nanotube film has a thickness in the range of 0.1 μm to 800 μm and a density of less than 5mg/cm 3 。
8. The method according to any one of claims 1 to 5, wherein the density-adjustable self-supporting carbon nanotube film target is obtained by pressing a low-density carbon nanotube film into a high-density carbon nanotube film and then transferring the film.
9. The method of claim 8, wherein the substrate coated with the carbon nanotube film is taken out of the tube furnace, inverted, placed on a coupling/nesting target frame comprising a base and a target, compressed by a film press until reaching a specified height, removed, and the base is withdrawn to obtain a self-supporting carbon nanotube film target.
10. An apparatus for implementing the method for preparing a self-supporting carbon nanotube film target according to any one of claims 1 to 9, comprising a carbon nanotube or a carbon nanotube film preparing apparatus and a coupling target frame, wherein the coupling target frame is composed of a base and a target piece coupled with the base in a nesting/complementary manner, the base comprises an aluminum alloy flat plate and a cylindrical bulge array on the surface of the aluminum alloy flat plate, the height of the cylinder is the thickness of the target piece, and the diameter of the cross section is the inner diameter of a target hole on the target piece.
11. The apparatus of claim 10, wherein the base is formed of an aluminum alloy plate and an array of cylindrical protrusions on a surface thereof, and the upper surfaces of the cylindrical protrusions are subjected to precision polishing, and the spatial arrangement of the cylindrical protrusions is consistent with the arrangement of the target holes on the target.
12. The apparatus of claim 10 or 11, wherein the sizes of the target and the base can be adjusted according to actual requirements, and the inner diameter of the target hole, i.e. the diameter of the columnar bulge, d, is 1-3mm; the thickness of the target piece, namely the height of the columnar bulge, h is 0.5-1mm, the sizes of the target piece and the base are equal, the target piece is square, and the side length is 25-50mm.
13. The device of claim 12, wherein the side length is 35-40mm.
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| CN202010763009.3A CN114057184B (en) | 2020-07-31 | 2020-07-31 | Density regulation and control method and preparation device of self-supporting carbon nanotube film target |
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| CN202010763009.3A CN114057184B (en) | 2020-07-31 | 2020-07-31 | Density regulation and control method and preparation device of self-supporting carbon nanotube film target |
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| CN114057184A CN114057184A (en) | 2022-02-18 |
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| CN101723349A (en) * | 2008-10-24 | 2010-06-09 | 中国科学院金属研究所 | Method for preparing carbon nano-tube macroscopic body |
| CN103367185A (en) * | 2013-07-25 | 2013-10-23 | 中国科学院微电子研究所 | Method for manufacturing carbon nano tube flexible micro-bumps through transfer method |
| CN104176722A (en) * | 2014-08-06 | 2014-12-03 | 北京航空航天大学 | High-oriented high-strength array drawn carbon nanotube film and preparation method thereof |
| CN109925891A (en) * | 2019-03-22 | 2019-06-25 | 北京工业大学 | A kind of carbon nanotube low-pressure membrane and preparation method thereof of small-bore high throughput |
| CN110274803A (en) * | 2019-05-30 | 2019-09-24 | 中国科学院金属研究所 | Can accuracy controlling nanometer grade thickness forming thin film thickness and area film-forming method |
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| JP5327899B2 (en) * | 2008-02-29 | 2013-10-30 | 独立行政法人産業技術総合研究所 | Carbon nanotube film structure and manufacturing method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101723349A (en) * | 2008-10-24 | 2010-06-09 | 中国科学院金属研究所 | Method for preparing carbon nano-tube macroscopic body |
| CN103367185A (en) * | 2013-07-25 | 2013-10-23 | 中国科学院微电子研究所 | Method for manufacturing carbon nano tube flexible micro-bumps through transfer method |
| CN104176722A (en) * | 2014-08-06 | 2014-12-03 | 北京航空航天大学 | High-oriented high-strength array drawn carbon nanotube film and preparation method thereof |
| CN109925891A (en) * | 2019-03-22 | 2019-06-25 | 北京工业大学 | A kind of carbon nanotube low-pressure membrane and preparation method thereof of small-bore high throughput |
| CN110274803A (en) * | 2019-05-30 | 2019-09-24 | 中国科学院金属研究所 | Can accuracy controlling nanometer grade thickness forming thin film thickness and area film-forming method |
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