CN114057184A - Density regulating method and preparation device of self-supporting carbon nanotube film target - Google Patents
Density regulating method and preparation device of self-supporting carbon nanotube film target Download PDFInfo
- Publication number
- CN114057184A CN114057184A CN202010763009.3A CN202010763009A CN114057184A CN 114057184 A CN114057184 A CN 114057184A CN 202010763009 A CN202010763009 A CN 202010763009A CN 114057184 A CN114057184 A CN 114057184A
- Authority
- CN
- China
- Prior art keywords
- target
- carbon nanotube
- nanotube film
- density
- tube
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/16—Preparation
- C01B32/162—Preparation characterised by catalysts
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Manufacturing & Machinery (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention discloses a self-supporting carbon nanotube film, a self-supporting carbon nanotube film target, a preparation method and a density control method thereof, and a correspondingly adopted preparation device. The device and/or the method provided by the invention prepare the microcosmic uniform low-density carbon tube film by a floating catalytic chemical vapor deposition method, then compress and transfer the film by a high-precision film pressing machine to obtain the self-supporting film target with the specified density, realize the self-supporting of the target hole and the regulation and control of the specified density in a large range, and can be used for laser targeting experiments or application.
Description
Technical Field
The invention relates to a density-adjustable self-supporting carbon nanotube film target, a density regulating method or a preparation method of the film target and an adopted device, belonging to the technical field of novel nano material manufacturing and application.
Background
The interaction of ultrashort and ultrastrong laser pulses and a self-supporting thin film target can realize ion acceleration, and the method has the advantages of high acceleration gradient, low manufacturing cost, no breakdown threshold limit and the like, and has attracted wide attention due to potential application values in the fields of proton imaging, nuclear fusion fast ignition and the like. Experimental research shows that the quality of the film target has key influence on the quality of cut-off energy, strong current, energy dispersion and the like of the ion beam obtained by acceleration. The self-supporting carbon nanotube film is micro-uniform and porous, and can generate uniform plasma with high temperature and high energy density when acting with super-strong laser pulse. When carbon tube films with different densities interact with the ultra-strong laser pulse, a new acceleration mechanism can be induced to form, and proton/carbon ion beams with high average energy and small energy dispersion are obtained. The proton/carbon ion obtained by accelerating has Bragg peak in the energy deposition effect in organisms, and has unique advantages in radiotherapy and cancer treatment.
At present, the preparation methods of the self-supporting carbon nanotube film mainly include a solution method and a chemical vapor deposition method. The carbon tube prepared by the solution method has the property of oleophobic and hydrophobic property of large pi bond on the surface, and the method is difficult to prepare a uniformly dispersed homogeneous carbon tube film unless complicated and complicated carbon tube functionalization treatment is carried out. In order to realize a peelable self-supporting film independent of a substrate, most of carbon nanotubes prepared by a chemical vapor deposition method have high density and thickness, and a low-density self-supporting film is difficult to realize. Patent CN105271163A discloses a continuous preparation and film-forming method of carbon nanotube macroscopic body, and the success rate of self-supporting of the prepared carbon tube film is low by adopting mechanical stripping or dissolution stripping. Considering the problem that the film is self-supported and easy to damage, the self-supporting carbon tube film prepared by the method has high density generally, and the density of the carbon tube film can be changed in a certain range only by controlling reaction conditions, so that the carbon tube film is difficult to perform large-range specified 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 desired to provide a self-supporting carbon nanotube film target with low density, easy peeling, and easy and flexible adjustment of density, thereby meeting the requirements of laser acceleration experiments.
Disclosure of Invention
The invention aims to solve the problems and provides a self-supporting carbon nanotube film, a self-supporting carbon nanotube film target, a preparation method and a density control method thereof and a correspondingly adopted preparation device aiming at the application requirement of the self-supporting carbon nanotube film in the field of laser acceleration. The device and/or the method provided by the invention prepare the microcosmic uniform low-density carbon tube film by a floating catalytic chemical vapor deposition method, then compress and transfer the film by a high-precision film pressing machine to obtain the self-supporting film target with the specified density, realize the self-supporting of the target hole and the regulation and control of the specified density in a large range, and can be used for laser targeting experiments or application, thereby completing the invention.
Therefore, according to the first aspect of the present invention, a method for preparing a self-supporting carbon nanotube thin film target is provided, wherein a carbon nanotube film is prepared first, then pressed into a high-density carbon nanotube film, and finally transferred, thereby preparing a self-supporting carbon nanotube thin film target with adjustable density.
In the present invention, the production of the carbon nanotube or the carbon nanotube film is carried out in a production apparatus comprising a tube furnace, preferably a high-temperature tube furnace, such as a quartz tube.
According to the present invention, the preparation of carbon nanotubes or carbon nanotube films comprises the steps of:
step 1, preparing a carbon source and a catalyst,
step 2, carrying out catalytic cracking reaction to form carbon nano-tubes,
and 3, forming the carbon nano tube film on the substrate.
In step 1, the carbon source is a carbohydrate, particularly a hydrocarbon compound, and it is preferable to use a mixed gas containing a carbon source in which a gas inert to the reaction (e.g., nitrogen or a rare gas such as argon) is mixed as a carrier gas, wherein, 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 the catalyst, preferably a mixed catalyst of ferrocene and a sulfur-containing compound, which may be sulfur powder, is 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.
In step 2, the cracking reaction is carried out in a preparation device comprising a tubular furnace, the temperature of the central high-temperature region of the furnace tube can reach more than 1000 ℃, preferably 1100-1200 ℃, the tubular furnace is preferably a quartz tube, the tube length of the tubular furnace is between 100-300cm, preferably 120-200cm, for example 150cm, and the diameter of the tubular furnace is between 30-90mm, preferably 40-80mm, for example 60 mm. The mixed gas containing carbon source contacts with catalyst, the catalyst is heated to above 100 deg.C in heating zone, such as 120-.
In step 3, the substrate is a conductive monocrystalline silicon wafer, which is horizontally inserted into a deposition boat at the tail of the furnace tube, the carbon nanotubes floating on the carrier gas and moving together with the carrier gas are mutually lapped, and a carbon nanotube film is formed on the substrate along with the reduction of the temperature at the tail of the furnace tube, the thickness of the carbon nanotube film is 0.05-1000 μm, preferably 0.1-800 μm, and the density is lower than 10mg/cm3Preferably less than 5mg/cm3Even as low as 1mg/cm3。
In the preparation method, a low-density carbon nanotube film is pressed into a high-density carbon nanotube film, then the high-density carbon nanotube film is transferred to obtain a self-supporting carbon nanotube film target with adjustable density, preferably, a substrate (or a deposited silicon wafer or a conductive silicon wafer) coated with the carbon nanotube film is taken out of a tube furnace, is reversely buckled and is placed on a coupling/nesting target frame comprising a base and a target wafer, a film pressing machine is used for compressing the substrate until the specified height is reached, the silicon wafer is removed, and the base is extracted to obtain the self-supporting carbon nanotube film target.
According to a second aspect of the present invention, a method for controlling the density of a self-supporting carbon nanotube thin film target is provided, which is implemented by mechanical compression and adhesive transfer, preferably, a conductive silicon wafer coated with carbon tubes is placed on a coupling target holder in a flush manner, and then transferred to a film pressing machine for compression, wherein the compression height (i.e. thickness) is set according to the required density, i.e. by compressing to a specified height 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 holder, wherein the coupling target holder is composed of a base and a target sheet coupled and nested/complementary thereto, wherein the base of the coupling target holder comprises an aluminum alloy flat plate and a cylindrical protrusion array on the surface thereof, preferably only composed of the two parts, the height of the cylinder is the thickness of the target sheet, the diameter of the cross section is the inner diameter of a target hole on the target sheet, and preferably, the upper surface of the cylindrical protrusion is subjected to precision polishing treatment. The spatial arrangement of the target holes is consistent with the arrangement of the target holes on the target plate.
In the invention, the sizes of the target sheet 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 1-3 mm; the thickness of the target, i.e. the height of the stud bumps, h, may be 0.5-1mm, the target and the base being of equal size and may be square, for example 25-50mm, more preferably 35-40mm, on a side.
Compared with the prior art, the invention has the following advantages:
1) the carbon nano tube film prepared has the carbon tubes arranged in a uniform and disordered way, good microscopic isotropic uniformity and very low film density (as low as 1 mg/cm)3)。
2) The method realizes the successful preparation of the self-supporting carbon nano tube film target in the low-density interval by matching with the subsequent processes of mechanical compression and self-supporting transfer, and solves the problems of easy damage and low success rate when the self-supporting is realized by the low-density carbon nano tube film target.
3) The density regulation and control method provided by the invention does not depend on the regulation of preparation parameters, can carry out large-scale specified density regulation and control on the carbon nano tube film target on a low-density starting point, prepares the self-supporting carbon nano tube film target with specific density, and well meets the requirements of laser accelerated experiments and application
Drawings
FIG. 1 is a schematic view of an apparatus for manufacturing a carbon nanotube film;
FIG. 2 is a schematic diagram of the compression and transfer process of carbon tube thin film target density control;
FIG. 3 is a drawing of a base of a coupling target and a target coupled and nested therewith;
FIG. 4 is an SEM photograph of a carbon tube thin film target obtained in example 1.
Detailed Description
The invention is explained in more detail below with reference to the figures and examples. The features and advantages of the present invention will become more apparent from the description.
The word "exemplary" is used exclusively 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. While the various aspects of the embodiments are presented in drawings, the drawings are not necessarily drawn to scale unless specifically indicated.
The invention is explained in more detail below with reference to the drawings and preferred embodiments. The features and advantages of the present invention will become more apparent from the description.
According to the invention, the preparation method or the density control method of the self-supporting carbon nanotube film target is provided, the carbon nanotube film is firstly prepared, then the carbon nanotube film with high density is pressed, and finally the transfer is carried out, so that the self-supporting carbon nanotube film target with adjustable density is prepared.
In the present invention, the carbon nanotubes or carbon nanotube films are produced in a production apparatus comprising a tube furnace, preferably a high-temperature tube furnace, such as a quartz tube, in which a high-temperature region can be formed in the middle of the tube furnace, i.e., in the center of the tube furnace, a catalyst heating region is provided on one side of the production apparatus, and a deposition region is provided on the other side of the tube furnace opposite thereto, in which a deposition boat is placed, into which substrates can be inserted.
The carbon nanotube film preparation device provided by the invention is shown in figure 1, wherein inlet gas 1 carries a catalyst 2 heated by a heater 3 to enter a tube furnace, the reaction is carried out in a high-temperature area 4 in the furnace, the generated carbon nanotube moves to the tail part of the tube furnace, and a carbon nanotube film is formed on a deposition 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 produce carbon nanotubes by catalytic cracking, and it is preferable to use a carbohydrate, particularly a hydrocarbon compound such as an alkane like methane, ethane, propane, butane, etc., and an aromatic hydrocarbon like benzene, toluene, xylene, etc., and it is preferable to use methane as the carbon source.
In the present invention, the catalyst can catalyze the cracking of carbon source, and ferrocene can be used as the catalyst, preferably a mixed catalyst of ferrocene and a sulfur-containing compound, which can be sulfur powder, and the catalyst is used in the form of mixed powder, wherein the ferrocene and the sulfur powder are mixed in a weight ratio of 90-95:1, preferably 91-94:1, more preferably 92-93:1, and optionally ground 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, half an hour, so as to be mixed well.
According to a preferred embodiment of the present invention, a mixed gas containing a carbon source in which a gas inert to the reaction (such as nitrogen or a rare gas) is mixed as a carrier gas in addition to the hydrocarbon compound as the carbon source is used, and preferably a rare gas such as helium, neon, argon, and more preferably argon is used.
According to the invention, the mixed gas is mixed in a gas mixing box, wherein methane is added at a flow rate of 2-20 sccm, preferably 5-15 sccm, and an inert gas, such as argon, is added at a flow rate of 500-2000 sccm, preferably 800-1200 sccm, and the mixed gas is introduced into the preparation device as inlet gas 1.
And 2, carrying out catalytic cracking reaction to form the carbon nano tube.
In the present invention, the cracking reaction is carried out in the above-mentioned preparation apparatus comprising a tube furnace, and the temperature of the central high-temperature region of the furnace tube can reach 1000 ℃ or more, preferably 1100 ℃ to 1200 ℃, above which the furnace tube is easily broken. The tube furnace is preferably a quartz tube having a tube length of between 100 and 300cm, preferably 120 and 200cm, for example 150cm, and a diameter of between 30 and 90mm, preferably 40 and 80mm, for example 60 mm.
According to the present invention, before the reaction, the air in the quartz tube is evacuated, for example, the quartz tube may be purged with gas, preferably the mixed gas or one of the gases is evacuated, for example, argon gas (preferably at a flow rate of 800 to 1200sccm) is introduced for several seconds to several minutes, for example, 5 seconds to 2 minutes, preferably 10 seconds before the reaction, and then the gas is exhausted from the furnace tube through the exhaust 6.
According to the invention, after being uniformly mixed by a gas mixing box, the mixed gas containing the carbon source is introduced into the quartz tube with the air being exhausted through an 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 ℃ by a heater 3 in a heating zone, for example, at the temperature of 120-.
In the invention, hydrocarbon compounds such as methane and the like as carbon sources are reaction gases, are catalytically cracked, are reconstructed and grown into carbon nanotubes, and float in carrier gas, so that the carbon nanotubes move in the quartz tube, for example, the carbon nanotubes can move along the tail part of the tube along with the airflow in the same direction.
And 3, forming the carbon nano tube film on the substrate.
In the invention, the substrate is a conductive monocrystalline silicon piece, and the monocrystalline silicon piece 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.
Along with the temperature reduction of the tail part of the furnace tube, the carbon nanotubes floating on the carrier gas and moving together with the carrier gas are mutually lapped, and a carbon nanotube film is formed on the substrate.
Therefore, by utilizing 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 disorderly distributed, the microcosmic isotropic 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 disorderly arranged.
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 can be controlled, for example, by the deposition time. In addition, the carbon nano tubes of the film are microscopically distributed in a disordered and uniform manner, and the density is low and is generally less than 10mg/cm3Preferably less than 5mg/cm3Even as low as 1mg/cm3。
According to the method, 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 density-adjustable self-supporting carbon nanotube film target is obtained.
According to a preferred embodiment of the invention, the substrate (or deposited silicon wafer, conductive silicon wafer) covered or attached with the carbon nanotube film is taken out of the tube furnace, reversed, placed on a coupling/nesting target stand comprising a base and a target, compressed by a laminator until a specified height is reached, the silicon wafer is removed, and the base is extracted to obtain the self-supporting carbon tube film target.
In the invention, the density regulation and self-support of the carbon tube film are realized by mechanical compression and bonding transfer, and the specific realization mode is as follows:
the conductive silicon wafer coated with carbon tubes is placed on the coupling target frame in a flush manner, and then the conductive silicon wafer is transferred to a film pressing machine for compression, wherein the compression height (namely the thickness) is set according to the required density, namely the conductive silicon wafer is compressed to the specified height to meet the specified density requirement.
In 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 carbon tube is tightly adhered on the target sheet while being compressed by utilizing the viscosity of the carbon tube and the difference between the surface roughness of the target sheet and the substrate, namely the surface of the target sheet is far rougher than the surface of a silicon wafer, so that the nondestructive transfer of the film and the self-support of a target hole are realized, and the self-supporting carbon nanotube film which is attached to the target sheet and has the specified density is obtained and can be directly installed for laser targeting experiments or practical application.
The process of compressing and transferring the carbon tube film target density regulation is 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 a target sheet on the base, as shown in the right figure of figure 3.
In the invention, the coupling target frame is composed of a base and a target sheet which is coupled and nested/complementary with the base. The base comprises a flat plate of aluminium alloy and an array of cylindrical protrusions on its surface, preferably consisting of only said two parts. The height of the column is the thickness of the target, the diameter of the cross section is the inner diameter of the target hole on the target, and the upper surface of the columnar bulge is subjected to precision polishing treatment. The spatial arrangement of the target holder is consistent with the arrangement of the target holes on the target, so that the target can be tightly buckled on the base to form the target holder with a smooth upper surface.
According to the preferred embodiment of the invention, the sizes of the target sheet and the base can be adjusted according to actual requirements. The target hole inner diameter, i.e. the diameter of the columnar projection, d, may be 0,5-5mm, preferably 1-3mm, most preferably 2 mm; the thickness of the target, i.e. the height of the stud bumps, h, may be from 0.1 to 3mm, preferably from 0.5 to 1mm, most preferably 0.7mm, the target and the base being of equal size and may be square, for example 10 to 100mm on a side, preferably 25 to 50mm, more preferably 35 to 40mm, for example 38mm x 38mm in size.
The present invention will be further described with reference to the following examples.
Example 1
The silicon wafer to be deposited with the carbon tube is placed into a film pressing machine for zeroing, then a deposition boat is inserted, and the silicon wafer is placed into a deposition area of a tube furnace. As shown in FIG. 1, a quartz boat containing a catalyst (mixed powder of ferrocene and sulfur powder in a weight ratio of 92: 1) was placed on the gas inlet side of a tube furnace, above a heater, heated to 130 ℃ while introducing 1000sccm argon gas to remove the gas in the furnace tube, thereby forming an inert atmosphere. After 10 seconds, methane is introduced together with argon gas at the flow rate of 10sccm, the methane and the argon gas carry a heated and sublimed catalyst to enter the center of a furnace tube at 1100 ℃, and the methane is catalytically cracked, reconstructed and grown into carbon nanotubes which are deposited on a silicon wafer along with carrier gas to form a film. And closing all gas valves after 30 minutes, finishing 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 chip, and determining the compression height according to the experimental density requirement. The coated silicon wafer is carefully reversed on a coupling target frame as shown in the right diagram of fig. 3, placed on a compression table with zero calibration, 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 holder to obtain a self-supporting carbon nanotube film target. The film target is intact, has no crack, and is uniform and flat through visual observation.
The initial thickness of the prepared carbon nanotube film was measured to be 188 μm, and the corresponding initial density was measured to be 1.24mg/cm3Height after compression of 17 μm, corresponding to a density of 13.71mg/cm3。
The scanning electron microscope image of the prepared carbon tube film is shown in fig. 4, and it can be seen that the carbon nanotubes in the film are in disordered and uniform distribution under the micron scale, the surface is clean, the granular impurities are few, and the requirements of laser acceleration experiments are well met.
Example 2
The silicon wafer to be deposited with the carbon tube is placed into a film pressing machine for zeroing, then a deposition boat is inserted, and the silicon wafer is placed into a deposition area of a tube furnace. As shown in FIG. 1, a quartz boat containing a catalyst (mixed powder of ferrocene and sulfur powder at a weight ratio of 93: 1) was placed on the gas inlet side of a tube furnace, above a heater, heated to 140 ℃ while introducing 800sccm argon gas to remove the air in the furnace tube, thereby forming an inert atmosphere. After 10 seconds, methane is introduced together with argon at the flow rate of 12sccm, the methane and the argon carry the heated and sublimated catalyst to enter the center of a furnace tube at 1100 ℃, the methane is catalytically cracked, reconstructed and grown into carbon nanotubes, and the carbon nanotubes deposit on a silicon wafer along with carrier gas to form a film. And closing all gas valves after 20 minutes, finishing 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 chip, and determining the compression height according to the experimental density requirement. The coated silicon wafer is carefully reversed on a designed coupling target frame as shown in the right diagram of fig. 3, placed on a compression table with zero calibration, 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 holder to obtain a self-supporting carbon nanotube film target.
The initial thickness of the prepared carbon nanotube film was measured to be 127 μm, and the corresponding initial density was measured to be 2.68mg/cm3Height after compression of 26 μm, corresponding to a density of 13.10mg/cm3。
The present invention has been described above in connection with preferred embodiments, but these embodiments are merely exemplary and merely illustrative. On the basis of the above, the invention can be subjected to various substitutions and modifications, and the substitutions and the modifications are all within the protection scope of the invention.
Claims (10)
1. A preparation method of a self-supporting carbon nanotube film target is characterized in that a carbon nanotube film is prepared firstly, then the carbon nanotube film is pressed into a high-density carbon nanotube film, and finally the carbon nanotube film target is transferred, so that the self-supporting carbon nanotube film target with adjustable density is prepared.
2. The method according to claim 1, wherein the production of the carbon nanotubes or carbon nanotube films is carried out in a production apparatus comprising a tube furnace, preferably a high temperature tube furnace, such as a quartz tube.
3. The production method according to claim 1 or 2, characterized in that the production of the carbon nanotube or the carbon nanotube film comprises the steps of:
step 1, preparing a carbon source and a catalyst,
step 2, carrying out catalytic cracking reaction to form carbon nano-tubes,
and 3, forming the carbon nano tube film on the substrate.
4. The production method according to claim 3, wherein, in step 1,
the carbon source is a carbohydrate, particularly a hydrocarbon compound, and it is preferable to use a mixed gas containing a carbon source in which a gas inert to the reaction (e.g., nitrogen or a rare gas such as argon) is mixed as a carrier gas, the mixed gas containing methane at a flow rate of 5 to 15sccm and argon at a flow rate of 800 to 1200sccm,
ferrocene is used as the catalyst, preferably a mixed catalyst of ferrocene and a sulfur-containing compound, which may be sulfur powder, is 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.
5. The production method according to claim 3 or 4, wherein, in step 2,
the cracking reaction is carried out in a preparation apparatus comprising a tube furnace, the temperature of the central high-temperature region of the furnace tube can reach more than 1000 ℃, preferably 1100-1200 ℃, the tube furnace is preferably a quartz tube, the tube length of the tube furnace is between 100-300cm, preferably 120-200cm, such as 150cm, the diameter of the tube furnace is between 30-90mm, preferably 40-80mm, such as 60mm,
the mixed gas containing carbon source contacts with catalyst, the catalyst is heated to above 100 deg.C in heating zone, such as 120-.
6. The production method according to any one of claims 3 to 5, wherein in the step 3, the substrate is a conductive single crystal silicon wafer which is horizontally inserted into a deposition boat at the end of a furnace tube, and the carbon nanotubes floating on the carrier gas and moving together therewith are lapped with each other, and a carbon nanotube film having a thickness in the range of 0.05 μm to 1000 μm, preferably 0.1 μm to 800 μm and a density lower than 10mg/cm is formed on the substrate as the temperature at the end of the furnace tube decreases3Preferably less than 5mg/cm3Even as low as 1mg/cm3。
7. The method of any one of claims 1 to 6, wherein the low-density carbon nanotube film is pressed into a high-density carbon nanotube film and then transferred to obtain a density-tunable self-supporting carbon nanotube film target, and preferably, the substrate (or the deposited silicon wafer, the conductive silicon wafer) coated with the carbon nanotube film is taken out of the tube furnace, reversed, placed on a coupling/nesting target stand comprising a base and a target plate, compressed by a laminator until a designated height is reached, the silicon wafer is removed, and the base is extracted to obtain a self-supporting carbon nanotube film target.
8. A method for regulating and controlling the density of self-supporting carbon nanotube film target includes such steps as mechanically compressing, adhering and transferring, putting the conductive silicon wafers on the coupling target frame, covering them with carbon tubes, aligning them, transferring them to film pressing machine, and compressing to a certain height.
9. A preparation device of a 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 sheet coupled and nested/complemented with the base, the base comprises an aluminum alloy flat plate and a cylindrical protrusion array on the surface of the aluminum alloy flat plate, preferably only composed of two parts, the height of a cylinder is the thickness of the target sheet, the diameter of the cross section is the inner diameter of a target hole in the target sheet, preferably, the upper surface of the cylindrical protrusion is subjected to precision polishing treatment, and the spatial arrangement of the cylindrical protrusion is consistent with the arrangement of the target hole in the target sheet.
10. The manufacturing apparatus as set forth in claim 9, wherein the target and the pedestal are adjustable in size, and the inner diameter of the target hole, i.e., the diameter of the columnar projection, d, is 1-3 mm; the thickness of the target, i.e. the height of the stud bumps, h, may be 0.5-1mm, the target and the base being of equal size and may be square, for example 25-50mm, more preferably 35-40mm, on a side.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN114057184A true CN114057184A (en) | 2022-02-18 |
| CN114057184B CN114057184B (en) | 2023-06-09 |
Family
ID=80227987
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202010763009.3A Active CN114057184B (en) | 2020-07-31 | 2020-07-31 | Density regulation and control method and preparation device of self-supporting carbon nanotube film target |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN114057184B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| US20110111177A1 (en) * | 2008-02-29 | 2011-05-12 | Kenji Hata | Carbon nanotube film structure and method for manufacturing the same |
| 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 |
-
2020
- 2020-07-31 CN CN202010763009.3A patent/CN114057184B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110111177A1 (en) * | 2008-02-29 | 2011-05-12 | Kenji Hata | Carbon nanotube film structure and method for manufacturing the same |
| 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 |
Also Published As
| Publication number | Publication date |
|---|---|
| CN114057184B (en) | 2023-06-09 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| JP5553353B2 (en) | Monoatomic film manufacturing method | |
| EP1413550B1 (en) | Method and device for synthesizing high orientationally arranged carbon nanotubes by using organic liquid | |
| KR20010085509A (en) | Process for controlled growth of carbon nanotubes | |
| JPH0477711B2 (en) | ||
| US20070224364A1 (en) | Plasma processing apparatus, plasma processing method, plasma film deposition apparatus, and plasma film deposition method | |
| CN111943130B (en) | Nano needle array and preparation method and application thereof | |
| CN1282801A (en) | Chemical vapour phase deposition equipment and method of synthesizing nanometer pipe using said equipment | |
| US10961123B2 (en) | Apparatus and method for synthesizing vertically aligned carbon nanotubes | |
| US5961719A (en) | Nucleation of diamond films using an electrode | |
| CN114057184A (en) | Density regulating method and preparation device of self-supporting carbon nanotube film target | |
| WO2004048258A2 (en) | Method for forming carbon nanotubes | |
| JPS6136200A (en) | Method for vapor-phase synthesis of diamond | |
| US7883927B2 (en) | Method and apparatus to sort nanotubes | |
| Fang et al. | Carbon nanotubes on nanoporous alumina: from surface mats to conformal pore filling | |
| TW502307B (en) | Method for preparation of diamond film | |
| CN114908338B (en) | Apparatus and method for depositing carbon nanotube foam on self-supporting film | |
| WO1993005207A1 (en) | Method of nucleating diamond and article produced thereby | |
| KR100513713B1 (en) | Growth method for vertically aligned carbon nanotubes by changing the morphologies of a transition metal thin films | |
| JP3028121B2 (en) | How to make diamond thin film | |
| KR20010049546A (en) | Synthesis method of highly purified carbon nanotubes | |
| JPS63169387A (en) | Formation of thin film | |
| JP4781617B2 (en) | Method for producing diamond film | |
| CN1559892A (en) | Process of carbon nano-structure body transforming into nano-diamond | |
| JP3291273B2 (en) | Carbon coating method | |
| JPS63169386A (en) | Formation of thin film |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |