CN107253714A - A kind of production method of km level overlength carbon nano pipe and overlarge area graphene - Google Patents
A kind of production method of km level overlength carbon nano pipe and overlarge area graphene Download PDFInfo
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- CN107253714A CN107253714A CN201710498669.1A CN201710498669A CN107253714A CN 107253714 A CN107253714 A CN 107253714A CN 201710498669 A CN201710498669 A CN 201710498669A CN 107253714 A CN107253714 A CN 107253714A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B2204/00—Structure or properties of graphene
- C01B2204/20—Graphene characterized by its properties
- C01B2204/32—Size or surface area
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- 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
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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
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/13—Nanotubes
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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
- C01P2004/60—Particles characterised by their size
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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
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Abstract
The present invention " production method of a kind of km level overlength carbon nano pipe and overlarge area graphene " belongs to carbon nanomaterial field, the caliber that the inventive method has abandoned conventional preparation method of carbon nano-tube is irregular, length is in micron dimension, complex process, it is unable to scale and continuous production, and the graphene unit area in irregular shape of existing method production is small, complex process, it is unable to scale and continuous production some problem, and invented method, technical scheme is to use nano level carbon dust and metal dust to be that raw material makes hollow cylinder solid target, when using laser bombardment hollow cylinder solid target, the method for giving hollow cylinder solid target loading current one step ahead simultaneously, overlength carbon nano pipe and overlarge area graphene are obtained after collection, main application：The two is mainly used as carbon nano superconductive material, makes cryomotor, generator, it may also be used for nanometer electronic device, photon sensor, ultra light aircraft, superpower flak jackets, the field such as space elevator.
Description
Technical field
Originally it is new to be related to carbon nanomaterial, superconductor, and in particular to a kind of km level overlength carbon nano pipe and super large face
The production method of product graphene.
Background technology
The Crow of houston, U.S.A Rice University in 1985 takes off（Kroto, H.W.）And Shi Molai（Smalley, R.E.）
The use of wavelength is 532 nanometers, Nd:YAG. pulse laser bombardment graphite surface is so as to be found that football alkene, 1993
S.lijima and DS Bethune are found that nano material, CNT etc., Univ Manchester UK's physics in 2004 again
Family An Deliehaimu and Constantine's Nuo Woxiao loves, are successfully isolated from graphite using mechanical means in an experiment
Flake graphite alkene, CNT before is all that, in Laboratory Production, CNT has size is short, and shape is undesirable etc.,
Only several or hundreds of nanometers is long, the bidimensional that the basic structure of graphene is made up of carbon hexatomic ring（2D）Cycle is cellular
Lattice structure, although graphene is own through can largely produce, unit area is too small;Current scientific research is found：CNT
For monodimension nanometer material, lightweight, the coaxitron for mainly constituting several layers to tens of layers by the carbon atom of hexagonal arrangement is constituted,
Fixed distance, about 0.34nm are kept between layers, and diameter is generally 2-20nm；Its radial dimension is nanometer scale, axially
Size is micron dimension, and pipe two ends are substantially sealed；If regarding CNT as graphene sheet layer curling form, according to
The number of plies of graphene film can be divided into single-walled carbon nanotube and multi-walled carbon nanotube, and the representative diameter of single-walled pipe also has in 0.6 ~ 2nm
In 0.6 ~ 6nm, multi-walled pipes innermost layer is most thick up to hundreds of nanometers but typical caliber is 2 ~ 100nm up to 0.4nm；Up to now
Untill, the production method of CNT has：Arc discharge method, laser evaporization method, chemical meteorology deposition method, ion or laser splash
Method etc., these methods obtain multi-walled carbon nanotube MWNT and single-walled carbon nanotube SWNT under varying experimental conditions respectively；
（One）Arc discharge method：It is the method for earliest most typical production CNT, its advantage and disadvantage is：With succinct, institute
Obtained CNT Guan Zhi, crystallinity are high, have the disadvantage that CNT has been sintered in one because temperature is up to 3000 ~ 3700 DEG C
Rise, defect is more；
（Two）Laser evaporization method or laser ablation method：It is a kind of simple and effective new method for preparing CNT, it is substantially former
Reason is：1. the light beam for being focused into 6 ~ 7mm using laser is exposed in the graphite target containing metal, 2. control of the laser in computer
Under system, the gentle quantitative surface that carbon atom or atomic group are inspired to target, the cigarette ash of evaporation is taken away by nitrogen from body of heater, is carrying
These carbon atoms or atomic group are collided with each other to form CNT in body gas, and 3. CNT is finally deposited on outside stove
Water-cooled copper
Collector surface, CNT is present in the graphite evaporation product of inert gas entrainment, the formation of CNT
Journey is exactly
The process of the carbon atom rearrangement of free state, the advantage of laser evaporization method is：It can produce high-quality single wall carbon and receive
Mitron, the purity of CNT prepared by this method reaches 70% ~ 90%, 0.81 ~ 1.51nm of radial dimension, is easy to raw than arc process
Production, need not purify, by changing the diameter of temperature-controllable tubulation, have the disadvantage substantially：Equipment complexity energy consumption is big, cost of investment
It is high；
（Three）Chemical meteorology deposition method：It is exactly by hydro carbons（Methane, ethene, propylene and benzene etc.）Or carbon oxide（Such as Co
Deng）Cracked under the catalysis of catalyst, the conventional metallic element for making catalyst has a Fe, Co, Ni etc., research shows that carbon is received
The diameter of mitron is largely dependent upon the diameter of catalyst granules, therefore the selection by catalyst type and granularity and work
The limitation of skill condition, can obtain purity height, the CNT of even size distribution, and advantage and disadvantage are：Although yield is high, degree of purity can
Control, but cost is high, earlier stage treatment process is complicated, and preparation condition is harsh, temperature generally at 700 ~ 800 DEG C, catalyst and carrier
Effort during handling；
（Four）Ion or Laser vaporization：Though the method is easy to continuous production, because Equipment limits its scale,
（Five）" laser bombardment prepares CNT and its related nano material "《Fujian University of Technology's journal》, 2004,2（1）：8-
11, " using iron as catalyst, optical maser wavelength is 1064nm, and laser power density is 4.5 × 109W/cm2、Nd:Can under conditions of YAG
CNT is successfully prepared, and, the CNT caliber of transmission electron microscope observing to gained is about 20~50nm, length about hundreds of
Nm, most long up to more than 1 μm ", the CNT obtained by above method all haves the shortcomings that axial length is micron dimension.
The content of the invention
In order to which the purity for the CNT for solving existing preparation method of carbon nano-tube production is low, caliber is irregular, length
In micron dimension, complex process, it is impossible to scale and continuous production some problem, and the production of existing graphene preparation method
Graphene unit area in irregular shape is small, and complex process has waste liquor contamination and defect, it is impossible to scale and continuous production
Some problem, and invented method：A kind of km level overlength carbon nano pipe and the production method of overlarge area graphene, we
Method has the advantages that technique simply largely and can be prepared quickly, is a kind of km level overlength carbon nano pipe of production and overlarge area
A kind of new method of graphene,
The method of the production km level overlength carbon nano pipe of the present invention comprises the following steps：
The first step, using nano level carbon dust and metal dust as raw material, metal powder is mixed in proportion with carbon dust or graphite, such as with original
Son ratio fully carries out being mixed and made into mixed-powder for 1 ~ 2: 1,
The carbon dust raw material is nano level graphite particle or carbon black pellet, and its particle diameter is less than or equal to 1000nm, and metal dust is former
Material is nano level iron, cobalt or nickel particle, and its particle diameter is less than or equal to 100nm,
Second step, by graphite rod adhesive, such as pitch or plant organic gel add water, and the mixed-powder with the first step is in heating
Under the conditions of stir --- be made for a kind of pasty mixture, then further a kind of pasty mixture be made
Hollow cylinder solid target,
The hollow cylinder solid target be made be by using etc. quiet die pressing or compression molding method or extruding rotation section into
A kind of pasty mixture is made for hollow cylinder solid target by shape method, or after being baked again through such as 1300 DEG C or so of high temperature
Hollow cylinder solid target is made, or uses the commercially available hollow cylinder nano-carbon powder section bar for being mixed with nano metal powder
As hollow cylinder solid target,
3rd step, the laser beam sent using laser bombards the side surface of hollow cylinder solid target, while one step ahead
It is subject to electric current to hollow cylinder solid target, wherein hollow cylinder of the laser beam that sends of the laser in horizontal positioned
Shape solid target upper vertical bombards hollow cylinder solid target, and the laser beam focal plane converges at hollow cylinder
On the side surface of solid target,
The laser beam is pulse laser or continuous laser, and its focus converges the laser power density in region（Refer to the defeated of laser
The numerical value gone out obtained by the facula area at power divided by laser spot）About in 10mW/mm2To 1010W/cm2Left and right, laser is made
With the time in 1 ~ 4 hour,
During the laser beam is acted on, hollow cylinder solid target, battery, lighting bulb, switch, outer surface
Or scribble the metal cylinder of conducting resinl and connected always by wire, hollow cylinder solid target and outer surface or scribble conducting resinl
Between metal cylinder, is produced from the surface that the laser beam sent by the laser bombards hollow cylinder solid target by condenser
Raw overlength carbon nano pipe connects and constitutes a closed-loop path with said elements, separately by hollow cylinder solid target, illumination
Bulb, switch, batteries hollow cylinder solid target and outer surface or are scribbled into another closed-loop path and constantly powered-up
Individually or collectively Constant Linear Velocity is rotated the metal cylinder of conducting resinl under the drive of motor, perpendicular to hollow cylinder solid target
The focus of laser beam can be slowly moving to the other end from one end of hollow cylinder solid target, in the process or
Can without using condenser,
When laser beam starts bombardment hollow cylinder solid target, the air-flow of air blower is from hollow cylinder solid target
The focus of laser beam is pointed to or blows to outer surface or scribble the metal cylinder of conducting resinl, and closes air blast after lighting bulb is lighted
The power supply of machine,
4th step, is collected to the product that the 3rd step laser beam is bombarded after hollow cylinder solid target and obtains overlength carbon and receive
Mitron,
A kind of device for the above method, the device includes laser, such as can excitation pulse laser or continuous laser laser
Device and its power supply, including air blower, motor, separately have, hollow cylinder solid target, battery, lighting bulb, switch, outer
Surface scribbles the metal cylinder of conducting resinl by wired in series, hollow cylinder solid target and outer surface or scribbles conducting resinl
Between metal cylinder, is produced from the surface that the laser beam sent by the laser bombards hollow cylinder solid target by condenser
Raw overlength carbon nano pipe connects and constitutes a closed-loop path with said elements, separately by hollow cylinder solid target, illumination
Bulb, switch, batteries are into another closed-loop path, and hollow cylinder solid target is with outer surface or scribbles the gold of conducting resinl
Belonging to cylinder, individually or collectively Constant Linear Velocity is rotated under the drive of motor, perpendicular to the laser beam of hollow cylinder solid target
Focus can be slowly moving to the other end from one end of hollow cylinder solid target, wherein, outer surface or scribble conducting resinl
Metal cylinder be used for adhere to collect overlength carbon nano pipe.
The beneficial effects of the invention are as follows：The inventive method has abandoned the CNT of conventional preparation method of carbon nano-tube production
Purity it is low, caliber is irregular, and length is in micron dimension, complex process, it is impossible to large-scale production some problem, it is possible to achieve thousand
The large-scale industrial production of meter level overlength carbon nano pipe.
The production method of a kind of km level overlength carbon nano pipe and overlarge area graphene, present invention production overlarge area stone
The method of black alkene comprises the following steps：
The first step, using nano level carbon dust and metal dust as raw material, metal powder is mixed in proportion with carbon dust or graphite, such as with original
Son ratio fully carries out being mixed and made into mixed-powder for 1 ~ 2: 1,
The carbon dust raw material is nano level graphite particle or carbon black pellet, and its particle diameter is less than or equal to 1000nm, and metal dust is former
Material is nano level iron, cobalt or nickel particle, and its particle diameter is less than or equal to 100nm,
Second step, by graphite rod adhesive, such as pitch or plant organic gel add water, and the mixed-powder with the first step is in heating
Under the conditions of stir --- be made for a kind of pasty mixture, then further a kind of pasty mixture be made
Hollow cylinder solid target,
The hollow cylinder solid target be made be by using etc. quiet die pressing or compression molding method or extruding rotation section into
A kind of pasty mixture is made for hollow cylinder solid target by shape method, or after being baked again through such as 1300 DEG C or so of high temperature
Hollow cylinder solid target is made, or uses the commercially available hollow cylinder nano-carbon powder section bar for being mixed with nano metal powder
As hollow cylinder solid target,
3rd step, is that the laser beam that rectangular laser is sent bombards hollow cylinder solid target using focus or burnt bar
Side surface, while being subject to electric current to hollow cylinder solid target one step ahead, wherein the laser beam that the laser is sent
Hollow cylinder solid target is bombarded in the hollow cylinder solid target upper vertical of horizontal positioned, what the laser was sent
The focus of laser beam or burnt bar plane are converged on the side surface of hollow cylinder solid target,
The laser beam is pulse laser or continuous laser, and its focus or burnt bar converge the laser power density in region（Refer to and swash
The numerical value obtained by facula area at the power output divided by laser spot of light）In 10mW/mm2To 1010W/cm2, laser work
With the time in 1 ~ 4 hour,
During the laser beam is acted on, hollow cylinder solid target, battery, lighting bulb, switch, outer surface
Or scribble the metal cylinder of conducting resinl and connected always by wire, hollow cylinder solid target and outer surface or scribble conducting resinl
It is that the laser beam that rectangular laser is sent is hollow by the bombardment of rectangle condenser by focus or burnt bar between metal cylinder
The overlarge area graphene strip that the surface of circular cylindrical solid target is produced connects and constitutes a closed-loop path with said elements,
It is another by hollow cylinder solid target, lighting bulb, switch, batteries into another closed-loop path and constantly powered-up, it is hollow
Circular cylindrical solid target and outer surface scribble the metal cylinder of the conducting resinl individually or collectively Constant Linear Velocity under the drive of motor
Rotate, the long side of the focus of the laser beam or burnt bar is parallel with the axle of outer surface or the metal cylinder for scribbling conducting resinl, herein
During or can without using rectangle condenser,
When laser beam starts bombardment hollow cylinder solid target, the air-flow of air blower is from hollow cylinder solid target
Laser beam focus or burnt bar point to or blow to outer surface or scribble the metal cylinder of conducting resinl, and after lighting bulb is lighted
The power supply of the air blower is closed,
Product after 4th step, the laser beam bombardment hollow cylinder solid target sent to laser described in the 3rd step is carried out
Collection obtains overlarge area graphene strip,
A kind of device for the above method, the device includes laser, such as can excitation pulse laser or continuous laser focus
Or burnt bar is rectangular laser and its power supply, including air blower, motor, separately have, hollow cylinder solid target, electric power storage
Pond, lighting bulb, switch, outer surface scribble the metal cylinder of conducting resinl by wired in series, hollow cylinder solid target with
Outer surface is scribbled between the metal cylinder of conducting resinl, and the laser beam sent by the laser is bombarded by rectangle condenser
The overlarge area graphene strip that the surface of hollow cylinder solid target is produced connects and constitutes a closure with said elements
Loop, separately by hollow cylinder solid target, lighting bulb, switch, batteries into another closed-loop path, hollow cylinder
Solid target and outer surface or the metal cylinder individually or collectively Constant Linear Velocity rotation, institute under the drive of motor for scribbling conducting resinl
State laser beam focus or burnt bar long side it is parallel with the axle of outer surface or the metal cylinder for scribbling conducting resinl, wherein, outer surface
Or the metal cylinder of conducting resinl is scribbled for adhering to collection overlarge area graphene strip.
The beneficial effects of the invention are as follows：The inventive method has abandoned the graphene shape of existing graphene preparation method production
Irregular unit area is small, and complex process has waste liquor contamination and defect, it is impossible to scale and continuous production some problem,
The large-scale industrial production of km level length overlarge area graphene can be realized.
Brief description of the drawings：
Fig. 1 is a kind of production method block diagram of km level overlength carbon nano pipe,
Fig. 2 is a kind of production method block diagram of overlarge area graphene,
Fig. 3 is a kind of production method schematic device of km level overlength carbon nano pipe,
Fig. 4 is a kind of production method schematic device of overlarge area graphene,
Fig. 5 is a kind of km level overlength carbon nano pipe structural representation,
Fig. 6 is a kind of overlarge area graphene-structured schematic diagram,
Fig. 7 is that a kind of local transmission Electronic Speculum of km level overlength carbon nano pipe refers to photo,
Description of reference numerals：
1 --- a kind of first step of km level overlength carbon nano pipe of production,
2 --- a kind of second step of km level overlength carbon nano pipe of production,
3 --- a kind of 3rd step of km level overlength carbon nano pipe of production,
4 --- a kind of 4th step of km level overlength carbon nano pipe of production,
5 --- the laser needed for a kind of km level overlength carbon nano pipe of production,
6 --- the laser beam of laser needed for a kind of km level overlength carbon nano pipe of production,
7 --- condenser, 8 --- lighting bulb, 9 --- overlength carbon nano pipe,
10 --- outer surface or the metal cylinder for scribbling conducting resinl,
11 --- the laser needed for a kind of overlarge area graphene of production,
12 --- focus or Jiao's bar are rectangular laser beam,
13 --- focus or the rectangle condenser that burnt bar is rectangular laser beam,
14 --- overlarge area graphene, 15 --- battery,
17 --- hollow cylinder solid target, 18 --- switches,
20 --- a kind of first step of overlarge area graphene of production,
21 --- a kind of second step of overlarge area graphene of production,
22 --- a kind of 3rd step of overlarge area graphene of production,
23 --- a kind of 4th step of overlarge area graphene of production.
Embodiment：
Embodiment 1, as shown in figure 3,
Device used in the method for present invention production km level overlength carbon nano pipe 9 includes laser 5, can such as excite and continuously swash
The Nd of light:YAG laser 5（Optical maser wavelength is 1064nm）And its power supply, including air blower, motor, separately have, hollow cylinder
Solid target 17, battery 15, lighting bulb 8, switch 18, outer surface scribble the metal cylinder 10 of conducting resinl and pass through wire string
Connection, hollow cylinder solid target 17 and outer surface or is scribbled between the metal cylinder 10 of conducting resinl, by the Nd:YAG laser 5
The overlength carbon nano pipe 9 that the surface that the laser beam 6 sent bombards hollow cylinder solid target 17 by condenser 7 is produced connects
Connect and constitute a closed-loop path with said elements, separately by hollow cylinder solid target 17, lighting bulb 8, switch 18, electric power storage
Pond 15 constitutes another closed-loop path, hollow cylinder solid target 17 and outer surface or scribbles the metal cylinder 10 of conducting resinl and distinguishes
Or the common Constant Linear Velocity under the drive of motor is rotated, perpendicular to Jiao of the laser beam 6 of hollow cylinder solid target 17
Point can be slowly moving to the other end from one end of hollow cylinder solid target 17, wherein, outer surface or scribble conducting resinl
Metal cylinder 10, which is used to adhere to, collects overlength carbon nano pipe 9, and the CNT caliber of gained is in 5nm ~ 15nm or so, and length is 1080
Rice.
The step of producing overlength carbon nano pipe 9 is as follows：
The first step, using nano level carbon dust and metal dust as raw material, metal powder is filled with carbon dust or graphite using atomic ratio as 1 ~ 2: 1
Progress is divided to be mixed and made into mixed-powder,
The carbon dust raw material is nano level graphite particle or carbon black pellet, and its particle diameter is less than or equal to 5nm ~ 20nm, metal dust
Raw material is nano level iron, cobalt or nickel particle, and its particle diameter is less than or equal to 5nm,
Second step, the mixed-powder of graphite rod binder pitch and the first step is sufficiently stirred under conditions of heating
It is even --- a kind of pasty mixture is made for, then further by a kind of pasty mixture using extruding rotation section shaping legal system
Into hollow cylinder solid target 17, the overall diameter of hollow cylinder solid target 17 is 20cm, and interior diameter is 2cm, length or
Highly it is 20cm,
3rd step, the laser beam 6 sent using laser 5 bombards the side surface of hollow cylinder solid target 17, while first
One step is subject to 0.1A electric current to hollow cylinder solid target 17, wherein the laser beam 6 that the laser 5 is sent is in level
The upper vertical of the hollow cylinder solid target 17 bombardment hollow cylinder solid target 17 of placement, the focus of laser beam 6
Plane is converged on the side surface of hollow cylinder solid target 17,
The laser beam 6 is continuous laser, and the laser power density in its focus convergence region is about in 500mW/mm2To 109W/
cm2Left and right, the laser action time in 2 hours,
During the laser beam 6 is acted on, hollow cylinder solid target 17, battery 15, lighting bulb 8, switch
18th, outer surface or scribble the metal cylinder 10 of conducting resinl and connected always by wire, hollow cylinder solid target 17 and outer surface
Or scribble between the metal cylinder 10 of conducting resinl, the laser beam 6 sent by the laser 5 bombards open circles by condenser 7
The overlength carbon nano pipe 9 that the surface of cylindricality solid target 17 is produced connects and constitutes a closed-loop path with said elements, separately by
Hollow cylinder solid target 17, lighting bulb 8, switch 18, battery 15 constitute another closed-loop path and constantly powered-up, empty
Heart circular cylindrical solid target 17 and outer surface or scribble conducting resinl metal cylinder 10 it is individually or collectively inferior in the drive of motor
The meter per second of linear velocity 0.15 is rotated, and the focus perpendicular to the laser beam 6 of hollow cylinder solid target 17 can be from hollow cylinder
One end of solid target 17 is slowly moving to arrive the other end,
When laser beam 6 starts bombardment hollow cylinder solid target 17, the air-flow of air blower is from hollow cylinder solid target
The focus of laser beam 6 is pointed to or blows to outer surface or scribble the metal cylinder 10 of conducting resinl on material 17, and is lighted in lighting bulb 8
The power supply of air blower is closed afterwards,
4th step, is collected to the product that the 3rd step laser beam 6 is bombarded after hollow cylinder solid target 17 and obtains overlength
CNT 9.The power supply of the laser 5 is first closed at the end of production, the power supply of 2 lighting bulbs 8 is then turned off.
Embodiment 2, as shown in figure 4, used in the method for present invention production km level length overlarge area graphene 14
Device includes laser 11, and the focus or burnt bar that can such as excite continuous laser are rectangular Nd:YAG laser 11（Laser wave
A length of 1064nm, focus or burnt bar are less than or equal to 5cm for the long side of the burnt bar of rectangular laser beam）And its power supply, including
Air blower, motor, separately have, hollow cylinder solid target 17, battery 15, lighting bulb 8, switch 18, outer surface or painting
The metal cylinder 10 for having conducting resinl passes through wired in series, hollow cylinder solid target 17 and outer surface or the metal for scribbling conducting resinl
Between cylinder 10, by the Nd:The laser beam 12 that YAG laser 11 is sent bombards hollow cylinder by rectangle condenser 13
The strip of overlarge area graphene 14 that the surface of solid target 17 is produced connects and constitutes a closed-loop path with said elements, separately
Another closed-loop path, hollow cylinder are constituted by hollow cylinder solid target 17, lighting bulb 8, switch 18, battery 15
Solid target 17 and outer surface scribble the metal cylinder 10 of conducting resinl individually or collectively Constant Linear Velocity turn under the drive of motor
Dynamic, the long side of the burnt bar of the laser beam 12 is parallel with the axle of outer surface or the metal cylinder 10 for scribbling conducting resinl, wherein, appearance
Face scribbles the metal cylinder 10 of conducting resinl for adhering to the strip of collection overlarge area graphene 14, the overlarge area graphene of gained
14 strip widths are less than or equal to 5cm, and length is at 1080 meters or so.
Production overlarge area graphene 14 has the following steps：
The first step, using nano level carbon dust and metal dust as raw material, metal powder is filled with carbon dust or graphite using atomic ratio as 1 ~ 2: 1
Progress is divided to be mixed and made into mixed-powder,
The carbon dust raw material is nano level graphite particle or carbon black pellet, and its particle diameter is in 5nm ~ 20nm, metal dust raw material
Nano level iron, cobalt or nickel particle, its particle diameter in 5nm or so,
Second step, the mixed-powder of graphite rod binder pitch and the first step is sufficiently stirred under conditions of heating
It is even --- a kind of pasty mixture is made for, then further by a kind of pasty mixture using extruding rotation section shaping legal system
Into hollow cylinder solid target 17, the overall diameter of hollow cylinder solid target 17 is 20cm, and interior diameter is 2cm, length or
Highly be more than or equal to 5cm,
3rd step, is rectangular Nd using focus or burnt bar:The bombardment hollow cylinder of laser beam 12 that YAG laser 11 is sent
The side surface of shape solid target 17, while being subject to 0.1A electric current to hollow cylinder solid target 17 one step ahead, wherein described
The laser beam 12 that laser 11 is sent bombards hollow cylinder in the upper vertical of hollow cylinder solid target 17 of horizontal positioned
Shape solid target 17, the focus for the laser beam 12 that the laser 11 is sent or burnt bar plane converge at hollow cylinder solid
On the side surface of target 17,
The laser beam 12 is continuous laser, and the laser power density in its focus or burnt bar convergence region is in 500mW/mm2Extremely
109W/cm2, the laser action time in 2 hours,
During the laser beam 12 is acted on, hollow cylinder solid target 17, battery 15, lighting bulb 8, switch
18th, outer surface or scribble the metal cylinder 10 of conducting resinl and connected always by wire, hollow cylinder solid target 17 and outer surface
Or scribble between the metal cylinder 10 of conducting resinl, it is rectangular Nd by focus or burnt bar:The laser beam that YAG laser 11 is sent
The strip of overlarge area graphene 14 that 12 surfaces for bombarding hollow cylinder solid target 17 by rectangle condenser 13 are produced
Connect and constitute a closed-loop path with said elements, separately by hollow cylinder solid target 17, lighting bulb 8, switch 18, storage
It is simultaneously constantly powered-up that battery 15 constitutes another closed-loop path, hollow cylinder solid target 17 and outer surface or scribbles conducting resinl
Individually or collectively the meter per second of Constant Linear Velocity 0.15 is rotated metal cylinder 10 under the drive of motor, the focus of the laser beam 12
Or the long side of burnt bar is parallel with the axle of outer surface or the metal cylinder 10 for scribbling conducting resinl,
When laser beam 12 starts bombardment hollow cylinder solid target 17, the air-flow of air blower is from hollow cylinder solid target
The focus of laser beam 12 on material 17 or burnt bar point to or blow to outer surface or scribble the metal cylinder 10 of conducting resinl, and in illumination
Bulb 8 closes the power supply of the air blower after lighting,
Production after 4th step, the bombardment hollow cylinder solid of laser beam 12 target 17 sent to laser 11 described in the 3rd step
Thing, which is collected, obtains the strip of overlarge area graphene 14.
The power supply of the laser 11 is first closed at the end of production, the power supply of 2 lighting bulbs 8 is then turned off.
In summary, including but not limited to those skilled in the art is it should be appreciated that the above embodiment of the present invention and parameter,
And the limitation present invention is not used to, the engineers and technicians of this area can on an equal basis be replaced to above-mentioned 2 kinds of process units structures
Or improve, progress one when also can be to raw material type and its proportioning, raw material particle size size parameter, laser power density, laser action
Successive step, the production method of a kind of km level overlength carbon nano pipe described in the invention and overlarge area graphene and its any
Improve, including use pulse laser instead, including it is close to raw material type and its proportioning and raw material particle size size parameter, laser power
Degree, any adjustment of laser action duration and improvement will all fall inside the protection domain of application claims.
Claims (10)
1. the production method of a kind of km level overlength carbon nano pipe and overlarge area graphene, it is characterised in that production km level is super
Long CNT comprises the following steps：
The first step, using nano level carbon dust and metal dust as raw material, metal powder is mixed in proportion with carbon dust or graphite, such as with original
Son ratio fully carries out being mixed and made into mixed-powder for 1 ~ 2: 1,
Second step, by graphite rod adhesive, such as pitch or plant organic gel add water, and the mixed-powder with the first step is in heating
Under the conditions of stir --- be made for a kind of pasty mixture, then further a kind of pasty mixture be made
Hollow cylinder solid target,
3rd step, the laser beam sent using laser bombards the side surface of hollow cylinder solid target, wherein described swash
The laser beam that light device is sent bombards hollow cylinder solid target in the hollow cylinder solid target upper vertical of horizontal positioned
Material, the laser beam focal plane is converged on the side surface of hollow cylinder solid target,
4th step, is collected to the product that the 3rd step laser beam is bombarded after hollow cylinder solid target and obtains overlength carbon and receive
Mitron.
2. a kind of production method of km level overlength carbon nano pipe and overlarge area graphene, it is characterised in that production overlarge area
Graphene comprises the following steps：
The first step, using nano level carbon dust and metal dust as raw material, metal powder is mixed in proportion with carbon dust or graphite, such as with original
Son ratio fully carries out being mixed and made into mixed-powder for 1 ~ 2: 1,
Second step, by graphite rod adhesive, such as pitch or plant organic gel add water, and the mixed-powder with the first step is in heating
Under the conditions of stir --- be made for a kind of pasty mixture, then further a kind of pasty mixture be made
Hollow cylinder solid target,
3rd step, is that the laser beam that rectangular laser is sent bombards hollow cylinder solid target using focus or burnt bar
Side surface, wherein the laser beam that sends of the laser horizontal positioned hollow cylinder solid target upper vertical Hong
Hollow cylinder solid target is hit, the focus for the laser beam that the laser is sent or burnt bar plane converge at hollow cylinder
On the side surface of solid target,
Product after 4th step, the laser beam bombardment hollow cylinder solid target sent to laser described in the 3rd step is carried out
Collection obtains overlarge area graphene strip.
3. method according to claim 1 or 2, it is characterised in that the carbon dust raw material is nano level graphite particle or charcoal
Black particle, its particle diameter is less than or equal to 1000nm, and metal dust raw material is nano level iron, cobalt or nickel particle, and its particle diameter is less than etc.
In 100nm.
4. method according to claim 1 or 2, it is characterised in that being made for the hollow cylinder solid target is to pass through
Using etc. quiet die pressing or compression molding method or extruding rotation section forming process a kind of pasty mixture is made for hollow cylinder
Shape solid target, or be made hollow cylinder solid target after being baked again through such as 1300 DEG C or so of high temperature, or using commercially available mixed
Conjunction has the hollow cylinder nano-carbon powder section bar of nano metal powder as hollow cylinder solid target.
5. method according to claim 1 or 2, it is characterised in that bombard hollow cylinder solid using the laser beam
During the side surface of target, while being subject to electric current to hollow cylinder solid target one step ahead.
6. method according to claim 1 or 2, it is characterised in that the laser beam is continuous laser or pulse laser,
The laser power density in its focus or burnt bar convergence region is about in 10mW/mm2To 1010W/cm2Left and right.
7. according to the method described in claim 1, it is characterised in that during the laser beam is acted on, hollow cylinder
Solid target, battery, lighting bulb, switch, outer surface scribble the metal cylinder of conducting resinl and connected always by wire, hollow
Circular cylindrical solid target and outer surface are scribbled between the metal cylinder of conducting resinl, and the laser beam sent by the laser passes through
The overlength carbon nano pipe that the surface of condenser bombardment hollow cylinder solid target is produced connects and constitutes one with said elements
Closed-loop path, separately by hollow cylinder solid target, lighting bulb, switch, batteries into another closed-loop path and always
Power-up, hollow cylinder solid target and outer surface or scribbles the metal cylinder of conducting resinl individually or collectively under the drive of motor
Constant Linear Velocity is rotated, and the focus perpendicular to the laser beam of hollow cylinder solid target can be from hollow cylinder solid target
One end is slowly moving to arrive the other end, in the process or can be without using condenser.
8. method according to claim 2, it is characterised in that during the laser beam is acted on, hollow cylinder
Solid target, battery, lighting bulb, switch, outer surface scribble the metal cylinder of conducting resinl and connected always by wire, hollow
Circular cylindrical solid target and outer surface are scribbled between the metal cylinder of conducting resinl, are rectangular laser hair by focus or burnt bar
The overlarge area graphene that the surface that the laser beam gone out bombards hollow cylinder solid target by rectangle condenser is produced
Strip connects and constitutes a closed-loop path with said elements, separately by hollow cylinder solid target, lighting bulb, switch, storage
Battery constitutes another closed-loop path and constantly powered-up, hollow cylinder solid target and outer surface or the metal for scribbling conducting resinl
Individually or collectively Constant Linear Velocity is rotated cylinder under the drive of motor, the long side and appearance of the focus of the laser beam or burnt bar
Face or scribble conducting resinl metal cylinder axle it is parallel, in the process or can be without using rectangle condenser.
9. a kind of device for claim 1 methods described, it is characterised in that the device includes laser, such as can excitation pulse
The laser and its power supply of laser or continuous laser, including air blower, motor, separately have, hollow cylinder solid target, electric power storage
Pond, lighting bulb, switch, outer surface scribble the metal cylinder of conducting resinl by wired in series, hollow cylinder solid target with
Outer surface is scribbled between the metal cylinder of conducting resinl, and the laser beam sent by the laser bombards open circles by condenser
The overlength carbon nano pipe that the surface of cylindricality solid target is produced connects and constitutes a closed-loop path with said elements, separately by hollow
Circular cylindrical solid target, lighting bulb, switch, batteries into another closed-loop path, hollow cylinder solid target with it is outer
Surface or the metal cylinder individually or collectively Constant Linear Velocity rotation under the drive of motor for scribbling conducting resinl, perpendicular to hollow cylinder
The focus of the laser beam of shape solid target can be slowly moving to the other end from one end of hollow cylinder solid target.
10. a kind of device for claim 2 methods described, it is characterised in that the device includes laser, can such as excite arteries and veins
The focus of impulse light or continuous laser or burnt bar are rectangular laser and its power supply, including air blower, motor, are separately had,
Hollow cylinder solid target, battery, lighting bulb, switch, outer surface scribble the metal cylinder of conducting resinl and pass through wire string
Connection, hollow cylinder solid target and outer surface or is scribbled between the metal cylinder of conducting resinl, the laser sent by the laser
The overlarge area graphene strip that the surface that light beam bombards hollow cylinder solid target by rectangle condenser is produced is connected
And with said elements constitute a closed-loop path, separately by hollow cylinder solid target, lighting bulb, switch, batteries into
Another closed-loop path, hollow cylinder solid target and outer surface or scribbles the metal cylinder of conducting resinl individually or collectively electronic
Constant Linear Velocity is rotated under the drive of machine, the focus of the laser beam or the long side and outer surface of burnt bar or the gold for scribbling conducting resinl
The axle for belonging to cylinder is parallel.
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| CN113113184A (en) * | 2021-03-29 | 2021-07-13 | 深圳先进技术研究院 | Carbon-based superconducting material and preparation method thereof |
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| CN104495793A (en) * | 2014-10-25 | 2015-04-08 | 王德龙 | Laser-based production method of kilometer-scale super-long carbon nanotubes and super-large area graphene |
| CN104860678A (en) * | 2015-04-29 | 2015-08-26 | 萝北奥星新材料有限公司 | Method for producing ultra-high power graphite electrode through natural graphite |
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| CN1273215A (en) * | 2000-05-23 | 2000-11-15 | 广东工业大学 | Process for preparing nm-class single-wall carbon tubes by high-power continuous CO2 laser |
| CN104495793A (en) * | 2014-10-25 | 2015-04-08 | 王德龙 | Laser-based production method of kilometer-scale super-long carbon nanotubes and super-large area graphene |
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