CN109231162B - A kind of method of seamless welding carbon nanotube - Google Patents
A kind of method of seamless welding carbon nanotube Download PDFInfo
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- CN109231162B CN109231162B CN201811043933.3A CN201811043933A CN109231162B CN 109231162 B CN109231162 B CN 109231162B CN 201811043933 A CN201811043933 A CN 201811043933A CN 109231162 B CN109231162 B CN 109231162B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82B—NANOSTRUCTURES FORMED BY MANIPULATION OF INDIVIDUAL ATOMS, MOLECULES, OR LIMITED COLLECTIONS OF ATOMS OR MOLECULES AS DISCRETE UNITS; MANUFACTURE OR TREATMENT THEREOF
- B82B3/00—Manufacture or treatment of nanostructures by manipulation of individual atoms or molecules, or limited collections of atoms or molecules as discrete units
- B82B3/0042—Assembling discrete nanostructures into nanostructural devices
- B82B3/0047—Bonding two or more elements
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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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- 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
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
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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
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/158—Carbon nanotubes
- C01B32/168—After-treatment
- C01B32/176—Cutting
Abstract
A kind of method of seamless welding carbon nanotube, is related to carbon nanotube.It chooses a carbon nanotube and is burnt into two sections using high current, or arbitrarily choose two different carbon nanotubes；Using electron beam is focused, amorphous carbon is deposited to connect two sections of carbon nanotubes in the gap of carbon nanotube port；It is annealed using Joule heating to the total after connection, obtains height crystallization and the continuous carbon nano tube structure of tube wall, realize the seamless welding of carbon nanotube.For the caliber direction of carbon nanotube, tube wall number, caliber and chiral equal no requirement (NR), other than it can carry out welded in place reparation to the same root carbon pipe blown in device, the seamless welding between any two with different tube diameters direction, tube wall number, caliber and chirality or more carbon nanotubes is applied also for.
Description
Technical field
The present invention relates to carbon nanotubes, more particularly, to a kind of method of seamless welding carbon nanotube.
Background technique
Basis of the microelectronic component as Modern Information and automation is dimensionally to become small, the following Xiang Na electricity
Sub- device development is a critically important trend.With the raising of device integration in chip, individual devices and connecting lead wire
Size will all reduce.For some traditional metal lead wires (such as copper, aluminium etc.), when size it is small to a certain extent when will face one
The challenge of series, heat dissipation problem and electromigration effect can damage connecting lead wire.Carbon nanotube is due to its excellent property
Can, had received widespread attention in related fields.The thermal conductivity of itself is very high, and SP2Carbon-carbon bond can effectively press down
The destruction of electromigration effect processed, makes it possible to the current density for bearing three orders of magnitude higher than common metal.Carbon nanotube is
Many relevant researchs have been carried out as FETs and connecting lead wire etc. through studied personnel.It can be seen that future electronic device can
It can develop from " silicon substrate " to " carbon-based ", and then " full carbon " electronic device may be developed into.
For carbon-based or full carbon electronic device, after the interconnection and carbon nanotube wire breaking between carbon nanotube
Reparation will be several big problems to be faced.There is electron beam high-temperature soldering for the method for carbon nanotube connection at present
[Terrones M,Banhart F,Grobert N,et al.Molecular junctions by joining single-
Walled carbon nanotubes [J] .Physical review letters, 2002,89 (7): 075505.], electric current adds
Thermal weld [Jin C, Suenaga K, Iijima S.Plumbing carbon nanotubes [J] .Nature
Nanotechnology, 2008,3 (1): 17.], amorphous carbon formula connect [Wang M S, Wang J Y, Chen Q, et
al.Fabrication and electrical and mechanical properties of carbon nanotube
Interconnections [J] .Advanced Functional Materials, 2005,15 (11): 1825-1831.], gold
Metal particles bridging formula connects [Rodr í guez-Manzo J A, Wang M S, Banhart F, et al.Multibranched
junctions of carbon nanotubes via cobalt particles[J].Advanced Materials,
2009,21 (44): 4477-4482.] etc., but all cut both ways.Such as some are only applicable to single wall or double-walled carbon nano-tube, weldering
Connect simple coarse, the auxiliary for needing respective metal particle etc..
Summary of the invention
The purpose of the present invention is to provide the welded in place that may be not only suitable for after blowing in device with root carbon nanotube to repair
Nothing that is multiple, and being applicable between any two of different tube diameters, tube wall number, caliber direction and chirality or more carbon nanotubes
Seam welding, a kind of method of seamless welding carbon nanotube with broad applicability.
The present invention the following steps are included:
1) it chooses a carbon nanotube and is burnt into two sections using high current, or arbitrarily choose two different carbon and receive
Mitron；
2) using electron beam is focused, amorphous carbon is deposited to connect two sections of carbon nanometers in the gap of carbon nanotube port
Pipe；
3) it is annealed using Joule heating to the total after connection, obtains height crystallization and the continuous carbon of tube wall is received
Nanotube structures realize the seamless welding of carbon nanotube.
In step 1), a piece carbon nanotube of the selection is simultaneously burnt into two sections, or any selection using high current
The specific method of two different carbon nanotubes can are as follows: mobile tungsten tip in situ makes tungsten tip and is sticked to one of spun gold edge
Carbon nanotube end contact, by applying multiple current impulse, making carbon nanometer in tungsten tip and spun gold electrode both ends making alive
Pipe is connect with two end electrodes, and then one bigger to carbon nanotube application, suitable current impulse again, makes carbon nanotube and two
Termination electrode is blown；One section of carbon nanotube is sticked on tungsten tip, and another section of carbon nanotube is sticked to spun gold edge, as to be welded two
Root carbon nanotube, or select a different carbon nanotube again, with the carbon nanotube that is sticked on tungsten tip as to be welded two
Root carbon nanotube.
The tungsten tip is the tungsten wire corrosion gained using electrochemical erosion method to 0.2mm diameter, in order to seek tungsten tip
The good electrical contact between carbon nanotube can carry out In-Situ Cleaning processing to tungsten tip usually before experiment, in tungsten tip
The constant pressure of 3V is added with spun gold both ends, mobile tungsten tip is gone close to spun gold edge, when tungsten tip and spun gold contact, tungsten needle sharp
End moment is melt into smooth spherical, and surface contaminant is cleaned out；The spun gold is for another termination electrode and adherency carbon nanometer
The substrate of pipe, diameter 0.25mm, front end pliers is pressed from both sides at flat, then front edge is cut, and obtains smoother front end
Edge；The carbon nanotube can prepare sample by removing the powder of scratch carbon nanotube with spun gold front end, i.e., can be there are many carbon
Nanotube is stained with and stretches out from spun gold edge, and one end is hanging.
It is described using electron beam is focused in step 2), amorphous carbon is deposited in the gap of carbon nanotube port with even
The specific method for connecing two sections of carbon nanotubes can are as follows:
(1) position of mobile tungsten tip, the port for keeping two carbon nanotubes obtained by step 1) to be welded are in same
The height of sample, and the gap of suitable distance is reserved between port；
(2) using the electron beam of suitable spot size, by Electron Beam Focusing port at one end, beam spot size is controlled, one section
Size and the consistent amorphous carbon nano dot of carbon nanotube caliber are deposited after time at port, once heavy at port
When product goes out amorphous carbon nano dot, slowly evenly to other port mobile spot, the track moved along beam spot can be deposited
A bit of amorphous carbon " nanometer bridge " structure out makes both ends port pass through the amorphous carbon with caliber approx. dimension deposited
" nanometer bridge " connects.
It is described to be annealed using Joule heating to the total after connection in step 3), obtain height crystallization and
The continuous carbon nano tube structure of tube wall realizes that the specific method of the seamless welding of carbon nanotube can are as follows: in tungsten tip and spun gold
Both ends apply constant pressure, are annealed using the Joule heat of generation to total, manually adjusting voltage gradually increases it, with this
The Joule heat generated simultaneously is also gradually increased, and keeps the crystallization degree of amorphous carbon and total higher and higher, by one section
After the Joule heating of time, it is seamlessly connected the fracture tube wall at two sections of carbon nanotube ports by continuous tubular graphene
Come, forms height crystallization and the continuous carbon nano tube structure of tube wall.
The present invention carries out the growth of amorphous carbon " nanometer bridge " by the motion track that control focuses electron beam, makes two sections of carbon
Nanotube connects；So that entire connection structure is carried out sufficient crystallization by Joule heating again, eventually forms seamless connection
Tube wall reaches to the seamless welding between carbon nanotube.Two or more carbon nanotubes no matter caliber direction, tube wall number, caliber
It is whether identical with chirality, it may be by this technology and carry out seamless welding.Due to the structure of last sufficiently crystallization, after making welding
Structure and original carbon nanotubes poorly conductive it is few.
Compared with existing carbon nanotube interconnection technique, the present invention is had the advantage that and technical effect is as follows:
1) present invention is for the caliber direction of carbon nanotube, tube wall number, caliber and chiral equal no requirement (NR), in addition to can be to device
The same root carbon pipe blown in part apply also for except welded in place reparation with different tube diameters direction, tube wall number, caliber
Seamless welding between chiral any two or more carbon nanotubes.
2) present invention is not welded with amorphous carbon packaging type not instead of simply, is taken using amorphous carbon " nanometer bridge "
Bridge-type connects, and forms the seamless connection between tube wall and tube wall after Annealing Crystallization, is almost no different with complete carbon nano tube structure.
3) present invention does not need to complete by the auxiliary of other metallic particles.
Detailed description of the invention
Fig. 1 is the process schematic of the embodiment of the present invention.
Fig. 2 be with tungsten tip be sticked to gold electrode edge and stretch out the Electronic Speculum after the hanging carbon nanotube end in one end contacts
Figure.
Fig. 3 is the electron microscope that carbon nanotube is burnt into two sections.
Fig. 4 is the Electronic Speculum for being connected two carbon pipes in port gap deposition amorphous carbon using electron beam is focused
Figure.
Fig. 5 for dotted rectangle institute target amorphous carbon junction in Fig. 4 high resolution electron microscopy figure.
Fig. 6 is the height crystallization obtained after being annealed using Joule heating and the continuous carbon nano tube structure of the several layers of tube walls of outer layer
Electron microscope.
Fig. 7 is the electron microscope of the carbon nanotube of two different tube diameters sizes.
Fig. 8 is several for the height crystallization and outer layer obtained after the carbon nanotube progress seamless welding to two different tube diameters sizes
The layer continuous carbon nano tube structure electron microscope of tube wall.
Fig. 9 is the electron microscope of the carbon nanotube in two different tube diameters directions.
Figure 10 is to carry out the height crystallization obtained after seamless welding and outer layer to the carbon nanotube in two different tube diameters directions
The electron microscope of several layers of continuous carbon nano tube structures of tube wall.
Specific embodiment
Below by the specific implementation of several examples and attached drawing, the invention will be further described, will receive to by same root carbon
Detailed implementation method introduction is made in welded in place reparation after mitron is blown, in addition respectively to different tube diameters size and different tube diameters
Two embodiments in direction are briefly introduced and Detailed description of the invention.
1, it chooses a carbon nanotube and is burnt into two sections using high current
A kind of method of seamless welding carbon nanotube provided by the invention is carried out in transmission electron microscope, the party
The process schematic of method as shown in Figure 1, wherein tungsten tip electrode can be three-dimensional mobile, fix, can at electrode both ends by spun gold electrode
Apply electric signal.First tungsten tip in situ mobile connects it with being sticked to spun gold edge and stretch out the hanging carbon nanotube end in one end
Touching, as shown in Figure 2.In order to make contact of the carbon nanotube with metal electrode improve, then applied in tungsten tip and spun gold electrode both ends
The pulse signal of time 0~2.5V is added, electric current limits below 100 μ A.Then, current limitation is changed to 1mA hereinafter, in electrode two
End applies the pulse signal of 0~3.5V, and carbon nanotube blows into two sections, and one section is sticked on tungsten tip, and another section still in spun gold
Over there, as shown in Figure 3.
2, using electron beam is focused, amorphous carbon is deposited to connect two sections of carbon nanotubes in the gap of carbon nanotube port
Mobile tungsten tip, the port for keeping two sections of carbon nanotubes to be welded is in same height, and reserves between port suitable
When the gap of distance.Suitable spot size (generally using 6~10) is chosen, adjusts Electronic Speculum to suitable amplification factor, and make
Port is in positive burnt.Adjustment electron beam spot is reduced to minimum, at the carbon nanotube port for focusing on it on tungsten tip, every one section
Time scatter hot spot discovery size and the approximate amorphous carbon nanometer spot of carbon nanotube caliber are deposited at port.Then fast
Hot spot is reduced to minimum by speed again, and from this one end slowly evenly to other port mobile spot, the mobile speed of hot spot will make
The speed of amorphous carbon continuous deposition forward is got caught up in.Last hot spot is moved to other port and deposits above amorphous
When carbon, scatter rapidly hot spot and before spot size is adjusted back to photographing mode state.Both ends be pass through deposit with pipe
The amorphous carbon " nanometer bridge " of diameter approx. dimension connects, as shown in Figure 4.Fig. 5 be in Fig. 4 dotted rectangle institute's target without fixed
The High-Resolution Map of shape carbon junction.
3, it is annealed using Joule heating to the total after connection, obtains height crystallization and the continuous carbon of tube wall is received
Nanotube structures, to realize the seamless welding of carbon pipe
After being connected with amorphous carbon " nanometer bridge ", apply constant pressure in tungsten tip and spun gold both ends, electric current is limited 100
μ A or less.The amplification factor of Electronic Speculum, which is transferred to 630K or other, can observe the multiple of carbon nanotube high-resolution photo, use phase
Machine observes the variation of connection structure in real time.First since 0.5V, then gradually up making alive, electric current also can gradually increase manually
Greatly, the Joule heat of generation can anneal to total.It is alive and meanwhile want the moment concern current value variation and
The variation of carbon nano tube structure, with the progress of Joule heating, unbodied structure can gradually crystallization, the electric conductivity of structure also can
Improve, corresponding electric current also will increase.The size of current that different carbon nanotubes can be born is different, so generally limiting electric current
100 μ A are hereinafter, prevent structure in crystallization process from maintaining great constant pressure to come to structure depending on actual conditions by considerable damage
It carries out Joule heating (voltage is typically maintained between 1.5~2V).After annealing after a period of time, original two sections of carbon nanometers
Some fracture tube walls at pipe port are connected by continuous tubular graphene, form height crystallization and the several layers of pipes of outer layer
The continuous carbon nano tube structure of wall, as shown in fig. 6, to realize the seamless welding of carbon nanotube.The side of this seamless welding
Method has finally obtained the structure almost the same with original multi-walled carbon nanotube, and electric conductivity is also similar.
The present invention is applicable not only to the welded in place reparation after same root carbon nanotube is blown in device, and can be used for having
There is the seamless welding between any two of different tube diameters direction, tube wall number, caliber and chirality or more carbon nanotubes.Here,
It respectively shows and two carbon nanotubes with different tube diameters size (Fig. 7) and different tube diameters direction (Fig. 9) is carried out without seam weld
The example connect.Both examples are compared with the seamless welding reparation in situ after same root carbon nanotube is blown, in specific embodiment party
It is unique different exactly after blowing carbon pipe using high current in method, new carbon pipe is chosen at spun gold edge and is sticked to tungsten tip
On carbon nanotube carry out welded in place.The result of welding as shown in figures 8 and 10, equally realizes seamless between carbon nanotube
Welding.
The present invention carries out relevant welding in transmission electron microscope, using manipulation in situ platform.The manipulation in situ is flat
Platform has two end electrodes, and one end is tungsten tip that can be three-dimensional mobile, and the other end is fixed spun gold, and carbon nanotube is to be sticked to spun gold
Edge.It is contacted by mobile tungsten tip with carbon nanotube, applying bias appropriate in two end electrodes blows carbon nanotube, In
The preceding paragraph carbon nanotube is glued on tungsten tip.Formed two sections can will be blown by same root carbon pipe, or arbitrarily another at spun gold edge
The carbon pipe on a carbon nanotube and tungsten tip is selected, as two carbon nanotubes to be welded.Mobile tungsten tip is adjusted, is made to be welded
There are suitable gaps at the two sections of carbon nanotube ports connect, using with focusing electron beam controllable precise in port gap deposition nothing
Setting carbon carries out bridging connection.Being biased later by both ends makes amorphous carbon crystallization using Joule heat, finally with original pipe
Wall forms seamless welding.
Claims (6)
1. a kind of method of seamless welding carbon nanotube, it is characterised in that the following steps are included:
1) it chooses a carbon nanotube and is burnt into two sections using high current, or arbitrarily choose two different carbon nanometers
Pipe；
2) using electron beam is focused, amorphous carbon is deposited to connect two sections of carbon nanotubes in the gap of carbon nanotube port, is had
Body method:
(1) position of mobile tungsten tip, the port for keeping two carbon nanotubes obtained by step 1) to be welded are in same
Highly, and between port the gap of suitable distance is reserved；
(2) Electron Beam Focusing port at one end is controlled into beam spot size, a period of time using the electron beam of suitable spot size
Size and the consistent amorphous carbon nano dot of carbon nanotube caliber are deposited at port afterwards, once depositing at port
When amorphous carbon nano dot, to other port mobile spot, the track moved along beam spot can deposit a bit of amorphous
Carbon " nanometer bridge " structure has connect both ends port with the amorphous carbon " nanometer bridge " of caliber approx. dimension by what is deposited
Come；
3) it is annealed using Joule heating to the total after connection, obtains height crystallization and the continuous carbon nanotube of tube wall
Structure realizes the seamless welding of carbon nanotube.
2. a kind of method of seamless welding carbon nanotube as described in claim 1, it is characterised in that in step 1), the selection
A piece carbon nanotube is simultaneously burnt into two sections using high current, or arbitrarily chooses the specific method of two different carbon nanotubes
Are as follows: tungsten tip in situ mobile contacts tungsten tip with a carbon nanotube end for being sticked to spun gold edge, by tungsten tip with
Spun gold electrode both ends making alive, applies multiple current impulse, connect carbon nanotube with two end electrodes, then again to carbon nanometer
Pipe applies current impulse, blows carbon nanotube with two end electrodes；One section of carbon nanotube is sticked on tungsten tip, another section of carbon nanometer
Pipe is sticked to spun gold edge, as two carbon nanotubes to be welded, or selects a different carbon nanotube again, and is sticked to tungsten needle
Carbon nanotube on point is as two carbon nanotubes to be welded.
3. a kind of method of seamless welding carbon nanotube as claimed in claim 2, it is characterised in that the tungsten tip is to utilize electricity
Chemical corrosion method corrodes gained to the tungsten wire of 0.2mm diameter, In-Situ Cleaning processing is carried out to tungsten tip before experiment, in tungsten tip
The constant pressure of 3V is added with spun gold both ends, mobile tungsten tip is gone close to spun gold edge, when tungsten tip and spun gold contact, tungsten needle sharp
End moment is melt into smooth spherical, and surface contaminant is cleaned out.
4. a kind of method of seamless welding carbon nanotube as claimed in claim 2, it is characterised in that the spun gold is for electrode
With the substrate of adherency carbon nanotube, diameter 0.25mm, front end pliers is pressed from both sides at flat, then front edge is cut, and is obtained
Smooth front edge.
5. a kind of method of seamless welding carbon nanotube as claimed in claim 2, it is characterised in that the carbon nanotube passes through use
Spun gold front end goes the powder of scratch carbon nanotube to prepare sample, so that carbon nanotube is stained with and is stretched out from spun gold edge, one end is outstanding
It is empty.
6. a kind of method of seamless welding carbon nanotube as described in claim 1, it is characterised in that in step 3), the utilization
Joule heating anneals to the total after connection, obtains height crystallization and the continuous carbon nano tube structure of tube wall, realizes
The seamless welding of carbon nanotube method particularly includes: apply constant pressure at the both ends of tungsten tip and spun gold, utilize the Joule heat of generation
It anneals to total, manually adjusting voltage gradually increases it, and the Joule heat generated at the same time is also gradually increased, and makes
Amorphous carbon and the crystallization degree of total are higher and higher, after Joule heating after a period of time, two sections of carbon are made to receive
Fracture tube wall at mitron port is got up by the seamless connection of continuous tubular graphene, forms height crystallization and the continuous carbon of tube wall
Nano tube structure.
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| GB0304623D0 (en) * | 2003-02-28 | 2003-04-02 | Univ Surrey | Methods for the fabrication of nanoscale structures and semiconductor devices |
| CN101481086B (en) * | 2009-01-22 | 2011-03-23 | 上海交通大学 | Non-damaged in situ construction method for nano-node |
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| CN103693634B (en) * | 2013-12-08 | 2015-10-28 | 北京工业大学 | E-beam induced deposition prepares the method for carbon nanotube |
| CN106301280B (en) * | 2016-07-26 | 2018-07-17 | 厦门大学 | A kind of adjusting method of cantilever beam carbon nanotube resonant device frequency |
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| CN102053180A (en) * | 2010-11-26 | 2011-05-11 | 天津大学 | Method for reinforcing lateral rigidity of hanging nanotube device through electron beam induced metal deposition |
| WO2015063413A1 (en) * | 2013-11-04 | 2015-05-07 | Arkema France | Black polymer composition suitable for laser welding |
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