CN104942455B - Low-temperature self-welding method of carbon-coating copper nanowires - Google Patents
Low-temperature self-welding method of carbon-coating copper nanowires Download PDFInfo
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- CN104942455B CN104942455B CN201510246707.5A CN201510246707A CN104942455B CN 104942455 B CN104942455 B CN 104942455B CN 201510246707 A CN201510246707 A CN 201510246707A CN 104942455 B CN104942455 B CN 104942455B
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B23—MACHINE TOOLS; METAL-WORKING NOT OTHERWISE PROVIDED FOR
- B23K—SOLDERING OR UNSOLDERING; WELDING; CLADDING OR PLATING BY SOLDERING OR WELDING; CUTTING BY APPLYING HEAT LOCALLY, e.g. FLAME CUTTING; WORKING BY LASER BEAM
- B23K31/00—Processes relevant to this subclass, specially adapted for particular articles or purposes, but not covered by only one of the preceding main groups
- B23K31/02—Processes relevant to this subclass, specially adapted for particular articles or purposes, but not covered by only one of the preceding main groups relating to soldering or welding
Abstract
The invention discloses a low-temperature self-welding method of carbon-coating copper nanowires, and relates to the field of nano welding. According to the technical scheme of the welding method, the copper nanowires wrapped with carbon shells and provided with five-fold twinned crystal structures are synthesized through a hydrothermal method. When the copper nanowires are in lap joint to form point contact and heated under a low-vacuum condition to 40-70% of a bulk copper melting point, namely 300-725 DEG C, copper atoms diffuse and are accumulated at contact points through a channel formed by the carbon shells, and accordingly under the condition that no other welding flux is used, self-welding is achieved, and the effect that the copper nanowires are connected is achieved. The nano welding technology has the advantages that work temperature is low, flow speed is high, the range is adjustable, welding can be achieved at multiple points on a large scale at the same time, no welding flux is needed, and pollution is not caused. Tests prove that welding points have excellent mechanical and electric characteristics, and the method is expected to be widely used in the fields of flexible electronic systems, semiconductor integrated circuits, micro-nano electronic packaging, transparent electrodes and the like.
Description
Technical field
The present invention relates to nano-weld technical field is and in particular to a kind of low temperature of carbon coating copper nano-wire is from the side of welding
Method.
Background technology
Nano material is due to physical propertys such as its unique optics, electricity, magnetics by extensive concern, scientist and engineering
Teachers have gone out multiple nano materials by various synthetic method controllable standbies, but if these nano materials tool to be formed
There is the device of certain 26S Proteasome Structure and Function, be necessary for being assembled these materials using certain solder technology.Yet with biography
The macroscopical welding method of system cannot operate to the material of nanoscale, and therefore nano-weld technology becomes research in nanotechnology at present
One focus in field and difficulties.
Interconnection technique in nanoscale mainly has three classes at present, i.e. electron beam/ion beam assisted depositing (Electron/
Ion Beam Induced Deposition, EBID/IBID), nanometer melting and cold welding.Electron beam/ion beam assisted depositing
Principle similar to chemical vapor deposition prepare thin-film material (Electron/Ion Beam Induced Deposition,
EBID/IBID)(Reyntjens S,Puers R.A review of focused ion beam applications in
microsystem technology[J].Journal of Micromechanics and Microengineering,
2001).This method is that (presoma containing deposited material is typically contained the metallo-organic compound of deposited element
Gas, such as W (CO)6、PtC7H17、Al(CH3)3Deng), the electricity consumption while nozzle needle of the intracavity that works sprays to deposition substrate surface
Son or ion beam carry out induction and irradiate, and these metallo-organic compound precursors divide after the bombardment by electron beam or ion beam
Solution, metallic element is enriched in substrate in a large number, and volatile element (as oxygen and hydrogen) is taken away by vacuum pump, the metal of these enrichments
Element regroups in the presence of ion beam, forms sedimentary.The advantage of this method is can to carry out high-precision fixed spot deposition,
But less efficient, expensive, amorphous carbon and diffusion into the surface can be produced with deposition process, and ion is also readily injected into
In sample, sample is polluted.
Nanometer melting is to produce Joule heat by electric current, by solder fusing, thus being attached to welding object.One
Typical case is the copper nano-wire two ends energising that carbon shell is wrapped in, and when voltage reaches to a certain degree, copper nano-wire is in Jiao
Melt in the presence of having burning ears, increase voltage further, the copper atom of fusing occurs directional transmissions to realize under electromigratory effect
Nano-weld (Dong L, Tao X, Zhang L, et al.Nanorobotic spot welding:controlled metal
deposition with attogram precision from copper-filled carbon nanotubes[J]
.Nano Letters,2007).The welding precision of this method is high, and minimum mass flow rate is only 120ag/s, plus bigger electricity
During pressure, can reach 500ag/s the soonest, flow velocity changes over substantially (Golberg D, Costa PMFJ, Mitome M, et
al.Copper-Filled Carbon Nanotubes:Rheostatlike Behavior and Femtogram Copper
Mass Transport[J].Advanced Materials,2007；One-dimensional tin silver bielement nano material for micro-/ nano welding
Material：China, CN103406685A, 2013.11.27).Another typical case be a root bead material nano wire is placed on to be welded
Material on, by being energized to solder nano wire two ends, will be in the big place of resistance (i.e. solder and Nanowire contacts to be welded
Place) produce more Joule heat, from but solder local melting.Profit can be welded and fixed to nano wire in this way
(Peng Y,Cullis T,Inkson B.Bottom-up nanoconstruction by the welding of
individual metallic nanoobjects using nanoscale solder[J].Nano Letters,2009).
Compared to electron beam/ion beam assisted deposition, the advantage that nanometer melts welding technology is low cost, pollutes little, high precision.
But because this kind of welding method is all carried out on far above metal material fusing point, therefore easily treat welding material and make
Become certain damage；And it is difficult to control to the flow rate of solder, so this technology still has some problems.
Cold welding is by by two nanometer rods/linear contact lay together, heating or apply higher stress, just can be in
At normal temperatures two nanometer rods/lines are linked together in short time, the mechanics of nanometer rods/line and electric property are not subject to shadow simultaneously
Ring (Lu Y, Huang JY, et al.Cold welding of untrathin gold nanowires [J] .Nature
Nanotechnology,2010.2.14).This method is successfully carried out in silver/silver, gold/silver and gold/nanowires of gold.Its
Advantage be pollution-free on sample, be not required to that heating, speed is fast, mechanics electric property is not affected by welding.But, the shortcoming of cold welding
It is, this welding manner has high demands for the clean-up performance of sample；Sample size has high demands, and the diameter of nanometer rods/line needs
In below 10nm；Can not many together welding it is difficult to scale application.
Additionally, the common ground of above-mentioned micro/nano-scale solder technology is in the same time, limited junction point can only to be welded
Connect, be not suitable for carrying out high flux welding to large area solder joint simultaneously, and the latter to the industrial applications of micro-nano electron trade is
Necessary.This patent is intended to invent a kind of reliable solder technology so that nano-weld can be real when far below material melting point
Now on a large scale, multiple spot high flux welding, because solder is derived from material itself, thus its mass velocity does not change over and changes
Become, and solder joint has excellent mechanics, electric property.
Content of the invention
Present invention is generally directed to the shortcoming and defect of current nano-weld technical field, occurred after the heating based on copper atom
Diffusing phenomenon, a kind of low temperature of carbon coating copper nano-wire is proposed from welding method, the method has that operating temperature is low, flow velocity is big
The advantages of scope is adjustable, solder is high and multiple spot welds simultaneously on a large scale, is expected in flexible electronics system, quasiconductor is integrated
The fields such as circuit, micro-nano electron device package, transparency electrode are extensively applied.
In order to achieve the above object, the present invention adopts the following technical scheme that：
From welding method, synthesize Surface coating using hydro-thermal method has the copper of carbon shell to a kind of low temperature of carbon coating copper nano-wire
Nano wire, is mutually lapped formation point contact between nano wire, is heated to the 40%-70% of block copper fusing point under vacuum
When i.e. 300 DEG C～725 DEG C, copper nano-wire will not melt, but copper atom realizes mass transport by diffusion, in copper nano-wire
The place contacting with each other is accumulated, thus under conditions of no additional solder, realizing being connected with each other of copper nano-wire.
A kind of low temperature of carbon coating copper nano-wire described above, from welding method, specifically includes following steps：
(1) use raw material copper chloride, glucose and surfactant octadecylamine, coated by hydro-thermal method synthetic surface
There is the copper nano-wire of carbon shell；
(2) in order to prevent copper nano-wire from aoxidizing, by copper nano-wire distributed and saved in organic solvent, drop on warm table,
After organic solvent volatilizees completely, under the conditions of coarse vacuum, copper nano-wire is heated, heating-up temperature is 300 DEG C～725 DEG C,
Control heat time heating time in a few minutes to dozens of minutes, copper atom realizes mass transport by diffusion, contacts with each other in copper nano-wire
Place accumulate, realize being connected with each other of copper nano-wire；By controlling heating-up temperature and controlling solder joint heat time heating time
Size.
The copper nano-wire of what step (1) synthesized be coated with carbon shell has quintic system structure copper nano-wire for carbon coating, its
Specifically building-up process is：Copper chloride, glucose and surfactant octadecylamine are sequentially added in deionized water, and three
Person's molar concentration is respectively：Copper chloride be 0.0078～0.0234mol/L, glucose be 0.0136～0.0408mol/L, 18
Alkylamine is 0.0334～0.1002mol/L, is sufficiently mixed 5h～12h to uniform using magnetic agitation；Transfer the solution into again
In autoclave, make solution account for the 40～60% of reactor volume, heat 2～8h at 120 DEG C；Treat the laggard of solution cooling
Row centrifugation, by precipitate respectively using deionized water, after ethanol and normal hexane flushing, reuses filtration membrane and sample is entered
Row is filtered to remove the copper nano particles produce in synthesis.
The copper nano-wire diameter that step (1) synthesizes is mainly distributed between 20～70nm, and length, in hundreds of micron, is received
Rice noodle outer wrapping a layer thickness 1nm～10nm amorphous carbon shell.
Described coarse vacuum condition refers to that the vacuum order of magnitude is 1～10Pa.
In order to ensure the dependable with function of the present invention, electricity is carried out respectively to the solder joint being obtained by this solder technology
Sign with mechanical property.Characterized using the electric conductivity of two-point method butt welding point first in scanning electron microscope.Tool
Body method is：Two copper nano-wires using two nano-machine handss and solder joint two ends form good electrical contact, and with
Keithley source table forms closed-loop path, more simultaneously monitoring circuit electric current enters by Keithley table butt welding point region applied voltage
And calculating the resistance obtaining solder joint, the resistance of single solder joint is less than 30 Ω.Test result indicate that should be obtained by this welding method
Solder joint there is good electric conductivity.Secondly, it has been also carried out characterizing by the mechanical property of nano-machine handss butt welding point.Using electricity
The copper nano-wire at solder joint two ends is fixed by beamlet assistant depositing metal platinum respectively with two nano-machine handss, then lentamente
The copper nano-wire at mobile manipulator butt welding point and two ends is stretched, and experiment finds to rupture until copper nano-wire, solder joint according to
So intact.Test result indicate that solder joint has excellent mechanical firmness.
Compared to the prior art relatively, it is an advantage of the current invention that：Whole welding process need not add other solders, using copper
The diffusion of atom itself can complete, therefore pollution-free, and operating temperature is low, flow rate regulation scope is big, copper atom utilization rate is high,
The mechanics of solder joint and electric conductivity are outstanding, are capable of multiple spot on a large scale and weld simultaneously, are expected in flexible electronics system, quasiconductor
The fields such as integrated circuit, micro-nano electron device package, transparency electrode are extensively applied.
Brief description
Fig. 1 is hydrothermal synthesis of carbon cladding phenogram under transmission electron microscope for the copper nano-wire used in the present invention
Piece, wherein：Fig. 1 (a) is photo under relatively low multiple for the copper nano-wire, and Fig. 1 (b) is the micro- photograph of high-resolution electronic of copper nano-wire
Piece.
Fig. 2 is the schematic diagram and pictorial diagram pattern before and after the copper nano-wire welding of the present invention, wherein：Fig. 2 (a) is copper nanometer
Line heat under vacuum conditions before schematic diagram and pictorial diagram；Fig. 2 (b) heat under vacuum conditions for copper nano-wire after signal
Figure and pictorial diagram, wherein Fig. 2 (b) is that temperature is increased to 400 DEG C, control heat time heating time in 5min about solder joint scanning electron microscope
Photo.
Specific embodiment
Below in conjunction with specification drawings and specific embodiments, the present invention is described further.
Accompanying drawing 1 is the saturating of the copper nano-wire by there being amorphous carbon shell in the present invention by the Surface coating that hydro-thermal method synthesizes
Penetrate electron micrograph：Fig. 1 (a) is photo under relatively low multiple for the nano wire, and diffraction spot demonstrates what copper nano-wire possessed
Quintic system structure, Fig. 1 (b) is the high-resolution electronic microphotograph of nano wire it can be seen that the surface of copper nano-wire is by one layer
Amorphous shell coats.The building-up process details of whole copper nano-wire are as follows：
Copper chloride 21mg and glucose 49mg is added sequentially in 10mL deionized water, adds surfactant ten afterwards
Eight alkylamine 180mg, are sufficiently mixed 5h using magnetic agitation；Transfer the solution in 25mL autoclave again, at 120 DEG C
Heating 2h；It is centrifuged after treating solution cooling, by precipitate respectively using deionized water, ethanol and normal hexane rinse
Afterwards, reuse filtration membrane sample to be carried out be filtered to remove the copper nano particles produce in synthesis.In order to prevent copper nano-wire oxygen
Change, final product will be obtained and be saved in normal hexane.The copper nano-wire of synthesis under this experiment condition, diameter is mainly distributed on 20～
Between 70nm, length is in hundreds of micron.In nanowire surface because glucose occurs polycondensation reaction, produce amorphous carbon shell,
Thickness is about between 1～10nm.Nanowire diameter, length etc. can be by changing response time, reactant concentration, surface activity
Agent etc. is regulated and controled.
The copper nano-wire of the amorphous carbon shell being saved in normal hexane cladding is dropped on warm table, treats that organic solvent is evaporated completely
Quan Hou, the warm table with copper nano-wire is heated in vacuum environment.
Accompanying drawing 2 is the schematic diagram and pictorial diagram pattern before and after the copper nano-wire welding of the present invention：
Fig. 2 (a) and upper right corner illustration are respectively the schematic diagram before copper nano-wire heats under vacuum conditions and pictorial diagram；Figure
2 (b) and upper right corner illustration are respectively the schematic diagram after copper nano-wire heats under vacuum conditions and pictorial diagram, and wherein Fig. 2 (b) is right
Upper angle illustration is is that temperature is increased to 400 DEG C, control heat time heating time in 5min about solder joint stereoscan photograph.
Claims (4)
1. a kind of low temperature of carbon coating copper nano-wire from welding method, receive by the copper that synthesizing Surface coating using hydro-thermal method has carbon shell
Rice noodle, is mutually lapped formation point contact between nano wire, is heated to the 40%-70% of block copper fusing point under vacuum
When, copper nano-wire will not melt, but copper atom can realize mass transport by diffusion, the ground contacting with each other in copper nano-wire
Fang Fasheng accumulates, thus under conditions of no additional solder, realizing being connected with each other of copper nano-wire；It is characterized in that：Concrete bag
Include following steps：
(1) use raw material copper chloride, glucose and surfactant octadecylamine, carbon is coated with by hydro-thermal method synthetic surface
The copper nano-wire of shell；
(2) in order to prevent copper nano-wire from aoxidizing, by copper nano-wire distributed and saved in organic solvent, drop on warm table, treated
After machine solvent volatilizees completely, under vacuum copper nano-wire is heated, heating-up temperature is 300 DEG C～725 DEG C, during heating
Between control in a few minutes to dozens of minutes, copper atom realizes mass transport by diffusion, the place contacting with each other in copper nano-wire
Accumulate, realize being connected with each other of copper nano-wire；By controlling heating-up temperature and the size controlling solder joint heat time heating time.
2. a kind of low temperature of carbon coating copper nano-wire according to claim 1 from welding method it is characterised in that：Step
(1) copper nano-wire being coated with carbon shell synthesizing has quintic system structure copper nano-wire for carbon coating, and it specifically synthesized
Cheng Wei：Copper chloride, glucose and surfactant octadecylamine are sequentially added in deionized water, and three's molar concentration is divided
It is not：Copper chloride is 0.0078～0.0234mol/L, glucose is 0.0136～0.0408mol/L, octadecylamine is
0.0334～0.1002mol/L, is sufficiently mixed 5h～10h using magnetic agitation；Transfer the solution into again in autoclave, make
Solution accounts for the 40～60% of reactor volume, heats 2～8h at 120 DEG C；It is centrifuged after treating solution cooling, will sink
Starch, respectively using deionized water, after ethanol and normal hexane flushing, reuses filtration membrane and sample is carried out being filtered to remove synthesis
The copper nano particles of middle generation.
3. a kind of low temperature of carbon coating copper nano-wire according to claim 1 from welding method it is characterised in that：Step
(1) the copper nano-wire diameter synthesizing is mainly distributed between 20～70nm, and length in hundreds of micron, nano wire outer wrapping
A layer thickness 1nm～10nm amorphous carbon shell.
4. a kind of low temperature of carbon coating copper nano-wire according to claim 1 from welding method it is characterised in that：Described true
Empty condition refers to that the vacuum order of magnitude is 1～10Pa.
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| CN105772938A (en) * | 2016-03-18 | 2016-07-20 | 浙江大学 | Nano-welding method adopting welding fluxes on basis of photothermal effect |
| CN106098401B (en) * | 2016-07-08 | 2018-06-08 | 武汉工程大学 | A kind of preparation method of carbon copper-clad combination electrode material |
| CN106971771A (en) * | 2017-05-10 | 2017-07-21 | 江汉大学 | A kind of preparation method of carbon-clad metal nano wire conductive film |
| CN109909493A (en) * | 2019-02-25 | 2019-06-21 | 华中科技大学 | A kind of method that electron beam irradiation improves metal material stability |
| CN111540535A (en) * | 2020-03-10 | 2020-08-14 | 河南大学 | Preparation method of carbon-coated copper nanowire |
| CN113634743B (en) * | 2021-08-04 | 2022-08-26 | 湖南大学 | Ostwald nano welding method |
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| CN103215575A (en) * | 2013-04-26 | 2013-07-24 | 中国矿业大学(北京) | Novel welding method for metal nanowire |
| CN103449359A (en) * | 2013-08-16 | 2013-12-18 | 西安交通大学 | Welding method for micron/nano scale conducting materials |
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| CN104078164A (en) * | 2014-07-10 | 2014-10-01 | 厦门大学 | Manufacturing method of copper nano wire network wrapped by graphene carbon film |
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| CN103215575A (en) * | 2013-04-26 | 2013-07-24 | 中国矿业大学(北京) | Novel welding method for metal nanowire |
| CN103449359A (en) * | 2013-08-16 | 2013-12-18 | 西安交通大学 | Welding method for micron/nano scale conducting materials |
| CN103586590A (en) * | 2013-11-12 | 2014-02-19 | 温州大学 | Nanometer welding method based on joule heat |
| CN104078164A (en) * | 2014-07-10 | 2014-10-01 | 厦门大学 | Manufacturing method of copper nano wire network wrapped by graphene carbon film |
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