CN104942455A - 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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- CN104942455A CN104942455A CN201510246707.5A CN201510246707A CN104942455A CN 104942455 A CN104942455 A CN 104942455A CN 201510246707 A CN201510246707 A CN 201510246707A CN 104942455 A CN104942455 A CN 104942455A
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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, be specifically related to a kind of low temperature of carbon coated copper nano wire from welding method.
Background technology
Nano material due to the physical property such as optics, electricity, magnetics of its uniqueness by extensive concern, scientists and engineers have gone out multiple nano material by various synthetic method controlled synthesis, if but these nano materials will form the device with certain 26S Proteasome Structure and Function, certain solder technology just must be utilized to be assembled by these materials.But cannot operate the material of nanoscale due to traditional macro welding method, therefore nano-weld technology becomes a focus and the difficulties in research in nanotechnology field at present.
Three classes are mainly contained at present, i.e. electron beam/ion beam assisted depositing (Electron/Ion Beam Induced Deposition, EBID/IBID), nanometer melting and cold welding in the interconnection technique of nanoscale.The principle of electron beam/ion beam assisted depositing is similar to chemical vapour deposition (CVD) and prepares 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 by containing being deposited the presoma of material (normally containing the metallo-organic compound gas being deposited element, as W (CO)
6, PtC
7h
17, Al (CH
3)
3deng), spray from the nozzle needle in working chamber and carry out induction irradiation with electronics or ion beam while deposition substrate surface, these metallo-organic compound precursors decompose after the bombardment being subject to electron beam or ion beam, metallic element is enriched in substrate in a large number, and volatile element (as oxygen and hydrogen) is taken away by vavuum pump, the metallic element of these enrichments regroups under the effect of ion beam, forms sedimentary deposit.The advantage of this method to carry out high-precision fixed spot deposition, but efficiency is lower, expensive, can produce amorphous carbon and diffusion into the surface, and ion is also easily injected in sample, pollutes sample with deposition process.
Nanometer melting produces Joule heat by electric current, by solder fusing, thus connects welding object.A typical case is the copper nano-wire two ends energising be wrapped in carbon shell, when voltage acquires a certain degree, copper nano-wire melts under the effect of Joule heat, further increase voltage, directional transmissions is there is and realizes nano-weld (Dong L in the copper atom of fusing under electromigratory effect, 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, minimum mass flow rate is only 120ag/s, when adding larger voltage, 500ag/s can be reached the soonest, flow velocity changes obviously (Golberg D, Costa PMFJ, Mitome M in time, 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: China, CN103406685A, 2013.11.27).Another typical case is placed on material to be welded by a root bead material nano wire, by being energized to solder nano wire two ends, more Joule heat will be produced in the place (i.e. solder and Nanowire contacts place to be welded) that resistance is large, from but solder local melting.Profit can be welded and fixed (Peng Y in this way to nano wire, 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 of nanometer melting technology is that cost is low, it is little to pollute, precision is high.But because this kind of welding method is all being carried out far above on metal material fusing point, therefore easily treat welding material and cause certain damage; And be difficult to the flow rate controlling solder, so this technology still also exists some problems.
Cold welding is by by two nanometer rods/linear contact lay together, without the need to heating or applying higher stress, just at normal temperatures two nanometer rods/lines can be linked together within the short time, the simultaneously mechanics of nanometer rods/line and unaffected (the Lu Y of electric property, 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, do not need that heating, speed are fast, mechanics electric property does not affect by welding.But the shortcoming of cold welding is, this welding manner requires high for the clean-up performance of sample; Sample size requires high, and the diameter of nanometer rods/line needs at below 10nm; Can not many weld together, be difficult to scale application.
In addition, the common ground of above-mentioned micro/nano-scale solder technology to weld limited tie point at one time, be not suitable for and carry out high flux welding to large area solder joint simultaneously, and the industrial applications of the latter to micro-nano electron trade is necessary.This patent is intended to a kind of solder technology reliably of invention, make nano-weld can far below during material melting point realize on a large scale, multiple spot high flux welds, because solder is from material itself, thus its mass velocity does not change in time and changes, and solder joint has excellent mechanics, electric property.
Summary of the invention
The present invention is mainly for the shortcoming and defect of current nano-weld technical field, based on the diffusion phenomena that copper atom occurs after the heating, a kind of low temperature of carbon coated copper nano wire is proposed from welding method, the method has that operating temperature is low, flow velocity on a large scale adjustable, solder is high and multiple spot such as to weld at the advantage simultaneously on a large scale, be expected at flexible electronics system, the field extensive uses such as semiconductor integrated circuit, micro-nano electron device package, transparency electrode.
In order to achieve the above object, the present invention adopts following technical scheme:
A kind of low temperature of carbon coated copper nano wire is from welding method, utilize water heat transfer to go out copper nano-wire that Surface coating has carbon shell, between nano wire, overlap joint forms point cantact mutually, when being heated to the 40%-70% that is 300 DEG C ~ 725 DEG C of block copper fusing point under vacuum, copper nano-wire can not melt, but copper atom realizes mass transport by diffusion, and the place contacted with each other at copper nano-wire is accumulated, thus under the condition without additional solder, realize being interconnected of copper nano-wire.
The low temperature of a kind of carbon coated copper nano wire described above, from welding method, specifically comprises the steps:
(1) use raw material copper chloride, glucose and surfactant octadecylamine, had the copper nano-wire of carbon shell by water heat transfer Surface coating;
(2) in order to prevent copper nano-wire to be oxidized, by copper nano-wire distributed and saved in organic solvent, drop on warm table, after organic solvent volatilizees completely, heat under low vacuum condition to copper nano-wire, heating-up temperature is 300 DEG C ~ 725 DEG C, heat time controls in a few minutes to dozens of minutes, copper atom realizes mass transport by diffusion, and the place contacted with each other at copper nano-wire is accumulated, and realizes being interconnected of copper nano-wire; The size of solder joint is controlled by control heating-up temperature and heat time.
To be that carbon is coated have quintic system structure copper nano-wire to the copper nano-wire being coated with carbon shell that step (1) is synthesized, its concrete building-up process is: copper chloride, glucose and surfactant octadecylamine are added successively in deionized water, and three's molar concentration is respectively: copper chloride is 0.0078 ~ 0.0234mol/L, glucose is 0.0136 ~ 0.0408mol/L, octadecylamine is 0.0334 ~ 0.1002mol/L, magnetic agitation is used fully to mix 5h ~ 12h to even; Again solution is transferred in autoclave, make solution account for 40 ~ 60% of reactor volume, at 120 DEG C, heat 2 ~ 8h; Carry out centrifugation after treating solution cooling, sediment is used deionized water respectively, after alcohol and n-hexane rinse, re-use filtration membrane and carried out sample filtering the copper nano particles produced in synthesis.
The copper nano-wire diameter that step (1) is synthesized mainly is distributed between 20 ~ 70nm, and at hundreds of micron not etc., nano wire outer wrapping a layer thickness 1nm ~ 10nm amorphous carbon shell to length.
Described low vacuum condition refers to that the vacuum order of magnitude is 1 ~ 10Pa.
In order to ensure dependable with function of the present invention, the sign of electricity and mechanical property is carried out respectively to the solder joint obtained by this solder technology.First in SEM, utilize the electric conductivity of two-point method butt welding point to characterize.Concrete grammar is: utilize two copper nano-wires at two nano-machine hands and solder joint two ends to form good electrical contact, and show to form closed-loop path with Keithley source, by Keithley table butt welding point region applying voltage, also monitoring circuit electric current and then calculating obtain the resistance of solder joint again, and the resistance of single solder joint is no more than 30 Ω.Experimental result shows that the solder joint that this is obtained by this welding method has good electric conductivity.Secondly, also characterized by the mechanical property of nano-machine hand butt welding point.Electron beam-induced deposition metal platinum is utilized to be fixed with two nano-machine hands respectively by the copper nano-wire at solder joint two ends, then the copper nano-wire at mobile manipulator butt welding point and two ends stretches lentamente, experiment finds until copper nano-wire ruptures, and solder joint is still intact.Experimental result shows that solder joint has excellent mechanical firmness.
Compared to the prior art comparatively, the invention has the advantages that: whole welding process is without the need to adding other solders, the diffusion of copper atom self is utilized to complete, therefore pollution-free, and operating temperature is low, velocity of flow adjust scope large, copper atom utilization rate is high, mechanics and the electric conductivity of solder joint are outstanding, can realize multiple spot on a large scale and weld simultaneously, be expected at flexible electronics system, the field extensive uses such as semiconductor integrated circuit, micro-nano electron device package, transparency electrode.
Accompanying drawing explanation
Fig. 1 is the sign picture of hydrothermal synthesis of carbon coated copper nano wire under transmission electron microscope used in the present invention, wherein: Fig. 1 (a) is the photo of copper nano-wire under lower multiple, the high-resolution electronic microphoto that Fig. 1 (b) is copper nano-wire.
Fig. 2 be copper nano-wire of the present invention welding before and after schematic diagram and pictorial diagram pattern, wherein: Fig. 2 (a) for copper nano-wire heat under vacuum conditions before schematic diagram and pictorial diagram; Fig. 2 (b) for copper nano-wire heat under vacuum conditions after schematic diagram and pictorial diagram, wherein temperature is increased to 400 DEG C by Fig. 2 (b), and the heat time controls the solder joint stereoscan photograph at about 5min.
Detailed description of the invention
Below in conjunction with specification drawings and specific embodiments, the present invention is described further.
Accompanying drawing 1 is that the Surface coating by being gone out by water heat transfer in the present invention has the transmission electron microscope photo of the copper nano-wire of amorphous carbon shell: Fig. 1 (a) is the photo of nano wire under lower multiple, diffraction spot demonstrates the quintic system structure that copper nano-wire possesses, the high-resolution electronic microphoto that Fig. 1 (b) is nano wire, can see that the surface of copper nano-wire is coated by one deck amorphous shell.The building-up process details of whole copper nano-wire are as follows:
Copper chloride 21mg and glucose 49mg is joined in 10mL deionized water successively, adds surfactant octadecylamine 180mg afterwards, use magnetic agitation fully to mix 5h; Solution is transferred in 25mL autoclave again, at 120 DEG C, heat 2h; Carry out centrifugation after treating solution cooling, sediment is used deionized water respectively, after alcohol and n-hexane rinse, re-use filtration membrane and carried out sample filtering the copper nano particles produced in synthesis.In order to prevent copper nano-wire to be oxidized, end product will be obtained and be kept in n-hexane.The copper nano-wire synthesized under this experiment condition, diameter is mainly distributed between 20 ~ 70nm, and length is not at hundreds of micron etc.In nanowire surface due to glucose generation polycondensation reaction, produce amorphous carbon shell, thickness is between 1 ~ 10nm.Nanowire diameter, length etc. can regulate and control by changing reaction time, reactant concentration, surfactant etc.
Copper nano-wire coated for the amorphous carbon shell be kept in n-hexane is dropped on warm table, after organic solvent volatilization completely, the warm table with copper nano-wire is heated in vacuum environment.
Accompanying drawing 2 is schematic diagram and the pictorial diagram pattern of copper nano-wire of the present invention welding front and back:
Fig. 2 (a) and upper right corner illustration be respectively copper nano-wire heat under vacuum conditions before schematic diagram and pictorial diagram; Fig. 2 (b) and upper right corner illustration be respectively copper nano-wire heat under vacuum conditions after schematic diagram and pictorial diagram, wherein Fig. 2 (b) upper right corner illustration is for being that temperature is increased to 400 DEG C, and the heat time controls the solder joint stereoscan photograph at about 5min.
Claims (5)
1. the low temperature of a carbon coated copper nano wire is from welding method, it is characterized in that: utilize water heat transfer to go out copper nano-wire that Surface coating has carbon shell, between nano wire, overlap joint forms point cantact mutually, when being heated to the 40%-70% that is 300 DEG C ~ 725 DEG C of block copper fusing point under vacuum, copper nano-wire can not melt, but copper atom realizes mass transport by diffusion, the place contacted with each other at copper nano-wire is accumulated, thus under the condition without additional solder, realize being interconnected of copper nano-wire.
2. the low temperature of a kind of carbon coated copper nano wire according to claim 1 is from welding method, it is characterized in that: specifically comprise the steps:
(1) use raw material copper chloride, glucose and surfactant octadecylamine, had the copper nano-wire of carbon shell by water heat transfer Surface coating;
(2) in order to prevent copper nano-wire to be oxidized, by copper nano-wire distributed and saved in organic solvent, drop on warm table, after organic solvent volatilizees completely, heat under vacuum to copper nano-wire, heating-up temperature is 300 DEG C ~ 725 DEG C, heat time controls in a few minutes to dozens of minutes, copper atom realizes mass transport by diffusion, and the place contacted with each other at copper nano-wire is accumulated, and realizes being interconnected of copper nano-wire; The size of solder joint is controlled by control heating-up temperature and heat time.
3. the low temperature welding method of a kind of carbon coated copper nano wire according to claim 2, it is characterized in that: to be that carbon is coated have quintic system structure copper nano-wire to the copper nano-wire being coated with carbon shell that step (1) is synthesized, its concrete building-up process is: by copper chloride, glucose and surfactant octadecylamine add in deionized water successively, and three's molar concentration is respectively: copper chloride is 0.0078 ~ 0.0234mol/L, glucose is 0.0136 ~ 0.0408mol/L, octadecylamine is 0.0334 ~ 0.1002mol/L, magnetic agitation is used fully to mix 5h ~ 10h, again solution is transferred in autoclave, make solution account for 40 ~ 60% of reactor volume, at 120 DEG C, heat 2 ~ 8h, carry out centrifugation after treating solution cooling, sediment is used deionized water respectively, after alcohol and n-hexane rinse, re-use filtration membrane and carried out sample filtering the copper nano particles produced in synthesis.
4. the low temperature of a kind of carbon coated copper nano wire according to claim 2 is from welding method, it is characterized in that: the copper nano-wire diameter that step (1) is synthesized mainly is distributed between 20 ~ 70nm, at hundreds of micron not etc., nano wire outer wrapping a layer thickness 1nm ~ 10nm amorphous carbon shell to length.
5. the low temperature of a kind of carbon coated copper nano wire according to claim 2 is from welding method, it is characterized in that: described vacuum condition refers to that the vacuum order of magnitude is 1 ~ 10Pa.
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| CN106098401A (en) * | 2016-07-08 | 2016-11-09 | 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 |
| CN113634743A (en) * | 2021-08-04 | 2021-11-12 | 湖南大学 | Ostwald nano welding method |
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Cited By (7)
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| CN113634743A (en) * | 2021-08-04 | 2021-11-12 | 湖南大学 | Ostwald nano welding method |
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