CN101976594A - Composite conductor application of carbon nano tube fiber and preparation method thereof - Google Patents
Composite conductor application of carbon nano tube fiber and preparation method thereof Download PDFInfo
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Abstract
The invention discloses composite conductor application of carbon nano tube fiber and a preparation method thereof. The invention is characterized in that a high strength carbon nano tube fiber material is combined with electroplating or chemical plating surface treatment process, and conductive metal coating is compounded on the carbon nano tube fiber, thus obtaining a carbon nano tube composite conductor with light weight, high strength and high electric conduction. The preparation method includes the following steps: firstly high strength carbon nano tube fiber material is prepared, and then chemical plating or electroplating is adopted to prepare uniform metal coating on the surface of fiber, thus obtaining the carbon nano tube composite conductor. The type of metal coating and the thickness of metal coating are controlled, so that the conductivity of carbon nano tube conductor can be consistent with the conductivity of metal body. The application and preparation method of the invention are simple and feasible, step is simple, and repeatability is good, thus being applicable to mass production, thereby having significance in development of novel superfine conductor with light weight, high tenacity and high strength and in showing potential application value thereof in electronic industry.
Description
Technical field
The present invention relates to the application preparation field of nano material, be specifically related to a kind of lightweight, high strength carbon nano-tube fibre in application of compound wire and preparation method thereof.
Background technology
Carbon nano-tube from Ijima in 1991 since observing under the Electronic Speculum
[1], just enjoy the concern of scientists.Studies show that further carbon nano-tube is because its special graphite laminate structure, thereby have excellent mechanical property, and excellent conducting performance.Result of study shows that the hot strength of carbon nano-tube is 150Gpa at present
[2], Young's modulus is 1Tpa
[3]In recent years, people are by spining technology, with the carbon nano-tube aerosol
[4]But, the spinning carbon nano pipe array
[5]And cotton shape carbon nano-tube raw material
[6]In processing obtained the carbon nano-tube fibre material formed by pure nano-carbon tube.At present, but classify the carbon nano-tube fibre hot strength best result that raw material obtain as with carbon nano-tube aerosol and spinning carbon nano-pipe array and can not reach 8.8Gpa and 3.3Gpa
[7,8]
Because carbon nano-tube fibre has so high hot strength and extraordinary chemical stability, makes it have very remarkable advantages aspect Composite Preparation, thereby play a significant role aspect preparing at high performance material.Adopt the metal material of good conductivity to be prepared from mostly as in the market ultrafine wire, but exist complex manufacturing technology, strength and toughness is relatively poor, lead is easy to the weakness of fracture failure.Carbon nano-tube fibre is a kind of novel high-performance carbon back fiber material, it is except having as chemical stability height, the carbon fiber intrinsic property such as corrosion resistance is strong and temperature coefficient is low, also has, intensity lower than carbon fiber density and toughness is higher, electric property is easy to improve advantage.
[list of references]
[1]S.Iijima，Nature，1991，354，56-.
[2]B.G.Demczyk，Y.M.Wang?et?al.，Mater.Sci.Eng.A?2002，334，173.
[3]M.F.Yu，B.S.Files?et?al.，Phys.Rev.Lett.2000，84，5552.
[4]Y.L.Li，A.Kinloch?et?al.，Science，2004，304，276.
[5]K.L.Jiang，Q.Q.Li，et?al.，Nature，2002，419，801.
[6]L.X.Zheng，X.F.Zhang?et?al.，Adv.Mater.2007，19，2567.
[7]K.Koziol，J.Vilatela?et?al.，Science，2007，318，1892.
[8]X.F.Zhang，Q.W.Li?et?al.，Adv.Mater.2007，19，4198.
Summary of the invention
Defective in view of above-mentioned existing ultrafine wire technology of preparing, purpose of the present invention is intended to propose the application of a kind of existing carbon nano-tube fibre in the compound wire preparation, to obtain a kind of carbon nano-tube fibre compound wire that had not only had the metal high conductivity but also had the carbon nano-tube fibre high structural strength.
Its technical solution is: carbon nano-tube fibre is used as the trunk core of compound wire, and its diameter range of choice is between 1 μ m～100 μ m; And described carbon nano-tube fibre surface is coated with the metal conducting layer of kind and controllable thickness.
Another object of the present invention is intended to propose simultaneously the above-mentioned application of a kind of realization, the preparation method of preparation compound wire.Its technical solution is: metal conducting layer is plating to the carbon nano-tube fibre surface equably, makes described compound wire, it comprises step:
But I, prefabricated carbon nano-tube aerosol or spinning carbon nano pipe array, or directly buy the cotton shape carbon nano-tube, and adopt spining technology therefrom to process to obtain the carbon nano-tube fibre material of forming by pure nano-carbon tube;
The method of one of II, employing plating and chemical plating needs the metal lining conductive layer on the carbon nano-tube fibre surface by length and thickness, makes the compound wire of sign an undertaking structure intensity and toughness.
Further, the compound wire preparation method of aforesaid a kind of carbon nano-tube fibre, the prefabricated carbon nano-tube aerosol of method of employing floating catalytic chemical vapour deposition (CVD) in the step I; But or chemical vapour deposition (CVD), the vertical-growth method prefabricated spinning carbon nano pipe array of employing on a smooth substrate.
Further, the compound wire preparation method of aforesaid a kind of carbon nano-tube fibre, metal conducting layer described in the step II is for adopting the electro-plating method plating in the single coat of metal on carbon nano-tube fibre surface or the composite deposite of two or more metallic elements, and wherein said two or more metallic elements are the while composite plating or divide composite plating successively.
Further, the composite deposite of described two or more metallic elements has a kind of as among major metal Cu, Ni, Au, Ag, Sn, Fe or the Zn of coating main body composition, and other minor metal Co or the nonmetal P that are used to regulate coating outward appearance, compactness and structure, described composite deposite is at least Au-Co alloy or Ni-P alloy.
Further, the compound wire preparation method of aforesaid a kind of carbon nano-tube fibre, metal conducting layer described in the step II for adopt chemical plating method with the metal plating liquid plating in the single coat of metal on carbon nano-tube fibre surface or two-layer more than composition metal coating, has the interface of distinguishing coating between the wherein said two-layer above composition metal coating, and each coating metal plating liquid plating not of the same race of serving as reasons makes, or by making with a kind of metal plating liquid branch precedence plating.
Further, described metal plating liquid is for only having the plating bath of single slaine as main salt; Or with special metal salt as main salt, and be mixed with other slaine or the nonmetalloid that is used to regulate coating outward appearance, compactness and structure.
The enforcement of above-mentioned application of the present invention and preparation method thereof, its outstanding beneficial effect is presented as:
This invention combines novel high-strength carbon nano-tube fibre material with plating and chemical plating process, by the variation of carbon nano-tube fibre diameter, coat of metal kind and thickness, be easy to make the compound wire that high-intensity carbon nano-tube fibre is used.This method is simple, step simple, good reproducibility, is suitable for mass production, embodies significant for the development of novel light high tenacity, high strength ultrafine wire and the potential using value in electronics industry thereof.
Description of drawings
Fig. 1 is the compound lead preparation method's of a high strength of the present invention schematic flow sheet;
Fig. 2 is the schematic diagram of carbon nano-tube fibre chemical plating mode among the present invention;
Fig. 3 is the schematic diagram of carbon nano-tube fibre plating mode among the present invention;
Fig. 4 is the ESEM picture of the preceding carbon nano-tube fibre of plating among the present invention;
Fig. 5 is the ESEM picture of carbon nano-tube fibre after the Electroless Cu Plating among the present invention;
Fig. 6 is the ESEM picture of carbon nano-tube fibre fracture place after the Electroless Cu Plating among the present invention;
Fig. 7 is the curve chart that the compound wire conductivity changed with the copper facing time in the carbon nano-tube fibre Electroless Cu Plating process among the present invention.
Embodiment
The present invention is based on the combination of the conduction property of high tensile strength properties of carbon nano-tube fibre and metal excellence, on the basis of fiber production, mode by chemical plating or plating obtains continuous metal coating uniformly on the carbon nano-tube fibre surface, thus preparation high strength carbon nanotube fiber composite lead.As shown in Figure 1, but be raw material, add to twist by spinning equipment and make the carbon nano-tube fibre material with carbon nano-tube material with spinnability.Can be with the in a fixed manner or continuous mode of preparation of fiber, immerse in chemical plating fluid or the electroplate liquid, the former metal ion generation autoreduction is reflected at fiber surface and obtains coating, the latter then need be with similar metal electrode as anode (except that Au), and carbon nano-tube fibre carries out negative electrode as negative electrode and electroplates the continuous coating of acquisition.On the basis that obtains single coating, can also obtain composite deposite by continuing chemical plating or plating mode.Thereby obtain the carbon nano-tube fibre compound wire of different structure.
Embodiment 1
As shown in Figure 2, carbon nano-tube fibre compound wire of the present invention is body with the carbon nano-tube fibre, obtains even metal coating through chemical plating process on the carbon nano-tube fibre surface.Concrete steps comprise that carbon nano-tube fibre preparation and fiber carry out two parts of chemical plating.
At first adopt the mode of electron beam evaporation, have thermal oxidation SiO at 2 inches
2The Si sheet on the uniform Fe film of deposition as the catalyst of carbon nano pipe array growth.Being placed on diameter then is in 3 inches quartz tube furnaces, but utilizes the thermal chemical vapor deposition technology to adopt acetylene gas to prepare the spinning carbon nano pipe array as carbon-source gas under 700 ℃ growth conditions, and the array height is 400 μ m.In spinning equipment pass through the direct fabrics technology, but from this spinning array, evenly pull out the carbon nano-tube film that fixed width is 3mm thereafter.The method that adopts twisting and shrink in conjunction with ethanolic solution, having prepared diameter is 12 μ m, length is the even carbon nano-tube fibre material (as shown in Figure 4) of 1m.Further Mechanical test results shows, the mechanics hot strength of this carbon nano-tube fibre is 800MPa.
The carbon nano-tube fibre for preparing is fixed on (as shown in Figure 2) on the PVC flat board, adopts CuCl
2Electroless Cu Plating technology as main salt.The plating bath that configures as in the bath trough, and is heated plating bath on the magnetic force heating station and stirs by magnet rotor.After treating that bath temperature reaches working temperature 25-35 ℃, carbon nano-tube fibre is together immersed in the plating bath together with the fixing PVC flat board of usefulness, and do bubbling by air pump bubbling air in plating bath simultaneously and handle.Cu
2+Can form Cu and be deposited on the carbon nano-tube fibre surface by the autoreduction mode, obtain uniform copper coating.Fig. 5 is the ESEM picture after the carbon nano-tube fibre Electroless Cu Plating, compares with Fig. 4, can find that there is tangible coating on the carbon nano-tube fibre surface, and diameter has increased 1-2um.Further composition characterizes and the analysis showed that this coating is metallic copper.The stereoscan photograph of carbon nano-tube fibre strip off can see that the Cu coat of metal and carbon nano-tube fibre surface have extraordinary associativity as shown in Figure 6.This compound wire is carried out the conductivity test analysis, and experimental result shows that the conductivity of the fiber of original not process Electroless Cu Plating is 6.45 * 10
4S/m, through the copper facing of 10min time, the conductivity of carbon nano-tube fibre compound wire can reach 8.65 * 10
6S/m.Further carbon nano-tube fibre compound wire conductivity has been carried out detailed measurement with the copper facing time relation, experimental result shows the increase along with surface metal copper amount as shown in Figure 7, and the conductivity of this compound wire obviously improves.The result shows and can modulate the conductivity of carbon nano-tube fibre compound wire by the control copper facing time.
As shown in Figure 3, carbon nano-tube compound wire of the present invention is body with the carbon nano-tube fibre, obtains the coat of metal equably through electroplating technology on the carbon nano-tube fibre surface.Concrete steps comprise that carbon nano-tube fibre preparation and fiber carry out two parts of electroplating.
The carbon nano-tube fibre preparation methods is with reference to specific embodiment 1.With the diameter for preparing is that the carbon nano-tube fibre of 12 μ m is fixed on the PVC flat board, is connected on the electrode with conductive silver glue at an end of carbon nano-tube fibre.Adopt CuSO
4Solution is electroplate liquid.As on the magnetic force heating stirrer, adopt the mode of agitating heating to make the temperature of electroplate liquid remain on 40-45 ℃ the electroplate liquid that configures.The carbon nano-tube fibre of predetermined fixed on the PVC flat board placed plating bath, and connection electrode one end as electroplating cathode, is connected in the negative pole of power supply as for more than the liquid level.Adopt 99.9999% copper coin as anode simultaneously, be connected in power anode one end.Distance between anode and the negative electrode is 10cm, adopts the constant voltage mode to carry out negative electrode and electroplates, and electroplating voltage is 5V, and electric current is 0.01A.Through after the plating of 10min, the conductivity of carbon nano-tube fibre compound wire to be measured, its size is 1.2 * 10
7S/m.
Except that above-mentioned two embodiment, the enforcement of the present invention's application and preparation method thereof has very wide range of choice.On using, according to the demand difference of compound wire, wherein the diameter of carbon nano-tube fibre can be chosen wantonly in scope 1 μ m～100 μ m, to satisfy the especially preparation requirement of ultrafine wire of various thickness leads;
Preparation method from carbon nano-tube fibre: but adopt the prefabricated spinning carbon nano pipe array of chemical vapour deposition (CVD), vertical-growth method on a smooth substrate and carry out the method for making of follow-up spinning except embodiment one, the present invention also can adopt the prefabricated carbon nano-tube aerosol of the method for floating catalytic chemical vapour deposition (CVD), or the method for making of carrying out follow-up spinning again after directly buying the cotton shape carbon nano-tube from market;
From the metal conducting layer plating technic: remove embodiment one, two adopt Cu as outside the main metal conducting layer, plating of the present invention can be the coat of metal of all kinds and component according to different plating processing modes in the electric conducting material on carbon nano-tube fibre surface, for electroplating technology, metal conducting layer can be the single coat of metal or the composite deposite of two or more metallic elements, and wherein two or more metallic elements are composite plating simultaneously both, can divide composite plating successively again, the material that is used to electroplate comprises the major metal Cu as coating main body composition, Ni, Au, Ag, Sn, a kind of among Fe or the Zn, and be used to regulate the coating outward appearance, other minor metal of compactness and structure or nonmetal P.For example: composite deposite can be Au-Co alloy or Ni-P alloy;
For chemical plating process, metal conducting layer for adopt chemical plating method with the metal plating liquid plating in the single coat of metal on carbon nano-tube fibre surface or two-layer more than composition metal coating, has the interface of distinguishing coating between the wherein two-layer above composition metal coating, and each coating metal plating liquid plating not of the same race of serving as reasons makes, or by making with a kind of metal plating liquid branch precedence plating, wherein metal plating liquid can be only to have the plating bath of single slaine as main salt, also can be as main salt (Cu for example with special metal salt, Ni, Au, Ag, Sn, and be mixed with and be used to regulate the coating outward appearance a kind of salt among Fe or the Zn),, other slaine or the nonmetalloid of compactness and structure.
Below, protection scope of the present invention is not constituted any limitation only in explanation technological means of the present invention.All employing equivalents or equivalence are replaced and the technical scheme of formation, all drop within the rights protection scope of the present invention.
Claims (10)
1. the compound wire of a carbon nano-tube fibre is used, and it is characterized in that: described carbon nano-tube fibre is used as the trunk core of compound wire, and described carbon nano-tube fibre surface is coated with the metal conducting layer of kind and controllable thickness.
2. the compound wire of a kind of carbon nano-tube according to claim 1 is used, and it is characterized in that: the diameter range of choice of described carbon nano-tube fibre is between 1 μ m～100 μ m.
3. the compound wire preparation method of a carbon nano-tube fibre, it is characterized in that: metal conducting layer is plating to the carbon nano-tube fibre surface equably, makes described compound wire, it comprises step:
But I, prefabricated carbon nano-tube aerosol or spinning carbon nano pipe array, or directly buy the cotton shape carbon nano-tube, and adopt spining technology therefrom to process to obtain the carbon nano-tube fibre material of forming by pure nano-carbon tube;
The method of one of II, employing plating and chemical plating needs the metal lining conductive layer on the carbon nano-tube fibre surface by length and thickness, makes the compound wire of sign an undertaking structure intensity and toughness.
4. the compound wire preparation method of a kind of carbon nano-tube fibre according to claim 3 is characterized in that: the prefabricated carbon nano-tube aerosol of method that adopts the floating catalytic chemical vapour deposition (CVD) in the step I.
5. the compound wire preparation method of a kind of carbon nano-tube fibre according to claim 3 is characterized in that: but adopt the prefabricated spinning carbon nano pipe array of chemical vapour deposition (CVD), vertical-growth method on a smooth substrate in the step I.
6. the compound wire preparation method of a kind of carbon nano-tube fibre according to claim 3, it is characterized in that: metal conducting layer described in the step II is for adopting the electro-plating method plating in the single coat of metal on carbon nano-tube fibre surface or the composite deposite of two or more metallic elements, and wherein said two or more metallic elements are the while composite plating or divide composite plating successively.
7. the compound wire preparation method of a kind of carbon nano-tube fibre according to claim 6, it is characterized in that: the composite deposite of described two or more metallic elements has a kind of as among major metal Cu, Ni, Au, Ag, Sn, Fe or the Zn of coating main body composition, and other minor metal Co or the nonmetal P that are used to regulate coating outward appearance, compactness and structure, described composite deposite is at least Au-Co alloy or Ni-P alloy.
8. the compound wire preparation method of a kind of carbon nano-tube fibre according to claim 3, it is characterized in that: metal conducting layer described in the step II for adopt chemical plating method with the metal plating liquid plating in the single coat of metal on carbon nano-tube fibre surface or two-layer more than composition metal coating, has the interface of distinguishing coating between the wherein said two-layer above composition metal coating, and each coating metal plating liquid plating not of the same race of serving as reasons makes, or by making with a kind of metal plating liquid branch precedence plating.
9. the compound wire preparation method of a kind of carbon nano-tube fibre according to claim 8 is characterized in that: described metal plating liquid is for only having the plating bath of single slaine as main salt.
10. the compound wire preparation method of a kind of carbon nano-tube fibre according to claim 8, it is characterized in that: described metal plating liquid as main salt, and is mixed with other slaine or the nonmetalloid that is used to regulate coating outward appearance, compactness and structure with special metal salt.
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