CN103219065A - Carbon nanotube-nanometer copper powder-based environment-friendly conductive paste - Google Patents
Carbon nanotube-nanometer copper powder-based environment-friendly conductive paste Download PDFInfo
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Abstract
The invention discloses a carbon nanotube-nanometer copper powder-based environment-friendly conductive paste, which consists of copper nanoparticles subjected to surface treatment, carbon nanotubes treated by carbon nanotube dispersion liquid, an additive and an organic solvent, wherein the surfaces of the copper nanoparticles subjected to surface treatment have negative charges and the average particle diameter is 50-150 nm; and the conductive paste comprises the components in percentage by mass: 10-20 percent of copper nanoparticles subjected to surface treatment, 1-10 percent of additive, 10-20 percent of organic solvent and the balance of carbon nanotubes treated by carbon nanotube dispersion liquid. The carbon nanotube-nanometer copper powder-based environment-friendly conductive paste has the advantages that the conductive paste has double advantages of the carbon nanotube and a noble metal material, the carbon nanotubes have better dispersion performance in the paste, do not settle and have good paste conductive performance, and all formula components used by the prepared conductive paste are all environment-friendly and pollution-free.
Description
Technical field
The present invention relates to technical field of electronic materials, be specifically related to a kind of environmental-friendly conductive sizing agent based on the carbon nanotube-nano copper powder.
Technical background
Along with electronics and information industry enters stage of high speed development, also allow the electric slurry industry that tremendous development has been arranged.Electric slurry integrates metallurgy, chemical industry, electronic technology, is a kind of electronic functional material with high-tech, therefore, has the status that can not be substituted in electron trade.Silver powder and electric slurry series of products thereof are to be most widely used in the electronics industry simultaneously that consumption also is maximum a kind of noble metal powder, be the basic function material of producing various electronic component products, make integrated circuit, capacitor, MLCC, electrode of solar battery, radio frequency identification label etc. but be mainly used in.Increase along with demand and kind, people for the development of electrocondution slurry also in continuous progress, various new-type electrocondution slurries emerge in an endless stream, wherein popular with copper slurry especially, be because its production cost is lower than the silver slurry, on the other hand on the one hand, though inferior slightly and silver paste aspect conductivity, but people still more are ready to select copper slurry, and therefore, the research that is directed to conductive copper paste in recent years emerges in an endless stream.But these slurry major parts are main conducting function phase with metal mutually all, especially in the majority especially with metal dusts such as silver powder, copper powder, nickel powders.In patent CN101593568, mention and in electrocondution slurry, add carbon nano-tube, and make its part that becomes conductive phase, and for its existence form and how to handle and not mentioned and not environmental protection of slurry.
Summary of the invention
The objective of the invention is at above-mentioned existing problems, a kind of environmental-friendly conductive sizing agent based on the carbon nanotube-nano copper powder is provided, this electrocondution slurry has excellent conducting performance and environmental protection.
Technical scheme of the present invention:
A kind of environmental-friendly conductive sizing agent based on the carbon nanotube-nano copper powder, carbon nano-tube, additive and the organic solvent handled by surface treated nano copper particle, through the carbon nano-tube dispersion liquid are formed, electronegative and the average grain diameter in described surface treated nano copper particle surface is 50-150nm, and the mass percent of each component is: surface treated nano copper particle 10-20wt%, additive 1-10wt%, organic solvent 10-20wt%, the carbon nano-tube of handling through the carbon nano-tube dispersion liquid are surplus.
Described carbon nano-tube is the mixture of one or both arbitrary proportions in Single Walled Carbon Nanotube and the multi-walled carbon nano-tubes.
Described carbon nano-tube dispersion liquid is a surface-active ion liquid, is specially dodecyl-3-methylimidazole bromine (C12mimBr) or myristyl-3-methylimidazole bromine (C14mimBr).
Described additive is binding agent and thickener and levelling agent, wherein binding agent is an epoxy powder coating, thickener and levelling agent are rheology modified thickener of polyurethane or hydrophobically-modified alkali swelling type thickener, and the mass ratio of binding agent and thickener and levelling agent is 1:1.
Described organic solvent is the mixture of one or both arbitrary proportions in ethyleneglycol monophenylether and the ethylene glycol phenyl ether acetate.
A kind of preparation method of described environmental-friendly conductive sizing agent based on the carbon nanotube-nano copper powder, step is as follows:
1) with chemical reduction method mantoquita is reduced, prepare the nano copper particle that particle diameter is 50-150nm, and make the nano copper particle surface of preparation be with negative electrical charge;
2) prepare the carbon nano-tube that the surface has positive charge with surface-active ion liquid, then it is evenly spread in the organic solvent;
3) nano copper particle that will handle and the adding of other additives contain in the organic solvent of carbon nano-tube, and ultrasonic mixing to each component can make electrocondution slurry.
A kind of application of described environmental-friendly conductive sizing agent based on the carbon nanotube-nano copper powder, can be used for electrode of solar battery, chip multilayer ceramic capacitor (MLCC), also can be used for the joining in the type of encapsulation, connection and wiring board of meticulous line pattern and multiple micro element.
Technical Analysis of the present invention:
1) why nano copper particle will be in order to allow copper powder be adsorbed on carbon nano tube surface better, to give full play to the advantage of carbon nano-tube and noble metal combination through negative electrical charge on the surface treatment band.
2) addition of nano copper particle is little, be not with it as main conducting function phase, but in order to auxiliary carbon nano-tube, make carbon nano-tube have metallic character with copper powder, and too much the copper powder of consumption can with treated carbon nano tube surface with positive charge all neutralize, cause the dispersiveness of carbon nano-tube to descend, tangle mutually or sedimentation, thereby make the stability decreases of electrocondution slurry.Therefore, only use copper powder slightly, can play booster action, can guarantee the dispersiveness that carbon nano-tube is good again carbon nano-tube.
3) the epoxy resin of binder powdery paints is in sintering process, just can solidify being no more than under 200 ℃ the temperature, can play equally and add institute's resin in other slurries as effect that binding agent played.
4) the present invention does not adopt traditional process for dispersing for carbon nano-tube, as add macromolecular compound etc. and make carbon nano-tube reach good dispersiveness, and adopt surface-active ion liquid that carbon nano-tube is disperseed, and use it in the electrocondution slurry simultaneously, be a kind of ionic liquid and the combining of electrocondution slurry, and for the also rare report of both being used in combination.
In advantage of the present invention be: the carbon nanotube adsorption in this electrocondution slurry behind a small amount of copper powder, on the basis of having improved electric conductivity, still can be scattered in preferably in the slurry and sedimentation phenomenon not take place.And selected epoxy powder coating binding agent can show good electric property after curing.In the carbon nano tube compound material of this slurry, not only comprise carbon nano-tube and can bring into play separately performance, and overall performance also improves to some extent at interior all material.In sintering process, the copper powder that is adsorbed on carbon nano tube surface can be become sheet by graininess, forms the coating to the carbon nano-tube part, and also can be connected to some extent between sheet and the sheet, more helps the formation of conductive network.All compositions of this electrocondution slurry are ep-type material, help environmental protection.
Embodiment
Embodiment 1-4:
A kind of preparation method of described environmental-friendly conductive sizing agent based on the carbon nanotube-nano copper powder, step is as follows:
1) with chemical reduction method mantoquita is reduced, prepare the nano copper particle that particle diameter is 50-150nm, and make the nano copper particle surface of preparation be with negative electrical charge;
2) prepare the carbon nano-tube that the surface has positive charge with surface-active ion liquid, then it is evenly spread in the organic solvent;
3) nano copper particle that will handle and the adding of other additives contain in the organic solvent of carbon nano-tube, and ultrasonic mixing to each component can make electrocondution slurry.
The electrocondution slurry of embodiment preparation is spin-coating film on equal glass substrate, behind 300 ℃ of following sintering 45min, obtains conductive layer, and its resistivity is measured.Each amounts of components and conducting performance test the results are shown in Table 1 among the embodiment 1-4.
Table 1
Testing result shows: this electrocondution slurry has excellent conducting performance and environmental protection.
The electrocondution slurry of preparation can be used for electrode of solar battery, chip multilayer ceramic capacitor (MLCC), also can be used for the joining in the type of encapsulation, connection and wiring board of meticulous line pattern and multiple micro element.
Claims (5)
1. environmental-friendly conductive sizing agent based on the carbon nanotube-nano copper powder, it is characterized in that: carbon nano-tube, additive and the organic solvent handled by surface treated nano copper particle, through the carbon nano-tube dispersion liquid are formed, electronegative and the average grain diameter in described surface treated nano copper particle surface is 50-150nm, and the mass percent of each component is: surface treated nano copper particle 10-20wt%, additive 1-10wt%, organic solvent 10-20wt%, the carbon nano-tube of handling through the carbon nano-tube dispersion liquid are surplus.
2. according to the described environmental-friendly conductive sizing agent based on the carbon nanotube-nano copper powder of claim 1, it is characterized in that: described carbon nano-tube is the mixture of one or both arbitrary proportions in Single Walled Carbon Nanotube and the multi-walled carbon nano-tubes.
3. according to the described environmental-friendly conductive sizing agent of claim 1 based on the carbon nanotube-nano copper powder, it is characterized in that: described carbon nano-tube dispersion liquid is a surface-active ion liquid, is specially dodecyl-3-methylimidazole bromine (C12mimBr) or myristyl-3-methylimidazole bromine (C14mimBr).
4. according to the described environmental-friendly conductive sizing agent of claim 1 based on the carbon nanotube-nano copper powder, it is characterized in that: described additive is binding agent and thickener and levelling agent, wherein binding agent is an epoxy powder coating, thickener and levelling agent are rheology modified thickener of polyurethane or hydrophobically-modified alkali swelling type thickener, and the mass ratio of binding agent and thickener and levelling agent is 1:1.
5. according to the described environmental-friendly conductive sizing agent based on the carbon nanotube-nano copper powder of claim 1, it is characterized in that: described organic solvent is the mixture of one or both arbitrary proportions in ethyleneglycol monophenylether and the ethylene glycol phenyl ether acetate.
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| CN201310105012.6A CN103219065B (en) | 2013-03-28 | 2013-03-28 | A kind of environmental-friendly conductive sizing agent based on carbon nanotube-nano copper powder |
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| CN201310105012.6A CN103219065B (en) | 2013-03-28 | 2013-03-28 | A kind of environmental-friendly conductive sizing agent based on carbon nanotube-nano copper powder |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106752804A (en) * | 2017-01-25 | 2017-05-31 | 山东凯盛新材料股份有限公司 | High temperature resistant, antistatic PEKK powdery paints and preparation method thereof |
| CN108628502A (en) * | 2018-04-12 | 2018-10-09 | 重庆市中光电显示技术有限公司 | Touch screen aqueous composite conducting slurry and its preparation method and application |
| CN110797186A (en) * | 2018-08-01 | 2020-02-14 | Ｊｘ金属株式会社 | Laminate of ceramic layer and copper powder paste sintered body |
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| CN1803352A (en) * | 2005-09-29 | 2006-07-19 | 江苏大学 | Method for preparing nanometer copper |
| CN101593568A (en) * | 2008-05-30 | 2009-12-02 | 三星电机株式会社 | The electrocondution slurry and the printed circuit board (PCB) that uses it that contain carbon nano-tube |
| EP2174910A1 (en) * | 2008-10-09 | 2010-04-14 | Exaenc Corp. | High conductive paste composite and method of producting the same |
| CN101864015A (en) * | 2010-06-25 | 2010-10-20 | 东华大学 | Method for preparing polyacrylonitrile/carbon nano tube composite material by taking ionic liquid as solvent |
| CN102198510A (en) * | 2011-04-27 | 2011-09-28 | 黑龙江大学 | Method for preparing nano copper/carbon nano tube composite powder by liquid phase method |
| CN102993820A (en) * | 2012-03-28 | 2013-03-27 | 杨阳 | Carbon nano material/metal nano material composite nano ink |
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| CN1803352A (en) * | 2005-09-29 | 2006-07-19 | 江苏大学 | Method for preparing nanometer copper |
| CN101593568A (en) * | 2008-05-30 | 2009-12-02 | 三星电机株式会社 | The electrocondution slurry and the printed circuit board (PCB) that uses it that contain carbon nano-tube |
| EP2174910A1 (en) * | 2008-10-09 | 2010-04-14 | Exaenc Corp. | High conductive paste composite and method of producting the same |
| CN101864015A (en) * | 2010-06-25 | 2010-10-20 | 东华大学 | Method for preparing polyacrylonitrile/carbon nano tube composite material by taking ionic liquid as solvent |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106752804A (en) * | 2017-01-25 | 2017-05-31 | 山东凯盛新材料股份有限公司 | High temperature resistant, antistatic PEKK powdery paints and preparation method thereof |
| CN108628502A (en) * | 2018-04-12 | 2018-10-09 | 重庆市中光电显示技术有限公司 | Touch screen aqueous composite conducting slurry and its preparation method and application |
| CN108628502B (en) * | 2018-04-12 | 2021-07-06 | 重庆市中光电显示技术有限公司 | Water-based composite conductive slurry for touch screen and preparation method and application thereof |
| CN110797186A (en) * | 2018-08-01 | 2020-02-14 | Ｊｘ金属株式会社 | Laminate of ceramic layer and copper powder paste sintered body |
| CN110797186B (en) * | 2018-08-01 | 2021-07-30 | Ｊｘ金属株式会社 | Laminate of ceramic layer and copper powder paste sintered body |
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