CN106448812A - Carbon-based water-based electroconductive slurry and preparation method thereof - Google Patents
Carbon-based water-based electroconductive slurry and preparation method thereof Download PDFInfo
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- CN106448812A CN106448812A CN201610931054.9A CN201610931054A CN106448812A CN 106448812 A CN106448812 A CN 106448812A CN 201610931054 A CN201610931054 A CN 201610931054A CN 106448812 A CN106448812 A CN 106448812A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
- H01B1/20—Conductive material dispersed in non-conductive organic material
- H01B1/24—Conductive material dispersed in non-conductive organic material the conductive material comprising carbon-silicon compounds, carbon or silicon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
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Abstract
The invention discloses carbon-based water-based electroconductive slurry. The carbon-based water-based electroconductive slurry is prepared from 0.3-0.5 wt% of helical carbon nanofiber, 0.7-1.4 wt% of carbon nano tubes, 1.5-2.6 wt% of fullerene soot, 0.2-0.5 wt% of a dispersing agent, 0.05-0.15 wt% of a defoaming agent and the balance a Na2CO3-NaHCO3 buffer solution. The invention further discloses a preparation method of the carbon-based water-based electroconductive slurry. The method comprises the steps that 1, the helical carbon nanofiber, the carbon nano tubes, the fullerene soot and the dispersing agent are placed into the Na2CO3-NaHCO3 buffer solution after being weighed; 2, all the materials are placed into a stirrer for low-speed stirring so as to achieve sufficient infiltration and preliminary mixing; 3, grinding is performed for 60-100 min to disperse the materials, and the defoaming agent is added dropwise in the grinding process. The carbon-based water-based electroconductive slurry is good in stability, a formed electroconductive film can be uniformly attached to the surface of a product, and the electroconductive performance is good.
Description
Technical field
The invention belongs to chemical field is and in particular to a kind of carbon-based waterborne conductive slurry and preparation method thereof.
Background technology
In technical fields such as electronics, the especially precision components such as flexible board and fine orifice plate require non-conductive substrate such as to mould
Material etc. has good conductive capability in local, to realize in technological operations such as its electroplating surfaces.Common process is first to lead non-
After electric base material activation process, allow electrocondution slurry in the hole wall on non-conductive substrate surface and micropore to spray the method soaking re-dry
Form layer of conductive film, then electroplated again.Additionally, some big-and-middle-sized non-conductive devices are also required to spray in use
Apply static electricity shield layer it is desirable to electrocondution slurry good fluidity, moderate and environmental friendliness.Slurry with metal as conductive materials will
Expensive, or chemical stability is poor；Slurry dispersiveness with carbon black as conductive materials and chemical stability are preferable, but
Electric conductivity is poor；With Graphene be main conductive materials slurry chemical stability and electric conductivity all preferable, but cost phase
To costliness, and because dispersion is more difficult needs introduce compared with multi-dispersant, subsequent applications may be impacted；Have
Electrocondution slurry solvent adopts organic solvent, has some specific uses, but is not suitable for very much the technique higher to environmental requirement.
Content of the invention
For prior art defect, it is an object of the invention to provide a kind of carbon-based waterborne conductive slurry and its preparation side
Method.The electric conductivity of this carbon-based waterborne conductive slurry is good.
The present invention seeks to be achieved through the following technical solutions：
Carbon-based waterborne conductive slurry of the present invention, is obtained by the raw material including following：
Balance of Na2CO3-NaHCO3Buffer solution.
Further, a diameter of 300～500nm of described coiled carbon fibers, draw ratio is 30～50.
Further, described carbon nanotube diameter is 5～20nm, 5～100 μm of length.
Fullerene soot of the present invention prepares, for combustion method, the extracted C of soot that fullerene obtains60Or C70Obtain afterwards
Remaining soot.Specifically preparation method is：With toluene as primary raw material, add a small amount of naphthalene and purified after carbolic oil, help in pure oxygen
Combustion, under high negative pressure environment (furnace pressure 40mmHg～70mmHg), generates soot in 1500-2500 DEG C of burning；Again with toluene is as molten
C is extracted in agent60Or C70, the when solvent due to extracting has been also carried out to soot washing, therefore gained remnants soot impurity is few.
Further, described fullerene soot content is 1.5wt%～1.8wt%
Preferably, the particle size of described fullerene soot is 30～70nm.
The species of dispersant of the present invention and defoamer is well known in the art, and its consumption is known in the art use
Amount.
Preferably, described dispersant be polyvinylpyrrolidone anionic dispersing agents and/or polyvinylpyrrolidone non-from
Sub- dispersant；Described defoamer is dimethicone.
The present invention also provides a kind of method preparing carbon-based waterborne conductive slurry, comprises the following steps：
(1) by after the weighing of coiled carbon fibers, CNT, fullerene soot and dispersant, it is placed in Na2CO3-NaHCO3Slow
Rush in liquid；
(2) step (1) resulting material is placed in stirring at low speed under agitator to infiltrate and tentatively mix with abundant；
(3) step (2) resulting material being ground 60～100min further makes it disperse, and drips froth breaking in process of lapping
Agent.
Further, in described step (1), the pH value of buffer solution controls 9.90～10.50 under 20 DEG C of environment.
Further, the Ginding process described in step (3) is sand milling, fineness≤5 μm.
The carbon-based waterborne conductive slurry that the present invention provides has the advantages that：
(1) good stability, standing is more than half a year still uniform, no precipitation and lamination；
(2) conductive film that this slurry is formed is evenly affixed to product surface；
(3) when CNT specifications control is in diameter 5-20nm, when in the range of length 5-100 μm, the electric conductivity of overlay film
Significantly increase.
Specific embodiment
Mode below by specific embodiment is further described to the present invention, but the scope of the present invention does not limit to
In these embodiments.All based on above-mentioned technological thought, the modification made using ordinary skill knowledge and customary means, replace
Change, change and belong to the scope of protection of present invention.
Embodiment 1
Weigh coiled carbon fibers 0.9g (a diameter of 300-500nm, draw ratio is 30-50), CNT 2.1g is (a diameter of
5-20nm, length 5-100 μm), fullerene soot 4.4g, polyvinylpyrrolidone anionic dispersing agents 0.9g, it is placed in cup.20
DEG C add Na2CO3-NaHCO3Buffer solution 291.5g control ph is 9.90～10.50.Stirred 5 minutes with 100r/min speed,
Rotating speed 200r/min stirs 5 minutes.Mixed material is poured in sand mill special stainless steel kettle.Add bead 200g, rotating speed
3500r/min sand milling 100min, adds 0.2g defoamer, so that material does not spill over stainless steel kettle.Sand milling uses stainless steel after terminating
Gauze filters bead, obtains carbon-based waterborne conductive slurry products.
Embodiment 2：
Weigh coiled carbon fibers 1.2g (a diameter of 300-500nm, draw ratio is 30-50), CNT 4.2g is (a diameter of
5-20nm, length 5-100 μm), fullerene soot 7.8g, polyvinylpyrrolidone anionic dispersing agents 0.9g and polyvinyl pyrrole
Alkanone non-ionic dispersing agent 1.5g, adds Na2CO3-NaHCO3Buffer solution 285g, control ph is 9.90～10.50.With 100r/
Min speed stirs 5 minutes, then is stirred 5 minutes with 200r/min speed.Mixed material is poured into sand mill special stainless steel kettle
In.Plus bead 200g, rotating speed 4000r/min sand milling 80min, drip 0.3g dimethicone defoamer.Sand milling is used after terminating
Stainless steel gauze filters bead, obtains carbon-based waterborne conductive slurry products.
Embodiment 3
Weigh coiled carbon fibers 1.5g (a diameter of 300-500nm, draw ratio is 30-50), CNT 2.8g is (a diameter of
5-20nm, length 5-100 μm), fullerene soot 6.3g, polyvinylpyrrolidone anionic dispersing agents 1.2g, it is placed in cup.20
DEG C add Na2CO3-NaHCO3Buffer solution 288g control ph is 9.90～10.50.Stirred 5 minutes with 100r/min speed, turn
Fast 200r/min stirs 5 minutes.Mixed material is poured in sand mill special stainless steel kettle.Add bead 200g, rotating speed
3500r/min sand milling 100min, adds 0.2g defoamer, so that material does not spill over stainless steel kettle.Sand milling uses stainless steel after terminating
Gauze filters bead, obtains carbon-based waterborne conductive slurry products.
Embodiment 4
The electrocondution slurry that embodiment 1 and embodiment 2 are obtained is contained in 200mL vial respectively, respectively drips salt of being fuming
Acid 8 simultaneously shakes up rear sealing preserve, and standing is observed and be the results are shown in Table 1 for 24 hours, 3 months, 6 months.
The stability of table 1 electrocondution slurry
Result shows, the electrocondution slurry obtained by the present invention, its good stability, places 3 months or even still uniform after half a year,
No precipitation and lamination.
Comparative example
(1) method with reference to embodiment 1-3 prepares electrocondution slurry, except that, it is not added with institute of the present invention in step (1)
State fullerene soot, correspondingly, prepared electrocondution slurry is respectively comparative example 1-3.Embodiment 1-3 and comparative example 1-3 are obtained
Slurry be respectively used to activate after plastic tab, carry out electroplating experiments, the long 50mm of plastic tab, wide 6mm.
Electro-plating method：Electrocondution slurry is placed in water-bath, keeps 50 DEG C of constant temperature, plastic tab is put into leaching in electrocondution slurry
Bubble 6min, proposes thin slice and erects 20s, allows the slurry failing on thin slice to adhere to instill beaker, then electricity consumption dries up thin slice,
Copper facing 3min under 2.6A electric current, observes and the results are shown in Table 2.
The uniformity of the electroplated rear finished product of table 2
Test result shows, compared with the slurry being not added with fullerene soot, is added the slurry of fullerene soot by the present invention
The finished product of material preparation, the uniformity of its overlay film significantly improves.
(2) method with reference to embodiment 1-3 prepares electrocondution slurry, except that, the specification of CNT in step (1)
Difference, tests the electrocondution slurry prepared by different size CNT, then makes the electric conductivity after overlay film, result is as shown in table 3.
The impact to overlay film electric conductivity for the table 3 different size CNT
Remarks："+" represents can be conductive, and " ++ " represents easily conductive.
Conclusion：The film-coating tool being obtained using inventive formulation gained slurry is conductive, and CNT specifications control exists
Diameter 5-20nm, when in the range of length 5-100 μm, the electric conductivity of overlay film significantly increases.
Claims (8)
1. a kind of carbon-based waterborne conductive slurry is it is characterised in that be obtained by including following raw material：
2. carbon-based waterborne conductive slurry according to claim 1 is it is characterised in that described coiled carbon fibers a diameter of 300
～500nm, draw ratio is 30～50.
3. carbon-based waterborne conductive slurry according to claim 1 it is characterised in that described carbon nanotube diameter be 5～
20nm, 5～100 μm of length.
4. carbon-based waterborne conductive slurry according to claim 1 is it is characterised in that described fullerene soot is burning legal system
The remaining soot obtaining after extracted C60 or C70 of soot that standby fullerene obtains, particle size is 30～70nm.
5. carbon-based waterborne conductive slurry according to claim 1 is it is characterised in that described dispersant is polyvinylpyrrolidine
Ketone anionic dispersing agents and/or polyvinylpyrrolidone non-ionic dispersing agent；Described defoamer is dimethicone.
6. a kind of method of the carbon-based waterborne conductive slurry prepared described in claim 1, comprises the following steps：
(1) by after the weighing of coiled carbon fibers, CNT, fullerene soot and dispersant, it is placed in Na2CO3-NaHCO3Buffer solution
In；
(2) step (1) resulting material is placed in stirring at low speed under agitator to infiltrate and tentatively mix with abundant；
(3) step (2) resulting material being ground 60～100min further makes it disperse, and drips defoamer in process of lapping.
7. carbon-based waterborne conductive slurry according to claim 6 preparation method it is characterised in that：In described step (1)
The pH value of buffer solution controls 9.90～10.50 under 20 DEG C of environment.
8. the preparation method of carbon-based waterborne conductive slurry according to claim 6 is it is characterised in that described in step (3)
Ginding process is sand milling, fineness≤5 μm.
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| CN201610931054.9A CN106448812B (en) | 2016-10-31 | 2016-10-31 | A kind of carbon-based waterborne conductive slurry and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107493613A (en) * | 2017-08-16 | 2017-12-19 | 杜启明 | A kind of electric heating produces the electric slurry and manufacturing process and methods for using them of far infrared |
| CN108735344A (en) * | 2018-05-23 | 2018-11-02 | 江苏时瑞电子科技有限公司 | A kind of carbon fiber/carbon nanotube composite conducting slurry and preparation method thereof |
| CN114883103A (en) * | 2022-04-28 | 2022-08-09 | 广州三则电子材料有限公司 | Method for manufacturing low-temperature sintered copper electrode alloy iron powder core power inductor |
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| JP2007023429A (en) * | 2005-07-19 | 2007-02-01 | Teijin Techno Products Ltd | Heat-resistant conductive paper and method for producing the same |
| WO2011019970A1 (en) * | 2009-08-14 | 2011-02-17 | Nano-C, Inc. | Solvent-based and water-based carbon nanotube inks with removable additives |
| KR20160032409A (en) * | 2014-09-16 | 2016-03-24 | 영진기술 주식회사 | High conductive Paste composition and producing Method thereof using high temperature heat treatment |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007023429A (en) * | 2005-07-19 | 2007-02-01 | Teijin Techno Products Ltd | Heat-resistant conductive paper and method for producing the same |
| WO2011019970A1 (en) * | 2009-08-14 | 2011-02-17 | Nano-C, Inc. | Solvent-based and water-based carbon nanotube inks with removable additives |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107493613A (en) * | 2017-08-16 | 2017-12-19 | 杜启明 | A kind of electric heating produces the electric slurry and manufacturing process and methods for using them of far infrared |
| CN108735344A (en) * | 2018-05-23 | 2018-11-02 | 江苏时瑞电子科技有限公司 | A kind of carbon fiber/carbon nanotube composite conducting slurry and preparation method thereof |
| CN114883103A (en) * | 2022-04-28 | 2022-08-09 | 广州三则电子材料有限公司 | Method for manufacturing low-temperature sintered copper electrode alloy iron powder core power inductor |
| CN114883103B (en) * | 2022-04-28 | 2023-06-23 | 广州三则电子材料有限公司 | Manufacturing method of low-temperature sintered copper electrode alloy iron powder core power inductor |
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| CN106448812B (en) | 2018-01-19 |
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