CN106448812B - A kind of carbon-based waterborne conductive slurry and preparation method thereof - Google Patents
A kind of carbon-based waterborne conductive slurry and preparation method thereof Download PDFInfo
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- CN106448812B CN106448812B CN201610931054.9A CN201610931054A CN106448812B CN 106448812 B CN106448812 B CN 106448812B CN 201610931054 A CN201610931054 A CN 201610931054A CN 106448812 B CN106448812 B CN 106448812B
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- carbon
- conductive slurry
- based waterborne
- waterborne conductive
- soot
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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
Abstract
The invention discloses a kind of carbon-based waterborne conductive slurry, its raw material includes：Coiled carbon fibers 0.3wt%~0.5wt%；CNT 0.7wt%~1.4wt%；Fullerene soot 1.5wt%~2.6wt%；Dispersant 0.2wt%~0.5wt%；Defoamer 0.05wt%~0.15wt%；Surplus is Na2CO3‑NaHCO3Buffer solution.The invention also discloses the preparation method of carbon-based waterborne conductive slurry：(1) after weighing coiled carbon fibers, CNT, fullerene soot and dispersant, it is placed in Na2CO3‑NaHCO3In buffer solution；(2) resulting material is placed under agitator stirring at low speed fully to infiltrate and tentatively mix；(3) 60~100min of grinding makes it scattered, and defoamer is added dropwise in process of lapping.The stability of carbon-based waterborne conductive slurry provided by the invention is good, and the conductive film formed can be evenly affixed to product surface, and electric conductivity is good.
Description
Technical field
The invention belongs to chemical field, and in particular to a kind of carbon-based waterborne conductive slurry and preparation method thereof.
Background technology
Require non-conductive substrate as moulded in the precision components such as the technical fields such as electronics, especially flexible board and fine orifice plate
Material etc. locally has good conductive capability, to realize in technological operations such as its electroplating surfaces.Common process is first to be led non-
After electric base material activation process, the method that re-dry is soaked with spraying allows electrocondution slurry in non-conductive substrate surface and the hole wall of micropore
Layer of conductive film is formed, is then electroplated again.In addition, 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 cost and environment-friendly.Slurry using metal as conductive materials will
It is expensive, otherwise chemical stability is poor；It is preferable as the slurry dispersiveness and chemical stability of conductive materials using carbon black, but
Electric conductivity is poor；It is all preferable as the slurry chemical stability and electric conductivity of main conductive materials using graphene, but cost phase
To costliness, and it is because scattered more difficult needing introducing to be impacted compared with multi-dispersant to subsequent applications；Have
Electrocondution slurry solvent uses organic solvent, has some specific uses, but be not suitable for very much the technique higher to environmental requirement.
The 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 the carbon-based waterborne conductive slurry is good.
The present invention seeks to what is be achieved through the following technical solutions：
Carbon-based waterborne conductive slurry of the present invention, is made by following raw material：
Surplus is Na2CO3-NaHCO3Buffer solution.
Further, a diameter of 300~500nm of the coiled carbon fibers, draw ratio are 30~50.
Further, the carbon nanotube diameter is 5~20nm, 5~100 μm of length.
Fullerene soot of the present invention is that combustion method prepares the extracted C of soot that fullerene obtains60Or C70Obtain afterwards
Remaining soot.Specifically preparation method is：Using toluene as primary raw material, add a small amount of naphthalene and it is purified after carbolic oil, helped in pure oxygen
Fire, under high negative pressure environment (furnace pressure 40mmHg~70mmHg), in 1500-2500 DEG C of burning generation soot；Again with toluene is as molten
C is extracted in agent60Or C70, because the when solvent of extraction is also washed to soot, therefore gained remnants soot impurity is few.
Further, the fullerene soot content is 1.5wt%~1.8wt%
Preferably, the particle size of the fullerene soot is 30~70nm.
The species of dispersant and defoamer of the present invention is well known in the art, and its dosage is known in the art use
Amount.
Preferably, the dispersant be polyvinylpyrrolidone anionic dispersing agents and/or polyvinylpyrrolidone it is non-from
Sub- dispersant；The defoamer is dimethicone.
The present invention also provides a kind of method for preparing carbon-based waterborne conductive slurry, comprises the following steps：
(1) after weighing coiled carbon fibers, CNT, fullerene soot and dispersant, it is placed in Na2CO3-NaHCO3It is slow
In fliud flushing；
(2) step (1) resulting material is placed under agitator stirring at low speed fully to infiltrate and tentatively mix；
(3) step (2) resulting material is further ground into 60~100min makes it scattered, and defoaming is added dropwise in process of lapping
Agent.
Further, the pH value of buffer solution is controlled 9.90~10.50 under 20 DEG C of environment in the step (1).
Further, the Ginding process described in step (3) is is sanded, fineness≤5 μm.
Carbon-based waterborne conductive slurry provided by the invention has the advantages that：
(1) stability is good, stands more than half a year still uniformly, no precipitation and lamination；
(2) conductive film that the slurry is formed is evenly affixed to product surface；
(3) when CNT specifications control is when in the range of diameter 5-20nm, 5-100 μm of length, the electric conductivity of overlay film
Significantly increase.
Embodiment
The present invention is further described below by the mode of specific embodiment, but the scope of the present invention does not limit to
In these embodiments.It is all to be 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
Coiled carbon fibers 0.9g (a diameter of 300-500nm, draw ratio 30-50) is weighed, CNT 2.1g is (a diameter of
5-20nm, 5-100 μm of length), 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 is stirred 5 minutes.Mixed material is poured into sand mill special stainless steel kettle.Add bead 200g, rotating speed
100min is sanded in 3500r/min, 0.2g defoamers is added, 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：
Coiled carbon fibers 1.2g (a diameter of 300-500nm, draw ratio 30-50) is weighed, CNT 4.2g is (a diameter of
5-20nm, 5-100 μm of length), fullerene soot 7.8g, polyvinylpyrrolidone anionic dispersing agents 0.9g and polyvinyl pyrrole
Alkanone non-ionic dispersing agent 1.5g, add Na2CO3-NaHCO3Buffer solution 285g, control ph are 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.Add bead 200g, rotating speed 4000r/min that 80min is sanded, 0.3g dimethicone defoamers are added dropwise.Sand milling is used after terminating
Stainless steel gauze filters bead, obtains carbon-based waterborne conductive slurry products.
Embodiment 3
Coiled carbon fibers 1.5g (a diameter of 300-500nm, draw ratio 30-50) is weighed, CNT 2.8g is (a diameter of
5-20nm, 5-100 μm of length), 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, turned with 100r/min speed
Fast 200r/min is stirred 5 minutes.Mixed material is poured into sand mill special stainless steel kettle.Add bead 200g, rotating speed
100min is sanded in 3500r/min, 0.2g defoamers is added, 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
Electrocondution slurry made from embodiment 1 and embodiment 2 is contained in 200mL vials, then each dropwise addition smoke salt respectively
Acid 8 drips and is sealed after shaking up, and standing is observed and the results are shown in Table 1 for 24 hours, 3 months, 6 months.
The stability of the electrocondution slurry of table 1
As a result showing, the electrocondution slurry obtained by the present invention, its stability is good, places 3 months even after half a year still uniformly,
Without precipitation and lamination.
Comparative example
(1) electrocondution slurry is prepared with reference to embodiment 1-3 method, except that, institute of the present invention is not added with step (1)
Fullerene soot is stated, correspondingly, obtained electrocondution slurry is respectively comparative example 1-3.Embodiment 1-3 and comparative example 1-3 are made
Slurry be respectively used to activation after plastic tab, carry out electroplating experiments, plastic tab long 50mm, wide 6mm.
Electro-plating method：Electrocondution slurry is placed in water-bath, 50 DEG C of constant temperature is kept, plastic tab is put into electrocondution slurry and soaked
6min is steeped, proposes that thin slice erects 20s, allows on thin slice the slurry for failing attachment to instill beaker, then electricity consumption blowing drying thin slice,
Copper facing 3min under 2.6A electric currents, observation the results are shown in Table 2.
The uniformity of finished product after table 2 is electroplated
Test result shows, compared with the slurry for being not added with fullerene soot, the slurry of fullerene soot is added by the present invention
Expect the finished product prepared, the uniformity of its overlay film significantly improves.
(2) electrocondution slurry is prepared with reference to embodiment 1-3 method, except that, the specification of CNT in step (1)
Difference, the electrocondution slurry prepared by different size CNT is tested, then the electric conductivity after overlay film is made, as a result as shown in table 3.
Influence of the different size CNT of table 3 to overlay film electric conductivity
Remarks："+" represents can be conductive, and " ++ " represents easily conductive.
Conclusion：It is conductive using overlay film made from slurry obtained by inventive formulation, and CNT specifications control exists
Diameter 5-20nm, when in the range of 5-100 μm of length, the electric conductivity of overlay film significantly increases.
Claims (8)
1. a kind of carbon-based waterborne conductive slurry, it is characterised in that be made by following raw material：
2. carbon-based waterborne conductive slurry according to claim 1, it is characterised in that the coiled carbon fibers a diameter of 300
~500nm, draw ratio are 30~50.
3. carbon-based waterborne conductive slurry according to claim 1, it is characterised in that the carbon nanotube diameter be 5~
20nm, 5~100 μm of length.
4. carbon-based waterborne conductive slurry according to claim 1, it is characterised in that the fullerene soot is burning legal system
The remaining soot obtained after the soot extracted C60 or C70 that standby fullerene obtains, particle size is 30~70nm.
5. carbon-based waterborne conductive slurry according to claim 1, it is characterised in that the dispersant is polyvinylpyrrolidine
Ketone anionic dispersing agents and/or polyvinylpyrrolidone non-ionic dispersing agent；The defoamer is dimethicone.
6. a kind of method for preparing the carbon-based waterborne conductive slurry described in claim 1, comprises the following steps：
(1) after weighing coiled carbon fibers, CNT, fullerene soot and dispersant, it is placed in Na2CO3-NaHCO3Buffer solution
In；
(2) step (1) resulting material is placed under agitator stirring at low speed fully to infiltrate and tentatively mix；
(3) step (2) resulting material is further ground into 60~100min makes it scattered, and defoamer is added dropwise in process of lapping.
7. the preparation method of carbon-based waterborne conductive slurry according to claim 6, it is characterised in that：In the step (1)
The pH value of buffer solution is controlled 9.90~10.50 under 20 DEG C of environment.
8. the preparation method of carbon-based waterborne conductive slurry according to claim 6, it is characterised in that described in step (3)
Ginding process is is sanded, fineness≤5 μm.
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| 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 |
| 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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| CA2770997C (en) * | 2009-08-14 | 2018-07-03 | Ramesh Sivarajan | Solvent-based and water-based carbon nanotube inks with removable additives |
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