CN113421694A - Graphene sheet/carbon black composite black pore liquid and preparation method thereof - Google Patents
Graphene sheet/carbon black composite black pore liquid and preparation method thereof Download PDFInfo
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- CN113421694A CN113421694A CN202110662009.9A CN202110662009A CN113421694A CN 113421694 A CN113421694 A CN 113421694A CN 202110662009 A CN202110662009 A CN 202110662009A CN 113421694 A CN113421694 A CN 113421694A
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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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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/54—Electroplating of non-metallic surfaces
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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
- H01B1/06—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors mainly consisting of other non-metallic substances
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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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- H—ELECTRICITY
- H05—ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
- H05K—PRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
- H05K3/00—Apparatus or processes for manufacturing printed circuits
- H05K3/40—Forming printed elements for providing electric connections to or between printed circuits
- H05K3/42—Plated through-holes or plated via connections
- H05K3/423—Plated through-holes or plated via connections characterised by electroplating method
- H05K3/424—Plated through-holes or plated via connections characterised by electroplating method by direct electroplating
Abstract
The invention belongs to the technical field of printed circuit board manufacturing, and particularly relates to a graphene sheet/carbon black composite black pore liquid and a preparation method thereof. The black hole liquid can keep the system stable within 300 days without sedimentation. And the black pore liquid preparation process is simple and efficient, low in cost, high in cost performance, environment-friendly and suitable for large-scale production.
Description
Technical Field
The invention belongs to the technical field of printed circuit board manufacturing, and particularly relates to a graphene sheet/carbon black composite black hole liquid and a preparation method thereof.
Background
The PCB is commonly called a printed circuit board, and its main function is to connect various electronic components through circuits, so as to perform the functions of conduction and transmission, and is a key electronic interconnection of electronic products. Both sides of the PCB are provided with wiring, and the connection of circuits on both sides is realized through the guide holes on the PCB. The PCB is an insulator, and in order to achieve conductive conduction on both sides of the board, the holes on the PCB must be metallized. Compared with a chemical copper plating method with complex process and high pollution, the direct electroplating of hole metallization is more in line with the development trend of environmental protection and energy conservation. The raw materials of the black hole method are graphite or carbon black, so that the black hole method is low in price and simple in process flow, and the used chemical reagents are few in types, non-toxic, harmless and the like, so that the black hole method has huge development potential.
The black hole liquid on the market at present is composed of conductive carbon black or graphite, a dispersing agent medium, a binder and other auxiliary agents, conductive nano or micron particles are obtained through mechanical grinding, and the conductive nano or micron particles are attached to through holes of a circuit board in the black hole process. However, the problems of unstable system, poor conductivity, large dosage and the like caused by easy agglomeration of the conductive carbon black nano particles in the system limit the practical application of the conductive carbon black nano particles; when graphite is used as a conductive agent, the graphite layer is too thick locally due to large particle size, so that the guide hole is blocked, and subsequent electroplating is affected. Therefore, whether carbon black or graphite has respective advantages and defects, and other conductive materials still need to be excavated and developed in order to solve the problems of the black hole fluid.
The graphene sheet is used as a two-dimensional carbon material with thin sheet layer and excellent current carrying capacity, can make up for the defects of carbon black and graphite, and has potential application value in black hole liquid. The conductive medium in the black pore liquid is required to have a small particle size (as small as possible to a nanometer level) and a good adsorbability to the substrate, in addition to excellent conductivity. At present, graphene sheet materials on the market are micron-sized, have excessively thick sheet layers and are not suitable for preparing black hole liquid.
At present, carbon black and graphite are mainly used as conductive media in the black pore liquid on the market, the median of the particle size of the carbon black is from dozens of nanometers to dozens of nanometers, and the median of the particle size of the graphite is about 1 mu m. The carbon black has small particle size and strong adsorbability, but has poor conductivity; graphite has good conductivity because the lone pair electrons of carbon in the layer form delocalized pi bonds, but because the particle diameter is larger than that of carbon black, a printed circuit board treated by the graphite conductive liquid may have an excessively thick graphite layer locally, and generally speaking, the existing black hole liquid system is unstable, easy to generate coagulation and poor in conductivity, and has obvious defects in the printed circuit board, so that a novel circuit board conductive liquid needs to be developed to solve the existing problems.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a graphene sheet/carbon black composite black pore liquid and a preparation method thereof, the adopted conductive agent is a graphene sheet and carbon black, the particle size of a conductive medium in a system is greatly reduced by optimizing the combination of a surfactant, selecting a proper water-soluble high polymer and carrying out three combined processes of ultrasound, sanding and high-pressure homogenization, and the black pore liquid with good conductivity, high stability, strong adsorbability to a base material and low cost is obtained, and the content of the black pore liquid is as follows:
the invention aims to provide a graphene sheet/carbon black composite black pore liquid, which is technically characterized in that: the graphene sheet/carbon black composite black pore liquid comprises, by weight, 3-8.4 parts of graphene sheets, 1.5-4.5 parts of carbon black, 1.5-3 parts of a surfactant, 1.5-3 parts of a water-based high polymer, 1.5-3 parts of a potassium hydroxide solution and 92.7-97 parts of deionized water.
In some embodiments of the invention, the number of graphene sheets in the graphene sheet/carbon black composite black pore liquid formula system is less than 8, the thickness of the graphene sheet layer is less than 3nm, and the single layer rate of the graphene sheet is greater than 80%.
In some embodiments of the invention, the surfactant in the graphene sheet/carbon black composite black pore liquid formula system is at least one of sodium dodecyl sulfate, nonylphenol polyoxyethylene ether phosphate, sodium dodecyl benzene sulfonate, fatty alcohol polyoxyethylene ether, nonylphenol polyoxyethylene ether, fatty alcohol polyoxyethylene sulfate, and potassium dodecyl phosphate.
In some embodiments of the invention, the aqueous high molecular polymer in the graphene sheet/carbon black composite black pore liquid formula system is at least one of polyethylene glycol, polyvinylpyrrolidone, polyvinyl alcohol, sodium carboxymethyl cellulose, sodium lignosulfonate, polyvinyl alcohol, sodium polyacrylate and polyacrylamide.
In some embodiments of the invention, the concentration of the potassium hydroxide solution in the graphene sheet/carbon black composite black pore liquid formulation system is 40 to 60 g/L.
The second purpose of the invention is to provide a preparation method of the graphene sheet/carbon black composite black pore liquid, which has the technical points that: the method comprises the following steps:
accurately weighing graphene sheets, carbon black, a surfactant, a water-based high polymer, potassium hydroxide and deionized water for later use;
step two, adding the surfactant and the water-based high molecular polymer into water, and stirring and mixing the mixture uniformly at a high speed at a rotating speed of 3000-;
step three, putting the graphene sheets and the carbon black into the mixture A obtained in the step two, and performing ultrasonic treatment for 10-30min to obtain a mixture B;
and step four, performing sanding and high-pressure homogenization treatment on the mixture B obtained in the step three, and then adding a potassium hydroxide solution into the treated mixture B to adjust the pH value to 9-11 to obtain the black pore liquid.
In some embodiments of the present invention, the ultrasonic treatment in step three of the preparation method of the graphene sheet/carbon black composite black pore liquid of the present invention specifically refers to: an ultrasonic frequency electric signal is generated by an ultrasonic generator, the electric signal is converted into mechanical wave with the same frequency by a piezoelectric transducer, the power of the ultrasonic generator is 1500-3000W, the working frequency of the ultrasonic generator is 80-100KHZ, and the working frequency of the transducer is 80KHZ or 100 KHZ.
In some embodiments of the invention, the rotation speed of the sanding treatment in step four of the preparation method of the graphene sheet/carbon black composite black pore liquid of the invention is 500-3000 rpm.
In some embodiments of the present invention, the pressure of the graphene sheet/carbon black composite black pore liquid in the fourth step of the preparation method of the present invention is 80 to 120Mpa during the high pressure homogenization treatment.
In some embodiments of the present invention, the black pore liquid particle size D90 of the sand grinding and high pressure homogenization treatment in step four of the preparation method of the graphene sheet/carbon black composite black pore liquid of the present invention is less than 2 μm.
Compared with the prior art, the graphene sheet/carbon black composite black pore liquid and the preparation method thereof have the beneficial effects that:
the black pore liquid graphene sheet/carbon black composite black pore liquid is prepared by mixing graphene sheets, carbon black, a surfactant, a water-based high-molecular polymer, a potassium hydroxide solution and deionized water, and the particle size of a conductive medium in a system is greatly reduced through three combined processes of ultrasound, sanding and high-pressure homogenization, so that the black pore liquid with good conductivity, high stability, strong substrate adsorbability and low cost is obtained. The black pore liquid is a conductive liquid taking graphene sheets and carbon black as conductive media, has the advantages of high dispersibility, good solution wettability, strong through-hole capability, small resistance, excellent binding force and the like, and has the performance far higher than that of the black pore liquid taking single carbon black as the conductive media. The black hole liquid can keep the system stable within 300 days without sedimentation. The black pore liquid of the invention has the advantages of simple and efficient preparation process, low cost, high cost performance, environment-friendly process and suitability for large-scale production.
Drawings
FIG. 1 is a graph of a black hole fluid of the present invention after being left for one week, compared with a black hole fluid of a comparative example;
FIG. 2 is a graph showing the adsorption properties of the black matrix according to the present invention and the black matrix according to the comparative example.
Detailed Description
Embodiments of the present invention will be described in detail below with reference to examples, but it will be understood by those skilled in the art that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer.
Example 1
The graphene sheet/carbon black composite black pore liquid comprises 3g of graphene sheets (the number of graphene sheets is less than 8, the thickness of the sheets is less than 3nm, the single-layer rate is greater than 80%), 1.5g of carbon black, 1.5g of surfactant (sodium dodecyl sulfate: nonylphenol polyoxyethylene ether phosphate is 1:1), 1.5g of polyethylene glycol, 1.5g of potassium hydroxide solution (the concentration is 40g/L) and 92.7g of deionized water.
According to the formula, the preparation method of the graphene sheet/carbon black composite black pore liquid comprises the following steps:
accurately weighing graphene sheets, carbon black, a surfactant, a water-based high polymer, potassium hydroxide and deionized water for later use;
adding a surfactant and a water-based high molecular polymer into water, and stirring and mixing uniformly at a high speed of 3000rmp to obtain a mixture A;
step three, putting the graphene sheets and the carbon black into the mixture A obtained in the step two, and performing ultrasonic treatment for 10min to obtain a mixture B, wherein the ultrasonic treatment specifically comprises the following steps: an ultrasonic frequency electric signal is generated by an ultrasonic generator, the electric signal is converted into mechanical waves with the same frequency through a piezoelectric transducer, the power of the ultrasonic generator is 1500W, the working frequency of the ultrasonic generator is 80KHZ, and the working frequency of the transducer is 80 KHZ;
and step four, performing sanding at the rotating speed of 500rpm and high-pressure homogenization at the pressure of 80MPa on the mixture B obtained in the step three until the granularity D90 of the black pore liquid is tested to be less than 2 mu m, and then adding a potassium hydroxide solution into the treated mixture B to adjust the pH value to 9 to obtain the black pore liquid.
Example 2
The graphene sheet/carbon black composite black pore liquid comprises 5g of graphene sheets (the number of graphene sheets is less than 8, the thickness of the sheets is less than 3nm, and the single-layer rate is greater than 80%), 2g of carbon black, 1.5g of surfactant (wherein sodium dodecyl sulfate: sodium dodecyl benzene sulfonate ═ 1:2), 2g of polyvinylpyrrolidone, 2g of potassium hydroxide solution (the concentration is 45g/L) and 93g of deionized water.
According to the formula, the preparation method of the graphene sheet/carbon black composite black pore liquid comprises the following steps:
accurately weighing graphene sheets, carbon black, a surfactant, a water-based high polymer, potassium hydroxide and deionized water for later use;
adding a surfactant and a water-based high molecular polymer into water, and stirring and mixing uniformly at a high speed of 3200rmp to obtain a mixture A;
step three, putting the graphene sheets and the carbon black into the mixture A obtained in the step two, and performing ultrasonic treatment for 15min to obtain a mixture B, wherein the ultrasonic treatment specifically comprises the following steps: an ultrasonic frequency electric signal is generated by an ultrasonic generator, the electric signal is converted into mechanical waves with the same frequency by a piezoelectric transducer, the power of the ultrasonic generator is 1800W, the working frequency of the ultrasonic generator is 85KHZ, and the working frequency of the transducer is 100 KHZ;
and step four, performing sand grinding at the rotating speed of 500-3000rpm and high-pressure homogenization at the pressure of 90MPa on the mixture B obtained in the step three until the granularity D90 of the black pore liquid is tested to be less than 2 mu m, and then adding a potassium hydroxide solution into the treated mixture B to adjust the pH value to 8 to obtain the black pore liquid.
Example 3
The graphene sheet/carbon black composite black pore liquid comprises 5g of graphene sheets (the number of graphene sheets is less than 8, the thickness of the sheet layer is less than 3nm, and the single-layer rate is greater than 80%), 3g of carbon black, 5g of surfactant (wherein sodium dodecyl sulfate: fatty alcohol-polyoxyethylene ether ═ 1:3), 2g of polyvinyl alcohol, 2g of potassium hydroxide solution (the concentration is 45g/L) and 94g of deionized water.
According to the formula, the preparation method of the graphene sheet/carbon black composite black pore liquid comprises the following steps:
accurately weighing graphene sheets, carbon black, a surfactant, a water-based high polymer, potassium hydroxide and deionized water for later use;
adding a surfactant and a water-based high molecular polymer into water, and stirring and mixing uniformly at a high speed at a rotating speed of 3500rmp to obtain a mixture A;
step three, putting the graphene sheets and the carbon black into the mixture A obtained in the step two, and performing ultrasonic treatment for 20min to obtain a mixture B, wherein the ultrasonic treatment specifically comprises the following steps: an ultrasonic frequency electric signal is generated by an ultrasonic generator, the electric signal is converted into mechanical waves with the same frequency by a piezoelectric transducer, the power of the ultrasonic generator is 2000W, the working frequency of the ultrasonic generator is 90KHZ, and the working frequency of the transducer is 80 KHZ;
and step four, performing sand grinding at the rotating speed of 500-3000rpm and high-pressure homogenization at the pressure of 100MPa on the mixture B obtained in the step three until the granularity D90 of the black pore liquid is tested to be less than 2 mu m, and then adding a potassium hydroxide solution into the treated mixture B to adjust the pH value to 8 to obtain the black pore liquid.
Example 4
The graphene sheet/carbon black composite black pore liquid comprises 6g of graphene sheets (the number of graphene sheets is less than 8, the thickness of the sheet layer is less than 3nm, the single-layer rate is greater than 80%), 1.5g of carbon black, 2.5g of surfactant (sodium dodecyl sulfate; nonylphenol polyoxyethylene ether is 1:2), 2g of sodium carboxymethylcellulose, 2g of potassium hydroxide solution (the concentration is 50g/L) and 95g of deionized water.
According to the formula, the preparation method of the graphene sheet/carbon black composite black pore liquid comprises the following steps:
accurately weighing graphene sheets, carbon black, a surfactant, a water-based high polymer, potassium hydroxide and deionized water for later use;
adding a surfactant and a water-based high molecular polymer into water, and stirring and mixing uniformly at a high speed at a rotating speed of 3500rmp to obtain a mixture A;
step three, putting the graphene sheets and the carbon black into the mixture A obtained in the step two, and performing ultrasonic treatment for 20min to obtain a mixture B, wherein the ultrasonic treatment specifically comprises the following steps: an ultrasonic frequency electric signal is generated by an ultrasonic generator, the electric signal is converted into mechanical waves with the same frequency by a piezoelectric transducer, the power of the ultrasonic generator is 2500W, the working frequency of the ultrasonic generator is 90KHZ, and the working frequency of the transducer is 100 KHZ;
and step four, performing sand grinding at the rotating speed of 500-3000rpm and high-pressure homogenization treatment at the pressure of 110MPa on the mixture B obtained in the step three until the granularity D90 of the black pore liquid is tested to be less than 2 mu m, and then adding a potassium hydroxide solution into the treated mixture B to adjust the pH value to 10 to obtain the black pore liquid.
Example 5
The graphene sheet/carbon black composite black pore liquid comprises 7g of graphene sheets (the number of graphene sheets is less than 8, the thickness of the sheet layer is less than 3nm, the single-layer rate is greater than 80%), 2g of carbon black, 2.7g of surfactant (sodium dodecyl sulfate: fatty alcohol polyoxyethylene sulfate is 1:1), 2.5g of aqueous high polymer sodium lignosulfonate, 2.5g of potassium hydroxide solution (the concentration is 55g/L) and 96g of deionized water.
According to the formula, the preparation method of the graphene sheet/carbon black composite black pore liquid comprises the following steps:
accurately weighing graphene sheets, carbon black, a surfactant, a water-based high polymer, potassium hydroxide and deionized water for later use;
adding a surfactant and a water-based high molecular polymer into water, and stirring and mixing uniformly at a high speed at a rotating speed of 3500rmp to obtain a mixture A;
step three, putting the graphene sheets and the carbon black into the mixture A obtained in the step two, and performing ultrasonic treatment for 25min to obtain a mixture B, wherein the ultrasonic treatment specifically comprises the following steps: an ultrasonic frequency electric signal is generated by an ultrasonic generator, the electric signal is converted into mechanical waves with the same frequency by a piezoelectric transducer, the power of the ultrasonic generator is 2500W, the working frequency of the ultrasonic generator is 90KHZ, and the working frequency of the transducer is 100 KHZ;
and step four, sanding the mixture B obtained in the step three at the rotating speed of 1000rpm and carrying out high-pressure homogenization treatment under the pressure of 120MPa until the granularity D90 of the black pore liquid is tested to be less than 2 mu m, and then adding a potassium hydroxide solution into the treated mixture B to adjust the pH value to 11 to obtain the black pore liquid.
Example 6
The graphene sheet/carbon black composite black pore liquid comprises 8.4g of graphene sheets (the number of graphene sheets is less than 8, the sheet thickness is less than 3nm, and the single-layer rate is greater than 80%), 4.5g of carbon black, 3g of surfactant (sodium dodecyl sulfate: potassium dodecyl phosphate is 1:3), 3g of polyvinyl alcohol, 3g of potassium hydroxide solution (the concentration is 50g/L) and 97g of deionized water.
According to the formula, the preparation method of the graphene sheet/carbon black composite black pore liquid comprises the following steps:
accurately weighing graphene sheets, carbon black, a surfactant, a water-based high polymer, potassium hydroxide and deionized water for later use;
adding a surfactant and a water-based high molecular polymer into water, and stirring and mixing uniformly at a high speed of 4000rmp to obtain a mixture A;
step three, putting the graphene sheets and the carbon black into the mixture A obtained in the step two, and performing ultrasonic treatment for 30min to obtain a mixture B, wherein the ultrasonic treatment specifically comprises the following steps: an ultrasonic frequency electric signal is generated by an ultrasonic generator, the electric signal is converted into mechanical wave with the same frequency by a piezoelectric transducer, the power of the ultrasonic generator is 3000W, the working frequency of the ultrasonic generator is 100KHZ, and the working frequency of the transducer is 80 KHZ;
and step four, performing sand grinding at the rotating speed of 3000rpm and high-pressure homogenization at the pressure of 100MPa on the mixture B obtained in the step three until the granularity D90 of the black pore liquid is tested to be less than 2 mu m, and then adding a potassium hydroxide solution into the treated mixture B to adjust the pH value to 10 to obtain the black pore liquid.
Test examples
The black pore liquid of the present invention prepared in examples 1 to 6 was tested for stability, conductivity and adsorption after black pore treatment of PCB, respectively, using a commercially available carbon black pore liquid as comparative example 1 and a commercially available graphite black pore liquid (hennoco HNX5) as comparative example 2, and the results of the test were shown in table 1, fig. 1 and fig. 2:
TABLE 1
The experimental results in table 1 show that compared with commercially available carbon black pore liquid and graphite black pore liquid, after the black pore liquid of examples 1 to 6 of the present invention is left for one week, the solid content of the upper layer solution is decreased by less than 2%, and the solid content of comparative examples 1 and 2 is decreased by 30% and 52%, respectively, which indicates that the graphene sheet/carbon black composite black pore liquid prepared by the present invention has better stability. After the specimen had been left for 1 week, the results are shown in FIG. 1.
From the experimental results in table 1, it can be seen that compared with commercially available carbon black pore liquid and graphite black pore liquid, the graphene/carbon black composite black pore liquid prepared by the present invention has better conductivity, and for examples 1 to 6, the resistance values of the pores after the black pore formation of the PCB panel are all lower than those of the commercially available products.
As can be seen from fig. 2, it can be seen from the observation of the via holes of the PCB that examples 1-6 can be uniformly absorbed in the via holes, the via holes absorbed in comparative example 1 have partial cracks, and the via holes absorbed in comparative example 2 have obvious phenomena of over-thickness and blockage of the film.
While particular embodiments of the present invention have been illustrated and described, it would be obvious that various other changes and modifications can be made without departing from the spirit and scope of the invention. It is therefore intended to cover in the appended claims all such changes and modifications that are within the scope of this invention.
Claims (10)
1. A graphene sheet/carbon black composite black pore liquid is characterized in that: the graphene sheet/carbon black composite black pore liquid comprises, by weight, 3-8.4 parts of graphene sheets, 1.5-4.5 parts of carbon black, 1.5-3 parts of a surfactant, 1.5-3 parts of a water-based high polymer, 1.5-3 parts of a potassium hydroxide solution and 92.7-97 parts of deionized water.
2. The graphene sheet/carbon black composite black pore liquid according to claim 1, wherein: the number of graphene sheets is less than 8, the thickness of the graphene sheet layer is less than 3nm, and the single-layer rate of the graphene sheet is greater than 80%.
3. The graphene sheet/carbon black composite black pore liquid according to claim 1, wherein: the surfactant is at least one of sodium dodecyl sulfate, nonylphenol polyoxyethylene ether phosphate, sodium dodecyl benzene sulfonate, fatty alcohol polyoxyethylene ether, nonanol polyoxyethylene ether, fatty alcohol polyoxyethylene sulfate and potassium dodecyl phosphate.
4. The graphene sheet/carbon black composite black pore liquid according to claim 1, wherein: the water-based high polymer is at least one of polyethylene glycol, polyvinylpyrrolidone, polyvinyl alcohol, sodium carboxymethyl cellulose, sodium lignosulfonate, polyvinyl alcohol, sodium polyacrylate and polyacrylamide.
5. The graphene sheet/carbon black composite black pore liquid according to claim 1, wherein: the concentration of the potassium hydroxide solution is 40-60 g/L.
6. A preparation method of a graphene sheet/carbon black composite black pore liquid is characterized by comprising the following steps: the method comprises the following steps:
accurately weighing graphene sheets, carbon black, a surfactant, a water-based high polymer, potassium hydroxide and deionized water for later use;
step two, adding the surfactant and the water-based high molecular polymer into water, and stirring and mixing the mixture uniformly at a high speed at a rotating speed of 3000-;
step three, putting the graphene sheets and the carbon black into the mixture A obtained in the step two, and performing ultrasonic treatment for 10-30min to obtain a mixture B;
and step four, performing sanding and high-pressure homogenization treatment on the mixture B obtained in the step three, and then adding a potassium hydroxide solution into the treated mixture B to adjust the pH value to 9-11 to obtain the black pore liquid.
7. The method for preparing the graphene sheet/carbon black composite black pore liquid according to claim 6, wherein the method comprises the following steps: the ultrasonic treatment in the third step specifically comprises the following steps: an ultrasonic frequency electric signal is generated by an ultrasonic generator, the electric signal is converted into mechanical wave with the same frequency by a piezoelectric transducer, the power of the ultrasonic generator is 1500-3000W, the working frequency of the ultrasonic generator is 80-100KHZ, and the working frequency of the transducer is 80KHZ or 100 KHZ.
8. The method for preparing the graphene sheet/carbon black composite black pore liquid according to claim 6, wherein the method comprises the following steps: the rotation speed of the sanding treatment in the fourth step is 500-3000 rpm.
9. The method for preparing the graphene sheet/carbon black composite black pore liquid according to claim 6, wherein the method comprises the following steps: the pressure in the high-pressure homogenization treatment in the fourth step is 80-120 Mpa.
10. The method for preparing the graphene sheet/carbon black composite black pore liquid according to claim 6, wherein the method comprises the following steps: the granularity D90 of the black pore liquid obtained by sanding and high-pressure homogenization treatment in the fourth step is less than 2 mu m.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114245613A (en) * | 2021-11-30 | 2022-03-25 | 武汉格智新材料有限公司 | Carbon black pore solution, preparation method thereof and black pore process |
| CN114466529A (en) * | 2021-12-31 | 2022-05-10 | 广东省科学院化工研究所 | Black hole liquid for electroplating through hole of printed circuit board and preparation method and application thereof |
| CN115594171A (en) * | 2022-07-29 | 2023-01-13 | 广东利尔化学有限公司（Cn） | Carbon pore process nano graphite dispersion liquid and preparation method thereof |
| CN115594171B (en) * | 2022-07-29 | 2024-04-30 | 广东利尔化学有限公司 | Carbon pore process nano graphite dispersion liquid and preparation method thereof |
-
2021
- 2021-06-15 CN CN202110662009.9A patent/CN113421694A/en not_active Withdrawn
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114245613A (en) * | 2021-11-30 | 2022-03-25 | 武汉格智新材料有限公司 | Carbon black pore solution, preparation method thereof and black pore process |
| CN114466529A (en) * | 2021-12-31 | 2022-05-10 | 广东省科学院化工研究所 | Black hole liquid for electroplating through hole of printed circuit board and preparation method and application thereof |
| CN115594171A (en) * | 2022-07-29 | 2023-01-13 | 广东利尔化学有限公司（Cn） | Carbon pore process nano graphite dispersion liquid and preparation method thereof |
| CN115594171B (en) * | 2022-07-29 | 2024-04-30 | 广东利尔化学有限公司 | Carbon pore process nano graphite dispersion liquid and preparation method thereof |
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