CN114937530A - Method for reducing viscosity of carbon fiber conductive slurry - Google Patents
Method for reducing viscosity of carbon fiber conductive slurry Download PDFInfo
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- CN114937530A CN114937530A CN202210704733.8A CN202210704733A CN114937530A CN 114937530 A CN114937530 A CN 114937530A CN 202210704733 A CN202210704733 A CN 202210704733A CN 114937530 A CN114937530 A CN 114937530A
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- 239000002002 slurry Substances 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 21
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 15
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 15
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 15
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 53
- 239000002041 carbon nanotube Substances 0.000 claims abstract description 47
- 229910021393 carbon nanotube Inorganic materials 0.000 claims abstract description 45
- 239000006185 dispersion Substances 0.000 claims abstract description 31
- 238000000227 grinding Methods 0.000 claims abstract description 29
- 238000009489 vacuum treatment Methods 0.000 claims abstract description 12
- 238000002360 preparation method Methods 0.000 claims abstract description 7
- 238000003825 pressing Methods 0.000 claims abstract description 7
- 238000005096 rolling process Methods 0.000 claims abstract description 5
- MCMNRKCIXSYSNV-UHFFFAOYSA-N Zirconium dioxide Chemical compound O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 claims description 32
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 16
- 239000000498 cooling water Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 9
- 239000004576 sand Substances 0.000 claims description 8
- 229920002134 Carboxymethyl cellulose Polymers 0.000 claims description 6
- 239000001768 carboxy methyl cellulose Substances 0.000 claims description 6
- 235000010948 carboxy methyl cellulose Nutrition 0.000 claims description 6
- 239000008112 carboxymethyl-cellulose Substances 0.000 claims description 6
- 239000003638 chemical reducing agent Substances 0.000 claims description 6
- 238000004140 cleaning Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 6
- 239000002270 dispersing agent Substances 0.000 claims description 4
- 230000007547 defect Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 abstract description 2
- 239000007787 solid Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 11
- 229910052799 carbon Inorganic materials 0.000 description 7
- 230000004048 modification Effects 0.000 description 7
- 238000012986 modification Methods 0.000 description 7
- 238000005303 weighing Methods 0.000 description 7
- 239000000047 product Substances 0.000 description 6
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 5
- 229910052744 lithium Inorganic materials 0.000 description 5
- 238000002156 mixing Methods 0.000 description 5
- 230000006872 improvement Effects 0.000 description 3
- 238000011085 pressure filtration Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000006258 conductive agent Substances 0.000 description 2
- 239000008188 pellet Substances 0.000 description 2
- 238000005086 pumping Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 230000004075 alteration Effects 0.000 description 1
- 239000006256 anode slurry Substances 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
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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
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- 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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a method for reducing the viscosity of carbon fiber conductive slurry, which comprises the steps of equipment preparation, carbon nanotube pretreatment, pre-dispersion treatment, vacuum treatment, grinding and filter pressing. According to the invention, the carbon nano tube is formed into a compacted solid shape through multiple times of rolling by the roller press, so that defects can be effectively formed on the carbon nano tube, and the specific surface area of the carbon nano tube is reduced; the vacuum treatment can remove its internal gases. The invention can fundamentally solve the problems that the carbon nano tube slurry has large viscosity and is difficult to disperse, and the carbon nano tube slurry with high specific surface area can not be applied to market.
Description
Technical Field
The invention relates to the technical field of carbon nanotubes, in particular to a method for reducing the viscosity of carbon fiber conductive slurry.
Background
In recent years, with the increasing influence of fossil energy on the global environment, clean energy is being widely used as a substitute, and a new energy battery as a main component of the clean energy is gradually becoming a first choice for storing electric energy in the fields of passenger cars, buses, energy storage and the like.
In the field of lithium batteries, carbon nanotubes are widely used by lithium battery manufacturers as a novel conductive agent by virtue of excellent conductivity, and are used for improving the energy density and the cycle life of lithium batteries. With the rapid development of new energy automobiles and the improvement of energy density of power lithium batteries, the replacement of traditional conductive agents by products is accelerated, and the demand of carbon nano tube conductive slurry products is certainly increased at a high speed.
The existing carbon nano tube conductive slurry has the problem of overlarge viscosity, and the slurry mixing viscosity of a lithium battery in the anode slurry mixing process and the viscosity of slurry transportation are directly influenced. The properties of the carbon nanotube height ratio table directly determine the slurry viscosity. At present, other carbon substances (SP and graphite) are mainly added in the market to solve the viscosity problem, but the method can cause impurity carbon to be added in the slurry, so that the conductivity of the slurry is influenced, and the viscosity problem of the pure carbon tube slurry cannot be solved in the prior art.
Disclosure of Invention
The invention aims to overcome the problems and provides a method for reducing the viscosity of carbon fiber conductive paste. In order to achieve the purpose, the invention adopts the following technical scheme:
a method for reducing the viscosity of carbon fiber conductive paste comprises the following steps:
s1. equipment preparation
Preparing a sand grinding tank and zirconia balls, cleaning and drying; placing the sanding tank and the stirring paddle, connecting a cooling water pipeline, and turning on a cooling water switch;
s2, pretreating the carbon nano tube
Introducing Carbon Nanotubes (CNTs) into a roller press, and performing rolling treatment;
s3, pre-dispersion treatment
Adding the rolled CNT into a sanding tank, and then adding N-methyl pyrrolidone (NMP) into the CNT and NMP according to the ratio of 1: 5; covering the cover of the sanding tank, and installing a high-speed dispersion disc for dispersion treatment;
s4, vacuum treatment
After dispersion, putting the tank body and the content thereof into a vacuum oven for vacuum treatment, wherein the vacuum degree of vacuumizing is less than 1 kpa;
s5, grinding
After the vacuum treatment is finished, adding the zirconia balls into a sanding tank, and additionally adding NMP, a dispersing agent and a viscosity reducer; then grinding treatment is carried out;
s6, filter pressing
After the grinding treatment, taking out the obtained slurry, and adding N 2 And (5) performing filter pressing to obtain the finished product of the conductive slurry.
As a modification, the diameter of the zirconia pellets in the step S5 is 0.8mm, and the amount of the zirconia pellets is 90-100 times the weight of the CNT.
As a modification, NMP additionally added in the S5 step was used in an amount of 18.75 times the weight of the CNTs; the amount of dispersant used was 18.75% by weight of the CNTs; the viscosity reducer is 6.25% of the weight of the CNT.
In the improvement, the dispersion in the step S5 is one or more of PVP, NCM and LB132, and the viscosity reducer is carboxymethyl cellulose.
As a modification, the S2 step rolls the CNTs multiple times using a roll press.
As a modification, the rotation speed of the dispersion treatment sand mill in the step S3 is 3000-4000rpm/min, and the dispersion time is 60 min.
As an improvement, the rotation speed of the grinding in the step S5 is 1000-1500rpm/min, and the grinding time is 4-6 hours.
As a modification, the sanding tank is subjected to the sealing process in the steps S3 and S5.
The invention has the advantages that:
the root cause of the inability of the current market conductive slurry polishing systems to reduce the viscosity of carbon nanotube slurry is the high specific surface area characteristic of carbon nanotubes. According to the invention, the carbon nano tube is formed into a compacted solid shape through multiple times of rolling by the roller press, so that defects can be effectively formed on the carbon nano tube, and the specific surface area of the carbon nano tube is reduced; the vacuum treatment can remove its internal gases. The invention can fundamentally solve the problems that the carbon nano tube slurry has large viscosity and is difficult to disperse, and the carbon nano tube slurry with high specific surface area can not be applied to market.
Drawings
FIG. 1 is a morphology of a conductive paste prepared in example 1;
FIG. 2 is a shape of the carbon nanotube of example 1 after being rolled;
fig. 3 is a morphology of the conductive paste prepared in comparative example 1;
fig. 4 is a morphology of the conductive paste prepared in comparative example 2;
fig. 5 shows the morphology of the conductive paste prepared in comparative example 3.
Detailed Description
The present invention will be described in detail and specifically by the following examples so as to better understand the present invention, but the following examples do not limit the scope of the present invention.
Example 1
The embodiment discloses a method for reducing the viscosity of carbon fiber conductive paste, which comprises the following steps:
s1. equipment preparation
Preparing a sand grinding tank and zirconia balls, cleaning and drying; placing the sanding tank and the stirring paddle, connecting a cooling water pipeline, and turning on a cooling water switch;
s2, pretreating the carbon nano tube
Introducing Carbon Nanotubes (CNT) into a roller press, and repeatedly rolling for 5 times;
s3, pre-dispersion treatment
Accurately weighing 16g of the milled CNTs into a sanding jar and adding 80g of n-methylpyrrolidone (NMP); covering the cover of the sanding tank, and installing a high-speed dispersion disc for dispersion treatment; the rotation speed of the sand mill for dispersion treatment is 4000rpm/min, and the dispersion time is 60 min.
S4, vacuum treatment
After the dispersion is finished, putting the tank body and the content thereof into a vacuum oven for vacuum treatment, wherein the vacuum degree of vacuum pumping is less than 1kpa, and the vacuum pumping time is 30 min;
s5, grinding
After the vacuum treatment, 1.5kg of zirconia balls (diameter 0.8mm) were added into the sanding tank, and 300g of NMP, 3g of PVP and 1g of carboxymethylcellulose were additionally added; then grinding treatment is carried out; the rotation speed of the grinding is 1000-;
s6, filter pressing
After the grinding treatment, taking out the obtained slurry, and adding N 2 And (5) performing filter pressing to obtain the finished product of the conductive slurry.
This embodiment performs the sealing process for the sanding tank in steps S3 and S5.
Comparative example 1
The preparation method of the comparative example includes the following steps:
1. preparing a sanding tank and zirconia balls, cleaning and drying; placing the sanding tank and the stirring paddle, connecting a cooling water pipeline, and turning on a cooling water switch;
2. accurately weighing 16g of ordinary untreated CNT, 3g of PVP and 1g of carboxymethyl cellulose, uniformly mixing, adding into a sanding tank, accurately weighing 380g of NMP, adding into the sanding tank for dispersion treatment, wherein the rotation speed of a dispersion treatment sanding machine is 1500rpm/min, and the stirring time is 5 min;
3. after the dispersion is finished, adding 1.5kg of zirconia balls (the diameter is 0.8mm), and grinding for 4 hours at the rotating speed of 4000 rpm/min;
4. and after the grinding treatment is finished, taking out the obtained slurry, and performing pressure filtration by using N2 to obtain the finished product conductive slurry.
Comparative example 2
The preparation method of the comparative example includes the following steps:
1. preparing a sanding tank and zirconia balls, cleaning and drying; placing the sanding tank and the stirring paddle, connecting a cooling water pipeline, and turning on a cooling water switch;
2. accurately weighing ordinary 12g of untreated CNT, 4gSP, 3g of PVP and 1g of carboxymethyl cellulose, uniformly mixing, adding into a sanding tank, accurately weighing 380g of NMP, adding into the sanding tank for dispersion treatment, wherein the rotation speed of a dispersion treatment sanding machine is 1500rpm/min, and stirring time is 5 min;
3. after the dispersion is finished, adding 1.5kg of zirconia balls (the diameter is 0.8mm), and grinding for 4 hours at the rotating speed of 4000 rpm/min;
4. and after the grinding treatment is finished, taking out the obtained slurry, and performing pressure filtration by using N2 to obtain the finished product conductive slurry.
Comparative example 3
The preparation method of the comparative example includes the following steps:
1. preparing a sand grinding tank and zirconia balls, cleaning and drying; placing a sanding tank and a stirring paddle, connecting a cooling water pipeline, and turning on a cooling water switch;
2. accurately weighing ordinary 12g of unprocessed CNT, 3g of PVP and 1g of carboxymethyl cellulose, uniformly mixing, adding into a sanding tank, accurately weighing 384g of NMP, adding into the sanding tank for dispersion treatment, wherein the rotation speed of a dispersion treatment sanding machine is 1500rpm/min, and the stirring time is 5 min;
3. after the dispersion is finished, adding 1.5kg of zirconia balls (the diameter is 0.8mm), and grinding for 4 hours at the rotating speed of 4000 rpm/min;
4. and after the grinding treatment is finished, taking out the obtained slurry, and performing pressure filtration by using N2 to obtain the finished product conductive slurry.
The results of the experiment are shown in the following table:
the conductive slurry is prepared by adopting the method in the embodiment 1, and the conductive slurry is prepared by adopting direct grinding, grinding after replacing a carbon source and grinding after reducing the carbon content in the comparative examples 1, 2 and 3 respectively. It can be seen that the discharge viscosity of the slurry of example 1 is significantly reduced compared to the slurries of comparative examples 1, 2 and 3.
As can be seen from fig. 1, in the conductive paste prepared by using the present invention, the carbon nanotubes are uniformly distributed and distributed in a relatively spread state in the paste, and the carbon nanotubes are mutually hooked to each other to maintain good stability and conductivity, and the paste can maintain a long-term dispersion state when standing.
As can be seen from fig. 3, the conductive paste prepared by the direct refining method has carbon nanotubes wound into a ball shape inside, and different carbon nanotubes are entangled with each other, resulting in a high viscosity. As shown in fig. 4 and 5, although the viscosity of the slurry can be reduced to some extent by adding an additional carbon source or reducing the carbon content, the carbon nanotubes inside the slurry are not uniformly distributed, and a problem that the carbon nanotubes are not present in a part of the carbon nanotubes occurs, resulting in a decrease in the conductivity and stability of the slurry.
In summary, example 1 has significant technical advantages over conventional methods.
The embodiments of the present invention have been described in detail above, but they are merely exemplary, and the present invention is not equivalent to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, it is intended that all equivalent alterations and modifications be included within the scope of the invention, without departing from the spirit and scope of the invention.
Claims (8)
1. A method for reducing the viscosity of carbon fiber conductive slurry is characterized by comprising the following steps:
s1. equipment preparation
Preparing a sand grinding tank and zirconia balls, cleaning and drying; placing the sanding tank and the stirring paddle, connecting a cooling water pipeline, and turning on a cooling water switch;
s2, pretreating the carbon nano tube
Introducing Carbon Nanotubes (CNTs) into a roller press for rolling treatment;
s3, pre-dispersion treatment
Adding the rolled CNT into a sanding tank, and then adding N-methylpyrrolidone (NMP) into the CNT and NMP according to the ratio of 1: 5; covering the cover of the sanding tank, and installing a high-speed dispersion disc for dispersion treatment;
s4, vacuum treatment
After the dispersion is finished, putting the tank body and the content thereof into a vacuum oven for vacuum treatment, wherein the vacuum degree of vacuumizing is less than 1 kpa;
s5, grinding
After the vacuum treatment is finished, adding the zirconia balls into the sand grinding tank, and additionally adding NMP, a dispersing agent and a viscosity reducer; then grinding treatment is carried out;
s6, filter pressing
After the grinding treatment, taking out the obtained slurry, and adding N 2 And (5) performing filter pressing to obtain the finished product of the conductive slurry.
2. The method for reducing the viscosity of carbon fiber conductive paste according to claim 1, wherein the diameter of the zirconia balls in the step of S5 is 0.8mm, and the amount of the zirconia balls is 90-100 times the weight of the CNTs.
3. The method for reducing the viscosity of carbon fiber conductive paste according to claim 1, wherein the amount of NMP additionally added in the step of S5 is 18.75 times the weight of the CNT; the amount of dispersant used was 18.75% by weight of the CNTs; the viscosity reducer is 6.25% of the weight of the CNT.
4. The method for reducing the viscosity of the carbon fiber conductive paste according to claim 1, wherein the dispersion in the step of S5 is one or more of PVP, NCM and LB132, and the viscosity reducer is carboxymethyl cellulose.
5. The method for reducing the viscosity of the carbon fiber conductive paste according to claim 1, wherein the step S2 rolls the CNTs a plurality of times using a roll press.
6. The method for reducing the viscosity of the carbon fiber conductive paste as claimed in claim 1, wherein the rotation speed of the dispersion treatment sand mill of the step S3 is 3000-4000rpm/min, and the dispersion time is 60 min.
7. The method for reducing the viscosity of the carbon fiber conductive paste as claimed in claim 1, wherein the rotation speed of the grinding in the step S5 is 1000-1500rpm/min, and the grinding time is 4-6 hours.
8. The method for reducing the viscosity of carbon fiber conductive paste according to claim 1, wherein the sanding tank is sealed in steps S3 and S5.
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