CN114023969A - 3D creeper-type high-performance conductive agent and preparation method and application thereof - Google Patents
3D creeper-type high-performance conductive agent and preparation method and application thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 241000219098 Parthenocissus Species 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 14
- 239000007774 positive electrode material Substances 0.000 claims abstract description 13
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 claims abstract description 9
- 241000727913 Parthenocissus tricuspidata Species 0.000 claims abstract description 9
- 229910001416 lithium ion Inorganic materials 0.000 claims abstract description 9
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims abstract description 5
- 229910052744 lithium Inorganic materials 0.000 claims abstract description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 34
- 238000000034 method Methods 0.000 claims description 24
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- 229910052751 metal Inorganic materials 0.000 claims description 10
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- 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
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- 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
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- 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
- H01M10/058—Construction or manufacture
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
-
- 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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
-
- 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
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- 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
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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The invention discloses a 3D creeper-type high-performance conductive agent which comprises a sheet conductive agent, a point conductive agent and a linear conductive agent, wherein the point conductive agent is in the shape of feet of the creeper, the linear conductive agent is in the shape of branch diameters of the creeper, and the sheet conductive agent is in the shape of leaves of the creeper. The invention also provides a preparation method of the 3D boston ivy type high-performance conductive agent and application of the conductive agent in a lithium ion battery. The invention disperses the point conductive agent, the linear conductive agent and the sheet conductive agent in the CMC solution to form the 3D creeper-type high-performance conductive agent, the coexistence symbiosis of the feet, the diameters and the leaves can achieve the point-line-surface synergistic effect, so that a 3D conductive network with stable structure and good conductivity can be formed, and particularly the part conforming to the point conductive agent can obviously improve the low-temperature performance of materials and cells; the conductive agent is less in usage amount, so that the energy density of a single battery cell can be effectively improved, and the positive electrode material, the multiplying power performance and the low-temperature performance of the lithium battery can be improved.
Description
Technical Field
The invention relates to the technical field of lithium ion battery materials, in particular to a 3D creeper-type high-performance conductive agent and a preparation method and application thereof.
Background
With the rapid development of the power lithium battery industry, higher requirements are put forward on the performance of the lithium ion battery anode material and the performance of the finished battery. The gram capacity exertion, rate capability, cycle performance and the like of the material can be improved by adding the conductive agent with excellent conductivity and stable structure in the preparation process of the positive electrode material, and the energy density, rate capability, cycle performance and the like of the battery can be improved by adding the conductive agent with excellent conductivity and stable structure in the preparation process of the battery.
Patent application No. CN201310448084.0 discloses that graphene oxide, a graphene semi-finished product, is mixed with a granular carbon material such as carbon black, and a chemical bond is formed in a graphene precursor through high-temperature heat treatment and weak oxidation treatment, so that the structural stability of the mixed material is improved. However, with the common conductive agent materials (conductive graphite, conductive carbon black, multi-walled carbon nanotubes and vapor grown carbon fibers), even if the usage amount is increased, a more developed and effective conductive network is difficult to form, and the excellent performances of the two novel anode and cathode materials are difficult to be fully exerted. Therefore, it is difficult to find a conductive agent which can form a developed and effective conductive network and has a very small addition amount.
Disclosure of Invention
The technical problem to be solved by the invention is how to realize a conductive agent which can form a developed effective conductive network and has a very small addition amount.
The invention solves the technical problems through the following technical means:
A3D creeper-type high-performance conductive agent comprises a sheet conductive agent, a point conductive agent and a linear conductive agent, wherein the mass ratio of the sheet conductive agent to the linear conductive agent to the point conductive agent is 0.02-0.025:0.07-0.08: 1;
the point-shaped conductive agent is in the shape of feet of the parthenocissus tricuspidata, the linear conductive agent is in the shape of branch diameters of the parthenocissus tricuspidata, and the sheet conductive agent is in the shape of leaves of the parthenocissus tricuspidata; the point-shaped conductive agent, the linear conductive agent and the sheet-shaped conductive agent are dispersed in the CMC solution to form the 3D creeper-type high-performance conductive agent.
The invention forms a 3D creeper-type high-performance conductive agent by dispersing a point conductive agent, a linear conductive agent and a sheet conductive agent in a CMC solution, wherein the point conductive agent is in the shape of feet of the creeper, the linear conductive agent is in the shape of branch diameters of the creeper, and the sheet conductive agent is in the shape of leaves of the creeper, and the coexistence of the feet, the diameters and the leaves achieves the point-line-surface synergistic effect, so that a 3D conductive network with stable structure and good conductivity is formed, and particularly the low-temperature performance of materials and a battery cell can be obviously improved according to the point conductive agent part; the conductive agent is less in usage amount, so that the energy density of a single battery cell can be effectively improved, and the positive electrode material, the multiplying power performance and the low-temperature performance of the lithium battery can be improved.
Preferably, the dot-shaped conductive agent comprises SP @ TiN, 350G @ TiN, Ks-6@ TiN, Ks-15@ TiN, MCMB @ TiN, Ketjenblack @ TiN or AB @ TiN.
Preferably, the linear conductive agent includes CNTs metal nanowire, VGCF metal nanowire, Ni metal nanowire, Pt metal nanowire or Au metal nanowire.
Preferably, the sheet-like conductive agent includes graphene, nitrogen-doped graphene, boron-nitrogen co-doped graphene, reduced graphene oxide, carboxylated graphene, hydroxylated graphene or aminated graphene.
The invention also provides a preparation method of the 3D creeper-type high-performance conductive agent, which comprises the following steps: dispersing a sheet conductive agent, a point conductive agent and a linear conductive agent in a CMC solution with the concentration of 3-8% according to the proportion, and performing ultrasonic stirring treatment to form uniformly dispersed conductive slurry; wherein the temperature of ultrasonic stirring is 25-35 ℃, the time of ultrasonic stirring is 1-3h, and the speed of ultrasonic stirring is 500-1200 r/min.
A lithium ion battery comprises a positive pole piece, a negative pole piece, electrolyte, a diaphragm and a shell; the positive electrode piece comprises the 3D partridge type high-performance conductive agent according to claim 1; the negative electrode tab comprises the 3D partridge type high-performance conductive agent of claim 1.
Further, the positive pole piece also comprises an LFP positive pole material and PVDF.
Further, the preparation method of the positive pole piece comprises the following steps: mixing the 3D parthenocissus tricuspidata type conductive agent, an LFP positive electrode material and PVDF according to the mass ratio of 0.8:98:1.2 to prepare slurry, and then sequentially performing coating, rolling and sheet-making processes on the slurry to prepare the positive electrode sheet.
Further, the negative pole piece also comprises a graphite negative pole material, SBR and CMC.
Further, the preparation method of the negative pole piece comprises the following steps: mixing the 3D creeper type with a graphite negative electrode material, SBR and CMC to prepare slurry according to a mass ratio of 0.5:96.8:1.5:1.2, and then sequentially carrying out coating, rolling and sheet-making on the slurry to prepare a negative electrode sheet.
The invention has the following beneficial effects: the invention forms a 3D creeper-type high-performance conductive agent by dispersing a point conductive agent, a linear conductive agent and a sheet conductive agent in a CMC solution, wherein the point conductive agent is in the shape of feet of the creeper, the linear conductive agent is in the shape of branch diameters of the creeper, and the sheet conductive agent is in the shape of leaves of the creeper, and the coexistence of the feet, the diameters and the leaves achieves the point-line-surface synergistic effect, so that a 3D conductive network with stable structure and good conductivity is formed, and particularly the low-temperature performance of materials and a battery cell can be obviously improved according to the point conductive agent part; the conductive agent is less in usage amount, so that the energy density of a single battery cell can be effectively improved, and the positive electrode material, the multiplying power performance and the low-temperature performance of the lithium battery can be improved.
Drawings
Fig. 1 is a schematic diagram of a 3D parthenocissus type high performance conductive agent according to an embodiment of the present invention;
fig. 2 is an SEM image of the 3D parthenocissus type conductive agent prepared in example 1 of the present invention applied to a slurry mixing process in the preparation of an LFP positive electrode material battery.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings and the embodiments of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Test materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
The specific techniques or conditions not specified in the examples can be performed according to the techniques or conditions described in the literature in the field or according to the product specification.
Example 1
Dispersing 1000g of SP @ TiN, 70g of CNTs and 20g of graphene in a 3% CMC solution, and ultrasonically stirring for 3 hours at the temperature of 25 ℃ at 500r/min to form uniformly dispersed conductive slurry; then taking the slurry to perform SEM characterization observation and comparing with the figure 1, and observing that the dispersion states of SP @ TiN, CNTs and Graphene are similar to the 'foot diameter leaf' at the lower right corner of the figure 1, namely forming the 3D creeper-tiger type conductive agent with stable structure and good conductivity; the prepared 3D parthenocissus tricuspidata-type conductive agent, an LFP positive electrode material and PVDF are processed according to the mass ratio of 0.8:98:1.2 to prepare a positive electrode piece through the procedures of coating, rolling, flaking and the like, and the prepared 3D parthenocissus tricuspidata-type graphite negative electrode material, SBR and CMC are processed according to the mass ratio of 0.5:96.8:1.5:1.2 to prepare a negative electrode piece through the procedures of coating, rolling, flaking and the like; the positive and negative pole pieces are processed by the procedures of assembly, liquid injection, formation, capacity grading and the like to obtain the finished battery.
Example 2
Dispersing 1000G of 350G @ TiN, 75G of VGCF and 23G of graphene in a 3.5% CMC solution, and ultrasonically stirring at the temperature of 28 ℃ for 2.5 hours at the speed of 800r/min to form uniformly dispersed conductive slurry, namely the 3D creeper-type conductive agent; the prepared 3D parthenocissus tricuspidata-type conductive agent, an LFP positive electrode material and PVDF are processed according to the mass ratio of 0.8:98:1.2 to prepare a positive electrode piece through the procedures of coating, rolling, flaking and the like, and the prepared 3D parthenocissus tricuspidata-type graphite negative electrode material, SBR and CMC are processed according to the mass ratio of 0.5:96.8:1.5:1.2 to prepare a negative electrode piece through the procedures of coating, rolling, flaking and the like; the positive and negative pole pieces are processed by the procedures of assembly, liquid injection, formation, capacity grading and the like to obtain the finished battery.
Example 3
Dispersing 1000g of AB @ TiN, 77g of VGCF and 20g of nitrogen-doped graphene in a 5% CMC solution, and ultrasonically stirring for 2 hours at 30 ℃ at 1000r/min to form uniformly dispersed conductive slurry, namely the 3D creeper-tiger-type conductive agent; the prepared 3D parthenocissus tricuspidata-type conductive agent, an LFP positive electrode material and PVDF are subjected to pulping according to the mass ratio of 0.8:98:1.2, then a positive electrode piece is prepared by processing through the working procedures of coating, rolling, tabletting and the like, and meanwhile, the prepared 3D parthenocissus tricuspidata-type graphite negative electrode material, SBR and CMC are subjected to pulping according to the mass ratio of 0.5:96.8:1.5:1.2, and then the negative electrode piece is prepared by processing through the working procedures of coating, rolling, tabletting and the like; the positive and negative pole pieces are processed by the procedures of assembly, liquid injection, formation, capacity grading and the like to obtain the finished battery.
Example 4
Dispersing 1000g of MCMB @ TiN, 80g of Ni nanowires and 25g of nitrogen-doped graphene in 6% CMC solution, and ultrasonically stirring at the temperature of 33 ℃ for 1.5h at 1100r/min to form uniformly dispersed conductive slurry, namely the 3D creeper-tiger-type conductive agent; the prepared 3D parthenocissus tricuspidata-type conductive agent, an LFP positive electrode material and PVDF are processed according to the mass ratio of 0.8:98:1.2 to prepare a positive electrode piece through the procedures of coating, rolling, flaking and the like, and the prepared 3D parthenocissus tricuspidata-type graphite negative electrode material, SBR and CMC are processed according to the mass ratio of 0.5:96.8:1.5:1.2 to prepare a negative electrode piece through the procedures of coating, rolling, flaking and the like; the positive and negative pole pieces are processed by the procedures of assembly, liquid injection, formation, capacity grading and the like to obtain the finished battery.
Example 5
Dispersing 1000g of SP @ TiN, 75g of CNTs and 22g of boron-nitrogen co-doped graphene in 8% CMC solution, and ultrasonically stirring for 1h at the temperature of 27 ℃ at 1200r/min to form uniformly dispersed conductive slurry, namely the 3D creeper-tiger type conductive agent; mixing the prepared 3D boswellia creeper-type conductive agent, an LFP positive electrode material and PVDF according to a ratio of 0.8:98: pulping by the mass ratio of 1.2, then processing by the working procedures of coating, rolling, tabletting and the like to prepare a positive pole piece, and simultaneously pulping the prepared 3D partridge lizard type and graphite negative pole material, SBR and CMC according to the mass ratio of 0.5:96.8:1.5:1.2, then processing by the working procedures of coating, rolling, tabletting and the like to prepare a negative pole piece; the positive and negative pole pieces are processed by the procedures of assembly, liquid injection, formation, capacity grading and the like to obtain the finished battery.
Comparative example
Pulping common conductive agent SP, LFP positive electrode material and PVDF according to the mass ratio of 1.5:97:1.5, then processing the materials by coating, rolling, flaking and other procedures to prepare a positive electrode piece, and simultaneously mixing the common conductive agent SP, graphite negative electrode material, SBR and CMC according to the mass ratio of 1:96: 1.8: pulping by the mass ratio of 1.2, and then processing by the working procedures of coating, rolling, tabletting and the like to obtain a negative pole piece; the positive and negative pole pieces are processed by the procedures of assembly, liquid injection, formation, capacity grading and the like to obtain the finished battery.
Battery performance testing
The finished batteries prepared in examples 1 to 5 and comparative example are subjected to performance tests, and the results are shown in table 1, and it can be seen that under the same system and the same preparation conditions, the 3C and 5C rate discharge capacity retention rates of LFP batteries prepared by using a common conductive agent are 85.3 and 72.6%, respectively, the low-temperature discharge capacity retention rate at-20 ℃ is only 62.2%, and the energy density of a single battery is 182.4 Wh/kg; the mean values of the rate discharge capacity retention rates of 3C and 5C LFP batteries prepared by using the 3D parthenocissus type conductive agent are 96.42% and 89.66%, the low-temperature discharge capacity retention rate at-20 ℃ is only 83.86%, the energy density of a single battery reaches 213.94Wh/kg, and the LFP battery shows excellent rate performance, low-temperature performance and higher energy density.
Table 1 shows the results of the battery performance test
The above examples are only intended to illustrate the technical solution of the present invention, but not to limit it; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The utility model provides a 3D creeper type high performance conductive agent which characterized in that: the conductive paste comprises a sheet conductive agent, a point conductive agent and a linear conductive agent, wherein the mass ratio of the sheet conductive agent to the linear conductive agent to the point conductive agent is 0.02-0.025:0.07-0.08: 1;
the point-shaped conductive agent is in the shape of feet of the parthenocissus tricuspidata, the linear conductive agent is in the shape of branch diameters of the parthenocissus tricuspidata, and the sheet conductive agent is in the shape of leaves of the parthenocissus tricuspidata; the point-shaped conductive agent, the linear conductive agent and the sheet-shaped conductive agent are dispersed in the CMC solution to form the 3D creeper-type high-performance conductive agent.
2. The 3D parthenocissus tricuspidata-type high-performance conductive agent according to claim 1, wherein: the dotted conductive agent comprises SP @ TiN, 350G @ TiN, Ks-6@ TiN, Ks-15@ TiN, MCMB @ TiN, Ketjenblack @ TiN or AB @ TiN.
3. The 3D parthenocissus tricuspidata-type high-performance conductive agent according to claim 1, wherein: the linear conductive agent comprises CNTs metal nanowires, VGCF metal nanowires, Ni metal nanowires, Pt metal nanowires or Au metal nanowires.
4. The 3D parthenocissus tricuspidata-type high-performance conductive agent according to claim 1, wherein: the sheet conductive agent comprises graphene, nitrogen-doped graphene, boron-nitrogen co-doped graphene, reduced graphene oxide, carboxylated graphene, hydroxylated graphene or aminated graphene.
5. The method for preparing the 3D parthenocissus tricuspidata-type high-performance conductive agent according to claim 1, comprising the steps of: dispersing a sheet conductive agent, a point conductive agent and a linear conductive agent in a CMC solution with the concentration of 3-8% according to the proportion, and performing ultrasonic stirring treatment to form uniformly dispersed conductive slurry; wherein the temperature of ultrasonic stirring is 25-35 ℃, the time of ultrasonic stirring is 1-3h, and the speed of ultrasonic stirring is 500-1200 r/min.
6. A lithium ion battery, characterized by: the lithium battery comprises a positive pole piece, a negative pole piece, electrolyte, a diaphragm and a shell; the positive electrode piece comprises the 3D partridge type high-performance conductive agent according to claim 1; the negative electrode tab comprises the 3D partridge type high-performance conductive agent of claim 1.
7. The lithium ion battery of claim 6, wherein: the positive pole piece also comprises an LFP positive pole material and PVDF.
8. The lithium ion battery of claim 7, wherein: the preparation method of the positive pole piece comprises the following steps: mixing the 3D parthenocissus tricuspidata type conductive agent, an LFP positive electrode material and PVDF according to the mass ratio of 0.8:98:1.2 to prepare slurry, and then sequentially performing coating, rolling and sheet-making processes on the slurry to prepare the positive electrode sheet.
9. The lithium ion battery of claim 6, wherein: the negative pole piece also comprises a graphite negative pole material, SBR and CMC.
10. The lithium ion battery of claim 9, wherein: the preparation method of the negative pole piece comprises the following steps: mixing the 3D creeper type with a graphite negative electrode material, SBR and CMC to prepare slurry according to a mass ratio of 0.5:96.8:1.5:1.2, and then sequentially carrying out coating, rolling and sheet-making on the slurry to prepare a negative electrode sheet.
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