CN112635741A - Emulsified asphalt coated silicon-carbon negative electrode material and preparation method thereof - Google Patents

Emulsified asphalt coated silicon-carbon negative electrode material and preparation method thereof Download PDF

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Publication number
CN112635741A
CN112635741A CN202011589174.8A CN202011589174A CN112635741A CN 112635741 A CN112635741 A CN 112635741A CN 202011589174 A CN202011589174 A CN 202011589174A CN 112635741 A CN112635741 A CN 112635741A
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preparation
negative electrode
electrode material
emulsified asphalt
carbon negative
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施中新
胡胜初
张凯铭
圣开光
崔阳明
高鲲鹏
段永龙
蒋元旦
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Huhuang New Material Technology Group Co ltd
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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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • H01M2004/027—Negative 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

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
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  • Nanotechnology (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • General Physics & Mathematics (AREA)
  • Condensed Matter Physics & Semiconductors (AREA)
  • Physics & Mathematics (AREA)
  • Manufacturing & Machinery (AREA)
  • Inorganic Chemistry (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides an emulsified asphalt coated silicon carbon negative electrode material which comprises, by mass, 90% -95% of emulsified asphalt, 1% -2% of nano silicon powder and 3% -9% of graphite. The emulsified asphalt coated silicon-carbon negative electrode material disclosed by the invention is simple in preparation process, easy to obtain raw materials, convenient to popularize and popularize, environment-friendly, excellent in electrical performance of a formed battery, and capable of reaching 1850mAh/g in specific discharge capacity for the first time, and after the emulsified asphalt is adopted, the mixing uniformity of asphalt, graphite and silicon is improved, and the cycle life of the battery is prolonged.

Description

Emulsified asphalt coated silicon-carbon negative electrode material and preparation method thereof
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to an emulsified asphalt coated silicon-carbon negative electrode material and a preparation method thereof.
Background
Lithium ion batteries play an irreplaceable role in the field of new energy due to their excellent performance. With the rapid development of smart phones, tablet computers, electric vehicles and the like in recent years, the demand of lithium ion batteries is on a rising trend, a negative electrode material is one of indispensable components in the lithium ion batteries and has very important influence on the performance of the batteries, the application of a carbon negative electrode material in the aspect of commercial electronic products is very wide, but the carbon negative electrode material has the defects of low actual specific capacity, large first irreversible capacity, poor rate capability and the like, the further development of the carbon negative electrode material is hindered, a certain amount of silicon is doped or embedded in the carbon negative electrode material to form a C/Si composite negative electrode material, the specific capacity of the carbon negative electrode material can be effectively improved, and more research results and application effects show that whether the carbon and the silicon can form a compact binary system or not has a key effect on the stability and the electrical performance of the C/Si composite negative electrode material, this aspect of research has therefore attracted the attention of researchers both overseas and overseas.
Asphalt is a mixture with a very complex structure and components, but has good cohesiveness, so that the asphalt has wide application in many fields, and with the development of new energy industry, researchers try to apply asphalt materials to the fields of lithium ion battery cathodes and the like; for example: chinese patent zl201610164454.b discloses a method for preparing a lithium ion battery anode material by using sulfonated asphalt and graphite; chinese patent ZL201611190965.7 discloses a method for preparing asphalt for lithium ion batteries; in addition, in recent years, it has been reported that asphalt is used as a binder to coat a C/Si composite anode material for improving the stability and electrical properties of the anode material. However, in the current technology, asphalt powder is usually used as a medium to coat the C/Si composite negative electrode material, and in this way, the asphalt powder, graphite and silicon are difficult to be mixed uniformly, the adhesion effect of asphalt is poor, and the stability of the C/Si composite negative electrode material is difficult to be improved obviously.
Disclosure of Invention
The invention aims to overcome and supplement the defects in the prior art, and provides an emulsified asphalt coated silicon-carbon negative electrode material and a preparation method thereof, so that the coating effect of the C/Si composite negative electrode material is improved, and the electrical property of a battery is improved. The technical scheme adopted by the invention is as follows:
an emulsified asphalt coated silicon carbon negative electrode material, wherein: comprises 90-95% of emulsified asphalt, 1-2% of nano silicon powder and 3-9% of graphite by mass percent.
A preparation method of an emulsified asphalt coated silicon-carbon negative electrode material comprises the following steps: the method comprises the following steps:
s1, heating and melting asphalt, controlling the temperature to be 130-150 ℃, adding the polyisobutylene succinic anhydride derivative into the asphalt, uniformly stirring, dissolving the surfactant in water at the temperature of 80-90 ℃, then pouring the asphalt solution into the water, and stirring to form emulsified asphalt;
s2, mixing emulsified asphalt, nano silicon powder and graphite in a colloid mill for 6-8 hours to obtain a mixture, and then performing spray drying on the mixture to obtain mixed powder;
and S3, sintering the mixed powder at 800-1200 ℃, and cooling to form the emulsified asphalt coated silicon carbon negative electrode material.
Preferably, the preparation method of the emulsified asphalt coated silicon carbon negative electrode material comprises the following steps: the asphalt of the step S1 is coal-made asphalt or petroleum asphalt.
Preferably, the preparation method of the emulsified asphalt coated silicon carbon negative electrode material comprises the following steps: the polyisobutylene succinic anhydride derivative obtained in the step S1 is one or a mixture of polyisobutylene succinimide, polyisobutylene succinic anhydride-urea and polyisobutylene succinic anhydride-ethanolamine.
Preferably, the preparation method of the emulsified asphalt coated silicon carbon negative electrode material comprises the following steps: the surfactant of step S1 includes a first surfactant and a second surfactant, the first surfactant is selected from one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate, and the second surfactant is tween 80.
Preferably, the preparation method of the emulsified asphalt coated silicon carbon negative electrode material comprises the following steps: the mass ratio of the first surfactant to the second surfactant is 1: 3-4.
Preferably, the preparation method of the emulsified asphalt coated silicon carbon negative electrode material comprises the following steps: the particle size of the nano silicon powder in the step S2 is 10-100 nm.
Preferably, the preparation method of the emulsified asphalt coated silicon carbon negative electrode material comprises the following steps: the graphite of the step S2 is any one of artificial graphite and natural graphite.
Preferably, the preparation method of the emulsified asphalt coated silicon carbon negative electrode material comprises the following steps: the emulsified asphalt comprises the following components in percentage by mass: 50-70% of asphalt, 1-2% of polyisobutylene succinic anhydride derivative, 1-2% of surfactant and the balance of water, wherein the total amount is 100%.
The invention has the advantages that: the emulsified asphalt coated silicon-carbon negative electrode material disclosed by the invention is simple in preparation process, easy to obtain raw materials, convenient to popularize and popularize, environment-friendly, excellent in electrical performance of a formed battery, and capable of reaching 1850mAh/g in specific discharge capacity for the first time, and after the emulsified asphalt is adopted, the mixing uniformity of asphalt, graphite and silicon is improved, and the cycle life of the battery is prolonged.
Detailed Description
The present invention will be further described with reference to the following specific examples.
Example 1
A preparation method of an emulsified asphalt coated silicon carbon negative electrode material comprises the following steps:
heating 5kg of coal tar pitch to melt, controlling the temperature and keeping the temperature at 130 ℃, adding 100g of polyisobutylene succinimide into the coal tar pitch, stirring uniformly, adding 40g of sodium dodecyl sulfate and 160g of tween 80 into 4.7kg of water to form a water phase, and keeping the temperature at 80 ℃ for later use; slowly adding asphalt into a water phase, stirring and shearing through an emulsifier to form emulsified asphalt, then mixing 9kg of emulsified asphalt, 100g of nano silicon powder with the particle size of 10nm and 900g of artificial graphite, mixing in a colloid mill for 6 hours, immediately performing spray drying on the formed mixture after mixing to remove moisture, controlling the air temperature to be 70 ℃, finally sintering the mixture at 800 ℃, and cooling to form the emulsified asphalt coated silicon-carbon negative electrode material.
Example 2
A preparation method of an emulsified asphalt coated silicon carbon negative electrode material comprises the following steps:
heating 7kg of petroleum asphalt to melt, controlling the temperature at 150 ℃, adding 200g of polyisobutylene succinic anhydride-ethanolamine into the petroleum asphalt, and uniformly stirring; adding 25g of sodium dodecyl benzene sulfonate and 75g of Tween 80 into 2.7kg of water to form a water phase, and keeping the temperature at 90 ℃ for later use; slowly adding asphalt into the water phase, and stirring and shearing through an emulsifier to form emulsified asphalt; then, 9.5kg of emulsified asphalt, 200g of nano silicon powder with the particle size of 100nm and 300g of natural graphite are mixed in a colloid mill for 8 hours, after mixing, the formed mixture is immediately subjected to spray drying to remove water, the air temperature is 80 ℃, finally, the mixture is sintered at 1200 ℃, and the emulsified asphalt coated silicon carbon negative electrode material is formed after cooling.
Example 3
Heating and melting 6.5kg of petroleum asphalt, controlling the temperature to be 140 ℃, adding 150g of polyisobutylene succinic anhydride-urea, uniformly stirring, adding 35g of sodium dodecyl sulfate and 115g of tween 80 into 3.2kg of water to form a water phase, and preserving heat at 85 ℃ for later use; slowly adding asphalt into a water phase, stirring and shearing through an emulsifier to form emulsified asphalt, then mixing 9.3kg of emulsified asphalt with 150g of nano silicon powder with the particle size of 60nm and 550g of natural graphite, mixing in a colloid mill for 7 hours, immediately performing spray drying on the formed mixture to remove moisture, controlling the air temperature to be 75 ℃, finally, sintering the mixture at 1000 ℃, and cooling to form the emulsified asphalt coated silicon-carbon negative electrode material.
Example 4
Heating and melting 5kg of coal tar pitch, controlling the temperature at 130 ℃, adding 50g of polyisobutylene succinimide and 50g of polyisobutylene succinic anhydride-ethanolamine, uniformly stirring, adding 40g of sodium dodecyl sulfate and 160g of tween 80 into 4.7kg of water to form a water phase, keeping the temperature at 80 ℃ for later use, slowly adding the pitch into the water phase, stirring and shearing through an emulsifier to form emulsified pitch, then mixing 9kg of emulsified pitch with 100g of nano silicon powder with the particle size of 10nm and 900g of artificial graphite, mixing in a colloid mill for 6 hours, immediately performing spray drying on the formed mixture after mixing to remove moisture, controlling the wind temperature at 70 ℃, finally sintering the mixture at 800 ℃, and cooling to form the emulsified pitch coated silicon carbon negative electrode material.
Example 5
Heating and melting 5kg of coal tar pitch, controlling the temperature at 130 ℃, adding 50g of polyisobutylene succinimide and 50g of polyisobutylene succinic anhydride-urea, uniformly stirring, adding 40g of sodium dodecyl sulfate and 160g of tween 80 into 4.7kg of water to form a water phase, keeping the temperature at 80 ℃ for standby, slowly adding the pitch into the water phase, stirring and shearing through an emulsifier to form emulsified pitch, then mixing 9kg of emulsified pitch, 100g of nano silicon powder with the particle size of 10nm and 900g of artificial graphite, mixing in a colloid mill for 6 hours, immediately performing spray drying on the formed mixture after mixing to remove moisture, controlling the wind temperature at 70 ℃, finally sintering the mixture at 800 ℃, and cooling to form the emulsified pitch coated silicon carbon negative electrode material.
Example 6
Heating and melting 5kg of coal tar pitch, controlling the temperature at 130 ℃, adding 50g of polyisobutylene succinic anhydride-ethanolamine and 50g of polyisobutylene succinic anhydride-ethanolamine, uniformly stirring, adding 40g of sodium dodecyl sulfate and 160g of tween 80 into 4.7kg of water to form a water phase, keeping the temperature at 80 ℃ for standby, slowly adding the pitch into the water phase, stirring and shearing through an emulsifier to form emulsified pitch, then mixing 9kg of emulsified pitch with 100g of nano silicon powder with the particle size of 10nm and 900g of artificial graphite, mixing in a colloid mill for 6 hours, immediately performing spray drying on the formed mixture after mixing to remove moisture, controlling the wind temperature at 70 ℃, finally sintering the mixture at 800 ℃, and cooling to form the emulsified pitch coated silicon carbon negative electrode material.
And (3) performance comparison:
the silicon-carbon negative electrode materials of examples 1 to 6 of the present invention and commercially available pitch-coated silicon-carbon negative electrode materials were respectively formed into batteries, and then the first discharge capacity and the reversible capacity after cycling were tested under the same conditions, and the electrical properties of the batteries were analyzed, and the test results are shown in table one, and it can be seen from table 1 that the batteries using the silicon-carbon negative electrode materials of the present invention have higher first discharge capacity and better cycling performance.
TABLE-Electrical Properties of different silicon-carbon negative electrode materials for forming batteries
Figure BDA0002868327190000051
The emulsified asphalt coated silicon carbon negative electrode material has the advantages of simple preparation process, readily available raw materials and convenience for popularization; the environment is friendly, the formed battery has excellent electrical performance, and the first discharge specific capacity can reach 1850 mAh/g; after the emulsified asphalt is adopted, the mixing uniformity of asphalt, graphite and silicon is improved, and the cycle life of the battery is prolonged.
Finally, it should be noted that the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to examples, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.

Claims (9)

1. The emulsified asphalt coated silicon-carbon negative electrode material is characterized in that: comprises 90-95% of emulsified asphalt, 1-2% of nano silicon powder and 3-9% of graphite by mass percent.
2. A preparation method of an emulsified asphalt coated silicon-carbon negative electrode material is characterized by comprising the following steps: the method comprises the following steps:
s1, heating and melting asphalt, controlling the temperature to be 130-150 ℃, adding the polyisobutylene succinic anhydride derivative into the asphalt, uniformly stirring, dissolving the surfactant in water at the temperature of 80-90 ℃, then pouring the asphalt solution into the water, and stirring to form emulsified asphalt;
s2, mixing emulsified asphalt, nano silicon powder and graphite in a colloid mill for 6-8 hours to obtain a mixture, and then performing spray drying on the mixture to obtain mixed powder;
and S3, sintering the mixed powder at 800-1200 ℃, and cooling to form the emulsified asphalt coated silicon carbon negative electrode material.
3. The preparation method of the emulsified asphalt coated silicon carbon negative electrode material as claimed in claim 2, wherein the preparation method comprises the following steps: the asphalt of the step S1 is coal-made asphalt or petroleum asphalt.
4. The preparation method of the emulsified asphalt coated silicon carbon negative electrode material as claimed in claim 2, wherein the preparation method comprises the following steps: the polyisobutylene succinic anhydride derivative obtained in the step S1 is one or a mixture of polyisobutylene succinimide, polyisobutylene succinic anhydride-urea and polyisobutylene succinic anhydride-ethanolamine.
5. The preparation method of the emulsified asphalt coated silicon carbon negative electrode material as claimed in claim 2, wherein the preparation method comprises the following steps: the surfactant of step S1 includes a first surfactant and a second surfactant, the first surfactant is selected from one of sodium dodecyl sulfate, sodium dodecyl benzene sulfonate and sodium dodecyl sulfate, and the second surfactant is tween 80.
6. The preparation method of the emulsified asphalt coated silicon carbon negative electrode material as claimed in claim 5, wherein the preparation method comprises the following steps: the mass ratio of the first surfactant to the second surfactant is 1: 3-4.
7. The preparation method of the emulsified asphalt coated silicon carbon negative electrode material as claimed in claim 2, wherein the preparation method comprises the following steps: the particle size of the nano silicon powder in the step S2 is 10-100 nm.
8. The preparation method of the emulsified asphalt coated silicon carbon negative electrode material as claimed in claim 2, wherein the preparation method comprises the following steps: the graphite of the step S2 is any one of artificial graphite and natural graphite.
9. The preparation method of the emulsified asphalt coated silicon carbon negative electrode material as claimed in claim 2, wherein the preparation method comprises the following steps: the emulsified asphalt comprises the following components in percentage by mass: 50-70% of asphalt, 1-2% of polyisobutylene succinic anhydride derivative, 1-2% of surfactant and the balance of water, wherein the total amount is 100%.
CN202011589174.8A 2020-12-29 2020-12-29 Emulsified asphalt coated silicon-carbon negative electrode material and preparation method thereof Pending CN112635741A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101244814A (en) * 2007-02-13 2008-08-20 深圳市比克电池有限公司 Method for producing lithium cell silicon carbon negative pole material and produced silicon carbon negative pole material
CN103208615A (en) * 2012-10-25 2013-07-17 郴州杉杉新材料有限公司 Silicon-carbon composite material, and preparation method and application thereof
CN104425802A (en) * 2013-09-11 2015-03-18 上海杉杉科技有限公司 Silicon-based composite material and preparation method and application thereof and prepared lithium ion battery
CN108054351A (en) * 2017-11-20 2018-05-18 海城申合科技有限公司 A kind of lithium ion battery, silicon-carbon cathode material used and preparation method thereof
CN108172812A (en) * 2018-01-30 2018-06-15 郑州中科新兴产业技术研究院 A kind of silicon-carbon cathode material available for power battery and preparation method thereof
CN111326723A (en) * 2020-02-26 2020-06-23 宁夏博尔特科技有限公司 Silicon-carbon composite negative electrode material for lithium ion battery and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101244814A (en) * 2007-02-13 2008-08-20 深圳市比克电池有限公司 Method for producing lithium cell silicon carbon negative pole material and produced silicon carbon negative pole material
CN103208615A (en) * 2012-10-25 2013-07-17 郴州杉杉新材料有限公司 Silicon-carbon composite material, and preparation method and application thereof
CN104425802A (en) * 2013-09-11 2015-03-18 上海杉杉科技有限公司 Silicon-based composite material and preparation method and application thereof and prepared lithium ion battery
CN108054351A (en) * 2017-11-20 2018-05-18 海城申合科技有限公司 A kind of lithium ion battery, silicon-carbon cathode material used and preparation method thereof
CN108172812A (en) * 2018-01-30 2018-06-15 郑州中科新兴产业技术研究院 A kind of silicon-carbon cathode material available for power battery and preparation method thereof
CN111326723A (en) * 2020-02-26 2020-06-23 宁夏博尔特科技有限公司 Silicon-carbon composite negative electrode material for lithium ion battery and preparation method thereof

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