CN112290004A - Expansion-resistant composite silicon, expansion-resistant composite silicon intermediate, preparation method and lithium battery - Google Patents
Expansion-resistant composite silicon, expansion-resistant composite silicon intermediate, preparation method and lithium battery Download PDFInfo
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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
- H01M4/364—Composites as mixtures
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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
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/60—Selection of substances as active materials, active masses, active liquids of organic compounds
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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- 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 belongs to the technical field of lithium battery manufacturing, and particularly relates to expansion-resistant composite silicon, an expansion-resistant composite silicon intermediate, a preparation method of the expansion-resistant composite silicon intermediate and a lithium battery, wherein the preparation method of the expansion-resistant composite silicon comprises the following steps: preparing a premix, namely, filling silicon into a reaction kettle, adding a silane coupling agent, and premixing by stirring; preparing an expansion-resistant composite silicon intermediate, namely heating the reaction kettle after vacuumizing to prepare the expansion-resistant composite silicon intermediate; and (3) preparing the expansion-resistant composite silicon, namely adding a lipophilic compound into the reaction kettle, vacuumizing the reaction kettle, and heating to obtain the expansion-resistant composite silicon. The expansion-resistant composite silicon prepared by the invention has low expansion rate, and has small volume change in the charge-discharge process of a lithium battery, so that the cycle stability of the lithium battery cathode material is improved.
Description
Technical Field
The invention belongs to the technical field of lithium battery manufacturing, and particularly relates to expansion-resistant composite silicon, an expansion-resistant composite silicon intermediate, a preparation method of the expansion-resistant composite silicon intermediate and a lithium battery.
Background
The lithium ion battery has the advantages of high energy density, long cycle life, small self-discharge, no memory effect, environmental friendliness and the like, is widely applied to the fields of smart phones, smart bracelets, digital cameras, notebook computers and the like, and has larger consumption requirements. Meanwhile, the electric vehicle is gradually popularized in the fields of pure electric vehicles, hybrid electric vehicles and extended-range electric vehicles, and the market share is the largest in increasing trend. In addition, the lithium ion battery has a good development trend in the large-scale energy storage fields of power grid peak shaving, household power distribution, communication base stations and the like.
The lithium ion battery mainly comprises a positive electrode, a negative electrode, electrolyte, a diaphragm and the like, wherein the selection of the negative electrode material is directly related to the energy density of the battery. The negative electrode material is a main body of lithium stored in the lithium ion battery, so that lithium ions are inserted and removed in the charging and discharging processes. When a lithium battery is charged, lithium atoms in a positive electrode are ionized into lithium ions and electrons, and the lithium ions move to a negative electrode to synthesize lithium atoms with the electrons. During discharge, lithium atoms are ionized from the surface of the negative electrode in the graphite crystal into lithium ions and electrons, and the lithium atoms are synthesized at the positive electrode. The negative electrode material mainly affects the first efficiency, the cycle performance and the like of the lithium battery, and the performance of the negative electrode material also directly affects the performance of the lithium battery.
Disclosure of Invention
The invention provides expansion-resistant composite silicon, an expansion-resistant composite silicon intermediate, a preparation method and a lithium battery.
In order to solve the technical problem, the invention provides a preparation method of expansion-resistant composite silicon, which comprises the following steps: preparing a premix, namely, filling silicon into a reaction kettle, adding a silane coupling agent, and premixing by stirring; preparing an expansion-resistant composite silicon intermediate, namely heating the reaction kettle after vacuumizing to prepare the expansion-resistant composite silicon intermediate; and (3) preparing the expansion-resistant composite silicon, namely adding a lipophilic compound into the reaction kettle, vacuumizing the reaction kettle, and heating to obtain the expansion-resistant composite silicon.
In a second aspect, the invention also provides the expansion-resistant composite silicon prepared by the preparation method, wherein the chemical formula of the expansion-resistant composite silicon is RSiOOM; r is an organic group of a silane coupling agent; m is silicon; and the particle size distribution D50 of the expansion-resistant composite silicon is 1-100 μm.
In a third aspect, the invention also provides an expansion-resistant composite silicon intermediate prepared by the preparation method, wherein the chemical formula of the expansion-resistant composite silicon intermediate is Y-RSiOOM; wherein Y is lipophilic compound such as long-chain fatty alcohol or long-chain fatty acid; r is an organic group of a silane coupling agent; m is silicon.
In a fourth aspect, the present invention also provides a lithium battery, including: and (3) expansion-resistant composite silicon.
The expansion-resistant composite silicon prepared by the invention has the beneficial effects that the expansion-resistant composite silicon has low expansion rate, the volume change is small in the charge-discharge process of a lithium battery, and the cycle stability of the lithium battery cathode material is improved.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
In order to make the aforementioned and other objects, features and advantages of the present invention comprehensible, preferred embodiments accompanied with figures are described in detail below.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a schematic structural view of the expansion-resistant composite silicon of the present invention.
In the figure:
1-silicon; 2-lipophilic compounds.
Detailed Description
To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings, and it is apparent that the described embodiments are some, but not all 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.
In order to improve the energy density of the lithium battery, as shown in fig. 1, the invention provides a preparation method of expansion-resistant composite silicon, which comprises the following steps: preparing a premix, namely, filling silicon into a reaction kettle, adding a silane coupling agent, and premixing by stirring; preparing an expansion-resistant composite silicon intermediate, namely vacuumizing a reaction kettle and heating to prepare the expansion-resistant composite silicon intermediate; and (3) preparing the expansion-resistant composite silicon, namely adding a lipophilic compound into the reaction kettle, vacuumizing the reaction kettle, and heating to obtain the expansion-resistant composite silicon.
Specifically, silicon is put into a reaction kettle, then a silane coupling agent is added, and premixing is carried out through stirring; vacuumizing the reaction kettle, heating for reaction, adding the lipophilic compound into the reaction kettle, vacuumizing the reaction kettle, and heating again to obtain the expansion-resistant composite silicon.
The expansion-resistant composite silicon prepared by the invention has low expansion rate, and has small volume change in the charge-discharge process of a lithium battery, so that the cycle stability of the lithium battery cathode material is improved.
Alternatively, the lipophilic compound may be, but is not limited to, one or more of a long chain fatty alcohol, a long chain fatty acid. Wherein the long-chain fatty alcohol and the long-chain fatty acid refer to fatty alcohol or fatty acid with molecular formula containing six or more carbon atoms.
Specifically, the reaction mechanism for preparing the expansion-resistant composite silicon intermediate is as follows:
RSiX3+H2O+M-OH→RSiOOM
the reaction mechanism for preparing the expansion-resistant composite silicon is as follows:
RSiOOM+Y→Y-RSiOOM
wherein, RSiX3Is a silane coupling agent, X is a hydrolyzable group, R is an organic group; m is silicon, and M-OH is silicon and free hydroxyl on the surface of the silicon; RSiOOM is an expansion-resistant composite silicon intermediate; y is lipophilic compound such as long-chain fatty alcohol or long-chain fatty acid; RSiOOM expansion resistant silicon composites.
Optionally, the mass ratio of the silicon to the silane coupling agent to the lipophilic compound is 10-20: 1: 1.25 to 4.
The silane coupling agent may be, but is not limited to, vinyltrimethoxysilane.
Optionally, the particle size distribution D50 of the silicon may be, but is not limited to, 0.5 to 50 μm.
Optionally, the stirring speed for preparing the pre-mixture can be, but is not limited to, 500-1000 revolutions, and the pre-mixing time is not less than 3 hours.
Optionally, the reaction temperature for preparing the expansion-resistant composite silicon intermediate can be but is not limited to 80-100 ℃, and the reaction time can be but is not limited to 2-3 hours.
Optionally, the reaction temperature for preparing the expansion-resistant composite silicon can be but is not limited to 90-110 ℃, and the reaction time can be but is not limited to 2-3 hours.
Furthermore, the invention also provides the expansion-resistant composite silicon prepared by the preparation method, wherein the chemical formula of the expansion-resistant composite silicon is RSiOOM; r is an organic group of a silane coupling agent; m is silicon; and the particle size distribution D50 of the expansion-resistant composite silicon is 1-100 μm.
Further, the invention also provides an expansion-resistant composite silicon intermediate prepared by the preparation method, wherein the chemical formula of the expansion-resistant composite silicon intermediate is Y-RSiOOM; wherein Y is lipophilic compound such as long-chain fatty alcohol or long-chain fatty acid; r is an organic group of a silane coupling agent; m is silicon.
Further, the present invention also provides a lithium battery, including: and (3) expansion-resistant composite silicon.
Example 1
500kg of silicon with the particle size distribution D50 of 10 mu m is added into a reaction kettle, 50kg of vinyl trimethoxy silane is added, and the mixture is stirred for 5 hours at the rotating speed of 800 revolutions; vacuumizing the reaction kettle, heating to 90 ℃, keeping the temperature constant, and reacting for 3 hours to obtain an expansion-resistant composite silicon intermediate; and adding 80kg of hexadecanol into the reaction kettle, vacuumizing the reaction kettle, heating to 95 ℃, keeping the temperature constant, and reacting for 3 hours to obtain the expansion-resistant composite silicon.
And preparing the prepared expansion-resistant composite silicon into a negative plate, taking lithium iron phosphate as a positive electrode material, taking lithium hexafluorophosphate as an electrolyte, and assembling the lithium battery by taking a PE film prepared by a wet method with the thickness of 12 microns as a diaphragm.
Example 2
Adding 600kg of silicon with the particle size distribution D50 of 0.5 mu m into a reaction kettle, adding 50kg of vinyl trimethoxy silane, and stirring for 6 hours at the rotating speed of 500 revolutions; vacuumizing the reaction kettle, heating to 80 ℃, keeping the temperature constant, and reacting for 3 hours to obtain an expansion-resistant composite silicon intermediate; and adding 150kg of hexadecanol into the reaction kettle, vacuumizing the reaction kettle, heating to 90 ℃, keeping the temperature constant, and reacting for 3 hours to obtain the expansion-resistant composite silicon.
And preparing the prepared expansion-resistant composite silicon into a negative plate, taking lithium iron phosphate as a positive electrode material, taking lithium hexafluorophosphate as an electrolyte, and assembling the lithium battery by taking a PE film prepared by a wet method with the thickness of 12 microns as a diaphragm.
Example 3
Adding 800kg of silicon with the particle size distribution D50 of 50 mu m into a reaction kettle, adding 50kg of vinyl trimethoxy silane, and stirring for 3 hours at the rotating speed of 1000 revolutions; vacuumizing the reaction kettle, heating to 100 ℃, keeping the temperature constant, and reacting for 2 hours to obtain an expansion-resistant composite silicon intermediate; and adding 200kg of tetracosanoic acid into the reaction kettle, vacuumizing the reaction kettle, heating to 110 ℃, keeping the temperature constant, and reacting for 2 hours to obtain the expansion-resistant composite silicon.
And preparing the prepared expansion-resistant composite silicon into a negative plate, taking lithium iron phosphate as a positive electrode material, taking lithium hexafluorophosphate as an electrolyte, and assembling the lithium battery by taking a PE film prepared by a wet method with the thickness of 12 microns as a diaphragm.
Example 4
Adding 1000kg of silicon with the particle size distribution D50 of 30 mu m into a reaction kettle, adding 50kg of vinyl trimethoxy silane, and stirring for 4 hours at the rotating speed of 900 revolutions; vacuumizing the reaction kettle, heating to 95 ℃, keeping the temperature constant, and reacting for 2.5 hours to obtain an expansion-resistant composite silicon intermediate; and adding 62.5kg of tetracosanoic acid into the reaction kettle, vacuumizing the reaction kettle, heating to 105 ℃, keeping the temperature constant, and reacting for 2.5 hours to obtain the expansion-resistant composite silicon.
And preparing the prepared expansion-resistant composite silicon into a negative plate, taking lithium iron phosphate as a positive electrode material, taking lithium hexafluorophosphate as an electrolyte, and assembling the lithium battery by taking a PE film prepared by a wet method with the thickness of 12 microns as a diaphragm.
Comparative example 1
And (2) preparing a negative plate by taking silicon as a negative material, preparing lithium iron phosphate as a positive material, taking lithium hexafluorophosphate as an electrolyte, and assembling the lithium battery by taking a PE film prepared by a wet method with the thickness of 12 microns as a diaphragm.
Comparative example 2
The lithium battery is assembled by using graphite as a negative electrode material to prepare a negative plate, lithium iron phosphate as a positive electrode material, lithium hexafluorophosphate as an electrolyte and a PE film prepared by a wet method with the thickness of 12 mu m as a diaphragm.
Comparative analysis of performance parameters
The swelling-resistant composite silicon prepared in examples 1 to 4 and the lithium batteries prepared in examples 1 to 4, comparative example 1 and comparative example 2 were tested in this section for their relevant performance, and the results are shown in table 1.
Table 1 summary table of performance test results of expansion-resistant composite silicon and lithium battery
As can be seen from the data in table 1, the expansion rate of the expansion-resistant composite silicon prepared in examples 1 to 4 is significantly reduced, and the soaking time of the electrolyte is shortened, and the service life of the lithium battery is prolonged.
In conclusion, the expansion-resistant composite silicon provided by the invention has the advantages of large specific capacity, low expansion rate, low reaction activity with electrolyte and no co-intercalation phenomenon of organic solvent; lithium dendrite is not formed when the lithium battery is charged, and the safety of the lithium battery is improved; the volume change is small in the charging and discharging process of the lithium battery, the cycling stability of the lithium battery cathode material is improved, and the service life of the lithium battery is prolonged.
In light of the foregoing description of the preferred embodiment of the present invention, many modifications and variations will be apparent to those skilled in the art without departing from the spirit and scope of the invention. The technical scope of the present invention is not limited to the content of the specification, and must be determined according to the scope of the claims.
Claims (10)
1. The preparation method of the expansion-resistant composite silicon is characterized by comprising the following steps of:
preparing a premix, namely, filling silicon into a reaction kettle, adding a silane coupling agent, and premixing by stirring;
preparing an expansion-resistant composite silicon intermediate, namely heating the reaction kettle after vacuumizing to prepare the expansion-resistant composite silicon intermediate;
and (3) preparing the expansion-resistant composite silicon, namely adding a lipophilic compound into the reaction kettle, vacuumizing the reaction kettle, and heating to obtain the expansion-resistant composite silicon.
2. The method according to claim 1, wherein the reaction mixture,
the lipophilic compound is one or more of long-chain fatty alcohol and long-chain fatty acid.
3. The method according to claim 1, wherein the reaction mixture,
the mass ratio of the silicon to the silane coupling agent to the lipophilic compound is 10-20: 1: 1.25 to 4.
4. The method according to claim 1, wherein the reaction mixture,
the particle size distribution D50 of the silicon is 0.5-50 μm.
5. The method according to claim 1, wherein the reaction mixture,
the stirring speed of the prepared premix is 500-1000 revolutions, and the premixing time is not less than 3 hours.
6. The method according to claim 1, wherein the reaction mixture,
the reaction temperature for preparing the expansion-resistant composite silicon intermediate is 80-100 ℃, and the reaction time is 2-3 h.
7. The method according to claim 1, wherein the reaction mixture,
the reaction temperature for preparing the expansion-resistant composite silicon is 90-110 ℃, and the reaction time is 2-3 h.
8. An expansion-resistant composite silicon obtained by the production method according to claim 1,
the chemical formula of the expansion-resistant composite silicon is RSiOOM;
r is an organic group of a silane coupling agent;
m is silicon; and
the particle size distribution D50 of the expansion-resistant composite silicon is 1-100 mu m.
9. An expansion-resistant composite silicon intermediate produced by the production method according to claim 1,
the chemical formula of the expansion-resistant composite silicon intermediate is Y-RSiOOM; wherein
Y is lipophilic compound such as long-chain fatty alcohol or long-chain fatty acid;
r is an organic group of a silane coupling agent;
m is silicon.
10. A lithium battery, comprising:
and (3) expansion-resistant composite silicon.
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