CN111430676A - Negative electrode material of lithium ion battery and preparation method thereof - Google Patents
Negative electrode material of lithium ion battery and preparation method thereof Download PDFInfo
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- H01M4/00—Electrodes
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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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- H01M4/36—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
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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- Y02E60/10—Energy storage using batteries
Abstract
The invention provides a negative electrode material of a lithium ion battery and a preparation method thereof. The cathode material has a core-shell structure, the material forming the core of the core-shell structure comprises a silicon material and a solid electrolyte material, and the shell of the core-shell structure is formed by graphene. According to the cathode material provided by the invention, silicon particles and solid electrolyte in the core-shell structure are uniformly dispersed and coated by the graphene layer, so that good ionic conductivity between the silicon particles in the cathode material can be ensured, the exertion of silicon capacity can be improved, and the rate capability can be improved.
Description
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a negative electrode material of a lithium ion battery and a preparation method thereof.
Background
With the rapid development of new energy vehicles, the requirements for the energy density and safety performance of the power battery for vehicles are continuously improved. It is expected that the energy density of the power battery will need to reach over 500Wh/kg by 2025. In order to realize further breakthrough of energy density of power batteries, the development of a next generation of novel battery system is urgent. The solid battery system uses the solid electrolyte material to replace the existing liquid electrolyte and the diaphragm, so that the safety of the battery is greatly improved. Meanwhile, the solid electrolyte material has good stability to the lithium metal negative electrode, and can inhibit the growth of dendrites, so that the solid-state battery can obtain higher energy density. Therefore, solid-state batteries are considered as an ideal choice for next-generation high-energy-density, high-safety power batteries.
However, there are significant problems with solid state batteries when matched to lithium metal cathodes. For example, the existing solid electrolyte, especially sulfide electrolyte, has poor stability to lithium metal and cannot be directly used; the electrolyte layer in the solid-state battery inevitably has certain pores and interparticle gaps, and lithium dendrites easily penetrate through the gaps to grow, so that the battery is short-circuited finally; the huge volume change in the charging and discharging process of the lithium metal cathode brings great challenge to the interface stability, so that the performances of the battery such as multiplying power, circulation and the like can not meet the use requirements.
In order to rapidly realize the breakthrough of the solid-state battery in energy density, the search for a high-performance negative electrode to replace a lithium metal negative electrode becomes a key point. The silicon negative electrode has a specific capacity (3600mAh/g) which is comparable to that of lithium metal, has stable chemical properties, receives great attention of people, and becomes the first choice of the negative electrode for the high-energy-density solid-state battery at present. However, the silicon negative electrode also has some problems, mainly that the volume change is serious, the volume expansion rate of the silicon negative electrode is 300%, and the silicon negative electrode also has serious interface problems in a solid-state battery system; in addition, the silicon negative electrode has poor cycle performance, the repeated change of the volume of the silicon negative electrode causes the breakage and falling of material particles, and a large amount of electrolyte is consumed to form a thick Solid Electrolyte Interface (SEI) layer, so that the impedance of the battery is increased and the cycle life of the battery is shortened.
Disclosure of Invention
The invention aims to provide a negative electrode material of a lithium ion battery, which has high ionic conductivity, higher silicon capacity utilization rate and higher rate capability.
In a first aspect of the invention, the invention provides a negative electrode material of a lithium ion battery.
According to the embodiment of the invention, the negative electrode material has a core-shell structure, the material forming the core of the core-shell structure comprises a silicon material and a solid electrolyte material, and the shell of the core-shell structure is formed by graphene.
The inventor finds that silicon particles and solid electrolyte in the core-shell structure of the negative electrode material are uniformly dispersed and coated by the graphene layer, so that good ionic conductivity between the silicon particles in the negative electrode material can be ensured, the exertion of silicon capacity can be improved, and the rate capability can be improved.
In addition, the anode material according to the above embodiment of the present invention may further have the following additional technical features:
according to an embodiment of the present invention, the silicon material includes at least one of elemental silicon and silicon oxide, wherein the elemental silicon includes single crystal silicon, polycrystalline silicon, and amorphous silicon.
According to the embodiment of the invention, the particle size of the silicon material is 0.01-5 microns.
According TO an embodiment of the present invention, the solid electrolyte material includes at least one of an oxide-based solid electrolyte including LL ZO, LL TO, LL 0L ZTO, L ATO, L ATP, L AGP, and L iPON, a sulfide-based solid electrolyte including L GPS, L PS, LPSI, and LPSCl, and a polymer-based solid electrolyte including PEO, PPC, PS, and PMMA.
According to an embodiment of the present invention, the particle size of the oxide-based solid electrolyte is 0.01 to 5 micrometers, the particle size of the sulfide-based solid electrolyte is 0.01 to 5 micrometers, and the molecular weight of the polymer-based solid electrolyte is 10 to 200 ten thousand.
According to the embodiment of the invention, the thickness of the shell is 2-200 nanometers.
According to the embodiment of the invention, the particle size of the anode material is 0.1-500 microns.
In a second aspect of the invention, a method of making a negative electrode material for a lithium ion battery is presented.
According to an embodiment of the invention, the method comprises: (1) preparing a dispersion liquid, wherein the dispersion liquid comprises a silicon material, a solid electrolyte material and graphene oxide; (2) and forming a negative electrode material by performing spray drying and calcination treatment on the dispersion liquid, wherein the negative electrode material has a core-shell structure, the core of the core-shell structure is formed by the silicon material and the solid electrolyte material, and the shell of the core-shell structure is formed by graphene.
The inventor finds that by adopting the preparation method provided by the embodiment of the invention, the graphene layer is coated on the outer layer of the uniformly mixed silicon particles and solid electrolyte particles, so that the prepared anode material has high electronic conductivity, and the volume expansion of silicon can be effectively relieved, and the preparation method is simple in step.
In addition, the preparation method according to the above embodiment of the present invention may further have the following additional technical features:
according to an embodiment of the present invention, the dispersion liquid is composed of the silicon material, the solid electrolyte material, the graphene oxide, and a solvent.
According to the embodiment of the invention, in the dispersion liquid, the mass content of the silicon material is 20-60%, the mass content of the solid electrolyte material is 5-30%, and the mass content of the graphene is 5-30%.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
The foregoing aspects of the invention are explained in the description of the embodiments with reference to the following drawings, in which:
fig. 1 is a schematic cross-sectional structure of an anode material according to an embodiment of the present invention;
fig. 2 is a schematic diagram of the lithium ion transport mechanism of the silicon/graphene composite (a) and the silicon/solid electrolyte/graphene composite (b) according to one embodiment of the present invention;
fig. 3 is a schematic flow chart of a method of preparing an anode material according to an embodiment of the present invention;
FIG. 4 is a schematic representation of the product before and after spray drying and high temperature calcination in a manufacturing process according to one embodiment of the present invention;
fig. 5 is a graph comparing charge and discharge rates of anode materials of an example of the present invention and a comparative example;
fig. 6 is a graph comparing cycle performance of the anode materials of one embodiment of the present invention and one comparative example.
Reference numerals
100 kernel
200 outer cover
Detailed Description
The following examples of the present invention are described in detail, and it will be understood by those skilled in the art that the following examples are intended to illustrate the present invention, but should not be construed as limiting the present invention. Unless otherwise indicated, specific techniques or conditions are not explicitly described in the following examples, and those skilled in the art may follow techniques or conditions commonly employed in the art or in accordance with the product specifications.
In one aspect of the invention, the invention provides a negative electrode material of a lithium ion battery.
According to an embodiment of the present invention, referring to fig. 1, the negative electrode material has a core-shell structure, the material forming the core 100 of the core-shell structure includes a silicon material and a solid electrolyte material, and the shell 200 of the core-shell structure is formed of graphene. In the research process, the inventor of the present invention finds that, although a carbon layer is coated on a silicon surface, the effects of alleviating silicon volume expansion and improving cycle stability can be achieved, when a silicon/graphene composite material is applied as a solid battery negative electrode, referring to fig. 2 (a), a solid electrolyte is only distributed on an outer surface of the silicon/graphene composite material and cannot enter into particles of the negative electrode material, so that ionic conductivity between silicon particles in the negative electrode material is low, silicon capacity is difficult to exert, and further rate capability is reduced.
Therefore, in order to solve the problem of low ionic conductivity inside the negative electrode material, the inventors refer to fig. 2 (b), in which silicon particles and a solid electrolyte are uniformly dispersed, and a graphene layer is coated on the outer surface of the silicon particles, so that the solid electrolyte can provide a high ionic conduction network for the silicon material, thereby ensuring that good ionic conductivity is maintained among the silicon particles inside the negative electrode material, improving the silicon capacity utilization rate, and further improving the rate capability. In addition, the graphene coating structure can also provide a buffer space for the volume expansion of the silicon material, so that the stability of an interface between a negative electrode and an electrolyte in the solid-state battery is ensured, and the cycle stability is improved.
In some embodiments of the present invention, the silicon material may include at least one of elemental silicon and silicon oxide, where the elemental silicon includes monocrystalline silicon, polycrystalline silicon and amorphous silicon, and the particle size of the silicon material is 0.01 to 5 micrometers, so that the specific surface inside the negative electrode material may be larger and the contact surface with the solid electrolyte may be more with the nano silicon particles, thereby obtaining higher ionic conductivity.
In some embodiments of the invention, the oxide-based solid state electrolyte may include lithium lanthanum zirconium oxide (LL ZO), lithium lanthanum titanium oxide (LL TO), lithium lanthanum zirconium titanium oxide (LL 0L ZTO), lithium aluminum titanium oxide (L ATO), titanium aluminum lithium phosphate (L ATP), germanium aluminum lithium phosphate (L AGP) and lithium nitrogen phosphate (L iPON), the sulfide-based solid state electrolyte may include lithium germanium phosphorus sulfide (L GPS), lithium phosphorus sulfide (L PS), Lithium Phosphorus Sulfur Iodide (LPSI) and lithium phosphorus sulfur chloride (SCLPl), and the polymer-based solid state electrolyte may include polyethylene glycol (PEO), carbon dioxide copolymer (PPC), Polystyrene (PS) and Polymethylmethacrylate (PMMA), such that the solid state electrolyte may be selected TO more closely match the solid state electrolyte TO the solid state electrolyte.
In some specific examples, the particle size of the oxide-based solid electrolyte may be 0.01 to 5 micrometers, the particle size of the sulfide-based solid electrolyte may be 0.01 to 5 micrometers, and the molecular weight of the polymer-based solid electrolyte may be 10 to 200 ten thousand. Thus, with the solid electrolyte having the above particle size or molecular weight, it is possible to mix well with the silicon particles.
According to the embodiment of the invention, the thickness of the shell can be 2-200 nanometers, so that the toughness of the thinner graphene layer is better, and the volume expansion of silicon in the negative electrode material is relieved more effectively. According to the embodiment of the invention, the particle size of the negative electrode material can be 0.1-500 microns, so that the prepared negative electrode material particles with high electronic conductivity and high ionic conductivity can be better coated into a negative electrode sheet.
In summary, according to the embodiments of the present invention, the present invention provides a negative electrode material, in which silicon particles and a solid electrolyte in a core-shell structure are uniformly dispersed, and the surface of the core-shell structure is coated by a graphene layer, so that good ionic conductivity between the silicon particles in the negative electrode material can be ensured, thereby improving the performance of silicon capacity and improving the rate capability.
In another aspect of the invention, a method of making a negative electrode material for a lithium ion battery is presented. According to an embodiment of the present invention, referring to fig. 3, the preparation method includes:
s100: and (4) preparing a dispersion liquid.
In this step, a dispersion is prepared, wherein the dispersion includes a silicon material, a solid electrolyte material, and graphene oxide.
According to the embodiment of the present invention, the specific composition of the dispersion liquid can be selected by those skilled in the art according to the properties of the finally prepared anode material. In some embodiments of the present invention, the dispersion may be composed of the silicon material, the solid electrolyte material, the graphene oxide, and the solvent, so that the silicon material, the solid electrolyte material, and the graphene oxide may be uniformly dispersed in water, tetrahydrofuran, Dimethylsulfoxide (DMSO), or toluene without an additional surfactant.
In some specific examples, in the dispersion liquid, the mass content of the silicon material may be 20 to 60%, the mass content of the solid electrolyte material may be 5 to 30%, and the mass content of the graphene may be 5 to 30%, so that the negative electrode material particles with high ionic conductivity and high rate performance can be obtained by using the dispersion liquid composed of the above proportions and then performing a spray drying process and a calcination process.
S200: and forming the negative electrode material by the dispersion liquid through a spray drying method and a calcining treatment.
In this step, referring to fig. 4, the dispersion liquid is subjected to spray drying and calcination treatment to form a negative electrode material, and the negative electrode material has a core-shell structure, wherein a core of the core-shell structure is formed by a silicon material and a solid electrolyte material, and a shell of the core-shell structure is formed by graphene.
According to the embodiment of the invention, spray drying or freeze drying is firstly performed, and the calcination treatment can be obtained by calcining at a high temperature of 850-950 ℃ for 2 hours under the protection of inert argon atmosphere, and a person skilled in the art can select the silicon material and the solid electrolyte material according to specific types in the dispersion liquid, which is not described herein again.
In summary, according to the embodiments of the present invention, the present invention provides a preparation method, in which the graphene layer is coated on the outer layer of the uniformly mixed silicon particles and solid electrolyte particles, so that the prepared anode material has high electronic conductivity, and the volume expansion of silicon can be effectively alleviated, and the preparation method has simple steps.
The invention will now be described with reference to specific examples, which are intended to be illustrative only and not to be limiting in any way.
Example 1
The preparation method comprises the specific steps of firstly dispersing 1.0g of graphene oxide in 500m L of water to form uniform dispersion liquid, then adding 2.0g of nano silicon and 0.5g of oxide solid electrolyte LL ZTO, fully stirring and dispersing for 2 hours to obtain dispersion liquid, then preparing the dispersion liquid into a composite material through a spray drying method, and finally calcining the composite material at the high temperature of 900 ℃ and in an argon atmosphere for 2 hours to obtain the nano silicon/LL ZTO/graphene cathode material.
Comparative example 1
Except that in this comparative example, the oxide solid electrolyte LL ZTO was not added to the dispersion, and thus, a nano silicon/graphene anode material was obtained.
Example 2
The preparation method comprises the specific steps of firstly dispersing 0.5g of graphene oxide into 500m L tetrahydrofuran to form uniform dispersion liquid, then adding 3.0g of SiOx and 0.5g of oxide solid electrolyte LL ZO, fully stirring and dispersing for 2 hours to obtain the dispersion liquid, then preparing the dispersion liquid into a composite material through a spray drying method, and finally calcining the composite material at the high temperature of 900 ℃ and in an argon atmosphere for 2 hours to obtain the SiOx/LL ZO/graphene negative electrode material.
Example 3
The preparation method comprises the specific steps of firstly dispersing 1.0g of graphene oxide into 1000m L DMSO to form uniform dispersion liquid, then adding 10.0g of nano silicon and 4.0g of oxide solid electrolyte L ATP, fully stirring and dispersing for 4 hours to obtain dispersion liquid, then preparing the dispersion liquid into a composite material through a freeze-drying method, and calcining the composite material at the high temperature of 900 ℃ and in an argon atmosphere for 2 hours to obtain the nano silicon/L ATP/graphene negative electrode material.
Example 4
In the embodiment, the negative electrode material is prepared by the specific steps of firstly dispersing 0.5g of graphene into 500m L toluene to form uniform dispersion liquid, then adding 3.0g of nano silicon, 2.0g of SiOx and 2.0g of sulfide solid electrolyte L GPS, fully stirring and dispersing for 4h to obtain dispersion liquid, and then preparing the negative electrode material of nano silicon/SiOx/L GPS/graphene from the dispersion liquid by a freeze drying method.
Summary of the invention
The rate capability and cycle capability of the nano-silicon/LL ZTO/graphene anode material of example 1 and the nano-silicon/graphene anode material of comparative example 1 are respectively shown in fig. 5 and fig. 6, it can be shown from fig. 5 and fig. 6 that after the solid electrolyte is added to the core in the core-shell structure of the anode material, the solid electrolyte can provide a high ion conductive network for the silicon material, thereby ensuring that good ionic conductivity is maintained among silicon particles in the anode material, improving the silicon capacity exertion rate, and further improving the rate capability.
In the description of the present invention, it is to be understood that the terms "central," "longitudinal," "lateral," "length," "width," "thickness," "upper," "lower," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," "clockwise," "counterclockwise," "axial," "radial," "circumferential," and the like are used in the orientations and positional relationships indicated in the drawings for convenience in describing the invention and to simplify the description, and are not intended to indicate or imply that the referenced device or element must have a particular orientation, be constructed and operated in a particular orientation, and are not to be considered limiting of the invention.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Although embodiments of the present invention have been shown and described above, it is understood that the above embodiments are exemplary and should not be construed as limiting the present invention, and that variations, modifications, substitutions and alterations can be made to the above embodiments by those of ordinary skill in the art within the scope of the present invention.
Claims (10)
1. The negative electrode material of the lithium ion battery is characterized in that the negative electrode material has a core-shell structure, materials forming an inner core of the core-shell structure comprise a silicon material and a solid electrolyte material, and an outer shell of the core-shell structure is formed by graphene.
2. The anode material according to claim 1, wherein the silicon material comprises at least one of elemental silicon and silicon oxide, wherein the elemental silicon comprises single crystal silicon, polycrystalline silicon, and amorphous silicon.
3. The negative electrode material as claimed in claim 1, wherein the silicon material has a particle size of 0.01 to 5 μm.
4. The anode material according to claim 1, wherein the solid electrolyte material includes at least one of an oxide-based solid electrolyte, a sulfide-based solid electrolyte, and a polymer-based solid electrolyte; wherein the content of the first and second substances,
the oxide-based solid electrolyte includes LL ZO, LL TO, LL ZTO, L ATO, L ATP, L AGP and L iPON,
the sulfide-based solid electrolyte includes L GPS, L PS, L PSI and L PSCl,
the polymer-based solid electrolyte includes PEO, PPC, PS, and PMMA.
5. The negative electrode material as claimed in claim 4, wherein the oxide-based solid electrolyte has a particle size of 0.01 to 5 μm, the sulfide-based solid electrolyte has a particle size of 0.01 to 5 μm, and the polymer-based solid electrolyte has a molecular weight of 10 to 200 ten thousand.
6. The anode material of claim 1, wherein the shell has a thickness of 2 to 200 nm.
7. The negative electrode material of claim 1, wherein the negative electrode material has a particle size of 0.1 to 500 μm.
8. A method of making a negative electrode material for a lithium ion battery, comprising:
(1) preparing a dispersion liquid, wherein the dispersion liquid comprises a silicon material, a solid electrolyte material and graphene oxide;
(2) and forming a negative electrode material by performing spray drying and calcination treatment on the dispersion liquid, wherein the negative electrode material has a core-shell structure, the core of the core-shell structure is formed by the silicon material and the solid electrolyte material, and the shell of the core-shell structure is formed by graphene.
9. The method of claim 8, wherein the dispersion consists of the silicon material, the solid state electrolyte material, the graphene oxide, and a solvent.
10. The method according to claim 8, wherein the dispersion liquid contains 20 to 60% by mass of the silicon material, 5 to 30% by mass of the solid electrolyte material, and 5 to 30% by mass of the graphene.
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| WO2022194089A1 (en) * | 2021-03-19 | 2022-09-22 | 比亚迪股份有限公司 | Negative electrode material and preparation method therefor, and all-solid-state lithium battery |
| CN112952035A (en) * | 2021-03-25 | 2021-06-11 | 蜂巢能源科技有限公司 | Negative electrode and preparation method and application thereof |
| CN112952035B (en) * | 2021-03-25 | 2022-04-22 | 蜂巢能源科技有限公司 | Negative electrode and preparation method and application thereof |
| WO2022199505A1 (en) * | 2021-03-25 | 2022-09-29 | 蜂巢能源科技股份有限公司 | Negative electrode, preparation method therefor, and application thereof |
| CN114730883A (en) * | 2021-09-15 | 2022-07-08 | 宁德新能源科技有限公司 | Negative electrode composite material and application thereof |
| WO2023039750A1 (en) * | 2021-09-15 | 2023-03-23 | 宁德新能源科技有限公司 | Negative electrode composite material and use thereof |
| DE102021213786A1 (en) | 2021-12-03 | 2023-06-07 | Volkswagen Aktiengesellschaft | Method of making an electrode, Electrode |
| CN116314834A (en) * | 2023-05-25 | 2023-06-23 | 四川新能源汽车创新中心有限公司 | Composite anode material, preparation method thereof and all-solid-state battery |
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