CN114628652B - Long-cycle quick-charging SiO graphite composite anode material and preparation method thereof - Google Patents
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Abstract
The invention relates to the field of battery cathode materials, and discloses a long-cycle quick-charging SiO graphite composite cathode material and a preparation method thereof, wherein the SiO graphite composite cathode material is prepared by kneading SiO, graphite, an adhesive and a nano porous elastic alloy at high temperature; according to the invention, the SiO and the nano elastic porous alloy are wrapped into balls to prepare primary SiO particles, and then the graphite is wrapped on the outer sides of the primary SiO particles to prepare the SiO graphite composite anode material, so that the cycle performance and the quick charge performance of the silicon-based anode lithium battery during quick charge are remarkably improved, the nano elastic porous alloy can play a role in buffering the volume expansion of the SiO, and the breakage speed of the anode material due to the volume expansion is slowed down; and the nano porous elastic alloy and graphite are sequentially coated on the outer side of SiO through twice granulation, so that a double-layer coating structure with SiO as an inner core, nano porous elastic alloy/carbon as an intermediate layer and graphite/carbon as an outer shell is more stable.
Description
Technical Field
The invention relates to the field of battery cathode materials, in particular to a long-cycle quick-charging SiO graphite composite cathode material and a preparation method thereof.
Background
Along with the rapid development of the lithium battery industry, the energy density requirement of the lithium ion battery is continuously improved, graphite is used as the negative electrode material of the traditional lithium ion battery, the theoretical energy density of the graphite is 372mAh/g, the increasing energy density requirement can not be met, in recent years, the theoretical energy density of the silicon-based negative electrode material can reach 4200mAh/g, which is 10 times of that of the graphite negative electrode, the theoretical energy density of the silicon-based negative electrode material is high, the storage of the synthesized raw materials is abundant and the price is low, and the graphite is an important research object of future negative electrode additive materials.
As disclosed in publication number CN109686957a, a preparation method of an artificial graphite and SiO-based silicon-carbon composite negative electrode material is disclosed, and the volume expansion of a lithium ion battery in the charge and discharge process can be effectively solved by using the artificial graphite and SiO-based silicon-carbon composite negative electrode material, so that the energy density of the negative electrode material is improved; the structure that the artificial graphite anode material and SiO are well combined together through asphalt can further improve the structural stability of the anode material, the whole process flow is simple, and the artificial graphite and SiO-based silicon-carbon composite anode material has good physical properties and electrochemistry in the lithium ion battery anode material and battery performance test.
Further, as disclosed in publication No. CN109037636A, a preparation method of a SiO/carbon/graphite composite anode material is disclosed, wherein SiO is moderately nanocrystallized by a sanding method, and then an inorganic carbon source is added for sanding, so that the dispersibility of the inorganic carbon source is improved; coating a layer of high-conductivity carbon material on the surface of the SiO nano-particles by a liquid-phase carbon coating technology, so that a large amount of binder is avoided being consumed in the electrode preparation process, and the processing performance of the material is improved; the SiO is subjected to disproportionation reaction through high-temperature heat treatment, so that the pulverization of the material caused by the local lithium intercalation of the material can be avoided, and the structural stability of the material is improved.
In the prior art, the silicon-based negative electrode material still has the problems of poor cycle performance and low quick charge performance during quick charge, so that a long-cycle quick charge SiO graphite composite negative electrode material and a preparation method thereof are needed to solve the problems.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a long-cycle fast-charging SiO graphite composite anode material and a preparation method thereof, wherein SiO and nano elastic porous alloy are wrapped into balls to prepare primary SiO particles by carbon prepared by high-temperature kneading of an adhesive, and graphite is wrapped on the outer sides of the primary SiO particles to prepare the SiO graphite composite anode material, so that the cycle performance and the conductivity of a silicon-based anode lithium battery during fast charging are remarkably improved.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
a long-circulation fast-charging SiO graphite composite anode material is prepared by kneading SiO, graphite, a binder and nano elastic porous alloy at high temperature.
According to the invention, siO and nano elastic porous alloy are wrapped into balls to prepare primary SiO particles, graphite is wrapped on the outer sides of the primary SiO particles to prepare the SiO graphite composite anode material, so that the cycle performance and the quick charge performance of the silicon-based anode lithium battery are remarkably improved, the elastic alloy has the characteristics of high conductivity, strong elasticity and corrosion resistance, the nano elastic alloy is wrapped on the surface of SiO to play a role in buffering the volume expansion of SiO, the elastic characteristic of the nano elastic alloy can form a layer of shell to change according to the volume change of SiO, the nano elastic alloy is firmly wrapped on the outer sides of the SiO particles to form a layer of protection net, electrolyte is blocked from contacting with SiO, and meanwhile, the porous structure of the nano elastic alloy can buffer the volume deformation quantity of the SiO particles when the SiO particles expand, so that the breakage speed of the anode material due to the volume expansion is slowed down, the cycle performance of the battery is remarkably improved, the nano elastic alloy is high in conductivity, the porous structure also shortens the path of lithium ion embedding SiO, the ion exchange rate of the anode material is remarkably increased, and the quick charge performance of the lithium battery is improved.
Preferably, the particle size of the nano porous elastic alloy is 70-100nm, and the particle size of SiO is 1-100 μm.
A preparation method of a long-cycle quick-charging SiO graphite composite anode material comprises the following preparation steps:
(1) Preparing a nano porous elastic alloy: uniformly mixing elastic alloy powder and a pore-forming agent according to a proportion, pressing into a green body, placing the green body in a vacuum inert atmosphere for calcination, heating for primary calcination, heating for secondary calcination, cooling to obtain porous elastic alloy, and ball-milling the porous elastic alloy to obtain the nano porous elastic alloy;
(2) Primary granulation: uniformly mixing SiO, nano porous elastic alloy and binder according to a proportion, and kneading at a high temperature to obtain primary SiO particles, wherein the kneading temperature is 100-300 ℃ and the kneading time is 30-300min;
(3) And (3) secondary granulation: uniformly mixing primary SiO particles, graphite and a binder according to a proportion, and kneading at a high temperature to obtain the SiO graphite composite material, wherein the kneading temperature is 100-300 ℃ and the kneading time is 30-300min.
The nano porous alloy is prepared by a template method, the SiO graphite composite material is prepared by a solid phase method, and the process is simple and easy to operate; the nano porous elastic alloy and graphite are sequentially coated on the outer side of SiO through twice granulation, so that a double-layer coating structure with SiO as an inner core, nano porous elastic alloy/carbon as an intermediate interlayer and graphite/carbon as an outer shell is formed, each layer of coating particles is more uniform and stable in structure, the structure is more stable when the volume of the buffer SiO expands, the breakage rate of a silicon negative electrode after being charged for many times can be delayed, and the cycle performance of a battery is remarkably improved.
Preferably, the elastic porous alloy is selected from one or more of Fe-Mn alloy, mn-Cu alloy and Mn-Ge alloy.
Preferably, the binder is selected from one or more of asphalt and resin.
Preferably, the pore-forming agent in the step (1) is selected from one or more of urea, ammonium chloride, ammonium carbonate and ammonium bicarbonate.
Preferably, the volume ratio of the elastic alloy powder to the pore-forming agent in the step (1) is 0.6-0.7:0.3-0.4.
Preferably, in the step (2), the mass portion ratio of SiO, the nano porous elastic alloy and the binder is 80-100:20-30:1-10.
Preferably, in the step (3), the mass part ratio of the primary SiO particles, the graphite and the binder is 20-25:1-3:0.1-0.5.
Therefore, the invention has the following beneficial effects:
(1) The nano porous elastic alloy can play a role in buffering the volume expansion of SiO, so that the damage speed of the anode material due to the volume expansion is slowed down, and the cycle performance of the battery is remarkably improved;
(2) The nano porous elastic alloy and graphite are sequentially coated on the outer side of SiO through twice granulation, so that a double-layer coating structure with SiO as an inner core, nano porous elastic alloy/carbon as an intermediate interlayer and graphite/carbon as an outer shell is formed, each layer of coating particles is more uniform and more stable in structure, the structure is more stable when the volume of the buffer SiO expands, the breakage rate of a silicon negative electrode after being charged for many times can be delayed, and the cycle performance of the battery is remarkably improved;
(3) The nano porous elastic alloy has high conductivity, the porous structure shortens the path of lithium ions for embedding SiO, the ion exchange rate of the anode material is obviously increased, and the quick charge performance of the lithium battery is improved.
Detailed Description
The invention is further described below in connection with the following detailed description.
In the present invention, all raw materials are commercially available or commonly used in the industry, and the methods in the following examples are conventional in the art unless otherwise specified.
Example 1:
the SiO-graphite composite negative electrode material is prepared by high-temperature kneading of SiO, graphite, a binder and a nano porous elastic Mn-Cu alloy, wherein the particle size of the nano porous elastic Mn-Cu alloy is 70nm, and the particle size of SiO is 1 mu m.
A preparation method of a long-cycle quick-charging SiO graphite composite anode material comprises the following preparation steps:
(1) Preparing a nano porous elastic alloy: uniformly mixing elastic Mn-Cu alloy powder and ammonia carbonate according to the volume ratio of 0.6:0.4, pressing into a green body, placing the green body in a vacuum inert atmosphere for calcination, heating for primary calcination, heating for secondary calcination, cooling to obtain porous elastic Mn-Cu alloy, and ball-milling the porous elastic alloy to prepare nano porous elastic Mn-Cu alloy;
(2) Primary granulation: the weight portion ratio is 80:20:1 evenly mixing SiO, nano porous elastic alloy and low-temperature asphalt and kneading at high temperature to prepare primary SiO particles, wherein the kneading temperature is 100 ℃ and the kneading time is 300min;
(3) And (3) secondary granulation: uniformly mixing primary SiO particles, graphite, low-temperature asphalt and resin according to a mass ratio of 20:1:0.05:0.05, and kneading at a high temperature to obtain the SiO graphite composite material, wherein the kneading temperature is 100 ℃, and the kneading time is 300min.
Example 2:
the SiO-graphite composite negative electrode material is prepared by high-temperature kneading of SiO, graphite, a binder and a nano porous elastic Mn-Cu alloy, wherein the particle size of the nano porous elastic Mn-Cu alloy is 83nm, and the particle size of the SiO is 10 mu m.
A preparation method of a long-cycle quick-charging SiO graphite composite anode material comprises the following preparation steps:
(1) Preparing a nano porous elastic alloy: uniformly mixing elastic Mn-Cu alloy powder and ammonia carbonate according to the volume ratio of 0.65:0.35, pressing into a green body, placing the green body in a vacuum inert atmosphere for calcination, heating for primary calcination, heating for secondary calcination, cooling to obtain porous elastic Mn-Cu alloy, and ball-milling the porous elastic alloy to prepare nano porous elastic Mn-Cu alloy;
(2) Primary granulation: the weight portion ratio is 85:26: uniformly mixing SiO, nano porous elastic alloy and asphalt, and kneading at high temperature to obtain primary SiO particles, wherein the kneading temperature is 285 ℃, and the kneading time is 60min;
(3) And (3) secondary granulation: uniformly mixing primary SiO particles, graphite, asphalt and resin according to a mass ratio of 22:1.8:0.1:0.1, and kneading at high temperature to obtain the SiO graphite composite material, wherein the kneading temperature is 285 ℃, and the kneading time is 60min.
Example 3:
the SiO-graphite composite negative electrode material is prepared by high-temperature kneading of SiO, graphite, a binder and a nano porous elastic Mn-Cu alloy, wherein the particle size of the nano porous elastic Mn-Cu alloy is 100nm, and the particle size of SiO is 100 mu m.
A preparation method of a long-cycle quick-charging SiO graphite composite anode material comprises the following preparation steps:
(1) Preparing a nano porous elastic alloy: uniformly mixing elastic Mn-Cu alloy powder and ammonia carbonate according to the volume ratio of 0.7:0.4, pressing into a green body, placing the green body in a vacuum inert atmosphere for calcination, heating for primary calcination, heating for secondary calcination, cooling to obtain porous elastic Mn-Cu alloy, and ball-milling the porous elastic alloy to prepare nano porous elastic Mn-Cu alloy;
(2) Primary granulation: the weight portion ratio is 100:30: uniformly mixing SiO, nano porous elastic alloy and low-temperature asphalt, and kneading at high temperature to obtain primary SiO particles, wherein the kneading temperature is 300 ℃ and the kneading time is 30min;
(3) And (3) secondary granulation: uniformly mixing primary SiO particles, graphite, low-temperature asphalt and resin according to a mass ratio of 25:3:0.5, and kneading at a high temperature to obtain the SiO graphite composite material, wherein the kneading temperature is 300 ℃, and the kneading time is 30min.
Example 4:
as compared with example 2, the elastic alloy was Fe-Mn alloy, and the other conditions were the same as in example 2.
Example 5:
as compared with example 2, mn-Ge alloy was used as the elastic alloy, and the other conditions were the same as those in example 2.
Comparative example 1: (common SiO graphite mixing)
A SiO graphite composite negative electrode material is prepared by kneading SiO, graphite and a binder at high temperature.
Comparative example 2: (direct granulation and mixing)
In comparison with example 2, siO, nanoporous elastic alloy, pitch, resin and graphite were all mixed directly with a Wen Zhicheng SiO graphite composite, the remaining conditions being the same as in example 2.
The prepared anode material is made into a lithium battery, the anode of the battery is NCM811, the diaphragm of the battery is a cellgard 2400 lithium battery diaphragm, and the electrolyte is EC/DEC/DMC/LiPF 6 The method comprises the steps of carrying out a first treatment on the surface of the And (3) charging the prepared lithium battery to 3.8V at a constant current of 5C and discharging the prepared lithium battery to 2.0V at a constant current of 1C, and respectively measuring the capacity retention rate of the lithium battery after 300 times, 500 times and 1000 times of cycling.
TABLE 1 cycle performance and cycle times of lithium batteries
| Cycle 300 times (%) | Cycle 500 times (%) | 1000 cycles (%) | |
| Example 1 | 91.57 | 89.88 | 82.43 |
| Example 2 | 92.23 | 90.02 | 83.15 |
| Example 3 | 91.84 | 89.52 | 82.79 |
| Example 4 | 90.22 | 88.54 | 81.46 |
| Example 5 | 90.54 | 88.98 | 81.88 |
| Comparative example 1 | 84.45 | 80.81 | 66.82 |
| Comparative example 2 | 88.52 | 85.26 | 75.14 |
As can be seen from table 1, the battery capacity retention rate of examples 1 to 5 after 1000 cycles was still 80% or more, which is significantly higher than that of comparative examples 1 and 2, and the battery cycle performance degradation rate of examples 1 to 5 was significantly lower than that of comparative example 1 with increasing cycle times;
in comparative example 2, graphite SiO, nano porous elastic alloy, asphalt, resin and graphite are directly mixed and made into a Wen Zhicheng SiO graphite composite material, and the structure of the composite material is poorer in buffering capacity and protective capacity for SiO compared with the invention of the embodiment of the invention, and is easier to break and crush along with the increase of the cycle times.
Claims (8)
1. The long-cycle quick-charging SiO graphite composite anode material is characterized by being prepared by kneading SiO, graphite, an adhesive and a nano porous elastic alloy at high temperature;
the preparation method of the long-cycle quick-charging SiO graphite composite anode material comprises the following preparation steps:
(1) Preparing a nano porous elastic alloy: uniformly mixing elastic alloy powder and a pore-forming agent according to a proportion, pressing into a green body, placing the green body in a vacuum inert atmosphere for calcination, heating for primary calcination, heating for secondary calcination, cooling to obtain porous elastic alloy, and ball-milling the porous elastic alloy to obtain the nano porous elastic alloy;
(2) Primary granulation: uniformly mixing SiO, nano porous elastic alloy and binder according to a proportion, and kneading at a high temperature to obtain primary SiO particles, wherein the kneading temperature is 100-300 ℃ and the kneading time is 30-300min;
(3) And (3) secondary granulation: uniformly mixing primary SiO particles, graphite and a binder according to a proportion, and kneading at a high temperature to obtain the SiO graphite composite material, wherein the kneading temperature is 100-300 ℃ and the kneading time is 30-300min.
2. The long-circulating fast-charging SiO graphite composite anode material according to claim 1, wherein the particle size of the nano porous elastic alloy is 70-100nm, and the particle size of SiO is 1-100 μm.
3. The long-circulating fast-charging SiO graphite composite anode material of claim 1, wherein said nanoporous elastic alloy is selected from one or more of Fe-Mn alloy, mn-Cu alloy and Mn-Ge alloy.
4. The long-circulating fast-charging SiO graphite composite anode material according to claim 1, wherein the binder is one or more selected from asphalt and resin.
5. The long-circulating fast-charging SiO graphite composite anode material according to claim 1, wherein the pore-forming agent in the step (1) is one or more selected from urea, ammonium chloride, ammonium carbonate and ammonium bicarbonate.
6. The long-circulating fast-charging SiO graphite composite anode material according to claim 1, wherein the volume ratio of the elastic alloy powder to the pore-forming agent in the step (1) is 0.6-0.7:0.3-0.4.
7. The long-cycle fast-charging SiO graphite composite anode material according to claim 1, wherein in the step (2), the mass ratio of SiO, nano porous elastic alloy and binder is 80-100:20-30:1-10.
8. The long-circulating fast-charging SiO graphite composite anode material according to claim 1, wherein the mass part ratio of primary SiO particles, graphite and binder in the step (3) is 25-20:1-3:0.1-0.5.
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