CN112803013A - Method for preparing silicon-copper alloy of lithium ion power battery as negative electrode material - Google Patents
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Abstract
本发明公开了锂离子电池电极材料制备技术领域的一种制备锂离子动力电池硅铜合金为负极材料的方法，包括以下步骤：(1)以质量比(3‑5):1称取硅粉和铜粉并混合，随后放入球磨罐中，以球料比(10‑30):1向球磨罐中加入钢球；(2)将球磨罐置于行星球磨机上，先以50‑200r/min低速球磨1‑2h，再以300‑500r/min高速球磨6‑18h，过滤后，得到复合材料；(3)将复合材料用玛瑙研钵充分研磨均匀，然后将研磨后的复合材料、乙炔黑和水性粘结剂按质量比8:1:1混合，得到混合料；(4)向混合料中加入超纯水和无水乙醇，超纯水和无水乙醇的体积比大于10:1，将其充分混合后调成粘度适宜的浆料，得到负极材料；本发明优化后的Si‑Cu3Si‑Cu纳米复合阳极具有良好的循环性能和可逆容量。
The invention discloses a method for preparing a lithium-ion power battery silicon-copper alloy as a negative electrode material in the technical field of lithium-ion battery electrode material preparation, comprising the following steps: (1) weighing silicon powder in a mass ratio of (3-5):1 Mix with the copper powder, then put it into the ball mill tank, add steel balls to the ball mill tank with a ball-to-material ratio (10-30): 1; (2) place the ball mill tank on the planetary ball mill, first use 50-200r/ min low-speed ball milling for 1-2 h, then high-speed ball milling at 300-500 r/min for 6-18 h, after filtration, the composite material was obtained; (3) the composite material was fully ground with an agate mortar and uniform, and then the ground composite material, acetylene The black and water-based binders are mixed in a mass ratio of 8:1:1 to obtain a mixture; (4) ultrapure water and absolute ethanol are added to the mixture, and the volume ratio of ultrapure water and absolute ethanol is greater than 10:1 , fully mixed and adjusted into a slurry with suitable viscosity to obtain a negative electrode material; the optimized Si-Cu 3 Si-Cu nano-composite anode of the present invention has good cycle performance and reversible capacity.
Description
Technical Field
The invention relates to the technical field of preparation of lithium ion battery electrode materials, in particular to a method for preparing a silicon-copper alloy cathode material of a lithium ion power battery.
Background
It is well known that energy density and long cycle life are important criteria for rechargeable Lithium Ion Batteries (LIBs). However, the graphite anode currently commercialized hardly meets the increasing demand for the new generation of lithium ion batteries due to its low capacity. Therefore, it is of great interest to explore materials with high energy density and long cycle life.
Among the numerous anode materials that are currently in existence, silicon-based anode materials are considered to be one of the most promising candidates for replacing commercial graphite anodes. The silicon-based material as the lithium ion battery cathode material has the following advantages: theoretical maximum specific capacity (about 4200mA h < -1 >), low working voltage (about 0.4V vs. Li/Li < + >), abundant natural resources and the like. However, lithium intercalation/deintercalation with cycling leads to a drastic volume expansion (300%) of the electrode, resulting in severe pulverization, separation, and conductivity degradation of the electrode material, which leads to a rapid capacity decrease and a decrease in the cycle life of the silicon negative electrode. In addition to nano modification of silicon, the method attempts to be compounded or alloyed with silicon to relieve volume change and improve conductivity, and for this reason, an environment-friendly and simple and convenient preparation method is provided, and an attempt is made by using a Si-Cu alloy as a negative electrode material. Conductive and inactive Cu formed in silicon3Si phase as buffer medium, Cu3Si has excellent mechanical flexibility and high electronic conductivity, and can slow down structural degradation and provide high conductivity. Optimized Si-Cu3The Si-Cu nano composite anode has good cycle performance and reversible capacity.
Disclosure of Invention
The invention aims to provide a method for preparing a silicon-copper alloy of a lithium ion power battery as a negative electrode material, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following scheme to realize the following steps:
the invention provides a method for preparing a silicon-copper alloy cathode material of a lithium ion power battery, which comprises the following steps:
(1) weighing silicon powder and copper powder according to the mass ratio of (3-5) to 1, mixing, then putting into a ball milling tank, and adding steel balls into the ball milling tank according to the ball material ratio of (10-30) to 1;
(2) placing the ball milling tank on a planetary ball mill, firstly carrying out low-speed ball milling for 1-2h at 50-200r/min, then carrying out high-speed ball milling for 6-18h at 500r/min with 300-;
(3) fully and uniformly grinding the composite material by using an agate mortar, and then mixing the ground composite material, acetylene black and a water-based binder according to a mass ratio of 8:1:1 to obtain a mixture;
(4) adding ultrapure water and absolute ethyl alcohol into the mixture, wherein the volume ratio of the ultrapure water to the absolute ethyl alcohol is more than 10:1, fully mixing the ultrapure water to the absolute ethyl alcohol, and then preparing into slurry with appropriate viscosity to obtain the cathode material.
Preferably, in the step (1), the particle size of the silicon powder is 5-20 μm, and the particle size of the copper powder is 200-500 meshes.
Preferably, in the step (1), the steel balls are placed into deionized water in advance, subjected to ultrasonic treatment, dried and then placed into a ball milling tank.
Preferably, in the step (3), the aqueous binder is a sodium alginate solution with a mass fraction of 3%.
The invention also provides an application of the silicon-copper alloy for preparing the lithium ion power battery as a negative electrode material, which specifically comprises the following steps:
s1: coating the prepared slurry on a current collector on a copper foil flatly and uniformly by using a full-automatic coating machine, and drying the coated copper foil in an oven;
s2: tabletting the copper foil dried in the step S1 by using a powder tabletting machine, controlling the gauge pressure to be 10MPa, and processing the compacted tablets into electrode plates by using a tablet punching machine;
s3: and drying the electrode plate, putting the electrode plate into a glove box filled with argon gas, assembling a battery, wherein the diaphragm is a polypropylene film, the electrolyte is the mixture of lithium hexafluorophosphate, ethylene carbonate and diethyl carbonate, the electrolyte is 10 wt% of vinyl fluoride carbonate, and the electrode plate is a negative electrode, and assembling the battery into the button cell with the model number of CR 2025.
In step S3, the concentration of lithium hexafluorophosphate is 1M, and the volume ratio of ethylene carbonate to diethyl carbonate is 1: 1.
The invention has the beneficial effects that:
(1) the method provided by the invention is a chemical mechanical synthesis method, the adopted raw materials are common chemicals such as commercial micron-sized silicon powder, copper powder and the like, and the raw materials are easy to obtain and low in cost;
(2) the composite material prepared by the simple solid-phase reaction has higher Initial Coulombic Efficiency (ICE) than the composite material prepared by the chemical method, because the composite material prepared by the chemical method contains residual impurities;
(3) the invention adopts a solid-state synthesis method which can be applied to the current production process, and has the advantages of improving the simplicity of the process and the possibility of large-scale production;
(4) the invention has no acid washing, no toxicity, no participation and discharge of organic solvents and gases such as pungent smell and the like in solid synthesis, and is beneficial to environmental protection in industrial production;
(5) in the invention, the high temperature generated by the ball milling collision of the silicon and copper phase interface is subjected to chemical reaction to generate Cu3A Si phase connecting the copper phase and the silicon phase, the structure between the particles being Si-Cu3Si-Cu nanocomposite anodes using conductive and inactive Cu formed in silicon3Si phase as buffer medium, highly conductive Cu3Si has excellent mechanical flexibility and high electronic conductivity, can slow down structural degradation, provides high conductivity, and is optimized to Si-Cu3The Si-Cu nano composite anode has good cycle performance and reversible capacity.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a scanning electron micrograph of a commercial pure silicon powder according to example 1 of the present invention;
FIG. 2 is a scanning electron microscope image of the composite material after ball milling of the silicon powder and the copper powder at different times in example 1 of the present invention;
FIG. 3 is a graph showing the cycle life of a half cell of a composite material and pure silicon powder after ball milling of silicon powder and copper powder at corresponding times in examples 1, 3 and 4 of the present invention;
FIG. 4 is a graph showing the cell impedance of the composite material and pure silicon powder after ball milling of the silicon powder and copper powder for the corresponding times in examples 1, 3 and 4 of the present invention.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. 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.
Example 1
A method for preparing a silicon-copper alloy of a lithium ion power battery as a negative electrode material specifically comprises the following steps:
(1) weighing 0.8g of silicon powder with the particle size of 20 mu m and 0.2g of copper powder with the particle size of 400 meshes, mixing, then putting into a ball milling tank, and adding 20g of steel balls into the ball milling tank;
(2) placing the ball milling tank on a planetary ball mill, firstly carrying out low-speed ball milling for 1h at 100r/min, then carrying out high-speed ball milling for 6h at 400r/min, and filtering to obtain a composite material;
(3) fully and uniformly grinding the composite material by using an agate mortar for 30min, and then mixing the ground composite material, acetylene black and a water-based binder according to a mass ratio of 8:1:1 to obtain a mixture;
(4) adding ultrapure water and absolute ethyl alcohol into the mixture, wherein the volume ratio of the ultrapure water to the absolute ethyl alcohol is more than 10:1, fully mixing the ultrapure water to the absolute ethyl alcohol, and then preparing into slurry with appropriate viscosity to obtain the cathode material.
Putting the steel ball into deionized water in advance, performing ultrasonic treatment, drying and then putting into a ball milling tank; the aqueous binder is sodium alginate solution with the mass fraction of 3%.
The application of the silicon-copper alloy for preparing the lithium ion power battery as the negative electrode material specifically comprises the following steps:
s1: coating the prepared slurry on a current collector on a copper foil flatly and uniformly by using a full-automatic coating machine, drying the coated copper foil in an oven, and drying at 60 ℃ for 12 hours;
s2: tabletting the copper foil dried in the step S1 by using a powder tabletting machine, controlling the gauge pressure to be 10MPa, and processing the compacted tablets into electrode plates by using a tablet punching machine;
s3: and drying the electrode plate in a vacuum oven at 120 ℃ for 12h, putting the electrode plate into a glove box filled with argon gas, assembling a battery, wherein a diaphragm is a polypropylene film, an electrolyte is a mixture of lithium hexafluorophosphate, ethylene carbonate and diethyl carbonate, an electrolyte is 10 wt% of vinyl fluoride carbonate, and the electrode plate is a negative electrode, and assembling the battery into a CR2025 button battery.
The concentration of lithium hexafluorophosphate was 1M and the volume ratio of ethylene carbonate to diethyl carbonate was 1: 1.
Example 2
A method for preparing a silicon-copper alloy of a lithium ion power battery as a negative electrode material specifically comprises the following steps:
(1) weighing 0.6g of silicon powder with the particle size of 20 mu m and 0.2g of copper powder with the particle size of 400 meshes, mixing, then putting into a ball milling tank, and adding 30g of steel balls into the ball milling tank;
(2) placing the ball milling tank on a planetary ball mill, firstly carrying out low-speed ball milling for 1h at 50r/min, then carrying out high-speed ball milling for 18h at 500r/min, and filtering to obtain a composite material;
(3) fully and uniformly grinding the composite material by using an agate mortar for 30min, and then mixing the ground composite material, acetylene black and a water-based binder according to a mass ratio of 8:1:1 to obtain a mixture;
(4) adding ultrapure water and absolute ethyl alcohol into the mixture, wherein the volume ratio of the ultrapure water to the absolute ethyl alcohol is more than 10:1, fully mixing the ultrapure water to the absolute ethyl alcohol, and then preparing into slurry with appropriate viscosity to obtain the cathode material.
Putting the steel ball into deionized water in advance, performing ultrasonic treatment, drying and then putting into a ball milling tank; the aqueous binder is sodium alginate solution with the mass fraction of 3%.
The application of the silicon-copper alloy for preparing the lithium ion power battery as the negative electrode material specifically comprises the following steps:
s1: coating the prepared slurry on a current collector on a copper foil flatly and uniformly by using a full-automatic coating machine, drying the coated copper foil in an oven, and drying at 60 ℃ for 12 hours;
s2: tabletting the copper foil dried in the step S1 by using a powder tabletting machine, controlling the gauge pressure to be 10MPa, and processing the compacted tablets into electrode plates by using a tablet punching machine;
s3: and drying the electrode plate in a vacuum oven at 120 ℃ for 12h, putting the electrode plate into a glove box filled with argon gas, assembling a battery, wherein a diaphragm is a polypropylene film, an electrolyte is a mixture of lithium hexafluorophosphate, ethylene carbonate and diethyl carbonate, an electrolyte is 10 wt% of vinyl fluoride carbonate, and the electrode plate is a negative electrode, and assembling the battery into a CR2025 button battery.
The concentration of lithium hexafluorophosphate was 1M and the volume ratio of ethylene carbonate to diethyl carbonate was 1: 1.
Example 3
On the basis of example 1, the ball milling time in step (2) was adjusted to 12 hours while keeping the other conditions unchanged.
Example 4
On the basis of example 1, the ball milling time in step (2) was adjusted to 18 hours while keeping the other conditions unchanged.
As can be seen from fig. 1: commercially pure silicon powders are irregular in shape but have a particle size of substantially between 20 and 25 μm.
As can be seen from fig. 3: compared with a pure silicon battery, the cycle life performance of the silicon-copper alloy is greatly improved. Under different ball milling time, Si-Cu is formed after ball milling for 6h3After the Si-Cu alloy negative electrode material is circulated for 50 circles under the current density of 100mA/g, the discharge specific capacity can be kept at 457.536mAh/g, and only pure silicon powder is leftLower 135.431 mAh/g.
As can be seen from fig. 4: the semicircle of the high frequency region represents the SEI film resistance (Rf) and the straight line at the low frequency represents the Warburg resistance (W) in the electrolyte. It is clear that the conductivity ratio of pure silicon Si-Cu3The Si-Cu alloy cathode material is much poorer, and among the four electrodes, the silicon-copper alloy electrode has the smallest resistance after ball milling for 6 hours, which is caused by the introduction of copper, and the high conductivity of the copper can provide mechanical strength, so that the charge transfer dynamics is enhanced, and the charge transfer resistance is reduced.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to 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 do not necessarily 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.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not exhaustive. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (7)
1. A method for preparing a silicon-copper alloy of a lithium ion power battery as a negative electrode material is characterized by comprising the following steps:
(1) weighing silicon powder and copper powder according to the mass ratio of (3-5) to 1, mixing, then putting into a ball milling tank, and adding steel balls into the ball milling tank according to the ball material ratio of (10-30) to 1;
(2) placing the ball milling tank on a planetary ball mill, firstly carrying out low-speed ball milling for 1-2h at 50-200r/min, then carrying out high-speed ball milling for 6-18h at 500r/min with 300-;
(3) fully and uniformly grinding the composite material by using an agate mortar, and then mixing the ground composite material, acetylene black and a water-based binder according to a mass ratio of 8:1:1 to obtain a mixture;
(4) adding ultrapure water and absolute ethyl alcohol into the mixture, wherein the volume ratio of the ultrapure water to the absolute ethyl alcohol is more than 10:1, fully mixing the ultrapure water to the absolute ethyl alcohol, and then preparing into slurry with appropriate viscosity to obtain the cathode material.
2. The method for preparing the silicon-copper alloy for the lithium ion power battery as the negative electrode material as claimed in claim 1, wherein in the step (1), the particle size of the silicon powder is 5-20 μm, and the particle size of the copper powder is 200-500 meshes.
3. The method for preparing the silicon-copper alloy cathode material of the lithium ion power battery as claimed in claim 1, wherein in the step (1), the steel ball is placed into deionized water in advance, is subjected to ultrasonic treatment, is dried and is then placed into a ball milling tank.
4. The method for preparing the silicon-copper alloy cathode material of the lithium ion power battery as claimed in claim 1, wherein in the step (3), the aqueous binder is a sodium alginate solution with a mass fraction of 3%.
5. The application of the silicon-copper alloy for preparing the lithium ion power battery as the negative electrode material in claim 1 is characterized in that the negative electrode material is applied to a button battery.
6. The application of the silicon-copper alloy for preparing the lithium ion power battery as the negative electrode material according to claim 5 is characterized by comprising the following steps:
s1: coating the prepared slurry on a current collector on a copper foil flatly and uniformly by using a full-automatic coating machine, and drying the coated copper foil in an oven;
s2: tabletting the copper foil dried in the step S1 by using a powder tabletting machine, controlling the gauge pressure to be 10MPa, and processing the compacted tablets into electrode plates by using a tablet punching machine;
s3: and drying the electrode plate, putting the electrode plate into a glove box filled with argon gas, assembling a battery, wherein the diaphragm is a polypropylene film, the electrolyte is the mixture of lithium hexafluorophosphate, ethylene carbonate and diethyl carbonate, the electrolyte is 10 wt% of vinyl fluoride carbonate, and the electrode plate is a negative electrode, and assembling the battery into the button cell with the model number of CR 2025.
7. The use of claim 6, wherein in step S3, the concentration of lithium hexafluorophosphate is 1M, and the volume ratio of ethylene carbonate to diethyl carbonate is 1: 1.
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| CN114695864A (en) * | 2022-04-25 | 2022-07-01 | 安徽工业大学 | Preparation method of phosphorus-doped silicon-copper alloy negative electrode material of lithium ion battery |
| CN114695864B (en) * | 2022-04-25 | 2023-09-08 | 安徽工业大学 | Preparation method of phosphorus-doped silicon-copper alloy negative electrode material of lithium ion battery |
| CN115275212A (en) * | 2022-08-10 | 2022-11-01 | 哈尔滨工业大学 | A kind of preparation method of copper-based current collector for anode-free lithium ion battery |
| CN115954443A (en) * | 2022-10-18 | 2023-04-11 | 贵州中水材料科技有限公司 | A preparation method of carbon-coated silicon-copper alloy negative electrode material for lithium ion battery |
| CN115954443B (en) * | 2022-10-18 | 2023-10-27 | 贵州中水材料科技有限公司 | Preparation method of carbon-coated silicon-copper alloy negative electrode material of lithium ion battery |
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Application publication date: 20210514 |