CN112786863A - Zn2SiO4Preparation method of high-rate lithium ion battery cathode material - Google Patents
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Abstract
The invention relates to the field of lithium ion batteries, in particular to Zn2SiO4The preparation method of the high-rate lithium ion battery cathode material solves the problem that the high-rate lithium ion battery cathode material has poor electrochemical performance. The invention adopts zinc acetate and tetraethyl orthosilicate as reaction raw materials, adopts a mixed solution of water and ethanol as a solvent, and synthesizes Zn with small grain size at lower temperature and in shorter time by using a microwave stirring and heating method2SiO4(ii) a Zn to be synthesized2SiO4And (3) carrying out carbon coating to improve the conductivity of the sample. Uniformly mixing the sample coated with carbon with a conductive agent, a binder and a dispersant to form slurry, and then coating the slurry on a collectorAnd (3) drying the fluid in vacuum, and carrying out electrochemical performance test, wherein the test result shows that the electrode material has good rate capability and cycle life.
Description
Technical Field
The invention relates to the field of lithium ion batteries, in particular to Zn2SiO4A preparation method of a high-rate lithium ion battery cathode material.
Background
The lithium ion battery mainly comprises a positive electrode and a negative electrode which can generate reactions of releasing and inserting lithium ions, electrolyte which can transmit the lithium ions and a diaphragm which allows the lithium ions to permeate. The anode and cathode materials are the most core parts of the lithium ion battery, and determine the performance of the lithium ion battery. The cathode material is an important component of the lithium ion battery, and the quality of the cathode material directly influences the comprehensive electrochemical performance of the lithium ion battery. At present, the commercialized negative electrode material is graphite, the high rate performance of the graphite is poor, and researchers strive to find a novel negative electrode material with the high rate performance.
The Chinese invention patent (No. CN102976344A) introduces a hydrothermal method for synthesizing Zn2SiO4The method comprises the steps of preparing suspension by using amorphous silicon dioxide and soluble zinc salt as raw materials, adjusting the pH value to 5-13, putting the suspension into a reaction kettle, preserving heat at 160-230 ℃ for 2-24 hours, cooling the reaction kettle, washing and drying the product to obtain the target product Zn2SiO4. Compared with a solid phase method, the method has the advantages that the synthesis temperature of a hydrothermal method is 200 ℃, the synthesis temperature is low, the reaction time is long, the yield is low, and the electrochemical performance characterization is not carried out.
Literature (Nano Energy 73, 2020, 104758) reports a hydrothermal synthesis of Zn2SiO4Method of (1) with Zn (NO)3)2·6H2O and SiO2Dissolving the raw materials in water to prepare a solution, adjusting the pH value of the solution to 10-11 by using NaOH, stirring the solution, putting the solution into a reaction kettle, and keeping the temperature at 220 ℃ for 24 hours. In order to improve the conductivity of the sample, the prepared sample is carbon-coated and is kept at 180 ℃ for 3h and then at 700 ℃ for 3h under the argon atmosphere. Button cells were assembled and tested for electrochemical performance at 0.1A g-1The specific discharge capacity is 640mAh g-1And at a higher magnification of 5A g-1The specific discharge capacity is only 280mAh g-1. The method has long heating and heat preservation period and low yield, and is not suitable for industrial production.
Disclosure of Invention
The invention aims to provide Zn2SiO4The preparation method of the high-rate lithium ion battery cathode material solves the problem that the high-rate lithium ion battery cathode material has poor electrochemical performance.
The technical scheme of the invention is as follows:
zn2SiO4Preparation of high-rate lithium ion battery cathode materialThe method comprises the following steps:
(1) dissolving zinc acetate in an aqueous solvent, and preparing a solution A after magnetic stirring;
(2) dissolving tetraethyl orthosilicate in ethanol, and preparing a solution B after magnetic stirring;
(3) pouring the solution B into the solution A to obtain a mixed solution, carrying out magnetic stirring, carrying out solvothermal synthesis on the mixed solution at 120-220 ℃ for 5-180 min, and carrying out solid-liquid separation on the suspension to obtain a white precipitate, namely Zn2SiO4；
(4) Zn to be synthesized2SiO4Washing with water, and then washing with alcohol; subsequently, a carbon source and Zn2SiO4Uniformly mixing the raw materials according to the mass ratio of (0.1-1) to (3-5), and putting the mixture into a tubular furnace for heat treatment to finally obtain the carbon-coated zinc silicate.
Said Zn2SiO4In the preparation method of the high-rate lithium ion battery negative electrode material, in the step (1), the used aqueous solvent is defined as water or an aqueous solution containing ions or organic solvents.
Said Zn2SiO4In the step (1), the molar ratio of the zinc acetate to the aqueous solvent is (0.5-1.0) - (1.5-3.0), and the magnetic stirring time is 0.5-10 h.
Said Zn2SiO4In the step (2), the mol ratio of tetraethyl orthosilicate to ethanol solvent is (0.5-1.0) - (3.0-6.0), and the magnetic stirring time is 0.5-10 h.
Said Zn2SiO4In the step (3), the mixed solution is magnetically stirred for 0.5 to 10 hours, the heating method is microwave heating, the heating temperature is 120 to 220 ℃, and the heat preservation time is 5 to 180 min.
Said Zn2SiO4In the step (4), the carbon source is one or more than two of sucrose, glucose, furfuryl alcohol and soluble starch, and the heat treatment temperature of the tube furnace is 6The heat preservation time is 1-10 h at 00-800 ℃, and the carbon content in the carbon-coated zinc silicate is 1-10 wt%.
The design idea of the invention is as follows:
the invention adopts zinc acetate and tetraethyl orthosilicate as reaction raw materials, adopts a mixed solution of water and ethanol as a solvent, and synthesizes Zn with small grain size at lower temperature and in shorter time by using a microwave stirring and heating method2SiO4(ii) a Zn to be synthesized2SiO4And (4) carrying out carbon coating to improve the conductivity of the sample. The sample coated with carbon, the conductive agent, the binder and the dispersant are uniformly mixed into slurry, then the slurry is coated on a current collector in a scraping mode, the current collector is dried in vacuum, and an electrochemical performance test is carried out.
The invention has the advantages and beneficial effects that:
1. the invention can synthesize pure-phase Zn with small grain size at lower synthesis temperature and in shorter synthesis time2SiO4。
2. Small grain size Zn synthesized by the invention2SiO4The high-rate electrochemical device has excellent high-rate electrochemical performance, including high specific charge-discharge capacity and good cycle performance, and has good application prospect in high-rate energy storage devices.
3. Zn prepared by the invention2SiO4The negative electrode material exhibits excellent rate capability, at 5A g-1The specific capacity of the current density can still reach 400mAh g-1。
Drawings
FIG. 1 shows that Zn is synthesized in the microwave stirring heating heat preservation of 0.5h at the temperature of 180 DEG C2SiO4XRD pattern of (a). In the figure, the abscissa 2 θ represents the diffraction angle (degree) and the ordinate Intensity represents the relative Intensity (a.u.).
FIG. 2 shows that Zn is synthesized in the microwave stirring heating heat preservation of 0.5h at 180 DEG C2SiO4Scanning electron microscope pictures.
FIG. 3 shows Zn after carbon coating2SiO4And C scanning electron microscope pictures.
FIG. 4 is Zn2SiO4a/C constant current charging and discharging curve map. In the figure, the abscissa Specific capacity represents the Specific capacity (mAh g)-1) The ordinate Voltage represents the Voltage (V vs. li)+/Li)。
FIG. 5 shows Zn2SiO4a/C rate performance test curve. In the figure, the abscissa Voltage represents the Voltage (V vs. li)+/Li), left ordinate Specific capacity represents the Specific capacity (mAh g)-1) The right ordinate of the Coulomb efficiency represents the Coulomb efficiency (%).
FIG. 6 shows Zn2SiO4Cycle stability test curve for/C. In the figure, the abscissa, Cycle number, and the left ordinate, Specific capacity, represent Specific capacity (mAh g)-1) The right ordinate of the Coulomb efficiency represents the Coulomb efficiency (%).
Detailed Description
In the concrete implementation process, Zn of the invention2SiO4The preparation method of the high-rate lithium ion battery negative electrode material comprises the following steps:
(1) dissolving zinc acetate in an aqueous solvent, and preparing a solution A after magnetic stirring;
(2) dissolving tetraethyl orthosilicate in ethanol, and preparing a solution B after magnetic stirring;
(3) pouring the solution B into the solution A to obtain a mixed solution, carrying out magnetic stirring, carrying out solvothermal synthesis on the mixed solution at 120-220 ℃ for 5-180 min, and carrying out solid-liquid separation on the suspension to obtain a white precipitate, namely Zn2SiO4；
(4) Zn to be synthesized2SiO4Washing with water, and then washing with alcohol; subsequently, a carbon source is reacted with Zn2SiO4Uniformly mixing the raw materials according to the mass ratio of (0.1-1) to (3-5), putting the mixture into a tube furnace for heat treatment, and finally obtaining the carbon-coated zinc silicate (Zn)2SiO4/C)。
The feasibility of the present invention is further demonstrated by the following examples.
Example 1
In this example, Zn2SiO4The preparation method of the high-rate lithium ion battery cathode material comprises the following stepsThe following:
(1) dissolving 7.06g of zinc acetate in 37.5mL of deionized water, and magnetically stirring for 30min to prepare a solution A;
(2) dissolving 3mL of tetraethyl orthosilicate in 22.5mL of ethanol, and magnetically stirring for 30min to prepare a solution B;
(3) pouring the solution B into the solution A, magnetically stirring for 40min, placing the mixed solution into a microwave workstation, keeping the temperature at 180 ℃ for 30min, and performing solid-liquid separation on the suspension to obtain a white precipitate, namely Zn2SiO4。
As shown in FIG. 1, after drying, pure phase Zn is obtained2SiO4. Zn observed under a scanning electron microscope, as shown in FIG. 22SiO4Are submicron particles.
(4) A carbon source is reacted with Zn2SiO4Uniformly mixing the raw materials according to the mass ratio of 1:4, putting the mixture into a tube furnace for heat treatment to finally obtain carbon-coated zinc silicate (Zn)2SiO4and/C). Wherein the carbon source is furfuryl alcohol, the heat treatment temperature of the tube furnace is 650 ℃, the heat preservation time is 3H, and the heat treatment protective atmosphere is 95 vol% Ar +5 vol% H2. The carbon-coated zinc silicate had a carbon content of 6 wt%.
As shown in fig. 3, Zn after carbon coating treatment2SiO4The morphology of the/C is not changed. The small grain size Zn, as shown in FIG. 4, was used to assemble the electrode materials into button cells and characterize their electrochemical performance2SiO4At 0.1A g-1The specific discharge capacity under the current density reaches 670mAh g-1. As shown in fig. 5, the electrode material still has good cycling stability under different multiplying factors. Electrode materials at 5A g-1The specific capacity of the mass can still reach 400mAh g under the current density-1And excellent rate performance is exhibited.
As shown in FIG. 6, the cycling stability test indicates Zn2SiO4the/C electrode exhibited excellent cycling stability at 1A g-1The specific capacity of 200 times of circulation under the current density is still higher than 500mAh g-1。
Example 2
In this example, Zn2SiO4The preparation method of the high-rate lithium ion battery negative electrode material comprises the following steps:
(1) dissolving 10g of zinc acetate in 55mL of deionized water, and magnetically stirring for 1h to prepare a solution A;
(2) dissolving 4.5mL of tetraethyl orthosilicate in 35.5mL of ethanol, and magnetically stirring for 1h to prepare a solution B;
(3) pouring the solution B into the solution A, magnetically stirring for 2 hours, putting the mixed solution into a microwave workstation, and preserving heat for 1 hour at 160 ℃. Separating the suspension liquid to obtain white precipitate Zn2SiO4Observation under a scanning electron microscope, Zn2SiO4Are submicron particles.
(4) A carbon source is reacted with Zn2SiO4Uniformly mixing the raw materials according to the mass ratio of 1:6, putting the mixture into a tube furnace for heat treatment, and finally obtaining the carbon-coated zinc silicate (Zn)2SiO4and/C). Wherein the carbon source is soluble starch, the heat treatment temperature of the tube furnace is 700 ℃, the heat preservation time is 5H, and the heat treatment protective atmosphere is 95 vol% Ar +5 vol% H2. The carbon-coated zinc silicate had a carbon content of 4 wt%.
Example 3
In this example, Zn2SiO4The preparation method of the high-rate lithium ion battery negative electrode material comprises the following steps:
(1) dissolving 5g of zinc acetate in 30mL of deionized water, and magnetically stirring for 2h to prepare a solution A;
(2) dissolving 2mL of tetraethyl orthosilicate in 15mL of ethanol, and magnetically stirring for 2 hours to prepare a solution B;
(3) pouring the solution B into the solution A, magnetically stirring for 4 hours, putting the mixed solution into a microwave workstation, and preserving the temperature for 15min at 200 ℃. Separating the suspension liquid to obtain white precipitate Zn2SiO4Observation under a scanning electron microscope, Zn2SiO4Are submicron particles.
(4) A carbon source is reacted with Zn2SiO4Uniformly mixing the raw materials according to the mass ratio of 1:8, putting the mixture into a tube furnace for heat treatment to finally obtain carbon-coated zinc silicate (Zn)2SiO4and/C). Wherein the carbon source is glucose, and the heat treatment temperature of the tube furnace isThe temperature is 750 ℃, the heat preservation time is 4H, and the heat treatment protective atmosphere is 95 vol% Ar +5 vol% H2. The carbon-coated zinc silicate had a carbon content of 8 wt%.
The example results show that the small grain size Zn produced by the present invention2SiO4Has excellent application prospect in the cathode material of the high-rate lithium ion battery.
Claims (6)
1. Zn2SiO4The preparation method of the high-rate lithium ion battery cathode material is characterized by comprising the following steps of:
(1) dissolving zinc acetate in an aqueous solvent, and preparing a solution A after magnetic stirring;
(2) dissolving tetraethyl orthosilicate in ethanol, and preparing a solution B after magnetic stirring;
(3) pouring the solution B into the solution A to obtain a mixed solution, carrying out magnetic stirring, carrying out solvothermal synthesis on the mixed solution at 120-220 ℃ for 5-180 min, and carrying out solid-liquid separation on the suspension to obtain a white precipitate, namely Zn2SiO4；
(4) Zn to be synthesized2SiO4Washing with water, and then washing with alcohol; subsequently, a carbon source and Zn2SiO4Uniformly mixing the raw materials according to the mass ratio of (0.1-1) to (3-5), and putting the mixture into a tubular furnace for heat treatment to finally obtain the carbon-coated zinc silicate.
2. Zn according to claim 12SiO4The preparation method of the high-rate lithium ion battery negative electrode material is characterized in that in the step (1), the used aqueous solvent is defined as water or an aqueous solution containing ions or organic solvents.
3. Zn according to claim 12SiO4The preparation method of the high-rate lithium ion battery cathode material is characterized in that in the step (1), the molar ratio of the zinc acetate to the aqueous solvent is (0.5-1.0) - (1.5-3.0), and the magnetic stirring time is 0.5-10 h.
4. Zn according to claim 12SiO4The preparation method of the high-rate lithium ion battery cathode material is characterized in that in the step (2), the molar ratio of tetraethyl orthosilicate to an ethanol solvent is (0.5-1.0) - (3.0-6.0), and the magnetic stirring time is 0.5-10 h.
5. Zn according to claim 12SiO4The preparation method of the high-rate lithium ion battery cathode material is characterized in that in the step (3), the magnetic stirring time of the mixed solution is 0.5-10 h, the heating method is microwave heating, the heating temperature is 120-220 ℃, and the heat preservation time is 5-180 min.
6. Zn according to claim 12SiO4The preparation method of the high-rate lithium ion battery cathode material is characterized in that in the step (4), the carbon source is one or more than two of sucrose, glucose, furfuryl alcohol and soluble starch, the heat treatment temperature of the tube furnace is 600-800 ℃, the heat preservation time is 1-10 hours, and the carbon content in the carbon-coated zinc silicate is 1-10 wt%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113809282A (en) * | 2021-09-17 | 2021-12-17 | 河北工业大学 | High-capacity nitrogen-doped carbon-coated SiOxPreparation method of nano-beam lithium ion battery cathode material |
| CN114373894A (en) * | 2022-01-11 | 2022-04-19 | 中国科学院金属研究所 | Zn with high multiplying power and long circulation stability2SiO4Preparation method of lithium ion battery cathode |
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| CN102206077A (en) * | 2011-03-21 | 2011-10-05 | 天津大学 | Preparation method of zinc cobalt sodium silicate nano powder |
| CN105502421A (en) * | 2016-01-08 | 2016-04-20 | 中山大学 | Preparation method of zinc silicate hollow micron ball |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113809282A (en) * | 2021-09-17 | 2021-12-17 | 河北工业大学 | High-capacity nitrogen-doped carbon-coated SiOxPreparation method of nano-beam lithium ion battery cathode material |
| CN113809282B (en) * | 2021-09-17 | 2023-02-14 | 河北工业大学 | High-capacity nitrogen-doped carbon-coated SiO x Preparation method of nano-beam lithium ion battery cathode material |
| CN114373894A (en) * | 2022-01-11 | 2022-04-19 | 中国科学院金属研究所 | Zn with high multiplying power and long circulation stability2SiO4Preparation method of lithium ion battery cathode |
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