CN110697788A - Method for synthesizing zinc ferrite lithium battery negative electrode material by carbonate coprecipitation method - Google Patents
Method for synthesizing zinc ferrite lithium battery negative electrode material by carbonate coprecipitation method Download PDFInfo
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Abstract
The invention discloses a method for synthesizing a zinc ferrite lithium battery cathode material by using a carbonate coprecipitation method, belonging to the technical field of preparation of lithium ion battery cathode materials. The invention adopts a carbonate coprecipitation technology, the prepared iron-zinc solution with certain concentration is added into a sodium carbonate solution with certain concentration at a constant speed, then an iron-zinc precursor is generated through coprecipitation, the obtained precursor is subjected to suction filtration, washing, ultrasonic treatment and spray drying, and then the high-capacity zinc ferrite lithium battery cathode material is obtained through high-temperature treatment in the air atmosphere. The zinc ferrite lithium ion battery cathode material prepared by the invention still maintains the capacity of more than 1000mAh/g after 100 cycle periods, and can obtain a high-capacity high-cycle zinc ferrite lithium battery cathode material.
Description
Technical Field
The invention belongs to the technical field of preparation of lithium ion battery cathode materials, and particularly relates to a method for synthesizing a zinc ferrite lithium battery cathode material by using a carbonate coprecipitation method.
Background
In recent years, with the rapid development of 3C digital products, energy storage, communication and new energy automobile fields, people have more and more stringent requirements on the performance of lithium ion batteries. With the progress of research, silicon is known to be the lithium ion battery anode material with the highest specific capacity at present (4200mAh/g), but due to the huge volume effect (> 300%), the electrochemical performance of the silicon electrode material is rapidly deteriorated. The graphite has excellent conductivity, and the problem of poor conductivity of the silicon-based material can be solved after the graphite is compounded with silicon. Under normal temperature, silicon and graphite have strong chemical stability and are difficult to generate strong acting force, so that a high-energy ball milling method and a chemical vapor deposition method are commonly used for preparing the silica-graphite composite material, but the cycle performance of the material is still not greatly improved. Therefore, there is a need to provide a new method for preparing a high-capacity high-cycle negative electrode material to promote the development of negative electrode materials for lithium ion batteries.
Disclosure of Invention
The invention solves the technical problem of providing the method for synthesizing the zinc ferrite lithium battery cathode material by using the carbonate coprecipitation method, which has simple process and convenient operation, and the zinc ferrite lithium battery cathode material prepared by the method has higher capacity and higher cycling stability.
The invention adopts the following technical scheme for solving the technical problems, and the method for synthesizing the zinc ferrite lithium battery cathode material by using the carbonate coprecipitation method is characterized by comprising the following specific processes:
step S1: dissolving soluble ferric salt and soluble zinc salt in deionized water to prepare a 1-2mol/L iron-zinc solution, and placing the prepared iron-zinc solution on a magnetic stirrer to be stirred at a constant speed for later use, wherein the soluble ferric salt is ferric nitrate, ferric sulfate, ferric chloride or ferric chloride hydrate, the soluble zinc salt is zinc nitrate, zinc nitrate hydrate, zinc chloride or zinc acetate, and the molar ratio of iron ions to zinc ions in the iron-zinc solution is 1.98-2.01: 1;
step S2: dissolving anhydrous sodium carbonate in deionized water to prepare a sodium carbonate solution with the concentration of 1-2.5mol/L, and placing the prepared sodium carbonate solution on a magnetic stirrer to stir at a constant speed for later use;
step S3: adding the iron-zinc solution obtained in the step S1 into a sodium carbonate solution through a peristaltic pump, reacting to generate a zinc ferrite precursor precipitate, monitoring the pH value of the mixed system, and controlling the pH value range of the mixed system to be 6.5-7.8 when the reaction is continuously carried out;
step S4: and (4) sequentially carrying out suction filtration and water washing on the zinc ferrite precursor precipitate obtained in the step (S3) to prepare a suspension, carrying out ultrasonic treatment on the suspension, carrying out spray drying on the suspension to obtain a precursor, heating the precursor to 700-900 ℃ at a heating rate of 2-3 ℃/min under the air condition, carrying out heat preservation for 2-4h, naturally cooling to room temperature, and sieving the obtained sintered product with a 250-mesh sieve to finally obtain the high-capacity high-cycle zinc ferrite lithium battery cathode material.
Further preferably, the concentration of the iron-zinc solution in step S1 is 1.2 mol/L.
Further preferably, the concentration of the sodium carbonate solution in step S2 is 2 mol/L.
Further preferably, the flow rate of the peristaltic pump in step S3 is set to be in the range of 0.5-3 mL/min.
The invention relates to a method for synthesizing a zinc ferrite lithium battery cathode material by using a carbonate coprecipitation method, which is characterized by comprising the following specific steps of:
step S1: weighing 0.03mol of ferric trichloride hexahydrate and 0.015mol of zinc chloride, dissolving in deionized water to prepare 1.2mol/L iron-zinc solution, and placing the solution on a magnetic stirrer to be stirred for later use;
step S2: weighing 0.08mol of anhydrous sodium carbonate, dissolving in deionized water to prepare 2mol/L sodium carbonate solution, and placing on a magnetic stirrer for stirring for later use;
step S3: adding the iron-zinc solution obtained in the step S1 into the sodium carbonate solution obtained in the step S2 through a peristaltic pump at the pump speed of 1mL/min, and reacting to generate a zinc ferrite precursor precipitate;
step S4: performing suction filtration and water washing on the zinc ferrite precursor obtained in the step S3 for 2 times to prepare 400mL of suspension, performing ultrasonic treatment for 1h, performing spray drying, finally placing the precursor obtained by spray drying in a muffle furnace, heating to 800 ℃ under the air condition, keeping the temperature for 2h, naturally cooling to room temperature, wherein the heating rate is 2.5 ℃/min, and sieving the obtained sintered material with a 250-mesh sieve to finally obtain the zinc ferrite lithium battery cathode material;
uniformly mixing the prepared zinc ferrite, superconducting carbon and polyvinylidene fluoride according to the mass ratio of 4:4:2, adding N-methyl pyrrolidone, continuously stirring until the material has fluidity, coating the mixed slurry on copper foil, drying and cutting into pieces to obtain pole pieces, putting the pole pieces into a glove box, taking a metal lithium piece as a counter electrode, adopting a polypropylene diaphragm and 1mol/L LiPF6The solution of EC, DEC and EMC is electrolyte, wherein EC is ethylene carbonate, DEC is diethyl carbonate, EMC is ethyl methyl carbonate, the volume ratio of EC to DEC to EMC is 1:1:1, and the solution is assembled into a CR2032 type button cell in a glove box filled with dry argon, the first charging specific capacity of the button cell is 1109.6mAh/g, the first efficiency is 70.12%, and the capacity retention rate after 100 charging and discharging at 0.1C is 127.3%.
Compared with the prior art, the invention has the following beneficial effects: the method is simple and easy to implement, can synthesize a pure spherical zinc ferrite sample with large grain size and regular appearance, and the spherical zinc ferrite sample can effectively buffer the volume expansion caused by charge and discharge, improve the lithium release and insertion channel of the material, give full play to the capacity of the material and have better circulation stability.
Detailed Description
The present invention is described in further detail below with reference to examples, but it should not be construed that the scope of the above subject matter of the present invention is limited to the following examples, and that all the technologies realized based on the above subject matter of the present invention belong to the scope of the present invention.
Example 1
1. Preparing a lithium battery negative electrode material:
weighing 0.03mol of ferric trichloride hexahydrate and 0.015mol of zinc chloride, dissolving in deionized water to prepare 1.2mol/L iron-zinc solution, and placing the solution on a magnetic stirrer to be stirred for later use; weighing 0.08mol of anhydrous sodium carbonate, dissolving the anhydrous sodium carbonate in deionized water to prepare 2mol/L sodium carbonate solution, and placing the solution on a magnetic stirrer to be stirred for later use; then adding the iron-zinc solution into the sodium carbonate solution through a peristaltic pump at the pump speed of 1mL/min, and reacting to generate zinc ferrite precursor precipitate.
And (3) precipitating, filtering and washing the obtained zinc ferrite precursor for 2 times to prepare 400mL of suspension, carrying out ultrasonic treatment for 1h, carrying out spray drying, finally placing the precursor obtained by spray drying in a muffle furnace, heating to 800 ℃ under the air condition, preserving the temperature for 2h, naturally cooling to room temperature at the heating rate of 2.5 ℃/min, and sieving the obtained sintered material with a 250-mesh sieve to finally obtain the zinc ferrite lithium battery negative electrode material.
2. And (3) testing electrical properties:
uniformly mixing the prepared zinc ferrite, superconducting carbon and polyvinylidene fluoride according to the mass ratio of 4:4:2, adding N-methyl pyrrolidone, continuously stirring until the material has fluidity, coating the mixed slurry on copper foil, drying and cutting into pieces to obtain pole pieces, putting the pole pieces into a glove box, taking a metal lithium piece as a counter electrode, adopting a polypropylene diaphragm and 1mol/L LiPF6And a solution of/EC + DEC + EMC (wherein EC is ethylene carbonate, DEC is diethyl carbonate, EMC is ethyl methyl carbonate, and the volume ratio of EC to DEC to EMC is 1:1:1) is used as an electrolyte, and the electrolyte is assembled into the CR2032 type button cell in a glove box filled with dry argon.
And (3) testing performance: the electrical property test of the button cell is carried out on a blue light test system or a Xinwei constant current tester, all the charge and discharge tests of the invention are constant current charge and discharge, the voltage interval is 0.005V-3.0V, and the test temperature is 25 +/-2 ℃. The test process and steps are as follows: (1)0.1C to 0.005V; (2) standing for 1 min; (3)0.1C to 3.0V; (4) standing for 1 min; (5) the cycle is 100 times. The test results are shown in Table 1.
Example 2
0.03015mol of ferric trichloride hexahydrate and 0.015mol of zinc chloride are weighed and dissolved in deionized water to prepare 1.2mol/L iron-zinc solution, and the iron-zinc solution is placed on a magnetic stirrer to be stirred for standby; weighing 0.08mol of anhydrous sodium carbonate, dissolving the anhydrous sodium carbonate in deionized water to prepare 2mol/L sodium carbonate solution, and placing the solution on a magnetic stirrer to be stirred for later use; then adding the iron-zinc solution into the sodium carbonate solution through a peristaltic pump at the pump speed of 1mL/min, and reacting to generate zinc ferrite precursor precipitate.
And (3) precipitating, filtering and washing the obtained zinc ferrite precursor for 2 times to prepare 400mL of suspension, carrying out ultrasonic treatment for 1h, carrying out spray drying, finally placing the precursor obtained by spray drying in a muffle furnace, heating to 700 ℃ under the air condition, preserving the temperature for 4h, naturally cooling to room temperature at the heating rate of 2.5 ℃/min, and sieving the obtained sintered material with a 250-mesh sieve to finally obtain the zinc ferrite lithium battery negative electrode material.
The electrical properties were measured in the same manner as in example 1, and the results are shown in Table 1.
Example 3
0.03008mol of ferric trichloride hexahydrate and 0.015mol of zinc chloride are weighed and dissolved in deionized water to prepare 1.2mol/L iron-zinc solution, and the iron-zinc solution is placed on a magnetic stirrer to be stirred for standby; weighing 0.08mol of anhydrous sodium carbonate, dissolving the anhydrous sodium carbonate in deionized water to prepare 2mol/L sodium carbonate solution, and placing the solution on a magnetic stirrer to be stirred for later use; then adding the iron-zinc solution into the sodium carbonate solution through a peristaltic pump at the pump speed of 1mL/min, and reacting to generate zinc ferrite precursor precipitate.
And (3) precipitating, filtering and washing the obtained zinc ferrite precursor for 2 times to prepare 400mL of suspension, carrying out ultrasonic treatment for 1h, carrying out spray drying, finally placing the precursor obtained by spray drying in a muffle furnace, heating to 900 ℃ under the air condition, preserving the temperature for 2h, naturally cooling to room temperature at the heating rate of 2.5 ℃/min, and sieving the obtained sintered material with a 250-mesh sieve to finally obtain the zinc ferrite lithium battery negative electrode material.
The electrical properties were measured in the same manner as in example 1, and the results are shown in Table 1.
Example 4
Weighing 0.03mol of ferric trichloride hexahydrate and 0.015mol of zinc chloride, dissolving in deionized water to prepare 1mol/L iron-zinc solution, and placing the solution on a magnetic stirrer to stir for later use; weighing 0.08mol of anhydrous sodium carbonate, dissolving the anhydrous sodium carbonate in deionized water to prepare a sodium carbonate solution with the concentration of 2.5mol/L, and placing the solution on a magnetic stirrer to be stirred for later use; then adding the iron-zinc solution into the sodium carbonate solution through a peristaltic pump at the pump speed of 1mL/min, and reacting to generate zinc ferrite precursor precipitate.
And (3) precipitating, filtering and washing the obtained zinc ferrite precursor for 2 times to prepare 400mL of suspension, carrying out ultrasonic treatment for 1h, carrying out spray drying, finally placing the precursor obtained by spray drying in a muffle furnace, heating to 800 ℃ under the air condition, preserving the temperature for 2h, naturally cooling to room temperature at the heating rate of 2.5 ℃/min, and sieving the obtained sintered material with a 250-mesh sieve to finally obtain the zinc ferrite lithium battery negative electrode material.
The electrical properties were measured in the same manner as in example 1, and the results are shown in Table 1.
Example 5
Weighing 0.03mol of ferric trichloride hexahydrate and 0.01515mol of zinc chloride, dissolving in deionized water to prepare 2mol/L iron-zinc solution, and placing the solution on a magnetic stirrer to stir for later use; weighing 0.08mol of anhydrous sodium carbonate, dissolving in deionized water to prepare 1mol/L sodium carbonate solution, and placing on a magnetic stirrer to stir for later use; then adding the iron-zinc solution into the sodium carbonate solution through a peristaltic pump at the pump speed of 1mL/min, and reacting to generate zinc ferrite precursor precipitate.
And (3) precipitating, filtering and washing the obtained zinc ferrite precursor for 2 times to prepare 400mL of suspension, carrying out ultrasonic treatment for 1h, carrying out spray drying, finally placing the precursor obtained by spray drying in a muffle furnace, heating to 800 ℃ under the air condition, preserving the temperature for 2h, naturally cooling to room temperature at the heating rate of 2.5 ℃/min, and sieving the obtained sintered material with a 250-mesh sieve to finally obtain the zinc ferrite lithium battery negative electrode material.
The electrical properties were measured in the same manner as in example 1, and the results are shown in Table 1.
Table 1 shows the results of testing 5 button cells of examples 1-5 assembled simultaneously
As can be seen from Table 1, the lithium ion battery cathode material prepared by the carbonate coprecipitation method has better capacity performance and cycle performance.
The foregoing embodiments illustrate the principles, principal features and advantages of the invention, and it will be understood by those skilled in the art that the invention is not limited to the foregoing embodiments, which are merely illustrative of the principles of the invention, and that various changes and modifications may be made therein without departing from the scope of the principles of the invention.
Claims (5)
1. The method for synthesizing the zinc ferrite lithium battery cathode material by using the carbonate coprecipitation method is characterized by comprising the following specific steps of:
step S1: dissolving soluble ferric salt and soluble zinc salt in deionized water to prepare a 1-2mol/L iron-zinc solution, and placing the prepared iron-zinc solution on a magnetic stirrer to be stirred at a constant speed for later use, wherein the soluble ferric salt is ferric nitrate, ferric sulfate, ferric chloride or ferric chloride hydrate, the soluble zinc salt is zinc nitrate, zinc nitrate hydrate, zinc chloride or zinc acetate, and the molar ratio of iron ions to zinc ions in the iron-zinc solution is 1.98-2.01: 1;
step S2: dissolving anhydrous sodium carbonate in deionized water to prepare a sodium carbonate solution with the concentration of 1-2.5mol/L, and placing the prepared sodium carbonate solution on a magnetic stirrer to stir at a constant speed for later use;
step S3: adding the iron-zinc solution obtained in the step S1 into a sodium carbonate solution through a peristaltic pump, reacting to generate a zinc ferrite precursor precipitate, monitoring the pH value of the mixed system, and controlling the pH value range of the mixed system to be 6.5-7.8 when the reaction is continuously carried out;
step S4: and (4) sequentially carrying out suction filtration and water washing on the zinc ferrite precursor precipitate obtained in the step (S3) to prepare a suspension, carrying out ultrasonic treatment on the suspension, carrying out spray drying on the suspension to obtain a precursor, heating the precursor to 700-900 ℃ at a heating rate of 2-3 ℃/min under the air condition, carrying out heat preservation for 2-4h, naturally cooling to room temperature, and sieving the obtained sintered product with a 250-mesh sieve to finally obtain the high-capacity high-cycle zinc ferrite lithium battery cathode material.
2. The method for synthesizing the negative electrode material of the zinc ferrite lithium battery by using the carbonate coprecipitation method according to claim 1, wherein the method comprises the following steps: the concentration of the iron-zinc solution in the step S1 is 1.2 mol/L.
3. The method for synthesizing the negative electrode material of the zinc ferrite lithium battery by using the carbonate coprecipitation method according to claim 1, wherein the method comprises the following steps: the concentration of the sodium carbonate solution in the step S2 is 2 mol/L.
4. The method for synthesizing the negative electrode material of the zinc ferrite lithium battery by using the carbonate coprecipitation method according to claim 1, wherein the method comprises the following steps: the flow rate of the peristaltic pump in step S3 is set to be in the range of 0.5-3 mL/min.
5. The method for synthesizing the negative electrode material of the zinc ferrite lithium battery by using the carbonate coprecipitation method according to claim 1, which is characterized by comprising the following specific steps of:
step S1: weighing 0.03mol of ferric trichloride hexahydrate and 0.015mol of zinc chloride, dissolving in deionized water to prepare 1.2mol/L iron-zinc solution, and placing the solution on a magnetic stirrer to be stirred for later use;
step S2: weighing 0.08mol of anhydrous sodium carbonate, dissolving in deionized water to prepare 2mol/L sodium carbonate solution, and placing on a magnetic stirrer for stirring for later use;
step S3: adding the iron-zinc solution obtained in the step S1 into the sodium carbonate solution obtained in the step S2 through a peristaltic pump at the pump speed of 1mL/min, and reacting to generate a zinc ferrite precursor precipitate;
step S4: performing suction filtration and water washing on the zinc ferrite precursor obtained in the step S3 for 2 times to prepare 400mL of suspension, performing ultrasonic treatment for 1h, performing spray drying, finally placing the precursor obtained by spray drying in a muffle furnace, heating to 800 ℃ under the air condition, keeping the temperature for 2h, naturally cooling to room temperature, wherein the heating rate is 2.5 ℃/min, and sieving the obtained sintered material with a 250-mesh sieve to finally obtain the zinc ferrite lithium battery cathode material;
mixing the obtained zinc ferrite with the zinc ferriteUniformly mixing carbon guide and polyvinylidene fluoride according to the mass ratio of 4:4:2, adding N-methyl pyrrolidone, continuously stirring until the material has fluidity, coating the mixed slurry on copper foil, drying and cutting into pieces to obtain a pole piece, putting the pole piece into a glove box, taking a metal lithium piece as a counter electrode, adopting a polypropylene diaphragm and 1mol/L LiPF6The solution of EC, DEC and EMC is electrolyte, wherein EC is ethylene carbonate, DEC is diethyl carbonate, EMC is ethyl methyl carbonate, the volume ratio of EC to DEC to EMC is 1:1:1, and the solution is assembled into a CR2032 type button cell in a glove box filled with dry argon, the first charging specific capacity of the button cell is 1109.6mAh/g, the first efficiency is 70.12%, and the capacity retention rate after 100 charging and discharging at 0.1C is 127.3%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112048194A (en) * | 2020-10-10 | 2020-12-08 | 武汉理工大学 | Yellow high-temperature-resistant composite pigment and preparation method thereof |
| CN112048194B (en) * | 2020-10-10 | 2021-11-23 | 武汉理工大学 | Yellow high-temperature-resistant composite pigment and preparation method thereof |
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