CN112259716A - High-specific-capacity carbon-coated lithium iron silicate material and preparation method thereof - Google Patents
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Abstract
The invention discloses a preparation method of a high-specific-capacity carbon-coated lithium iron silicate material, which comprises the following steps of: s1, dissolving a carbon source and a silicon source in an ethanol water solution to obtain a solution A; s2, dissolving lithium salt and ferric salt in deionized water to obtain a solution B; s3, dripping the solution B into the solution A for multiple times under the heating and stirring conditions, and continuing heating and stirring until gel is formed after dripping is finished; and S4, drying and grinding the gel to obtain precursor powder, calcining the precursor powder in an inert atmosphere, and cooling to obtain the product. The carbon-coated lithium iron silicate prepared by the method has the advantages of controllable shape, uniform particles and small particle size, and the prepared lithium iron silicate has higher electronic and ionic conductivity and can exert higher specific capacity.
Description
Technical Field
The invention relates to the technical field of lithium ion battery anode materials, in particular to a high-specific-capacity carbon-coated lithium iron silicate material and a preparation method thereof.
Background
Along with the development of society, people have more and more demand for energy, the exploitation and use amount of the traditional fossil energy is also more and more, the fossil energy is not renewable, and meanwhile, a large amount of pollution is generated to the environment in the using process, and the development of new energy is an effective method for solving the problem. Therefore, lithium ion batteries are widely used. The lithium ion battery mainly comprises a positive electrode, a negative electrode, a diaphragm and electrolyte. Wherein the specific capacity of the positive electrode material directly affects the energy density of the lithium ion battery. The current commercialized anode materials mainly comprise lithium iron phosphate and a ternary material, the ternary material has high specific capacity but has safety risk, and the lithium iron phosphate has high safety, but the theoretical specific capacity of the lithium iron phosphate is low, is 170mAh, and practically exerts 150 mAh. Directly affects the energy density of the lithium ion battery. The lithium iron silicate has high theoretical specific capacity which reaches 320mAh, but the ionic and electronic conductivity of the lithium iron silicate is lower, so that the lithium iron silicate has lower actual specific capacity and no actual use value.
Disclosure of Invention
Based on the technical problems in the prior art, the invention provides a high-specific-capacity carbon-coated lithium iron silicate material and a preparation method thereof, and aims to improve the practical exertion specific capacity of lithium iron silicate.
The invention provides a preparation method of a high-specific-capacity carbon-coated lithium iron silicate material, which comprises the following steps of:
s1, dissolving a carbon source and a silicon source in an ethanol water solution to obtain a solution A;
s2, dissolving lithium salt and ferric salt in deionized water to obtain a solution B;
s3, dripping the solution B into the solution A for multiple times under the heating and stirring conditions, and continuing heating and stirring until gel is formed after dripping is finished;
and S4, drying and grinding the gel to obtain precursor powder, calcining the precursor powder in an inert atmosphere, and cooling to obtain the product.
Preferably, in the step S3, the solution B is added into the solution a in 3 to 10 times, the time interval of each time of addition is 2 to 10min, and the addition amount of each time is 10 to 40% of the total volume of the solution B.
Preferably, in step S4, the specific method of calcining is: heating the mixture from room temperature to 300-500 ℃ at a heating rate of 1-5 ℃/min, preserving heat for 120-300 min, heating the mixture to 600-800 ℃ at a heating rate of 1-5 ℃/min, and preserving heat for 240-360 min.
Preferably, the inert atmosphere is at least one of argon, nitrogen and helium.
Preferably, in the step S4, the drying temperature is 60 to 100 ℃.
Preferably, the molar ratio of the silicon source to the lithium salt to the iron salt is 1 (0.5-2) to 0.5-2; the molar ratio of the silicon source to the carbon source is 1: (0.5-5).
Preferably, the ethanol aqueous solution is prepared by mixing absolute ethanol and deionized water in a volume ratio of 1: (0.2-1.6) mixing.
Preferably, the concentration of the carbon source in the solution A is 0.05-0.5 mol/L.
Preferably, in the solution B, the concentration of the lithium salt is 0.02-0.1 mol/L, and the concentration of the iron salt is 0.02-0.1 mol/L.
Preferably, the carbon source is tartaric acid, and the silicon source is tetraethoxysilane.
Preferably, the lithium salt is at least one of lithium nitrate, lithium oxalate and lithium formate, and the iron salt is at least one of ferric nitrate, ferric chloride and ferric sulfate.
A high specific capacity carbon-coated lithium iron silicate material is prepared by the preparation method.
The invention has the following beneficial effects:
the carbon-coated lithium iron silicate prepared by the method has the advantages of controllable shape, uniform particles and small particle size, and the prepared lithium iron silicate has higher electronic and ionic conductivity and can exert higher specific capacity.
Drawings
Fig. 1 is an SEM image of the carbon-coated lithium iron silicate material of example 1;
fig. 2 is an SEM image of the carbon-coated lithium iron silicate material of example 2;
fig. 3 is an SEM image of the carbon-coated lithium iron silicate material of example 3;
FIG. 4 is an XRD pattern of the carbon-coated lithium iron silicate material of example 1;
fig. 5 is a charge-discharge curve diagram of the button cell made of the carbon-coated lithium iron silicate material in example 1.
Detailed Description
The technical solution of the present invention will be described in detail below with reference to specific examples.
Example 1
A preparation method of a high-specific-capacity carbon-coated lithium iron silicate material comprises the following steps:
s1, mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:1 to obtain an ethanol aqueous solution, and then dissolving tartaric acid and tetraethoxysilane in a proper amount of ethanol aqueous solution to obtain a solution A, wherein the concentration of tartaric acid in the solution A is 0.1mol/L, and the concentration of tetraethoxysilane is 0.1 mol/L;
s2, dissolving lithium nitrate and ferric nitrate in a proper amount of deionized water to obtain a solution B, wherein the concentration of the lithium nitrate in the solution B is 0.1mol/L, and the concentration of the ferric nitrate is 0.1 mol/L;
s3, dropwise adding 100mL of solution B into 100mL of solution A for 3 times under the condition of heating and stirring at 80 ℃, wherein the time interval between the first dropwise adding and the second dropwise adding is 5min, the time interval between the second dropwise adding and the third dropwise adding is 5min, and heating and stirring are continued until gel is formed;
and S4, drying the gel at 60 ℃, grinding to obtain precursor powder, heating the precursor powder from room temperature to 300 ℃ at a heating rate of 2 ℃/min in a tube furnace under the argon atmosphere, preserving heat for 120min, heating to 650 ℃ at a heating rate of 2 ℃/min, preserving heat for 300min, and naturally cooling to room temperature to obtain the product.
Example 2
A preparation method of a high-specific-capacity carbon-coated lithium iron silicate material comprises the following steps:
s1, mixing absolute ethyl alcohol and deionized water according to a volume ratio of 7:3 to obtain an ethanol aqueous solution, and then dissolving tartaric acid and tetraethoxysilane in a proper amount of ethanol aqueous solution to obtain a solution A, wherein the concentration of tartaric acid in the solution A is 0.05mol/L, and the concentration of tetraethoxysilane is 0.1 mol/L;
s2, dissolving lithium nitrate and ferric nitrate in a proper amount of deionized water to obtain a solution B, wherein the concentration of the lithium nitrate in the solution B is 0.1mol/L, and the concentration of the ferric nitrate is 0.1 mol/L;
s3, dropwise adding 100mL of solution B into 100mL of solution A in 5 times under the condition of heating and stirring at 60 ℃, wherein the total volume of the solution B is 20% of the total volume of the solution B for the first time, 20% of the total volume of the solution B for the second time, 20% of the total volume of the solution B for the third time, 20% of the total volume of the solution B for the fourth time and 20% of the total volume of the solution B for the fifth time, the time interval between the first dropwise addition and the second dropwise addition is 5min, the time interval between the second dropwise addition and the third dropwise addition is 5min, the time interval between the third dropwise addition and the fourth dropwise addition is 5min, and heating and stirring are continued until gel is formed after the dropwise addition;
and S4, drying the gel at 60 ℃, grinding to obtain precursor powder, heating the precursor powder from room temperature to 300 ℃ at a heating rate of 2 ℃/min in a tube furnace under the argon atmosphere, preserving heat for 120min, heating to 650 ℃ at a heating rate of 2 ℃/min, preserving heat for 300min, and naturally cooling to room temperature to obtain the product.
Example 3
A preparation method of a high-specific-capacity carbon-coated lithium iron silicate material comprises the following steps:
s1, mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:1 to obtain an ethanol aqueous solution, and then dissolving tartaric acid and tetraethoxysilane in a proper amount of ethanol aqueous solution to obtain a solution A, wherein the concentration of tartaric acid in the solution A is 0.3mol/L, and the concentration of tetraethoxysilane is 0.1 mol/L;
s2, dissolving lithium nitrate and ferric nitrate in a proper amount of deionized water to obtain a solution B, wherein the concentration of the lithium nitrate in the solution B is 0.1mol/L, and the concentration of the ferric nitrate is 0.1 mol/L;
s3, dropwise adding 100mL of solution B into 100mL of solution A for 3 times under the condition of heating and stirring at 100 ℃, wherein the time interval between the first dropwise adding and the second dropwise adding is 5min, the time interval between the second dropwise adding and the third dropwise adding is 5min, and heating and stirring are continued until gel is formed after the dropwise adding is finished;
and S4, drying the gel at 80 ℃ and grinding the gel to obtain precursor powder, heating the precursor powder from room temperature to 300 ℃ at the heating rate of 1 ℃/min in a tube furnace under the argon atmosphere, preserving the heat for 180min, heating to 700 ℃ at the heating rate of 2 ℃/min, preserving the heat for 300min, and naturally cooling to room temperature to obtain the product.
Example 4
A preparation method of a high-specific-capacity carbon-coated lithium iron silicate material comprises the following steps:
s1, mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:0.2 to obtain an ethanol water solution, and then dissolving tartaric acid and tetraethoxysilane in a proper amount of ethanol water solution to obtain a solution A, wherein the concentration of tartaric acid in the solution A is 0.05mol/L, and the concentration of tetraethoxysilane is 0.01 mol/L;
s2, dissolving lithium formate and ferric chloride in a proper amount of deionized water to obtain a solution B, wherein the concentration of the lithium formate in the solution B is 0.02mol/L, and the concentration of the ferric chloride is 0.02 mol/L;
s3, dropwise adding 100mL of solution B into 100mL of solution A for 3 times under the condition of heating and stirring at 70 ℃, wherein the time interval between the first dropwise adding and the second dropwise adding is 5min, the time interval between the second dropwise adding and the third dropwise adding is 5min, and heating and stirring are continued until gel is formed;
and S4, drying the gel at 80 ℃ and grinding the gel to obtain precursor powder, heating the precursor powder from room temperature to 400 ℃ at a heating rate of 2 ℃/min in a tube furnace under the argon atmosphere, preserving the heat for 300min, heating to 600 ℃ at a heating rate of 1 ℃/min, preserving the heat for 360min, and naturally cooling to room temperature to obtain the product.
Example 5
A preparation method of a high-specific-capacity carbon-coated lithium iron silicate material comprises the following steps:
s1, mixing absolute ethyl alcohol and deionized water according to the volume ratio of 1:1.6 to obtain an ethanol water solution, and then dissolving tartaric acid and tetraethoxysilane in a proper amount of ethanol water solution to obtain a solution A, wherein the concentration of tartaric acid in the solution A is 0.5mol/L, and the concentration of tetraethoxysilane is 0.1 mol/L;
s2, dissolving lithium oxalate and ferric sulfate in a proper amount of deionized water to obtain a solution B, wherein the concentration of the lithium oxalate in the solution B is 0.05mol/L, and the concentration of the ferric sulfate is 0.05 mol/L;
s3, dropwise adding 100mL of solution B into 100mL of solution A for 10 times under the condition of heating and stirring at 60 ℃, wherein 10% of the total volume of the solution B is dropwise added each time, the time interval of dropwise adding each time is 2min, and after dropwise adding is finished, heating and stirring are continued until gel is formed;
s4, drying the gel at 100 ℃ and then grinding to obtain precursor powder, heating the precursor powder in a tube furnace at a heating rate of 5 ℃/min from room temperature to 500 ℃ in a nitrogen atmosphere, preserving heat for 120min, heating at a heating rate of 5 ℃/min to 800 ℃ in a tube furnace, preserving heat for 240min, and naturally cooling to room temperature to obtain the product.
The carbon-coated lithium iron silicate materials prepared in examples 1 to 3 are shown in fig. 1 to 3. As can be seen from fig. 1 to 3, the lithium iron silicate material is uniformly coated with carbon, and has controllable morphology, uniform particles and small particle size.
The XRD test result of the carbon-coated lithium iron silicate material prepared in example 1 is shown in fig. 4. As can be seen from fig. 4, each peak corresponds to lithium iron silicate, and a peak of carbon exists, indicating that the lithium iron silicate material is coated with carbon.
The carbon-coated lithium iron silicate material prepared in example 1 is used as a positive electrode active material, is pulped with PVDF and SP according to a mass ratio of 92:4:4, is coated on an aluminum foil to prepare a positive electrode sheet, and a lithium sheet is used as a negative electrode sheet to prepare a CR2025 button cell, and the electrochemical performance is tested under a current density of 100mA/g, and the test result is shown in FIG. 5.
As can be seen from fig. 5, the second discharge specific capacity of the battery reaches 208.5mAh, the third discharge specific capacity is 204.7mAh, and the tenth discharge specific capacity is 196.9mAh, which indicates that the prepared lithium iron silicate has high electronic and ionic conductivity, and can exert high specific capacity and good capacity retention rate.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (10)
1. A preparation method of a high-specific-capacity carbon-coated lithium iron silicate material is characterized by comprising the following steps of:
s1, dissolving a carbon source and a silicon source in an ethanol water solution to obtain a solution A;
s2, dissolving lithium salt and ferric salt in deionized water to obtain a solution B;
s3, dripping the solution B into the solution A for multiple times under the heating and stirring conditions, and continuing heating and stirring until gel is formed after dripping is finished;
and S4, drying and grinding the gel to obtain precursor powder, calcining the precursor powder in an inert atmosphere, and cooling to obtain the product.
2. The method for preparing the high-specific-capacity carbon-coated lithium iron silicate material according to claim 1, wherein in the step S3, the solution B is added into the solution A in 3-10 times, the time interval of each time of addition is 2-10 min, and the addition amount of each time of addition is 10-40% of the total volume of the solution B.
3. The method for preparing the high-specific-capacity carbon-coated lithium iron silicate material according to claim 1 or 2, wherein the molar ratio of the silicon source to the lithium salt to the iron salt is 1 (0.5-2) to 0.5-2; the molar ratio of the silicon source to the carbon source is 1: (0.5-5).
4. The method for preparing the high-specific-capacity carbon-coated lithium iron silicate material according to any one of claims 1 to 3, wherein in the step S4, the specific calcining method comprises: heating the mixture from room temperature to 300-500 ℃ at a heating rate of 1-5 ℃/min, preserving heat for 120-300 min, heating the mixture to 600-800 ℃ at a heating rate of 1-5 ℃/min, and preserving heat for 240-360 min.
5. The preparation method of the high-specific-capacity carbon-coated lithium iron silicate material according to any one of claims 1 to 4, wherein the ethanol aqueous solution is prepared from absolute ethanol and deionized water in a volume ratio of 1: (0.2-1.6) mixing.
6. The method for preparing the high-specific-capacity carbon-coated lithium iron silicate material according to any one of claims 1 to 5, wherein the concentration of the carbon source in the solution A is 0.05 to 0.5 mol/L.
7. The method for preparing the high-specific-capacity carbon-coated lithium iron silicate material according to any one of claims 1 to 6, wherein the concentration of the lithium salt in the solution B is 0.02 to 0.1mol/L, and the concentration of the iron salt in the solution B is 0.02 to 0.1 mol/L.
8. The method for preparing the high-specific-capacity carbon-coated lithium iron silicate material according to any one of claims 1 to 7, wherein the carbon source is tartaric acid, and the silicon source is ethyl orthosilicate.
9. The method for preparing the high-specific-capacity carbon-coated lithium iron silicate material according to any one of claims 1 to 8, wherein the lithium salt is at least one of lithium nitrate, lithium oxalate and lithium formate, and the iron salt is at least one of ferric nitrate, ferric chloride and ferric sulfate.
10. A high specific capacity carbon-coated lithium iron silicate material, which is characterized by being obtained by the preparation method of any one of claims 1 to 9.
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Application publication date: 20210122 |