CN110723718A - Preparation method of nitrogen-doped graphene/lithium iron phosphate composite material for lithium ion battery - Google Patents
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Abstract
The invention discloses a preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material. The method has simple process, is suitable for industrial mass production, and the prepared composite material has excellent and stable conductivity, can be used as a positive electrode material and applied to lithium ion batteries.
Description
Technical Field
The invention belongs to the field of composite materials, and particularly relates to a preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material for a lithium ion battery.
Background
Lithium ion batteries are a new generation of green high-energy batteries. Since the commercialization of lithium ion batteries, the study of the conductivity of the positive electrode material has been a hotspot of the study in the battery field, most of the positive electrode active materials currently used in lithium ion batteries are transition metal oxides or transition metal phosphates, most of the positive electrode active materials are semiconductors or insulators, and the conductivity is poor, so that a conductive agent needs to be added to improve the conductivity, and the positive electrode active materials and the active materials and a current collector play a role in collecting micro-current to reduce the contact resistance of electrodes, and simultaneously can effectively improve the mobility of lithium ions in the battery material, thereby improving the charge-discharge rate performance of the battery.
CN 106992301A discloses a nitrogen-doped graphene conductive agent and a preparation method thereof, wherein a chemical vapor deposition method is adopted to prepare the nitrogen-doped graphene and apply the nitrogen-doped graphene to a lithium ion battery, although the method successfully prepares the conductive agent with high conductivity, the conductive agent is dispersed in the slurry preparation process, and the graphene is easy to agglomerate to increase the internal resistance of the battery, thereby reducing the performance of the battery. CN 109103442a discloses a preparation method of a graphene-coated lithium iron phosphate positive electrode material, wherein a microwave hydrothermal method is adopted to prepare the graphene-coated lithium iron phosphate material, and the problem of graphene dispersion is solved by coating, but the graphene prepared by the method has low conductivity, so that the effect of improving the performance of a lithium iron phosphate battery is not ideal.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides a preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material for a lithium ion battery. The problem of uneven dispersion of graphene is solved, and the conductivity of the material is further improved by carrying out nitrogen modification on the graphene.
In order to realize the purpose of the invention, the technical scheme of the invention is as follows:
a preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material for a lithium ion battery is characterized by taking a carbon source, a lithium source, a phosphorus source and an iron source as raw materials and preparing the nitrogen-doped graphene/lithium iron phosphate composite material by a sol-gel method and a high-temperature calcination method, and specifically comprises the following steps:
(1) adding a lithium source, a phosphorus source, an iron source and a carbon source into deionized water for dispersing to prepare a dispersion liquid;
(2) adding citric acid into the dispersion liquid obtained in the step (1), adjusting the pH value to 11 by using ammonia water, and uniformly stirring;
(3) heating in water bath at certain temperature, and stirring until gel appears;
(4) and (4) calcining the gel obtained in the step (3) at high temperature in an ammonia atmosphere to obtain the nitrogen-doped graphene/lithium iron phosphate composite material.
Further, the molar ratio of the lithium source, the phosphorus source, the iron source and the carbon source in the step (1) is 0.8-1.2:1-1.5: 0.5-3.
Further, the method for preparing the dispersion liquid in the step (1) is high-power ultrasonic dispersion, and the power is 800W-1000W.
Further, the lithium source in step (1) is one of lithium hydroxide, lithium carbonate and lithium hydrogen phosphate.
Further, the phosphorus source in the step (1) is one of ammonium phosphate, diammonium hydrogen phosphate, ammonium monohydrogen phosphate and phosphoric acid.
Further, the iron source in the step (1) is one of ferrous sulfate, ferric phosphate, ferric oxide, ferric chloride and ferric acetate.
Further, the carbon source in the step (1) is one of glucose, fructose and sucrose.
Further, the water bath heating temperature in the step (3) is 80-100 ℃.
Further, the ammonia gas in the step (4) is high-purity ammonia gas.
Further, the calcination process in the step (4) is divided into two sections, wherein the first section is insulated for 3-5h at 600 ℃, the second section is insulated for 3-5h at 900 ℃ and 750 ℃ and the temperature rise rate is 3-5 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
the preparation method of the nitrogen-doped graphene/lithium iron phosphate composite material comprises the steps of preparing a precursor of the lithium iron phosphate and carbon source composite material by a sol-gel method, and then obtaining the nitrogen-doped graphene/lithium iron phosphate composite material by a high-temperature calcination method in an ammonia atmosphere. And (3) pyrolyzing and reducing glucose into nitrogen-doped graphene through high-temperature calcination, drying the gel into lithium iron phosphate, and compounding the nitrogen-doped graphene and the lithium iron phosphate in the reduction process. The preparation process is simple, the problem that graphene is not uniformly dispersed in the positive electrode slurry can be solved through the method, and the conductivity of the graphene is further improved by performing nitrogen modification on the graphene on the basis of the graphene, so that the charge-discharge and rate performance of the lithium iron phosphate battery are improved.
Drawings
Fig. 1 is the capacity retention of the lithium ion battery of example 1 after 100 cycles at 1C;
fig. 2 is an SEM image of the nitrogen-doped graphene/lithium iron phosphate composite.
Detailed Description
The specific preferred embodiments of the present invention will be further described with reference to the following examples:
example 1
A preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material comprises the following steps:
(1) according to the lithium source: a phosphorus source: weighing 0.01mol of lithium hydroxide, 0.01mol of diammonium phosphate, 0.01mol of ferric chloride and 0.01mol of glucose into deionized water according to the molar ratio of iron source =1:1:1:1, and preparing a dispersion liquid through high-power dispersion;
(2) adding 0.06mol of citric acid in the stirring process, and adding ammonia water to adjust the pH value to 11;
(3) heating the mixture in water bath at 80 ℃, and stirring the mixture to be gelatinous to obtain a precursor of the lithium iron phosphate/graphene composite material;
(4) and (4) transferring the material obtained in the step (3) into a vacuum heating furnace, introducing high-purity ammonia gas, heating to 600 ℃ at the heating rate of 3 ℃/min, preserving heat for 3h, then raising the temperature to 750 ℃ and preserving heat for 3h, and finally cooling to room temperature to obtain the nitrogen-doped graphene/lithium iron phosphate composite material.
The obtained composite material was dispersed in N-methylpyrrolidone (NMP) to obtain a dispersion liquid. According to PVDF: NMP = 5: mixing the PVDF binder in a mass ratio of 95 to obtain a PVDF binder, and mixing the PVDF binder with the dispersion liquid according to a ratio of 1: and 8, mixing and stirring the mixture according to the proportion to obtain the lithium ion battery anode slurry.
Example 2
A preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material comprises the following steps:
(1) according to the lithium source: a phosphorus source: weighing 0.01mol of lithium acetate, 0.01mol of ammonium phosphate, 0.01mol of iron acetate and 0.02mol of glucose into deionized water according to the molar ratio of iron source =1:1:1:2, and preparing a dispersion liquid through high-power dispersion;
(2) adding 0.06mol of citric acid in the stirring process, and adding ammonia water to adjust the pH value to 11;
(3) heating the mixture in water bath at 90 ℃, and stirring the mixture to be gelatinous to obtain a precursor of the lithium iron phosphate/graphene composite material;
(4) and (4) transferring the material obtained in the step (3) into a vacuum heating furnace, introducing high-purity ammonia gas, heating to 600 ℃ at the heating rate of 4 ℃/min, preserving heat for 3h, then raising the temperature to 700 ℃ and preserving heat for 3h, and finally cooling to room temperature to obtain the nitrogen-doped graphene/lithium iron phosphate composite material.
The obtained composite material was dispersed in N-methylpyrrolidone (NMP) to obtain a dispersion liquid. According to PVDF: NMP = 5: mixing the PVDF binder in a mass ratio of 95 to obtain a PVDF binder, and mixing the PVDF binder with the dispersion liquid according to a ratio of 1: and 8, mixing and stirring the mixture according to the proportion to obtain the lithium ion battery anode slurry.
Example 3
A preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material comprises the following steps:
(1) according to the lithium source: a phosphorus source: weighing 0.01mol of lithium acetate, 0.01mol of ammonium monohydrogen phosphate, 0.01mol of iron acetate and 0.03mol of glucose into deionized water according to the molar ratio of iron source =1:1:1:3, and preparing a dispersion liquid through high-power dispersion;
(2) adding 0.06mol of citric acid in the stirring process, and adding ammonia water to adjust the pH value to 11;
(3) heating in water bath at 100 ℃, and stirring to be gelatinous to obtain a precursor of the lithium iron phosphate/graphene composite material;
(4) and (4) transferring the material obtained in the step (3) into a vacuum heating furnace, introducing high-purity ammonia gas, heating to 600 ℃ at the heating rate of 5 ℃/min, preserving heat for 3h, then raising the temperature to 800 ℃ and preserving heat for 3h, and finally cooling to room temperature to obtain the nitrogen-doped graphene/lithium iron phosphate composite material.
The obtained composite material was dispersed in N-methylpyrrolidone (NMP) to obtain a dispersion liquid. According to PVDF: NMP = 5: mixing the PVDF binder in a mass ratio of 95 to obtain a PVDF binder, and mixing the PVDF binder with the dispersion liquid according to a ratio of 1: and 8, mixing and stirring the mixture according to the proportion to obtain the lithium ion battery anode slurry.
Example 4
A preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material comprises the following steps:
(1) according to the lithium source: a phosphorus source: weighing 0.01mol of lithium acetate, 0.01mol of ammonium monohydrogen phosphate, 0.01mol of iron acetate and 0.01mol of glucose into deionized water according to the molar ratio of iron source =1:1:1:1, and preparing a dispersion liquid through high-power dispersion;
(2) adding 0.06mol of citric acid in the stirring process, and adding ammonia water to adjust the pH value to 11;
(3) heating the mixture in water bath at 80 ℃, and stirring the mixture to be gelatinous to obtain a precursor of the lithium iron phosphate/graphene composite material;
(4) and (4) transferring the material obtained in the step (3) into a vacuum heating furnace, introducing high-purity ammonia gas, heating to 600 ℃ at the heating rate of 5 ℃/min, preserving heat for 3h, then raising the temperature to 900 ℃ and preserving heat for 3h, and finally cooling to room temperature to obtain the nitrogen-doped graphene/lithium iron phosphate composite material.
The obtained composite material was dispersed in N-methylpyrrolidone (NMP) to obtain a dispersion liquid. According to PVDF: NMP = 5: mixing the PVDF binder in a mass ratio of 95 to obtain a PVDF binder, and mixing the PVDF binder with the dispersion liquid according to a ratio of 1: and 8, mixing and stirring the mixture according to the proportion to obtain the lithium ion battery anode slurry.
Example 5
A preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material comprises the following steps:
(1) according to the lithium source: a phosphorus source: weighing 0.01mol of lithium acetate, 0.01mol of ammonium monohydrogen phosphate, 0.01mol of iron acetate and 0.01mol of glucose into deionized water according to the molar ratio of iron source =1:1:1:1, and preparing a dispersion liquid through high-power dispersion;
(2) adding 0.06mol of citric acid in the stirring process, and adding ammonia water to adjust the pH value to 11;
(3) heating the mixture in water bath at 90 ℃, and stirring the mixture to be gelatinous to obtain a precursor of the lithium iron phosphate/graphene composite material;
(4) and (4) transferring the material obtained in the step (3) into a vacuum heating furnace, introducing high-purity ammonia gas, heating to 600 ℃ at the heating rate of 5 ℃/min, preserving heat for 3h, then raising the temperature to 900 ℃ and preserving heat for 3h, and finally cooling to room temperature to obtain the nitrogen-doped graphene/lithium iron phosphate composite material.
The obtained composite material was dispersed in N-methylpyrrolidone (NMP) to obtain a dispersion liquid. According to PVDF: NMP = 5: mixing the PVDF binder in a mass ratio of 95 to obtain a PVDF binder, and mixing the PVDF binder with the dispersion liquid according to a ratio of 0.5: and 9, mixing and stirring the mixture according to the proportion to obtain the lithium ion battery anode slurry.
The positive electrode slurry prepared in examples 1 to 5 and mesocarbon microbeads as negative electrode materials were applied to a lithium battery to assemble a button cell.
Table 1 discharge capacity and coulombic efficiency after 100 cycles of nitrogen-doped graphene/lithium iron phosphate composite 1C for each example
Table 1 shows that the positive electrode conductive paste prepared from the nitrogen-doped graphene/lithium iron phosphate composite material prepared by the method has higher capacity retention rate and coulombic efficiency when applied to lithium ion batteries (1-5) under high rate, and the specific capacity of example 1 reaches 165mAh/g under low rate (0.5C), which is close to the theoretical specific capacity; FIG. 1 is a cycle chart of example 1 at 1C current density for 100 cycles, and the composite material prepared by the preparation method can still maintain high capacity retention after multiple cycles.
Claims (9)
1. A preparation method of a nitrogen-doped graphene/lithium iron phosphate composite material for a lithium ion battery is characterized by comprising the following steps of:
(1) adding a lithium source, a phosphorus source, an iron source and a carbon source into deionized water for dispersing to prepare a dispersion liquid;
(2) adding citric acid into the dispersion liquid obtained in the step (1), adjusting the pH value to 11 by using ammonia water, and uniformly stirring;
(3) heating in water bath at certain temperature, and stirring until gel appears;
(4) and (4) calcining the gel obtained in the step (3) at high temperature in an ammonia atmosphere to obtain the nitrogen-doped graphene/lithium iron phosphate composite material.
2. The method of claim 1, wherein: the molar ratio of the lithium source, the phosphorus source, the iron source and the carbon source in the step (1) is 0.8-1.2:1-1.5: 0:5-3.
3. The method of claim 1, wherein: the lithium source in the step (1) is one of lithium hydroxide, lithium carbonate and lithium hydrogen phosphate.
4. The method of claim 1, wherein: the phosphorus source in the step (1) is one of diammonium hydrogen phosphate, ammonium monohydrogen phosphate and phosphoric acid.
5. The method of claim 1, wherein: the iron source in the step (1) is one of ferrous sulfate, ferric phosphate, ferric oxide, ferric chloride and ferric acetate.
6. The method of claim 1, wherein: the carbon source in the step (1) is one of glucose, fructose and sucrose.
7. The method of claim 1, wherein: the dispersion mode of the dispersion liquid in the step (1) is high-power ultrasonic dispersion, and the power is 800W-1000W.
8. The method of claim 1, wherein: the water bath heating temperature in the step (3) is 80-100 ℃.
9. The method of claim 1, wherein: the calcination process in the step (4) is divided into two sections, wherein the first section is insulated for 3-5h at 600 ℃, the second section is insulated for 3-5h at 900 ℃ of 700-.
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| CN113072052A (en) * | 2021-03-29 | 2021-07-06 | 山东大学 | Waste lithium iron phosphate lithium supplement repair method and application |
| CN114122406A (en) * | 2022-01-25 | 2022-03-01 | 成都特隆美储能技术有限公司 | Preparation method of graphene modified lithium iron phosphate and lithium iron phosphate |
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