CN110957490A - Preparation method of carbon-coated sodium iron phosphate electrode material with hollow structure - Google Patents
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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Abstract
A preparation method of a carbon-coated sodium iron phosphate electrode material with a hollow structure relates to a preparation method of an electrode material. The invention solves the problem of the existing NaFePO4The electron conductivity and the ion diffusion coefficient are low, so that the sodium rate performance of the positive electrode material of the sodium-ion battery is poor. The preparation method comprises the following steps: dissolving an iron source, a sodium-phosphorus source and a nitrogen-containing organic high molecular compound in water to obtain a mixed solution; secondly, magnetically stirring to obtain a uniformly mixed solution; thirdly, preserving the heat of the uniformly mixed solution until the water is completely evaporated to obtain uniformly mixed powder; and fourthly, heat treatment in a tube furnace. The method is used for preparing the carbon-coated sodium iron phosphate electrode material with the hollow structure.
Description
Technical Field
The invention relates to a preparation method of an electrode material.
Background
Since the first discovery of lithium ion batteries, they have received much attention because of their advantages such as high energy density and good cycle performance. In the past decades, small and lightweight portable electronic devices (e.g., notebook computers, cellular phones) have been widely used around the world. In recent years, lithium ion batteries have been expanded from portable products to large-scale applications, particularly in the field of electric vehicles, driven by "green" technology. The amount of lithium resources on earth will not be sufficient to meet the increasing demand of mankind. Sodium is located below lithium in the periodic table, has many similar chemical properties to lithium, and the storage capacity of sodium resources is more abundant. Therefore, sodium ion batteries are also receiving attention. Sodium ion batteries depend to a large extent on the structure and properties of the materials inside the battery. The electrode material is the core component of the battery, and the negative electrode is generally made of carbon material, and the development is mature. The price and performance of sodium ion batteries depend mainly on the choice of the positive electrode material. Therefore, the development of positive electrode materials has become very important and has received great attention from researchers in the last decade.
LiFePO4The anode material has the advantages of high energy density, long cycle life, good safety, environmental friendliness and the like, and is successfully applied to the power supply of the electric vehicle by companies such as Biedi, Rongwei and the like. And with LiFePO4Similar NaFePO4The material has the highest theoretical specific capacity of 154mAh/g in the phosphate sodium-ion secondary battery cathode material, so the material is widely concerned.
However, NaFePO4The presence of intrinsic electronic conductivity is very low and is essentially considered to be an insulator. The extremely low electronic conductivity and ionic diffusion coefficient are the main reasons of poor rate performance of sodium iron phosphate, and in the prior art, the capacity retention rate under high rate is generally lower than 50%.
Disclosure of Invention
The invention aims to solve the problem of the existing NaFePO4The electron conductance and the ion diffusion coefficient are low, so that the cathode material of the sodium ion battery has poor sodium rate performance, and the preparation method of the carbon-coated iron phosphate sodium electrode material with the hollow structure is provided.
A preparation method of a carbon-coated sodium iron phosphate electrode material with a hollow structure comprises the following steps:
dissolving an iron source, a sodium-phosphorus source and a nitrogen-containing organic high molecular compound in water to obtain a mixed solution;
the mass ratio of the iron source to the nitrogen-containing organic high molecular compound is 1 (1-5); the molar ratio of the iron element in the iron source to the phosphorus element in the sodium-containing phosphorus source is 1 (1-5); the volume ratio of the mass of the iron source to the volume of the water is 1g (5-20) mL;
secondly, magnetically stirring the mixed solution for 1 to 5 hours at the temperature of between 10 and 40 ℃ to obtain a uniformly mixed solution;
thirdly, using a rotary evaporator to keep the temperature of the uniformly mixed solution at 60-120 ℃ until water is completely evaporated to obtain uniformly mixed powder;
and fourthly, placing the uniformly mixed powder in a tubular furnace, heating the uniformly mixed powder to 500-900 ℃ at a heating rate of 2-10 ℃/min under the condition of inert gas, and carrying out heat treatment for 1-4 h at the temperature of 500-900 ℃ to obtain the carbon-coated sodium iron phosphate electrode material with the hollow structure.
The invention has the beneficial effects that:
1. the invention adopts a chemical synthesis method to prepare the carbon-coated sodium iron phosphate electrode material with a hollow structure. The method has the advantages of simple process, easy operation, low cost and convenient industrial production.
2. NaFePO prepared by the invention4The electrochemical reaction device has extremely high theoretical specific capacity and stable working voltage, and the hollow structure increases the specific surface area and provides abundant active sites for electrochemical reaction.
3. According to the carbon-coated sodium iron phosphate electrode material with the hollow structure, the carbon coating layer can enhance the conductivity, promote the transmission of electrons/sodium ions, buffer the volume change, and realize excellent rate performance and cycle stability. When the current density is enlarged by 20 times, the capacity retention rate can reach 51.3%, higher coulombic efficiency (more than 95%) is always kept in a rate test, after 500 times of charge-discharge cycles, the specific capacity can be stabilized at 107.2mAh/g, and the capacity retention rate reaches 87%, which indicates that the battery has excellent rate performance and reversible performance.
The invention relates to a preparation method of a carbon-coated sodium iron phosphate electrode material with a hollow structure.
Drawings
FIG. 1 is an X-ray diffraction pattern, wherein 1 is a carbon-coated sodium iron phosphate electrode material with a hollow structure prepared in the first example, and 2 is NaFePO4The standard card of (1);
FIG. 2 is a scanning electron micrograph of a carbon-coated sodium iron phosphate electrode material with a hollow structure prepared in example one;
fig. 3 is a rate performance test chart of the carbon-coated sodium iron phosphate electrode material with a hollow structure prepared in the first embodiment at different current densities, wherein ■ is a charging specific capacity, ▲ is a discharging specific capacity, and ● is a coulombic efficiency;
fig. 4 is a graph of a cycle performance test result of the carbon-coated sodium iron phosphate electrode material with a hollow structure prepared in the first embodiment at a current density of 1A/g, where 1 is coulombic efficiency and 2 is specific capacity.
Detailed Description
The first embodiment is as follows: the embodiment provides a preparation method of a carbon-coated sodium iron phosphate electrode material with a hollow structure, which is carried out according to the following steps:
dissolving an iron source, a sodium-phosphorus source and a nitrogen-containing organic high molecular compound in water to obtain a mixed solution;
the mass ratio of the iron source to the nitrogen-containing organic high molecular compound is 1 (1-5); the molar ratio of the iron element in the iron source to the phosphorus element in the sodium-containing phosphorus source is 1 (1-5); the volume ratio of the mass of the iron source to the volume of the water is 1g (5-20) mL;
secondly, magnetically stirring the mixed solution for 1 to 5 hours at the temperature of between 10 and 40 ℃ to obtain a uniformly mixed solution;
thirdly, using a rotary evaporator to keep the temperature of the uniformly mixed solution at 60-120 ℃ until water is completely evaporated to obtain uniformly mixed powder;
and fourthly, placing the uniformly mixed powder in a tubular furnace, heating the uniformly mixed powder to 500-900 ℃ at a heating rate of 2-10 ℃/min under the condition of inert gas, and carrying out heat treatment for 1-4 h at the temperature of 500-900 ℃ to obtain the carbon-coated sodium iron phosphate electrode material with the hollow structure. .
Carbon is a common sodium iron phosphate surface coating material, and compared with pure carbon coating, nitrogen doping can obviously enhance the electron conduction performance of carbon materials such as carbon, graphene, carbon nano tubes and the like. However, it is difficult to obtain a uniform nitrogen-doped carbon material in the material by using a solid nitrogen source and a solid carbon source, so that the nitrogen-doped carbon obtained by the embodiment is uniformly coated on the surface of the sodium iron phosphate with a hollow structure by using a method of carbonizing a nitrogen-containing organic polymer compound, and the carbon coating layer can enhance the conductivity and buffer the volume change, thereby realizing excellent rate performance and cycle stability.
In the specific embodiment, the carbon-coated sodium iron phosphate electrode material with a hollow structure is prepared by a chemical synthesis method. The method has the advantages of simple process, easy operation, low cost and wide application prospect in the field of energy storage materials.
The beneficial effects of the embodiment are as follows:
1. in the embodiment, the carbon-coated sodium iron phosphate electrode material with a hollow structure is prepared by adopting a chemical synthesis method. The method has the advantages of simple process, easy operation, low cost and convenient industrial production.
2. NaFePO prepared by the present embodiment4The electrochemical reaction device has extremely high theoretical specific capacity and stable working voltage, and the hollow structure increases the specific surface area and provides abundant active sites for electrochemical reaction.
3. According to the carbon-coated sodium iron phosphate electrode material with the hollow structure, the carbon coating layer can enhance the conductivity, promote the transmission of electrons/sodium ions, buffer the volume change, and realize excellent rate performance and cycle stability. When the current density is enlarged by 20 times, the capacity retention rate can reach 51.3%, higher coulombic efficiency (more than 95%) is always kept in a rate test, after 500 times of charge-discharge cycles, the specific capacity can be stabilized at 107.2mAh/g, and the capacity retention rate reaches 87%, which indicates that the battery has excellent rate performance and reversible performance.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the iron source in the step one is Fe (NO)3)3·9H2O、FeCl3·6H2O or Fe2(SO4)3·9H2And O. The rest is the same as the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: the sodium-containing phosphorus source in the step one is NaH2PO2·H2O、Na2HPO4·12H2O or NaH2PO4·2H2And O. The other is the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the nitrogen-containing organic polymer compound in the first step is polyvinylpyrrolidone or polydopamine. The others are the same as the first to third embodiments.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: the inert gas in the fourth step is argon or nitrogen. The rest is the same as the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the mass ratio of the iron source to the nitrogen-containing organic high molecular compound in the first step is 1 (1-3). The rest is the same as the first to fifth embodiments.
The seventh embodiment: the difference between this embodiment and one of the first to sixth embodiments is: the molar ratio of the iron element in the iron source to the phosphorus element in the sodium-containing phosphorus source in the first step is 1 (1-3). The others are the same as the first to sixth embodiments.
The specific implementation mode is eight: the present embodiment differs from one of the first to seventh embodiments in that: the volume ratio of the mass of the iron source to the water in the step one is 1g (20-50) mL. The rest is the same as the first to seventh embodiments.
The specific implementation method nine: the present embodiment differs from the first to eighth embodiments in that: and in the third step, a rotary evaporator is utilized, and the uniformly mixed solution is kept at the temperature of 60-80 ℃ until water is completely evaporated, so that uniformly mixed powder is obtained. The other points are the same as those in the first to eighth embodiments.
The detailed implementation mode is ten: the present embodiment differs from one of the first to ninth embodiments in that: in the fourth step, the uniformly mixed powder is heated to 500-700 ℃ at the heating rate of 5-10 ℃/min, and is subjected to heat treatment for 1-3 h at the temperature of 500-700 ℃. The other points are the same as those in the first to ninth embodiments.
The following examples were used to demonstrate the beneficial effects of the present invention:
the first embodiment is as follows:
a preparation method of a carbon-coated sodium iron phosphate electrode material with a hollow structure comprises the following steps:
firstly, dissolving 1g of iron source, 1.33g of sodium-phosphorus source and 1g of nitrogen-containing organic high molecular compound in 50mL of water to obtain a mixed solution;
secondly, magnetically stirring the mixed solution for 4 hours at the temperature of 25 ℃ to obtain a uniformly mixed solution;
thirdly, using a rotary evaporator to evaporate the uniformly mixed solution until water is completely evaporated under the condition that the temperature is 80 ℃ to obtain uniformly mixed powder;
fourthly, placing the uniformly mixed powder in a tubular furnace, heating the uniformly mixed powder to 500 ℃ at the heating rate of 10 ℃/min under the condition of inert gas, and carrying out heat treatment for 1h under the condition of 500 ℃ to obtain the carbon-coated sodium iron phosphate electrode material with the hollow structure;
the iron source in the step one is FeCl3·6H2O；
The sodium-containing phosphorus source in the step one is Na2HPO4·12H2O；
The nitrogen-containing organic high molecular compound is polyvinylpyrrolidone;
the inert gas in the fourth step is argon.
FIG. 1 is an X-ray diffraction pattern1 is the carbon-coated sodium iron phosphate electrode material with a hollow structure prepared in the first embodiment, and 2 is NaFePO4The standard card of (1). NaFePO4The standard card of (2) corresponds to PDF #29-1216, and the main component of the material is sodium iron phosphate, and the crystallinity is good.
Fig. 2 is a scanning electron micrograph of the carbon-coated sodium iron phosphate electrode material with a hollow structure prepared in the first example. In the figure, sodium ferric phosphate can be seen to form a three-dimensional framework, and the sodium ferric phosphate is composed of nano hollow microspheres, and the surface of the nano hollow microspheres is uniformly coated with a nitrogen-doped carbon layer.
Fig. 3 is a rate performance test chart of the carbon-coated sodium iron phosphate electrode material with the hollow structure prepared in the first embodiment under different current densities, wherein ■ is a specific charge capacity, ▲ is a specific discharge capacity, and ● is a coulombic efficiency.
Fig. 4 is a graph of a cycle performance test result of the carbon-coated sodium iron phosphate electrode material with a hollow structure prepared in the first embodiment at a current density of 1A/g, where 1 is coulombic efficiency and 2 is specific capacity. As can be seen from the figure, after 500 charge-discharge cycles, the specific capacity can be stabilized at 107.2mAh/g, and the capacity retention rate reaches 87%, indicating that the lithium ion battery has excellent cycle stability.
Claims (10)
1. A preparation method of a carbon-coated sodium iron phosphate electrode material with a hollow structure is characterized by comprising the following steps:
dissolving an iron source, a sodium-phosphorus source and a nitrogen-containing organic high molecular compound in water to obtain a mixed solution;
the mass ratio of the iron source to the nitrogen-containing organic high molecular compound is 1 (1-5); the molar ratio of the iron element in the iron source to the phosphorus element in the sodium-containing phosphorus source is 1 (1-5); the volume ratio of the mass of the iron source to the volume of the water is 1g (5-50) mL;
secondly, magnetically stirring the mixed solution for 1 to 5 hours at the temperature of between 10 and 40 ℃ to obtain a uniformly mixed solution;
thirdly, using a rotary evaporator to keep the temperature of the uniformly mixed solution at 60-120 ℃ until water is completely evaporated to obtain uniformly mixed powder;
and fourthly, placing the uniformly mixed powder in a tubular furnace, heating the uniformly mixed powder to 500-900 ℃ at a heating rate of 2-10 ℃/min under the condition of inert gas, and carrying out heat treatment for 1-4 h at the temperature of 500-900 ℃ to obtain the carbon-coated sodium iron phosphate electrode material with the hollow structure.
2. The method according to claim 1, wherein the iron source in step one is Fe (NO)3)3·9H2O、FeCl3·6H2O or Fe2(SO4)3·9H2O。
3. The method for preparing a carbon-coated sodium iron phosphate electrode material with a hollow structure according to claim 1, wherein the sodium-containing phosphorus source in the step one is NaH2PO2·H2O、Na2HPO4·12H2O or NaH2PO4·2H2O。
4. The method according to claim 1, wherein the nitrogen-containing organic polymer compound in step one is polyvinylpyrrolidone or polydopamine.
5. The method according to claim 1, wherein the inert gas in step four is argon or nitrogen.
6. The method for preparing a carbon-coated sodium iron phosphate electrode material with a hollow structure according to claim 1, wherein the mass ratio of the iron source to the nitrogen-containing organic polymer compound in the step one is 1 (1-3).
7. The method for preparing the carbon-coated sodium iron phosphate electrode material with the hollow structure according to claim 1, wherein the molar ratio of the iron element in the iron source to the phosphorus element in the sodium-containing phosphorus source in the step one is 1 (1-3).
8. The preparation method of the carbon-coated sodium iron phosphate electrode material with the hollow structure according to claim 1, wherein the volume ratio of the mass of the iron source to the volume of the water in the step one is 1g (20-50) mL.
9. The method for preparing the carbon-coated sodium iron phosphate electrode material with the hollow structure according to claim 1, wherein the step three is to use a rotary evaporator to keep the temperature of the uniformly mixed solution at 60-80 ℃ until the water is completely evaporated to obtain uniformly mixed powder.
10. The method for preparing the carbon-coated sodium iron phosphate electrode material with the hollow structure according to claim 1, wherein the step four comprises heating the uniformly mixed powder to 500-700 ℃ at a heating rate of 5-10 ℃/min, and performing heat treatment at 500-700 ℃ for 1-3 h.
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Cited By (7)
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| CN113104828A (en) * | 2021-03-19 | 2021-07-13 | 三峡大学 | Preparation method of porous carbon modified sodium iron pyrophosphate phosphate/sodium carbonate ion battery positive electrode material |
| CN113548650A (en) * | 2021-07-26 | 2021-10-26 | 兰州理工大学 | Preparation method of bubble film-shaped graphene coated metal phosphide electrode material |
| CN113972364A (en) * | 2021-09-30 | 2022-01-25 | 广东邦普循环科技有限公司 | Preparation method of layered carbon-doped sodium iron phosphate cathode material |
| CN114050250A (en) * | 2021-11-18 | 2022-02-15 | 中国科学技术大学 | Carbon-coated sodium iron phosphate sodium ion battery positive electrode material, and preparation method and application thereof |
| CN114249311A (en) * | 2021-11-26 | 2022-03-29 | 广东邦普循环科技有限公司 | Preparation method of porous sodium ion battery positive electrode material sodium iron phosphate |
| CN114824205A (en) * | 2022-04-15 | 2022-07-29 | 宁波市稻禾科技有限公司 | Titanium-based fast ion conductor modified sodium iron phosphate positive electrode material, preparation method thereof and battery prepared from positive electrode material |
| GB2616234A (en) * | 2021-11-26 | 2023-08-30 | Guangdong Brunp Recycling Technology Co Ltd | Preparation method for porous sodium ion battery positive electrode material sodium iron phosphate |
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| CN114824205A (en) * | 2022-04-15 | 2022-07-29 | 宁波市稻禾科技有限公司 | Titanium-based fast ion conductor modified sodium iron phosphate positive electrode material, preparation method thereof and battery prepared from positive electrode material |
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