CN110943216B - Preparation method of cobalt-iron bimetallic selenide sodium-ion battery cathode material - Google Patents
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Abstract
The invention relates to a preparation method of a cobalt-iron bimetallic selenide sodium-ion battery cathode material, which synthesizes FeSe by a simple method2@CoSe2Heterostructures to enhance the electrochemical properties of sodium ion batteries. The method comprises the steps of firstly synthesizing a precursor of ZIF-67, then growing a Fe metal layer on the surface of the precursor through ion adsorption, and carrying out high-temperature selenizing calcination to obtain the core-shell structure material with a uniform heterogeneous interface. The cobalt-iron bimetallic selenide material prepared by the method is used as a negative electrode material to be applied to the sodium-ion battery, so that the cycle performance of the sodium-ion battery is obviously improved, the capacity and the service life of the battery are improved, and the volume expansion in the charging and discharging process is effectively inhibited.
Description
Technical Field
The technical scheme of the invention relates to a preparation method of a cobalt-iron bimetallic selenide sodium-ion battery cathode material, belonging to the field of material chemistry.
Background
Lithium ion batteries have attracted attention of researchers due to characteristics of high energy density, long cycle life, environmental friendliness, and the like, and are widely used in various fields such as portable electronic products and electric vehicles. However, the specific capacity of graphite as the negative electrode of the lithium ion battery is low, so that the requirement of rapid market development cannot be met. It is therefore imperative to find new systems to replace it. The storage capacity of the metal sodium on the earth is large, and the price is relatively low. Although sodium ions are similar to lithium ion batteries during charging and discharging,however, conventional negative electrode materials such as graphite materials used in lithium ion batteries are not suitable for sodium ion batteries because the ion radius of sodium is larger than that of lithium. Finding suitable anode materials is therefore a major challenge for sodium ion batteries. Among the anode materials that have been explored, metal selenides are considered to be anode materials for high-performance sodium-ion batteries because they have various structural types and excellent electrochemical activity. In past studies. FeSe2And CoSe2The sodium storage mechanism of (a) involves the conversion process. However, bulk FeSe results from the large volume change that occurs during charging and discharging of the cell2And CoSe2Exhibiting poor cycle life and stability performance.
Based on some theoretical foundations, we propose a simple method for synthesizing FeSe2@CoSe2Heterostructures to enhance the electrochemical properties of sodium ion batteries.
Disclosure of Invention
The invention mainly uses ZIF-67 as a precursor, grows a layer of Fe metal layer on the surface, then carries out selenylation calcination in Ar atmosphere to obtain the nuclear shell ferrocobalt bimetallic selenide, and applies the material to the cathode of a sodium ion battery. The main purpose of the metal layer with Fe growing on the surface is to grow a metal layer on the outer surface of the ZIF-67, and the material can form a layer of amorphous carbon in the calcining process due to a layer of PVP on the outer surface, so that the conductivity of the material can be enhanced, and meanwhile, the volume expansion of the sodium-ion battery caused in the charging and discharging processes can be effectively inhibited due to the existence of the carbon layer. Relative to pure CoSe2For the sample, the designed structure can more effectively improve the cycle performance and the coulomb efficiency of the sodium-ion battery. The invention overcomes the volume expansion of the sodium ion battery cathode material prepared in the prior art in the charging and discharging process, effectively improves the cycle performance of the battery, and simultaneously, the external carbon layer can also increase the conductivity of the battery, and improves the specific capacity and the cycle stability of the battery.
The preparation method of the cathode material of the cobalt-iron bimetallic selenide sodium-ion battery specifically comprises the following steps:
(1) preparation of ZIF-67 precursor:
cobalt nitrate was dissolved in methanol and stirred in a magnetic stirrer until completely dissolved, labeled as solution a. The 2-methylimidazole was dissolved in methanol and stirred in a magnetic stirrer until completely dissolved, labeled as solution B. And quickly pouring the solution B into the solution A, stirring, standing at room temperature, collecting a sample by centrifugation, washing with methanol for three times, and drying in an oven at 60 ℃ for later use.
Further, in the step (1), the mass of the cobalt nitrate is 0.291g, and the volume of methanol required for preparing the solution A is 20mL; the mass of the 2-methylimidazole is 0.658g, and the volume of methanol required for preparing the solution B is 20mL;
further, in the preparation process of the solution A and the solution B in the step (1), the stirring speed is 400r/min, and the stirring time is 5min;
further, A, B in the step (1) is stirred for 5min after mixing, the room temperature standing time is 24h, and the centrifugal speed is 8000r/min when the sample is collected by centrifugation.
(2) Synthesis of ZIF-67@ Fe-LDH structural material
And (2) dissolving the ZIF-67 precursor obtained in the step (1) in ethanol and marking the solution as C, and carrying out ultrasonic treatment for 10 min. Potassium ferricyanide and PVP were dissolved in ethanol solution and labeled as solution D. Quickly pouring the solution D into the solution C, stirring for 3h, then collecting a sample by centrifugal separation for 5min, wherein the centrifugal rotation speed is 8000r/min, washing with methanol for three times, and drying in a 60 ℃ oven for later use;
further, the mass of the ZIF-67 precursor required for preparing the solution C in the step (2) is 0.05g, and the volume of ethanol is 5mL; the mass of potassium ferricyanide required for preparing the solution D is 0.05g, the molecular weight of PVP is 10000 and 0.63g, and the volume fraction of the ethanol aqueous solution is 50 percent and the volume is 40mL;
further, C, D in the step (2) is stirred for 3 hours after mixing, the room temperature standing time is 24 hours, and the centrifugal speed is 8000r/min when the sample is centrifugally collected;
(3) preparation of FeSe2@CoSe2@ C negative electrode material
And respectively placing the ZIF-67@ Fe-LDH sample and the selenium powder at two ends of a porcelain boat, calcining in Ar atmosphere, and obtaining the cathode material of the cobalt-iron double-metal selenide sodium-ion battery after the reaction is finished.
Further, in the step (3), the mass ratio of the ZIF-67@ Fe-LDH sample to the selenium powder is 1:3-4, the selenium powder is arranged at a gas inlet of the gas, and the ZIF-67@ Fe-LDH sample is arranged at a gas outlet of the gas;
further, in the step (3), the calcination temperature in the Ar atmosphere is 400-500 ℃, the calcination time is 2h, and the heating rate is 2 ℃/min.
Compared with the prior art, the invention has the following beneficial effects:
firstly, the core-shell structure designed by the invention can provide more electronic channels for the charge and discharge process, and is beneficial to the implementation of the electrochemical reaction of the battery. Secondly, in the process of charging and discharging of the battery, due to the existence of the carbon layer, the volume expansion caused by the process of sodium ion sodium insertion and sodium removal is effectively inhibited. Thirdly, due to CoSe2The carbon layer outside the nano sheet has good conductivity, the specific capacity of the battery can be increased, and the electrochemical performance is improved. The core-shell nano structure designed by the invention can provide extra buffer space and pressure, effectively inhibits volume expansion in the charge and discharge process, and has important significance for the cycle performance of the sodium ion battery.
The bimetallic selenide sodium-ion battery cathode material prepared by the preparation method obviously improves the cycle performance of the sodium-ion battery due to the combined action of multiple aspects in the application process of the sodium-ion battery, improves the capacity and the service life of the battery, and has positive significance for realizing the industrialization of the sodium-ion battery.
Drawings
FIG. 1A is a scanning electron microscope image of the ZIF-67@ Fe-LDH precursor of example 1.
FIG. 2 shows FeSe obtained after selenization in example 12@CoSe2Scanning Electron micrograph of @ C.
FIG. 3 is FeSe prepared in example 12@CoSe2@ C as the negative electrode material of the sodium-ion battery at the current density of1A g-1Electrochemical cycling profile under discharging conditions.
The specific implementation mode is as follows:
the invention is further described with reference to the drawings and the detailed description.
Example 1:
the first step is as follows: preparation of ZIF-67 precursor:
0.291g of cobalt nitrate was dissolved in 20mL of methanol and then stirred in a magnetic stirrer at 400r/min for 5min to complete dissolution, labeled solution A. 0.658g of 2-methylimidazole was dissolved in 20mL of methanol and stirred in a magnetic stirrer at 400r/min for 5min until complete dissolution, labeled solution B. And quickly pouring the solution B into the solution A, stirring for 5min, standing for 24h at room temperature, centrifuging for 5min, collecting a sample, centrifuging at the rotating speed of 8000r/min, washing with methanol for three times, and drying in an oven at 60 ℃ for later use. As can be seen from the attached figure 1, the prepared precursor is hexagonal rhombus-shaped, uniform in size and approximately 300-400 nm in diameter. The figure shows a hexagonal diamond on the inside and a small granular iron layer on the outside.
The second step is that: synthesis of ZIF-67@ Fe-LDH structural material
0.05g of the resulting ZIF-67 was dissolved in 5mL of ethanol, labeled as solution C, and then sonicated for 10 min. 0.05g of potassium ferricyanide and 0.63g of PVP with a molecular weight of 10000 were dissolved in 40mL of 50% ethanol solution by volume fraction and labeled as solution D. And quickly pouring the solution D into the solution C, stirring for 3h, centrifuging for 5min, collecting a sample, centrifuging at the rotating speed of 8000r/min, washing with methanol for three times, and drying in an oven at the temperature of 60 ℃ for later use.
The third step: preparation of FeSe2@CoSe2@ C negative electrode material
Mixing the components in a mass ratio of 1:3, respectively placing the ZIF-67@ Fe-LDH sample and the selenium powder at two ends of the porcelain boat, wherein the selenium powder is arranged at a gas inlet, and the ZIF-67@ Fe-LDH sample is arranged at a gas outlet. Calcining under Ar atmosphere, wherein the calcining temperature is 400 ℃, the calcining time is 2h, the heating rate is 2 ℃/min, and the cathode material of the cobalt-iron bimetallic selenide sodium-ion battery is obtained after the reaction is finished. FIG. 2 is selenizationFeSe after chemical conversion2@CoSe2The scanning electron micrograph of @ C, from FIG. 2A, shows that the selenide preparation was successfully prepared and is a hexagonal rhombohedral structure. As can be seen from FIG. 2B, the prepared morphology is a hexagonal rhombus core-shell structure. As can be seen from FIG. 3, the prepared material has high and stable specific charge-discharge capacity of the battery. Pure CoSe2The capacity is relatively low and also less stable and the decay is relatively fast.
Example 2:
the first step is as follows: preparation of ZIF-67 precursor:
0.291g of cobalt nitrate was dissolved in 20mL of methanol and then stirred in a magnetic stirrer at 400r/min for 5min until the label A solution was completely dissolved. 0.658g of 2-methylimidazole was dissolved in 20mL of methanol and stirred in a magnetic stirrer at 400r/min for 5min until complete dissolution, labeled solution B. And quickly pouring the solution B into the solution A, stirring for 5min, standing for 24h at room temperature, centrifuging for 5min, collecting a sample, centrifuging at the rotating speed of 8000r/min, washing with methanol for three times, and drying in an oven at 60 ℃ for later use.
The second step is that: synthesis of ZIF-67@ Fe-LDH Structure
0.05g of the resulting ZIF-67 was dissolved in 5mL of ethanol, labeled as solution C, and sonicated for 10 min. 0.05g of potassium ferricyanide and 0.63g of PVP with a molecular weight of 10000 were dissolved in 40mL of 50% ethanol solution by volume fraction and labeled as solution D. And quickly pouring the solution B into the solution A, stirring for 3h, centrifuging for 5min, collecting a sample, centrifuging at the rotating speed of 8000r/min, washing with methanol for three times, and drying in an oven at the temperature of 60 ℃ for later use.
The third step: preparation of FeSe2@CoSe2@ C negative electrode material
Mixing the components in a mass ratio of 1: 4, respectively placing the ZIF-67@ Fe-LDH sample and the selenium powder at two ends of the porcelain boat, wherein the selenium powder is arranged at a gas inlet, and the sample is arranged at a gas outlet. Calcining under Ar atmosphere, wherein the calcining temperature is 400 ℃, the calcining time is 2h, the heating rate is 2 ℃/min, and the cathode material of the cobalt-iron bimetallic selenide sodium-ion battery is obtained after the reaction is finished.
Example 3:
the first step is as follows: preparation of ZIF-67 precursor:
0.291g of cobalt nitrate was dissolved in 20mL of methanol and then stirred in a magnetic stirrer at 400r/min for 5min to complete dissolution, labeled solution A. 0.658g of 2-methylimidazole was dissolved in 20mL of methanol and stirred in a magnetic stirrer at 400r/min for 5min until complete dissolution, labeled solution B. And quickly pouring the solution B into the solution A, stirring for 5min, standing for 24h at room temperature, centrifuging for 5min, collecting a sample, centrifuging at the rotating speed of 8000r/min, washing with methanol for three times, and drying in an oven at 60 ℃ for later use.
The second step is that: synthesis of ZIF-67@ Fe-LDH structural material
0.05g of the resulting ZIF-67 was dissolved in 5mL of ethanol, labeled as solution C, and sonicated for 10 min. 0.05g of potassium ferricyanide and 0.63g of PVP with a molecular weight of 10000 were dissolved in 40mL of 50% ethanol solution by volume fraction and labeled as solution D. And quickly pouring the solution D into the solution C, stirring for 3h, centrifuging for 5min, collecting a sample, centrifuging at the rotating speed of 8000r/min, washing with methanol for three times, and drying in an oven at the temperature of 60 ℃ for later use.
The third step: preparation of FeSe2@CoSe2@ C negative electrode material
Mixing the components in a mass ratio of 1:3, respectively placing the ZIF-67@ Fe-LDH sample and the selenium powder at two ends of the porcelain boat, wherein the selenium powder is arranged at a gas inlet, and the sample is arranged at a gas outlet. Calcining under Ar atmosphere, wherein the calcining temperature is 500 ℃, the calcining time is 2h, the heating rate is 2 ℃/min, and the cathode material of the cobalt-iron bimetallic selenide sodium-ion battery is obtained after the reaction is finished.
The above-mentioned method for preparing the negative electrode material for sodium ion battery, wherein the raw materials are all purchased from the group consisting of Aladdin reagent Co., Ltd and Michelin reagent Co., Ltd, and the equipment and process used are well known to those skilled in the art.
The invention is not the best known technology.
Claims (6)
1. A preparation method of a cobalt-iron bimetallic selenide sodium-ion battery cathode material is characterized by firstly synthesizing a precursor of ZIF-67, growing a Fe metal layer on the surface of the precursor through ion adsorption, and performing high-temperature selenization calcination to obtain the cobalt-iron bimetallic selenide material with a core-shell structure with a uniform heterogeneous interface, wherein the cobalt-iron bimetallic selenide material is used as the sodium-ion battery cathode material;
the preparation method comprises the following steps of (1) preparing a ZIF-67 precursor, namely dissolving cobalt nitrate in methanol, stirring in a magnetic stirrer until the cobalt nitrate is completely dissolved, marking as solution A, dissolving 2-methylimidazole in methanol, stirring in the magnetic stirrer until the 2-methylimidazole is completely dissolved, marking as solution B, quickly pouring the solution B into the solution A, stirring, standing for 24 hours at room temperature, collecting a sample by centrifugation, washing with methanol for three times, and drying in a 60-DEG C oven to obtain the ZIF-67 precursor;
(2) synthesis of ZIF-67@ Fe-LDH structural material
Dissolving the precursor of the ZIF-67 prepared in the step (1) in ethanol, marking as a solution C, performing ultrasonic treatment for 10min, dissolving potassium ferricyanide and PVP in the ethanol solution, marking as a solution D, quickly pouring the solution D into the solution C, stirring for 3h, performing centrifugal separation, collecting a sample, washing with methanol for three times, and drying in a 60 ℃ oven to obtain a ZIF-67@ Fe-LDH structural material;
(3) preparation of FeSe2@ CoSe2@ C cathode material
And (3) respectively placing the ZIF-67@ Fe-LDH sample and the selenium powder prepared in the step (2) at two ends of a porcelain boat, calcining the selenium powder at an air inlet of gas and the ZIF-67@ Fe-LDH sample at an air outlet of gas in Ar atmosphere, and obtaining the cathode material of the cobalt-iron double-metal selenide sodium-ion battery after the reaction is finished.
2. The method according to claim 1, wherein in the step (1), the solution A contains 0.291g of cobalt nitrate and 20mL of methanol, and the solution B contains 0.658g of 2-methylimidazole and 20mL of methanol.
3. The method according to claim 1 or 2, wherein the solution A and the solution B in the step (1) are stirred at a speed of 400r/min for 5min, and the solution A and the solution B are stirred at a speed of 5min after mixing at A, B, and the rotational speed is 8000r/min during the collection of the sample by centrifugation.
4. The preparation method according to claim 1, wherein the ZIF-67 precursor required for preparing the solution C in the step (2) has a mass of 0.05g and a volume of 5mL of ethanol, the potassium ferricyanide required for preparing the solution D has a mass of 0.05g, a PVP molecular weight of 10000 and a mass of 0.63g, a volume fraction of 50% of an ethanol aqueous solution is 40mL, the stirring time is 3 hours after mixing the solution with C, D, and the rotation speed of the centrifugal separation is 8000 r/min.
5. The preparation method according to claim 1, characterized in that the mass ratio of ZIF-67@ Fe-LDH sample to selenium powder in step (3) is 1: 3-4.
6. The production method according to claim 1 or 5, characterized in that in the step (3), the calcination temperature in Ar atmosphere is 400 ℃ to 500 ℃, the calcination time is 2 hours, and the temperature rise rate is 2 ℃ per minute.
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CN113823790B (en) * | 2021-08-23 | 2022-11-29 | 中南大学 | Cobalt iron selenide/graphene nanoribbon composite negative electrode material and preparation method thereof |
CN114671414B (en) * | 2022-03-25 | 2023-05-16 | 浙江大学 | Iron-copper-tin ternary selenide nano material for sodium ion battery and preparation method |
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