CN110867571A - Preparation method of hexagonal-prism-shaped iron-cobalt bimetallic selenide - Google Patents
Preparation method of hexagonal-prism-shaped iron-cobalt bimetallic selenide Download PDFInfo
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Abstract
The invention belongs to the field of inorganic materials, and particularly relates to a preparation method of hexagonal-prism-shaped iron-cobalt bimetallic selenide. The method comprises the following steps: s1, mixing and dissolving iron salt and cobalt salt in isopropanol; s2, preparing an isopropanol solution of PVP; s3, preparing NaHCO3An aqueous solution; s4, mixing the solutions obtained in the step S1 and the step S2 according to the volume ratio of 1: 1-3, and carrying out ultrasonic treatment for 10-20 min; s5, adding NaHCO into the mixed solution obtained in the step S43Obtaining an iron-cobalt metal precursor by using an aqueous solution;s6, mixing the iron-cobalt metal precursor and the selenium powder in the step S5 according to the mass ratio of 1: mixing 1-3, and calcining for 3-5 h. The Fe-Co bimetallic selenium composite carbon material prepared by the preparation method provided by the invention has stable cycle life and rate capability, and the carbon doping can enhance the conductivity of the material so as to improve the specific capacity of the battery.
Description
Technical Field
The invention belongs to the field of inorganic materials, and particularly relates to a preparation method of hexagonal-prism-shaped iron-cobalt bimetallic selenide.
Background
The energy storage problem is a hot point of discussion in the scientific research community today. The main energy storage technologies at present are physical, phase change, electromagnetic and electrochemical energy storage. The breakthrough of battery technology in electrochemical energy storage is large, particularly lithium ion batteries, the rapid development of which promotes the development of the whole energy market, opens up a new path for the energy market, and simultaneously, the development of new battery technology is continuously stimulated along with the rapid increase of the demand of the lithium ion batteries. However, since lithium is a scarce element on the earth, and the development demand technology is high, the cost of lithium ion batteries is high, and in addition, the lithium ion batteries are short of supply and demand in the vast energy market as commodities, the existing lithium resources cannot meet the demand of people, and the development of the lithium ion batteries is seriously hindered. Therefore, sodium ion batteries of the same family as lithium are gradually paid attention by the scientific research community, and attract a large number of researchers of energy storage materials. The abundance in the earth is far higher than that of lithium, and the property of the earth is very similar to that of lithium, namely Na+The standard electrode potential of the/Na couple is-2.71V, with Li+The Li electric pair is closer to-3.04V, has the advantages of high resource storage capacity, low development technical requirement, higher safety, low price, greenness, environmental protection and the like compared with the lithium element, and has the prospect of being the next generation capable of replacing lithium ion batteries in partial fields.
However, Na+Is 0.102nm, and Li+Has a radius of 0.076nm of aboutLi+1.34 times of the total amount of the lithium ion battery anode and cathode materials, the diffusion problem of the lithium ion battery anode and cathode materials in the working process of the battery is hindered, so that the energy storage mechanism of the lithium ion battery anode and cathode materials is greatly different from the crystal structure, and most of the lithium ion battery anode and cathode materials cannot be suitable for a sodium ion battery system. Various sodium ion battery cathode materials are researched and applied at present, mainly embodied in single metal, double metal oxide, selenide, sulfide, phosphide and doped materials thereof, in order to improve the problem of material expansion in the charging and discharging process so as to reduce the cycle reversibility and service life of the battery, the transition metal selenide has higher theoretical specific capacity than the oxide and has higher stability than the sulfide. The problem of the destruction of the material architecture during charging and discharging is still serious.
At present, most of the synthesized negative electrode materials are prepared by synthesizing a precursor by using a metal organic framework as a template and then performing high-temperature treatment on the precursor to obtain the final electrode material, the obtained material has different morphology structures, and the performances of the material when the material is used as a battery material have respective characteristics. Some materials are synthesized by using a coprecipitation method to synthesize a precursor through high-temperature treatment, compared with a hydrothermal method, the method is simpler in operation, safer, energy-saving, high in yield and short in synthesis period, but agglomeration is generated or the composition is not uniform enough due to overhigh local concentration, so that the material is irregular in appearance.
Disclosure of Invention
The invention aims to overcome the problems in the prior art and provides a preparation method of hexagonal-prism-shaped iron-cobalt bimetallic selenide.
Another object of the present invention is to provide a bimetal selenium compound with hexagonal prism-shaped iron cobalt prepared by the above preparation method.
The invention also aims to provide application of the iron-cobalt bimetallic selenium compound as a negative electrode material of a sodium-ion battery.
The purpose of the invention is realized by the following technical scheme:
hexagonal-prism-shaped iron-cobalt bimetallic selenide (FeSe)2/CoSe2@ C) in a process for the preparation of,the method comprises the following steps:
s1, preparing a solution A: mixing iron salt and cobalt salt, dissolving in isopropanol to obtain Fe3+And Co2+The concentration of (b) is 0.01-0.03M, preferably, the iron salt is Fe (NO)3)3•9H2O, cobalt salts being Co (NO)3)2•6H2O；
S2, preparing a solution B: preparing 0.01-0.03 g/mL of PVP (polyvinylpyrrolidone) in isopropanol solution, wherein the molecular weight of the PVP is 10000-150000, preferably, the concentration of the PVP is 0.02g/mL, for example, 1g of PVP is weighed and dissolved in 50mL of isopropanol solution;
s3, preparing a solution C: preparing 0.1-0.3M NaHCO3An aqueous solution;
s4, mixing the solution A and the solution B according to the volume ratio of 1: 1-3, and carrying out ultrasonic treatment for 10-20 min;
s5, dropwise adding the mixed solution obtained in the step S4 into the solution C while carrying out constant-temperature reaction, wherein the volume of the solution C is 1-2 times that of the mixed solution obtained in the step S4, and the constant-temperature reaction temperature is 0-100 ℃; filtering after the reaction is finished; washing the precipitate with deionized water for three times after filtering, collecting the precipitate, and performing vacuum drying, cleaning and drying at the temperature of 60-65 ℃, preferably 60 ℃;
s6, mixing the iron-cobalt metal precursor obtained in the step S5 with selenium powder according to the mass ratio of 1: 1-3 parts of the ceramic boat are placed at two ends of the same ceramic boat; calcining for 3-5 h at the temperature of 300-450 ℃ in the atmosphere of reducing gas.
In order to solve the problem that a material framework of a sodium ion battery is damaged in the charging and discharging processes, the invention firstly synthesizes the iron-cobalt bimetal precursor by the method. The shape of the precursor is regular hexagonal prism shape, the nano-particles are reasonably stacked, enough space is provided for storing sodium ions, and the precursor has large specific surface area and can be better in full contact with electrolyte. And then the bimetallic selenium compound composite carbon material is obtained by a calcination method, so that the stability of the nano material is further improved, and the application of the nano material to the cathode material of the sodium-ion battery is improved. The carbon layer formed by calcining the doped carbon source can effectively protect the material structure and inhibit the volume expansion of the material during the charging and discharging of the battery.
Preferably, the molecular weight of PVP in step S2 is 10000.
Preferably, the temperature rise rate of the calcination in the step S6 is 3-5 ℃/min.
Preferably, the reducing gas in the step S6 is H2And Ar, wherein the volume of the hydrogen is 8-15% of the volume of the mixed gas. The effect of the mixed gas is mainly H2Reacting with selenium powder to obtain hydrogen selenide gas, and reacting the obtained hydrogen selenide gas with a precursor to finally obtain the required selenide.
Preferably, the mass ratio of the iron-cobalt metal precursor to the selenium powder in the step S6 is 1: 2.
Compared with the prior art that an organic frame is adopted as a template and is used as a precursor or a coprecipitation method, the method adopts the steps of synthesizing a metal precursor, doping a carbon source, and calcining at high temperature in the atmosphere of reducing gas to obtain FeSe2/CoSe2@ C nanomaterial. And experiments show that the material synthesized by the method has better conductivity when used as an electrode material.
The iron-cobalt bimetallic selenide is applied as a cathode material of a sodium ion battery, the sodium ion battery has stable cycle life and rate capability, and the carbon doping can enhance the conductivity of the material so as to improve the specific capacity of the battery.
In summary, compared with the prior art, the invention has the following technical effects:
1. the iron-cobalt bimetallic precursor prepared by the scheme provided by the invention presents regular hexagonal prism-shaped nanoparticles, the particle size distribution is uniform, the specific surface area is larger, the framework structure is stable, and the iron-cobalt bimetallic precursor can be further functionally modified without changing the morphology. The carbon source is doped during the preparation of the precursor, the carbon layer formed after calcination can effectively protect the material structure, inhibit the volume expansion of the material during the charge and discharge of the battery, have stable cycle life and rate capability, and the carbon doping can enhance the conductivity of the material so as to improve the specific capacity of the battery.
2. The small hexagonal prism-shaped nano structure can be fully contacted with the electrolyte, and can be uniformly mixed with the conductive carbon black and the binder when the battery is assembled, so that the material and the carrier are combined more firmly, the phenomenon that the material is dispersed into the electrolyte along with the charging and discharging processes is avoided, and the material has great contribution to the cycle performance of the sodium-ion battery.
3. Compared with the oxide of the nano material obtained by selenizing the iron-cobalt bimetallic precursor at high temperature, the nano material has the advantages that the distance for sodium ions to be embedded into the material is smaller during charging and discharging, so that the resistance of a battery system is smaller, the coulomb efficiency of charging and discharging is improved, and the specific capacity of the material is also favorably improved.
Drawings
FIG. 1 is a scanning electron microscope image of a Fe-Co bimetallic precursor;
FIG. 2 FeSe2/CoSe2@ C scanning electron microscope pictures;
FIG. 3 FeSe2/CoSe2The XRD pattern of @ C is compared with a PDF standard card;
FIG. 4 FeSe2/CoSe2@ C as negative electrode material of sodium ion battery at current density of 1A g-1Electrochemical cycling profile under charge and discharge conditions; and
FIG. 5 FeSe2/CoSe2Rate performance graph of charging and discharging of @ C.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be described in detail below with reference to specific examples and comparative examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the examples given herein without any inventive step, are within the scope of the present invention.
Unless otherwise specified, the equipment used in the present examples, comparative examples and experimental examples was conventional experimental equipment, and the materials and reagents used were commercially available.
Example 1
A preparation method of hexagonal-prism-shaped iron-cobalt bimetallic selenide comprises the following steps:
s1, taking 0.4040g of Fe (NO)3)3•9H2O and 0.2911g Co (NO)3)2•6H2Dissolving O in 50mL of isopropanol, and marking as a solution A;
s2, dissolving 1.0g of PVP (Mw = 10000) in 50mL of isopropanol, and marking as a solution B;
s3, taking 1.6802g of NaHCO3Dissolving in 100mL of deionized water, and marking as solution C;
s4, mixing the solution B with the solution A, performing ultrasonic treatment for 15min, and dropwise adding the solution C under the magnetic stirring of an oil bath; keeping the oil bath temperature at 40 ℃ for reaction for 12h, centrifugally washing the reaction product for several times by using ethanol and deionized water after the reaction is finished, and carrying out vacuum drying at 60 ℃ for 24h to collect precipitates;
s6, respectively placing the prepared iron-cobalt precursor and selenium powder at two ends of a porcelain boat, and uniformly paving the iron-cobalt precursor and the selenium powder at a mass ratio of 1: 2;
s7 at H2/Ar(10vol% H2) Calcining under gas, raising the temperature to 400 ℃ at the temperature raising rate of 4 ℃/min, and keeping the reaction for 4 h. Cooling to room temperature to obtain FeSe2/CoSe2@ C negative electrode material compound.
Example 2
The procedure of example 1 was repeated to adjust the oil bath in S4 to a 0 ℃ ice bath.
Example 3
The procedure of example 1 was repeated to adjust the temperature of the oil bath to 20 ℃ in S4.
Example 4
The procedure of example 1 was repeated to adjust the temperature of the oil bath to 60 ℃ in S4.
Example 5
The procedure of example 1 was repeated to adjust the temperature of the oil bath to 80 ℃ in S4.
Example 6
The procedure of example 1 was repeated to adjust the temperature of the oil bath to 100 ℃ in S4.
Example 7
The procedure of example 1 was repeated to adjust the calcination temperature in S7 to 300 ℃.
Example 8
The procedure of example 1 was repeated to adjust the calcination temperature to 350 ℃ in S7.
Example 9
The procedure of example 1 was repeated to adjust the calcination temperature in S7 to 450 ℃.
Examples of the experiments
The iron-cobalt bimetallic composite carbon obtained in example 1 was used as an electrode material of a sodium ion battery for performance testing.
The iron-cobalt bimetallic precursor material obtained in example 1 was observed under a scanning electron microscope. As shown in fig. 1, the prepared iron-cobalt bimetallic precursor is hexagonal prism-shaped nanoparticles with uniform size. Sodium ion battery cathode material FeSe prepared by X-ray diffraction test2/CoSe2@ C from FeSe2/CoSe2Comparison of the XRD pattern of @ C with the PDF standard card shows that the synthesized material is indeed FeSe2/CoSe2@ C. FeSe is reacted with2/CoSe2@ C as negative electrode material of sodium ion battery at current density of 1A g-1The electrochemical cycle under the charge-discharge conditions of (1) and (2) is shown in fig. 4; the results of the rate performance test of the charge and discharge of the electrode material are shown in fig. 5. As can be seen from fig. 4 and 5, the synthesized material has not only higher and stable specific capacitance, but also charge-discharge efficiency substantially maintained at 100% and better rate performance as a sodium ion battery.
The same tests were carried out on the materials of examples 2 to 9, with results similar to those of example 1.
Claims (8)
1. The preparation method of the hexagonal-prism-shaped iron-cobalt bimetallic selenide is characterized by comprising the following steps of:
s1, preparing a solution A: mixing iron salt and cobalt salt, dissolving in isopropanol to obtain Fe3+And Co2+The concentration of the (A) is 0.01-0.03M;
s2, preparing a solution B: preparing an isopropanol solution of polyvinylpyrrolidone with the concentration of 0.01-0.03 g/mL, wherein the molecular weight of the polyvinylpyrrolidone is 10000-150000;
s3, preparing a solution C: preparing 0.1-0.3M NaHCO3An aqueous solution;
s4, mixing the solution A and the solution B according to the volume ratio of 1: 1-3, and carrying out ultrasonic treatment for 10-20 min;
s5, dropwise adding the mixed solution obtained in the step S4 into the solution C while carrying out constant-temperature reaction, wherein the volume of the solution C is 1-2 times that of the mixed solution obtained in the step S4, and the constant-temperature reaction temperature is 0-100 ℃; after the reaction is finished, filtering, cleaning and drying to obtain an iron-cobalt metal precursor;
s6, mixing the iron-cobalt metal precursor obtained in the step S5 with selenium powder according to the mass ratio of 1: 1-3, and calcining for 3-5 hours at the temperature of 300-450 ℃ in a reducing atmosphere.
2. The method for preparing Fe-Co-Bi-metal-Se compound of claim 1, wherein the Fe salt is Fe (NO) in step S13)3•9H2O; the cobalt salt is Co (NO)3)2•6H2O。
3. The method of claim 1, wherein the molecular weight of the polyvinylpyrrolidone in step S2 is 10000.
4. The method for preparing Fe-Co bimetallic selenide according to claim 1, wherein the temperature rise rate of calcination in the step S6 is 3-5 ℃/min.
5. The method of claim 1, wherein the inert gas in the step S6 is H2And Ar, wherein the volume of the hydrogen is 8-15% of the volume of the mixed gas.
6. The method of claim 1, wherein the mass ratio of the metal precursor of Fe-Co to the selenium powder in step S6 is 1: 2.
7. An Fe-Co bimetallic selenium compound prepared by the method of any one of claims 1 to 6.
8. The use of the Fe-Co-Bi-metallic selenium compound of claim 7 in the anode material of a sodium-ion battery.
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| CN112138685A (en) * | 2020-10-15 | 2020-12-29 | 吉林大学 | Composite catalytic material, preparation method thereof, electrode and application |
| CN113593922A (en) * | 2021-07-27 | 2021-11-02 | 陕西君普新航科技有限公司 | Super capacitor electrode powder material and preparation method thereof |
| CN113629245A (en) * | 2021-08-05 | 2021-11-09 | 肇庆市华师大光电产业研究院 | Novel compounding method of carbon material and transition metal compound, composite material and application |
| CN113823790A (en) * | 2021-08-23 | 2021-12-21 | 中南大学 | Cobalt iron selenide/graphene nanoribbon composite negative electrode material and preparation method thereof |
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| CN112138685A (en) * | 2020-10-15 | 2020-12-29 | 吉林大学 | Composite catalytic material, preparation method thereof, electrode and application |
| CN113593922A (en) * | 2021-07-27 | 2021-11-02 | 陕西君普新航科技有限公司 | Super capacitor electrode powder material and preparation method thereof |
| CN113629245A (en) * | 2021-08-05 | 2021-11-09 | 肇庆市华师大光电产业研究院 | Novel compounding method of carbon material and transition metal compound, composite material and application |
| CN113823790A (en) * | 2021-08-23 | 2021-12-21 | 中南大学 | Cobalt iron selenide/graphene nanoribbon composite negative electrode material and preparation method thereof |
| 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 |
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