CN111342016A - Sodium-selenium battery positive electrode material and preparation method thereof - Google Patents
Sodium-selenium battery positive electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of sodium-selenium batteries, and particularly relates to a sodium-selenium battery positive electrode material and a preparation method thereof. The anode material is a selenium-carbon-coated ferroferric oxide-graphene composite material. The cathode material is used for the sodium selenium battery and has excellent electrochemical stability and ideal specific discharge capacity.
Description
Technical Field
The invention belongs to the technical field of sodium-selenium batteries, and particularly relates to a sodium-selenium battery positive electrode material and a preparation method thereof.
Background
The sodium-selenium battery is a novel metal sodium secondary battery which adopts elemental selenium or a selenium-containing compound as a positive electrode and metal sodium as a negative electrode and realizes mutual conversion between chemical energy and electric energy through a two-electron electrochemical reaction between selenium and sodium. In the sodium selenium battery, selenium as a positive electrode and sodium as a negative electrode both have very high theoretical capacities, so that the sodium selenium battery has very high theoretical energy density and is suitable for the development trend of mobile equipment with strict volume limitation at present.
Selenium and sulfur are elements of the same main group, so sodium selenium batteries have many similarities with sodium sulfur batteries widely used in smart grids and distributed power stations at present. Although selenium has a lower theoretical capacity than sulfur, it has a higher voltage and greater density, resulting in a sodium selenium battery having a theoretical energy density comparable to that of a sodium sulfur battery. In the traditional sodium-sulfur battery, because the electrochemical reaction activity of sulfur and sodium is low at room temperature, and a series of polysulfide which is easily dissolved in electrolyte is easily formed in the charging and discharging processes, the problems of low utilization rate of a sulfur positive electrode and rapid cycle capacity attenuation (generally less than 20 circles) exist, and the performance and the practical application of the sodium-sulfur battery at room temperature are seriously influenced. Therefore, the working temperature of the traditional sodium-sulfur battery is above 300 ℃, so that the sodium-sulfur battery needs additional heating equipment to maintain the temperature in the working process, and the running cost of the sodium-sulfur battery is greatly increased.
Meanwhile, as sodium and sulfur are in liquid states when the sodium-sulfur battery works, once the ceramic tube is damaged, a short circuit is formed, and at the moment, the high-temperature liquid sodium and sulfur can be in direct contact and generate violent exothermic reaction, so that the operation safety of the sodium-sulfur battery is seriously influenced. Compared with sulfur, the conductivity of selenium is twenty orders of magnitude higher, so that the electrochemical reaction activity of selenium and sodium at room temperature is far higher than that of sulfur, the utilization rate of positive active substances is greatly improved, and the positive active substances can meet the requirements of large-current charging and discharging; in addition, the solubility of the polyselenide formed by selenium in the charging and discharging process in the electrolyte is low, so that the polyselenide has higher cycle stability than a sulfur positive electrode. Although the cost of selenium is high, the manufacturing cost of the battery can be effectively reduced by assembling selenium and sodium with low cost. Therefore, the sodium selenium battery can meet the requirement of room-temperature use, so that the sodium selenium battery has better safety and energy economy compared with the traditional sodium sulfur battery, and can replace the traditional sodium sulfur battery to meet the application requirements including large-scale fixed energy storage and electric automobiles.
Although the novel sodium-selenium battery has the advantages of high energy density, high safety and the like, the research on the sodium-selenium battery is very rare at present, and the reaction mechanism of selenium as an electrode material active substance in the charging and discharging process is not clear. Amine et al (j.am. chem. soc.2012,134,4505-4508) have conducted exploratory research work on the charge-discharge reaction mechanism of a selenium positive electrode in a sodium-selenium battery, and the developed sodium-selenium battery adopts metal sodium as a negative electrode and a mixture of selenium and carbon nanotubes as a positive electrode. Because the selenium particles have larger sizes and are not effectively compounded with the conductive substrate, the electrochemical activity of the selenium cannot be effectively exerted, and the cycle capacity of the obtained sodium-selenium battery is low. Meanwhile, as the conductive substrate has weak dispersion and restriction effects on selenium, part of selenium can form polyselenide to be dissolved in electrolyte in the circulation process, so that the capacity of the sodium-selenium battery is irreversibly attenuated along with the circulation, and the service life of the battery is influenced.
Thus, major problems with sodium selenium battery positive electrode materials to date include low availability of bulk selenium and irreversible active material decay due to shuttling effects of polyselenides during cycling. At present, the main method for solving the problems is to compound selenium and a conductive porous carbon material so as to relieve the problem of low utilization rate of the selenium, and meanwhile, the carbon material can have a certain adsorption effect on polyselenide due to the higher specific surface area of the carbon material so as to relieve the capacity loss caused by the shuttle effect. However, the currently applied porous carbon materials cannot effectively adsorb the polyselenide, and finding a material which has high conductivity, has enough space to store selenium and can effectively adsorb the polyselenide becomes a research focus of the sodium selenium battery.
In conclusion, the conductive substrate with a proper porous structure is selected, selenium is effectively compounded with the conductive substrate, and the selenium is limited in the pore channel of the substrate in a molecular form, so that the sodium-selenium battery electrode material with high volume energy density and cycling stability is prepared, the sodium-selenium battery with high capacity and stable cycling performance is developed, and the method has important significance for the development of the whole energy storage field.
Disclosure of Invention
The invention aims to provide a positive electrode material of a sodium selenium battery and a preparation method thereof, aiming at the defects, wherein the positive electrode material has excellent electrochemical stability and ideal specific discharge capacity when being used for the sodium selenium battery.
The technical scheme of the invention is as follows: a positive electrode material of a sodium-selenium battery is a selenium-carbon-coated ferroferric oxide-graphene composite material.
The preparation method of the sodium-selenium battery anode material comprises the steps of firstly preparing carbon-coated ferroferric oxide composite graphene; and then compounding with elemental selenium to prepare the selenium-carbon-coated ferroferric oxide-graphene composite material.
The preparation method of the sodium-selenium battery positive electrode material comprises the following steps:
(1) preparing carbon-coated ferroferric oxide-graphene: firstly, adding ferric nitrate nonahydrate, anhydrous glucose and graphene into deionized water to prepare a mixed solution, and stirring and ultrasonically dispersing the mixed solution to obtain a uniformly dispersed reaction solution; then transferring the reaction solution into a reaction kettle for hydrothermal reaction, and cooling along with the furnace after the reaction is finished; after the reaction kettle is cooled to room temperature, taking out a hydrothermal product, performing centrifugal separation, and drying at 60 ℃ for 12-24 hours to obtain carbon-coated ferroferric oxide-graphene precursor powder; flatly paving the obtained carbon-coated ferroferric oxide-graphene precursor powder in a quartz boat, and placing the quartz boat in a tube furnace for high-temperature calcination; after the reaction is finished, continuously introducing inert gas argon until the tubular furnace is cooled to room temperature, and obtaining carbon-coated ferroferric oxide-graphene;
(2) preparing a selenium-carbon coated ferroferric oxide-graphene composite material: firstly, mixing the carbon-coated ferroferric oxide-graphene obtained in the step (1) with elemental selenium powder, uniformly grinding, then transferring the mixture into a reaction kettle, preserving the heat for 12-24 hours at the temperature of 200-240 ℃, cooling, and uniformly grinding to obtain the selenium-carbon-coated ferroferric oxide-graphene composite material.
In the step (1), 1-2 g of ferric nitrate nonahydrate, 0.1-1 g of anhydrous glucose, 0.05-0.2 g of graphene and 10-100 mL of deionized water are added.
Stirring for 30-60 min in the step (1), and ultrasonically dispersing for 1-2 h.
The temperature of the hydrothermal reaction in the step (1) is 150-200 ℃, and the reaction time is 6-12 h.
The tubular furnace high-temperature calcination in the step (1) is specifically as follows: before the calcination reaction is started, introducing inert gas argon into the tubular furnace at the flow rate of 100-200 mL/min to remove air in the tubular furnace, then adjusting the flow rate of argon to 50-100 mL/min, placing the quartz boat in a constant-temperature reaction zone in the middle of the tubular furnace, heating to 400-600 ℃ at the heating rate of 5-10 ℃/min under the argon atmosphere, and preserving heat for 2-6 hours.
In the step (2), carbon-coated ferroferric oxide-graphene is prepared by the following steps: the simple substance selenium powder is 1: 3-5.
The invention has the beneficial effects that: the positive electrode material of the sodium-selenium battery is a selenium-carbon-coated ferroferric oxide-graphene composite material. The carbon-coated ferroferric oxide-graphene is used as a selenium simple substance carrier, wherein a carbon layer on the surface of the carbon-coated ferroferric oxide has an obvious microporous structure and can be used for bearing the selenium simple substance, and the structural stability of the carbon-coated ferroferric oxide-graphene can be enhanced by the carbon-coated ferroferric oxide-graphene. The graphene is introduced, so that the conductivity of the whole anode material is improved, and the volume change of selenium in the charging and discharging process is relieved.
Ferroferric oxide in the composite material mainly plays a role in effectively adsorbing polyselenides; the carbon coating layer and the graphene mainly play a supporting role, and in addition, a larger specific surface area and a microporous structure can be provided, so that the volume expansion effect brought in the circulation process can be relieved while the active material selenium is effectively stored. The three are mutually cooperated and matched to be completely and effectively compounded with the selenium, so that the electrochemical activity of the selenium is fully exerted.
Reasonable process parameters in the preparation method become a key for controlling the ferroferric oxide and the carbon coating layer, and the proportion of the ferroferric oxide and the carbon coating layer is mainly controlled by the proportion of ferric nitrate and glucose in the precursor synthesis process. Secondly, graphite alkene has played essential effect in the aspect of improving the electric conductivity and providing the support effect, and the content of graphite alkene is mainly controlled through how much of hydrothermal in-process addition, but through hydrothermal reaction back, the graphite alkene appears piling up easily, consequently through calcining under the argon atmosphere in the tube furnace, can avoid the piling up of graphite alkene in the material effectively, obtains bigger specific surface area and microporous structure to the volume expansion that brings in the adaptation charge-discharge process better.
Drawings
Fig. 1 is a discharge specific capacity cycle diagram of the selenium-carbon-coated ferroferric oxide-graphene composite material prepared in examples 1-3 as a positive electrode material applied to a sodium selenium battery.
Detailed Description
The present invention will be described in detail below with reference to examples.
Example 1
The positive electrode material of the sodium-selenium battery is a selenium-carbon-coated ferroferric oxide-graphene composite material.
The preparation method of the sodium-selenium battery positive electrode material is characterized by comprising the following steps:
(1) preparing carbon-coated ferroferric oxide-graphene: firstly, 1.5g of ferric nitrate nonahydrate, 0.5g of anhydrous glucose and 0.1g of graphene are added into 50mL of deionized water to prepare a mixed solution, the mixed solution is mechanically stirred for 40min, and ultrasonic dispersion is carried out for 1h to obtain a uniformly dispersed reaction solution; then transferring the reaction solution to a reaction kettle, covering and screwing, placing in an oven, preserving heat for 8 hours at 180 ℃, and cooling along with the oven after the reaction is finished; after the reaction kettle is cooled to room temperature, taking out a hydrothermal product, repeatedly performing centrifugal separation by using deionized water and absolute ethyl alcohol, placing the hydrothermal product in a constant-temperature drying box, and drying the hydrothermal product for 18 hours at the temperature of 60 ℃ to obtain carbon-coated ferroferric oxide-graphene precursor powder; flatly paving the obtained carbon-coated ferroferric oxide-graphene precursor powder in a quartz boat, placing the quartz boat in a constant-temperature reaction zone in the middle of a tubular furnace, carrying out high-temperature calcination in an argon atmosphere, introducing inert gas argon into the tubular furnace at a flow rate of 150mL/min before the start of the calcination reaction to remove air in the tubular furnace, then adjusting the flow rate of argon to 80mL/min, heating the tubular furnace to 600 ℃ at a heating rate of 8 ℃/min, and preserving the heat at the temperature for 4 hours; after the reaction is finished, continuously introducing inert gas argon until the tubular furnace is cooled to room temperature, and obtaining carbon-coated ferroferric oxide-graphene;
(2) preparing a selenium-carbon coated ferroferric oxide-graphene composite material: firstly, mixing the carbon-coated ferroferric oxide-graphene obtained in the step (1) with elemental selenium powder, and uniformly grinding, wherein the carbon-coated ferroferric oxide-graphene is prepared by the following steps in percentage by mass: the elemental selenium powder is 1: 4; and then transferring the mixture to a reaction kettle, preserving heat for 18 hours at the temperature of 230 ℃, cooling and then uniformly grinding to obtain the selenium-carbon coated ferroferric oxide-graphene composite material.
Example 2
The preparation method of the sodium-selenium battery positive electrode material is characterized by comprising the following steps:
(1) preparing carbon-coated ferroferric oxide-graphene: firstly, 1.5g of ferric nitrate nonahydrate, 0.3g of anhydrous glucose and 0.1g of graphene are added into 10mL of deionized water to prepare a mixed solution, the mixed solution is mechanically stirred for 30min, and ultrasonic dispersion is carried out for 1h to obtain a uniformly dispersed reaction solution; then transferring the reaction solution to a reaction kettle, covering and screwing, placing in an oven, preserving heat for 6 hours at 150 ℃, and cooling along with the oven after the reaction is finished; after the reaction kettle is cooled to room temperature, taking out a hydrothermal product, repeatedly performing centrifugal separation by using deionized water and absolute ethyl alcohol, placing the hydrothermal product in a constant-temperature drying box, and drying the hydrothermal product for 12 hours at the temperature of 60 ℃ to obtain carbon-coated ferroferric oxide-graphene precursor powder; flatly paving the obtained carbon-coated ferroferric oxide-graphene precursor powder in a quartz boat, placing the quartz boat in a constant-temperature reaction zone in the middle of a tubular furnace, carrying out high-temperature calcination in an argon atmosphere, introducing inert gas argon into the tubular furnace at a flow rate of 100mL/min before the start of the calcination reaction to remove air in the tubular furnace, then adjusting the flow rate of argon to 50mL/min, heating the tubular furnace to 400 ℃ at a heating rate of 5 ℃/min, and preserving the heat at the temperature for 4 hours; after the reaction is finished, continuously introducing inert gas argon until the tubular furnace is cooled to room temperature, and obtaining carbon-coated ferroferric oxide-graphene;
(2) preparing a selenium-carbon coated ferroferric oxide-graphene composite material: firstly, mixing the carbon-coated ferroferric oxide-graphene obtained in the step (1) with elemental selenium powder, and uniformly grinding, wherein the carbon-coated ferroferric oxide-graphene is prepared by the following steps in percentage by mass: the elemental selenium powder is 1: 3; and then transferring the mixture to a reaction kettle, preserving heat for 12 hours at the temperature of 200 ℃, cooling and then uniformly grinding to obtain the selenium-carbon coated ferroferric oxide-graphene composite material.
Example 3
The preparation method of the sodium-selenium battery positive electrode material is characterized by comprising the following steps:
(1) preparing carbon-coated ferroferric oxide-graphene: firstly, 1.5g of ferric nitrate nonahydrate, 1g of anhydrous glucose and 0.1g of graphene are added into 100mL of deionized water to prepare a mixed solution, the mixed solution is mechanically stirred for 60min, and ultrasonic dispersion is carried out for 2h to obtain a uniformly dispersed reaction solution; then transferring the reaction solution to a reaction kettle, covering and screwing, placing in an oven, preserving heat for 12 hours at 200 ℃, and cooling along with the oven after the reaction is finished; after the reaction kettle is cooled to room temperature, taking out a hydrothermal product, repeatedly performing centrifugal separation by using deionized water and absolute ethyl alcohol, placing the hydrothermal product in a constant-temperature drying box, and drying the hydrothermal product for 24 hours at the temperature of 60 ℃ to obtain carbon-coated ferroferric oxide-graphene precursor powder; flatly paving the obtained carbon-coated ferroferric oxide-graphene precursor powder in a quartz boat, placing the quartz boat in a constant-temperature reaction zone in the middle of a tubular furnace, carrying out high-temperature calcination in an argon atmosphere, introducing inert gas argon into the tubular furnace at a flow rate of 200mL/min before the start of the calcination reaction to remove air in the tubular furnace, then adjusting the flow rate of argon to 100mL/min, heating the tubular furnace to 500 ℃ at a heating rate of 10 ℃/min, and preserving the heat at the temperature for 4 hours; after the reaction is finished, continuously introducing inert gas argon until the tubular furnace is cooled to room temperature, and obtaining carbon-coated ferroferric oxide-graphene;
(2) preparing a selenium-carbon coated ferroferric oxide-graphene composite material: firstly, mixing the carbon-coated ferroferric oxide-graphene obtained in the step (1) with elemental selenium powder, and uniformly grinding, wherein the carbon-coated ferroferric oxide-graphene is prepared by the following steps in percentage by mass: the elemental selenium powder is 1: 5; and then transferring the mixture to a reaction kettle, preserving heat for 24 hours at the temperature of 240 ℃, cooling and grinding uniformly to obtain the selenium-carbon coated ferroferric oxide-graphene composite material.
As can be seen from fig. 1, the positive electrode material obtained in example 1 has a significant advantage over examples 2 and 3 in terms of specific discharge capacity and capacity fade rate when used in a sodium selenium battery. Therefore, the selection of proper process condition parameters and reagent dosage plays a crucial role in electrochemical performance, and the optimal process parameter range and reagent dosage are obtained through creative work.
Claims (8)
1. The sodium-selenium battery positive electrode material is characterized by being a selenium-carbon-coated ferroferric oxide-graphene composite material.
2. The preparation method of the sodium-selenium battery cathode material as claimed in claim 1, characterized by firstly preparing carbon-coated ferroferric oxide composite graphene; and then compounding with elemental selenium to prepare the selenium-carbon-coated ferroferric oxide-graphene composite material.
3. The preparation method of the positive electrode material of the sodium-selenium battery as claimed in claim 2, characterized by comprising the following steps:
(1) preparing carbon-coated ferroferric oxide-graphene: firstly, adding ferric nitrate nonahydrate, anhydrous glucose and graphene into deionized water to prepare a mixed solution, and stirring and ultrasonically dispersing the mixed solution to obtain a uniformly dispersed reaction solution; then transferring the reaction solution into a reaction kettle for hydrothermal reaction, and cooling along with the furnace after the reaction is finished; after the reaction kettle is cooled to room temperature, taking out a hydrothermal product, performing centrifugal separation, and drying at 60 ℃ for 12-24 hours to obtain carbon-coated ferroferric oxide-graphene precursor powder; flatly paving the obtained carbon-coated ferroferric oxide-graphene precursor powder in a quartz boat, and placing the quartz boat in a tube furnace for high-temperature calcination; after the reaction is finished, continuously introducing inert gas argon until the tubular furnace is cooled to room temperature, and obtaining carbon-coated ferroferric oxide-graphene;
(2) preparing a selenium-carbon coated ferroferric oxide-graphene composite material: firstly, mixing the carbon-coated ferroferric oxide-graphene obtained in the step (1) with elemental selenium powder, uniformly grinding, then transferring the mixture into a reaction kettle, preserving the heat for 12-24 hours at the temperature of 200-240 ℃, cooling, and uniformly grinding to obtain the selenium-carbon-coated ferroferric oxide-graphene composite material.
4. The method for preparing the sodium-selenium battery cathode material as claimed in claim 3, wherein in the step (1), 1-2 g of ferric nitrate nonahydrate, 0.1-1 g of anhydrous glucose, 0.05-0.2 g of graphene and 10-100 mL of deionized water are added.
5. The preparation method of the sodium-selenium battery cathode material as claimed in claim 3, wherein the stirring in the step (1) is carried out for 30-60 min, and the ultrasonic dispersion is carried out for 1-2 h.
6. The preparation method of the sodium-selenium battery cathode material as claimed in claim 3, wherein the temperature of hydrothermal reaction in the step (1) is 150-200 ℃, and the reaction time is 6-12 h.
7. The preparation method of the sodium-selenium battery cathode material as claimed in claim 3, wherein the tubular furnace high-temperature calcination in the step (1) is specifically: before the calcination reaction is started, introducing inert gas argon into the tubular furnace at the flow rate of 100-200 mL/min to remove air in the tubular furnace, then adjusting the flow rate of argon to 50-100 mL/min, placing the quartz boat in a constant-temperature reaction zone in the middle of the tubular furnace, heating to 400-600 ℃ at the heating rate of 5-10 ℃/min under the argon atmosphere, and preserving heat for 2-6 hours.
8. The preparation method of the sodium-selenium battery cathode material as claimed in claim 3, wherein in the step (2), the carbon-coated ferroferric oxide-graphene is prepared by the following steps in percentage by mass: the simple substance selenium powder is 1: 3-5.
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Application publication date: 20200626 |