CN113675458A - Sodium-magnesium double-salt battery with stable electrode form and improved capacity and multiplying power - Google Patents
Sodium-magnesium double-salt battery with stable electrode form and improved capacity and multiplying power Download PDFInfo
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- CN113675458A CN113675458A CN202110717414.6A CN202110717414A CN113675458A CN 113675458 A CN113675458 A CN 113675458A CN 202110717414 A CN202110717414 A CN 202110717414A CN 113675458 A CN113675458 A CN 113675458A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
- H01M10/0566—Liquid materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0564—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of organic materials only
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- H—ELECTRICITY
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- 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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
A sodium-magnesium double-salt battery with stable electrode shape and improved capacity and multiplying power belongs to the technical field of energy storage. Existing NaCrO2The specific capacity of the sodium-magnesium double-salt battery needs to be improved, the electrode form stability needs to be improved, the rate capability is poor, and the manufacturing cost is high. The negative electrode of the sodium-magnesium double-salt battery of the invention is Mg2+the/Mg electrode is characterized in that the positive electrode is a reduced graphene oxide composite SnSe electrode; the electrolyte has the formula of' x M NaBH4/y M Mg(BH4)2-ethereal solvents ", wherein x is 0.5, 1.0 or 1.5 and y is 0.1 or 0.2, M is the concentration unit mol/L. The invention can completely overcome the existing NaCrO2The deficiency of the sodium-magnesium double-salt battery.
Description
Technical Field
The invention relates to a sodium-magnesium double-salt battery with stable electrode form and improved capacity and multiplying power, belonging to the technical field of energy storage.
Background
In recent years, magnesium ion batteries become a new generation of energy storage batteries with great potential due to higher theoretical mass specific capacity and volume specific capacity. The transport of charge and the storage of energy inside magnesium ion batteries mainly rely on divalent magnesium ions. During the charging and discharging process, magnesium ions are embedded/de-embedded in the anode material, and the storage and release of energy are completed. However, due to the higher charge density of the divalent magnesium ions, the intercalation and migration of the magnesium ions in the positive electrode material are hindered, resulting in poor electrochemical performance of the magnesium ion battery.
In order to enhance the energy storage capacity of the magnesium ion battery, the prior art introduces a double-salt concept, and a magnesium-based double-salt battery appears. The magnesium-based double salt battery is similar to the magnesium ion battery, except that the electrolyte component in the magnesium-based double salt battery is two salts, namely a sodium salt and a magnesium salt. In the electrochemical process, magnesium ions and sodium ions respectively participate in electrochemical reaction at one side of the negative electrode of the battery and at one side of the positive electrode of the battery. Compared with divalent magnesium ions, monovalent sodium ions have higher ion diffusion kinetic properties and can be rapidly transferred and stored in the positive electrode material.
It has been reported (Frontiers in Chemistry,6,611, Magnesium-Sodium Hybrid With High Voltage, Capacity and Cyclability) as NaCrO2Is the anode of the battery, the cathode of magnesium, Na (CB)11H12) NaCrO constructed by adopting/APC as electrolyte2The sodium-magnesium double-salt battery is at 60mA g-1Can obtain 98mAh g at the current density of-1The specific capacity for initial discharge of (a) is shown in fig. 2. Although the NaCrO2Compared with a magnesium ion battery, the sodium-magnesium double-salt battery has the advantages that the energy storage capacity is improved, but the specific capacity is still required to be improved. Furthermore, as the charging and discharging processes proceeded, there was a significant attenuation in the battery capacity, as shown in FIG. 1, at 6mA g-1The current density of the lithium ion battery is cycled for 50 times, and the specific discharge capacity is 118mA h g-1Decaying to about 90mAh g-1The reason why the electrode has poor cycle stability (electrode morphology stability) is that NaCrO should be used2The shape stability of the anode is poor, and the electrode expands, cracks, falls off on the surface layer and is seriously pulverized along with the progress of the charging and discharging process. Meanwhile, the NaCrO2The rate capability of the sodium-magnesium double-salt battery is not good, namely, when the current density is gradually increased in multiples in the process of multiple charging and discharging, the specific discharge capacity is obviously reduced, as shown in table 1 and figure 2, the currentThe density is improved from 60 to 600, the current density is improved to 10 times, and the discharge specific capacity is reduced by more than two thirds. Furthermore, NaCrO2The material needs to be synthesized in high-temperature inert atmosphere, and the preparation difficulty is high; electrolyte component Na (CB)11H12) Is not commercially available, needs to be prepared separately and has complicated preparation process. Thus, the NaCrO2The manufacturing cost of the sodium-magnesium double-salt battery is high.
TABLE 1
Disclosure of Invention
In order to overcome the defects of the conventional sodium-magnesium double-salt battery, the invention provides the sodium-magnesium double-salt battery with stable electrode form and improved capacity and multiplying power.
The negative electrode of the sodium-magnesium double-salt battery of the invention has stable electrode shape and improved capacity and multiplying power and is Mg2+the/Mg electrode is characterized in that the positive electrode is a reduced graphene oxide composite SnSe electrode; the electrolyte has the formula of' x M NaBH4/y M Mg(BH4)2-ethereal solvents ", where x is 0.5, 1.0 or 1.5, y is 0.1 or 0.2, and M is the concentration unit mol/L.
The technical effects of the present invention are as follows.
Firstly, the capacity of the sodium-magnesium double-salt battery is obviously improved, as shown in figure 3 or figure 5, when the electrolyte is 1.0M NaBH4/0.1M Mg(BH4)2at-DGM, at 50mA g-1The discharge specific capacity of the current density discharge reaches the peak value of 252mA h g in the 5 th cycle-1Much higher than the prior art 98mA h g-1。
Secondly, the electrode form stability of the sodium-magnesium double-salt battery of the invention is improved, as shown in FIG. 3 or FIG. 5, when the electrolyte is 1.0M NaBH4/0.1M Mg(BH4)2at-DGM, at 50mA g-1From the 5 th cycle to the 40 th cycle, the specific discharge capacity of the discharge is from 252mA h g of the peak value-1Only down to 229mA hg-1The average capacity decay rate is only 0.2% per cycle by calculating the highest specific discharge capacity, which indicates that the reduced graphene oxide composite SnSe electrode has higher morphological stability.
Thirdly, the rate capability of the sodium-magnesium double-salt battery of the invention is also obviously improved, as shown in table 2 and fig. 6, the current density is improved from 50 to 500, and is also improved to 10 times, and the specific discharge capacity is only reduced by less than one half.
TABLE 2
Fourthly, the preparation of the cathode material only needs simple mixing and mechanical ball milling, does not need extreme conditions such as high temperature, high pressure and the like, and has short preparation period, simple preparation method and low preparation cost. The electrolyte preparation in the invention only needs to weigh two commercially available raw materials NaBH according to the ion concentration ratio4And Mg (BH)4)2Dissolving in ether solvent and stirring, easy preparation, short period and low cost. Therefore, the sodium-magnesium double-salt battery of the invention is easy to manufacture and low in cost.
Drawings
FIG. 1 shows a conventional NaCrO2Sodium magnesium double salt battery with 6mA g-1The cycle number of current density discharge and the discharge specific capacity curve chart.
FIG. 2 shows a conventional NaCrO2The relation curve diagram of the cycle times and the specific discharge capacity of the sodium-magnesium double-salt battery in the discharge process with different current densities in integral multiple relation.
FIG. 3 shows the formula of 1.0M NaBH when the electrolyte ratio is4/0.1M Mg(BH4)2at-DGM, at 50mA g-1The current density discharge of the battery adopts a relation curve graph of the cycle times and the discharge specific capacity of the SnSe-rGO laminated electrode, the SnSe laminated electrode and the sodium-magnesium double-salt battery respectively.
FIG. 4 is a linear sweep voltammetry test curve of the sodium-magnesium double-salt battery of the invention with different total ion concentrations of sodium and magnesium in the electrolyte.
FIG. 5 shows a sodium-magnesium double-salt battery of the present invention with different total sodium and magnesium ion concentrations in electrolyte, with 50mA g-1The graph of the relationship between the respective cycle times and the specific discharge capacity of the current density discharge is also taken as an abstract figure.
Fig. 6 is a graph showing the relationship between the cycle number and the specific discharge capacity of the sodium-magnesium double-salt battery of the present invention, in which the total sodium and magnesium ion concentrations of the electrolyte are different, during the discharging process at different current densities in an integral multiple relationship.
Detailed Description
In the sodium-magnesium double-salt battery with stable electrode shape and improved capacity and multiplying power, the composite mass percentage of the two components of the reduced graphene oxide composite SnSe electrode is as follows: 5-30% of original graphene oxide and 95-70% of SnSe, for example, 10% of original graphene oxide and 90% of SnSe. Electrolyte proportioning formula of' x M NaBH4/y MMg(BH4)2Ether solvents in "ether solvents" are diethylene glycol dimethyl ether (DGM) or tetraethylene glycol dimethyl ether, e.g. DGM; the molar concentration ratio of four ions between sodium ions and magnesium ions is (x, y) ═ 0.5, 0.1), (1.0, 0.1), (1.5, 0.1) or (1.0, 0.2), for example, (x, y) ═ 1.0, 0.1.
Regarding the positive electrode in the present invention:
the positive electrode material is prepared by compounding reduced graphene oxide and SnSe, and the preparation process is as follows. First, according to 1: 1, putting Sn powder and Se powder in a ball milling tank according to the molar ratio, filling argon gas, and then carrying out ball milling to prepare SnSe; secondly, mixing the prepared SnSe and the reduced graphene oxide rGO according to the mass percent of SnSe90 percent and original graphene oxide 10 percent, and carrying out ball milling to obtain the reduced graphene oxide composite SnSe electrode material. Then, doping conductive carbon powder into the obtained reduced graphene oxide composite SnSe electrode material, blending the conductive carbon powder into slurry by using PVDF glue, and coating the slurry on a carrier to prepare a SnSe-rGO layered electrode; for comparison, an SnSe layered electrode without the graphene protoxide was fabricated in the same manner as in this link.
With respect to the electrolyte in the present invention:
according to four types of sodium ions and magnesium ionsThe NaBH is weighed in four times according to the ion molar concentration ratio, namely (x, y) ═ 0.5, 0.1), (1.0, 0.1), (1.5, 0.1) and (1.0, 0.2)4、Mg(BH4)2And adding the electrolyte into a conical flask containing DGM for four times, and magnetically stirring for 12 hours respectively to finish the preparation of the electrolyte with four ionic molar concentration ratios.
The sodium-magnesium double-salt battery of the invention comprises:
using Mg2+a/Mg sheet electrode, a SnSe-rGO layered electrode or a SnSe layered electrode and a composition formula of' x M NaBH4/y M Mg(BH4)2The electrolyte solutions of-DGM and (x, y) are respectively (0.5, 0.1), (1.0, 0.1), (1.5, 0.1) and (1.0, 0.2) to assemble the sodium-magnesium double-salt battery of the invention.
And (4) inspecting the discharge specific capacity and the electrode form stability.
The positive electrodes are respectively an SnSe-rGO layered electrode and an SnSe layered electrode, and the electrolyte is 1.0M NaBH4/0.1M Mg(BH4)2DGM ", the electrode form stability of the positive electrodes of the two sodium-magnesium double-salt batteries is different. As shown in fig. 3, as the number of cycles increases, in contrast, the specific discharge capacity of the sodium-magnesium double-salt battery with the positive electrode being the SnSe-rGO layered electrode decreases slowly, which indicates that the presence of the reduced graphene oxide rGO inhibits the SnSe-rGO layer from growing on Na+、Mg2+The volume expansion and cracking caused in the electrochemical process of embedding, migration, storage and de-embedding relieve the pulverization of the SnSe-rGO layered electrode, namely the SnSe-rGO electrode material has higher morphological stability.
The positive electrode is also SnSe-rGO layered electrode, and the electrolytes are respectively in accordance with the matching formula of' x M NaBH4/y M Mg(BH4)2The electrochemical performances of four sodium-magnesium double-salt batteries with DGM and (x, y) of (0.5, 0.1), (1.0, 0.1), (1.5, 0.1) and (1.0, 0.2) are greatly different.
Firstly, the ionic conductivity is shown in the ionic conductivity, and as shown in table 3, as the total ionic concentration of sodium and magnesium in the electrolyte is increased, the ionic conductivity of the electrolyte is increased, so that the specific capacity of the sodium-magnesium double-salt battery is increased.
TABLE 3
Secondly, the electrolyte of the four sodium-magnesium double-salt batteries is tested by adopting a linear sweep voltammetry, as shown in fig. 4, with the rise of the test voltage, the rise of the output current of the sodium-magnesium double-salt batteries is increased due to the increase of the total ion concentration of sodium and magnesium, which is contrary to the description, the test voltage is also increased, the electrolyte with high total ion concentration of sodium and magnesium has low stability and strong side reactions, such as decomposition reaction and corrosion reaction, more released electrons and large output current, and meanwhile, the low stability of the electrolyte inevitably leads to the reduction of the electrode form stability.
Thus, the total ion concentration of sodium and magnesium is increased, which is beneficial to improving the specific capacity of the sodium-magnesium double-salt battery, but also reduces the stability of electrolyte and the stability of electrode form. Therefore, for the sake of compatibility, there is an optimum value for the total ion concentration of sodium and magnesium. As shown in fig. 5, the total ion concentration of sodium and magnesium is (1.0, 0.1), which is the best, not only the specific capacity is large, but also the electrode morphology stability is good; when the total ion concentration of sodium and magnesium is (0.5, 0.1), the specific capacity is small, although the electrode form stability is good; when the total ion concentration of sodium and magnesium is the highest, namely (1.5, 0.1), the specific capacity is only moderate, the electrode form stability is poor, and the first discharge specific capacity is up to 308mA h g-1The discharge specific capacity of the battery is obviously attenuated in the subsequent charging and discharging processes, and after 40 times of charging and discharging, the discharge specific capacity is attenuated to 192mA h g-1The discharge specific capacity retention rate is only 62%; when the total ion concentration of sodium and magnesium is (1.0, 0.2), the specific capacity is only moderate, although the electrode morphology stability is good.
And (5) inspecting the rate performance.
As shown in fig. 6, the current density is increased from 50 to 500, the discharge specific capacity is reduced by less than half, the rate capability of the sodium-magnesium double-salt battery is improved, and the rate capability of the total ion concentration of sodium and magnesium of the electrolyte is close to that of the total ion concentration of sodium and magnesium.
Claims (3)
1. The negative electrode of the sodium-magnesium double-salt battery with stable electrode form and improved capacity and multiplying power is Mg2+the/Mg electrode is characterized in that the positive electrode is a reduced graphene oxide composite SnSe electrode; the electrolyte has the formula of' x M NaBH4/y MMg(BH4)2-ethereal solvents ", where x is 0.5, 1.0 or 1.5, y is 0.1 or 0.2, and M is the concentration unit mol/L.
2. The sodium-magnesium double-salt battery with the stable electrode form and the improved capacity and the improved multiplying power according to claim 1, wherein the reduced graphene oxide and SnSe composite electrode comprises the following two components in percentage by mass: 5-30% of original graphene oxide and 95-70% of SnSe.
3. The sodium-magnesium double-salt battery with stable electrode form and improved capacity and multiplying power as claimed in claim 1, wherein the electrolyte has a formula of "x M NaBH4/y M Mg(BH4)2The ether solvent in the ether solvent is diethylene glycol dimethyl ether or tetraethylene glycol dimethyl ether; the molar concentration ratio of four ions between sodium ions and magnesium ions is (x, y) ═ 0.5, 0.1, (1.0, 0.1), (1.5, 0.1) or (1.0, 0.2).
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| CN106532111A (en) * | 2015-09-15 | 2017-03-22 | 中国科学院上海硅酸盐研究所 | Conversion reaction-based magnesium battery with high energy density |
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| CN109742353A (en) * | 2018-12-29 | 2019-05-10 | 陕西科技大学 | A kind of SnSe quantum dot/r-GO compound and its preparation method and application |
| CN110165154A (en) * | 2019-04-08 | 2019-08-23 | 陕西科技大学 | A kind of carbon quantum dot surface modification 1-dimention nano SnO2Double salt cell positive materials of magnesium-lithium and preparation method thereof and its application |
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- 2021-06-28 CN CN202110717414.6A patent/CN113675458A/en active Pending
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013061079A1 (en) * | 2011-10-26 | 2013-05-02 | Nexeon Limited | An electrode composition for a secondary battery cell |
| CN106532111A (en) * | 2015-09-15 | 2017-03-22 | 中国科学院上海硅酸盐研究所 | Conversion reaction-based magnesium battery with high energy density |
| US20170279151A1 (en) * | 2016-03-25 | 2017-09-28 | Toyota Motor Engineering & Manufacturing North America, Inc. | Magnesium battery having an electrolyte containing cations of magnesium and sodium |
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| CN106129461A (en) * | 2016-09-08 | 2016-11-16 | 吉林大学 | A kind of sodium Mg secondary cell and preparation method thereof |
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