CN111244561B - Preparation method of high-energy-density and high-voltage graphite-zinc-based ion battery based on aqueous electrolyte - Google Patents

Preparation method of high-energy-density and high-voltage graphite-zinc-based ion battery based on aqueous electrolyte Download PDF

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CN111244561B
CN111244561B CN202010154573.5A CN202010154573A CN111244561B CN 111244561 B CN111244561 B CN 111244561B CN 202010154573 A CN202010154573 A CN 202010154573A CN 111244561 B CN111244561 B CN 111244561B
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zinc
graphite
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battery
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CN111244561A (en
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师唯
刘洪文
杨皓
程鹏
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Nankai University
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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
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • 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
    • H01M10/36—Accumulators not provided for in groups H01M10/05-H01M10/34
    • H01M10/38—Construction or manufacture
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M2300/00—Electrolytes
    • H01M2300/0002—Aqueous electrolytes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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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
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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Abstract

The preparation method of the high-energy density and high-voltage graphite-zinc-based ion battery based on the water system electrolyte comprises the following steps: (1) Soluble bromine salt is dissolved in saturated zinc chloride solution to obtain high-concentration (30 mol/L) electrolyte. (2) And coating the graphite positive electrode material by using a wet film-making method to obtain the positive electrode piece. (3) And assembling the electrolyte, the positive pole piece and the negative metal zinc foil into the simple soft package battery. The invention designs novel high-concentration zinc chloride + bromine salt aqueous electrolyte as a core, and reversible intercalation reaction can be carried out in a graphite electrode based on the electrolyte, and the average potential is 1.71V (for Zn/Zn) 2+ ) In the case of (1), 257mAh g was obtained ‑1 High capacity of (2). The graphite-zinc-based dual-ion battery with the limit voltage of more than 2V is assembled, and the energy density of the battery can reach 440Wh kg ‑1 . The halogen anion intercalation mechanism combines the high energy density of the conversion reaction, and greatly improves the energy density of the water system zinc-based battery.

Description

Preparation method of high-energy-density and high-voltage graphite-zinc-based ion battery based on aqueous electrolyte
Technical Field
The invention belongs to the technical field of secondary ion battery preparation, and particularly relates to preparation of a water system electrolyte graphite-zinc base ion battery capable of realizing high voltage and high energy density.
Background
Since the invention of zinc-manganese batteries in the 60's of the 19 th century, zinc batteries have been widely used in the field of primary batteries. 20. In the 60's of the century, secondary alkaline zinc manganese batteries were widely developed, but their cycle life was short due to irreversible by-products generated during discharge. The development of electric vehicles and smart grids, and the increasing popularity of intermittent energy sources such as solar energy, wind energy and tides, has made it urgent to develop new large-scale energy storage systems. Secondary batteries are one of the important large-scale energy storage systems. An ideal secondary battery for large-scale energy storage needs to have excellent electrochemical performance, rich raw material reserves, low price, economic and social benefit indexes such as environmental protection, high safety and the like. Recently, rechargeable zinc-based ion batteries based on aqueous electrolytes have drawn attention due to advantages such as abundant and inexpensive raw material resources and safety of aqueous electrolytes. However, there is a significant gap in energy density between aqueous zinc-based ion cells and organic electrolyte system cells, and the narrow electrochemical stability window, mainly due to aqueous electrolytes, limits the choice of electrode materials, resulting in low cell voltages.
The existing water system electrolyte commonly used by the water system zinc-based ion battery can cause electrochemical side reaction and uncontrollable solid-liquid interface reaction due to the existence of a large amount of water with high reaction activity; an ideal aqueous zinc-based ion battery electrolyte should also have a wide and stable voltage window to match the zinc foil negative electrode with a positive electrode material with high theoretical capacity. The problems can be comprehensively solved by reducing the content of active water through the high-concentration electrolyte provided by the invention, and the electrolyte has an important promoting effect on the development of the water-based zinc-based ion battery.
Disclosure of Invention
The invention aims to provide a preparation method of a water system electrolyte graphite-zinc-based ion battery capable of realizing high voltage and high energy density, aiming at the problems of low energy density caused by low working voltage and narrow voltage window of the water system zinc-based ion at present. The invention designs the high-concentration electrolyte, remarkably improves the working voltage and the energy density of the water-based zinc-based ion battery, and provides good prospects for large-scale application of the water-based zinc-based ion battery. By the design of the electrolyte, the average working voltage of the water-based graphite zinc-based ion battery reaches 1.71V, the water-based graphite zinc-based ion battery respectively has two flat platforms at 1.80V and 1.65V, and 440Wh kg is obtained -1 High energy density and 257mAh g -1 High specific capacity of (2).
The technical scheme of the invention is as follows:
a preparation method of a high-energy-density and high-voltage graphite-zinc-based ion battery based on an aqueous electrolyte comprises the following steps:
(1) Dissolving 0.001-1 equivalent of soluble bromine salt (such as potassium bromide) in saturated zinc chloride solution to obtain high-concentration electrolyte;
(2) Coating the artificial graphite positive electrode material by a wet film-making method, and performing vacuum drying at 60-100 ℃ for 6-12 hours to obtain the positive electrode piece.
(3) And (3) assembling the electrolyte obtained in the step (1), the positive pole piece obtained in the step (2) and the negative metal zinc foil into a simple soft package battery. The zinc ion battery provided by the invention comprises a positive electrode, a negative electrode, a diaphragm and high-concentration electrolyte.
The battery test voltage is 1.0V-2.0V, the working voltage window of the electrolyte is 0.01V-2.1V, the working mode is constant current charging and discharging, and the current is set to be 0.01-100Ag -1 The results shown in FIG. 8 were obtained after 100 weeks of charge and discharge.
The invention has the advantages and beneficial effects that:
performance: the voltage window of the cheap combined electrolyte in the method is as high as 2.1V, which is much higher than the decomposition voltage of water by 1.23V. By the design of high-concentration electrolyte, the average working voltage of the water system graphite-zinc-based ion battery reaches 1.71V, two flat platforms are respectively arranged at 1.80V and 1.65V, the voltage is higher than that of a zinc-based ion battery based on common electrolyte, and 440Wh kg is obtained -1 Ultra high energy density and 257mAh g -1 The ultra-high specific capacity.
Cost: the electrolyte and the electrode material do not contain any transition metals other than the main salt zinc chloride. The element abundance of the used anode material is high, and the price is low. The battery electrolyte and the material are extremely simple in design, have no highly toxic components (especially no fluorine and fluoride components), are green batteries, are expected to be applied to energy storage equipment with low cost, high safety and high environmental protection, and are very important for large-scale energy collection/storage requirements. The battery can be directly assembled in the air, and is convenient and fast. The results presented provide new insights into alternative energy storage technologies.
Drawings
FIG. 1 is an X-ray powder diffraction pattern of artificial graphite in an example of the present invention;
FIG. 2 is a field emission scanning electron microscope image of an artificial graphite in an example of the present invention;
FIG. 3 is a graph showing a particle size distribution of artificial graphite in an example of the present invention;
FIG. 4 is a 77K nitrogen isothermal adsorption and desorption data graph of artificial graphite in the example of the invention;
FIG. 5 is a graph of the rate performance of an aqueous electrolyte graphite-zinc-based ion battery in different voltage windows according to an embodiment of the invention;
FIG. 6 is a graph of the discharge curves of an aqueous electrolyte graphite-zinc based ion battery at different voltage windows in accordance with an embodiment of the present invention;
FIG. 7 is a cyclic voltammogram of an aqueous electrolyte graphite-zinc-based ion battery in an example of the invention;
FIG. 8 is a graph of the cycling performance of an aqueous electrolyte graphite-zinc based ion battery in an example of the invention;
FIG. 9 is a charge-discharge curve diagram of an aqueous electrolyte graphite-zinc-based ion battery in an embodiment of the invention;
FIG. 10 is a graph of the rate performance of different concentrations of potassium bromide in an aqueous electrolyte graphite-zinc based ion battery in an embodiment of the invention;
FIG. 11 is a graph of the rate performance of an aqueous electrolyte graphite-zinc based ion battery with conductive additives in accordance with an embodiment of the present disclosure;
fig. 12 is a graph of the cycle performance of the gel-state electrolyte of the aqueous electrolyte graphite-zinc-based ion battery in an example of the invention.
Detailed Description
In order to facilitate an understanding of the invention, reference will now be made in detail to the present invention, examples of which are illustrated in the accompanying drawings, and the scope of the invention is not limited to the following specific examples.
The core of the invention is novel water system ZnCl 2 + KBr electrolyte, based on which reversible intercalation reactions can be carried out in graphite electrodes, at an average potential of 1.71V (for Zn/Zn) 2+ ) In the case of (1), 257mAh g was obtained -1 High specific capacity of (2). The graphite-zinc-based ion battery with the limit voltage of more than 2.0V is assembled, and the energy density of the battery can reach 440Wh kg -1 . The halogen anion intercalation mechanism combines the conversion reaction, and greatly improves the energy density of the water system zinc-based ion battery.
Example 1:
a preparation method of a high-energy density and high-voltage graphite-zinc-based ion battery based on an aqueous electrolyte comprises the following steps:
(1) Synthesis of aqueous electrolyte:
the preparation concentration is 5.89mol kg -1 (30 mol/L) Zinc chloride and 0.38mol kg -1 (0.4 mol/L) of an aqueous solution of potassium bromide, wherein the molar ratio of zinc chloride to potassium bromide in the aqueous solution is 750:1 as an electrolyte.
(2) 900mg of artificial graphite positive electrode material, 3.33g of a 3% sodium carboxymethylcellulose aqueous solution, was sufficiently stirred, and then coated with a film by a wet film-forming method, followed by vacuum drying at 80 ℃ for 10 hours to obtain a positive electrode sheet. The physical characterization of the used graphite cathode material is shown in figure 1, and the powder X-ray result shows the phase purity of graphite; FIG. 2 is a field emission scanning electron microscope image showing the morphology of graphite as micron-sized particles; FIG. 3 shows the particle size distribution of graphite in the range of about 8 microns; FIG. 4 is the adsorption and desorption curve of graphite under 77K nitrogen, which belongs to the characteristic curve without micropores. These results are consistent with the intrinsic characteristics of graphite.
(3) And (3) assembling the electrolyte obtained in the step (1), the positive electrode sheet obtained in the step (2) and the negative electrode metal zinc foil into a simple soft package battery. Fig. 5 is a multiplying power performance diagram of the graphite-zinc-based ion battery with the water system electrolyte in different voltage windows in the experiment; the result shows that the optimal voltage window is 1.0-2.0V. FIG. 6 is a graph of the discharge curves of the cell in this experiment at different voltage windows; the result shows that the optimal voltage window is 1.0-2.0V and has two stable discharge platforms. FIG. 7 is a cyclic voltammogram of the cell in this experiment; the result shows that the optimal voltage window is 1.0-2.0V and has two pairs of reversible redox peaks. FIG. 8 is a graph of the cycling performance of the cells in this experiment; the capacity of 83mAh/g can still be achieved after the capacitor is circulated for 100 circles under the current density of 0.25A/g. FIG. 9 is a graph showing the charge and discharge curves of the battery in this experiment; the charge and discharge still have two stable discharge platforms under the current density of 0.25A/g, and the performance is excellent.
Example 2:
a preparation method of a high-energy density and high-voltage graphite-zinc-based ion battery based on an aqueous electrolyte comprises the following steps:
(1) Synthesis of electrolyte:
dissolving zinc chloride (81.78g, 0.6 mol) and potassium bromide (0.47g, 0.004mol) in water (20 mL) to obtain an electrolyte containing potassium bromide (0.2 mol/L) and zinc chloride (30 mol/L);
dissolving zinc chloride (81.78g, 0.6 mol) and potassium bromide (0.95g, 0.008mol) in water (20 mL) to obtain an electrolyte containing potassium bromide (0.4 mol/L) and zinc chloride (30 mol/L);
dissolving zinc chloride (81.78g, 0.6 mol) and potassium bromide (1.90g, 0.016 mol) in water (20 mL) to obtain an electrolyte containing potassium bromide (0.8 mol/L) and zinc chloride (30 mol/L);
zinc chloride (81.78g, 0.6 mol) and potassium bromide (3.57g, 0.03mol) were dissolved in water (20 mL) to give an electrolyte containing potassium bromide (1.5 mol/L) and zinc chloride (30 mol/L).
(2) 900mg of artificial graphite positive electrode material, 3.33g of a 3% sodium carboxymethylcellulose aqueous solution, was sufficiently stirred and then coated by a wet film-forming method, and was vacuum-dried at 100 ℃ for 6 hours to obtain a positive electrode sheet. The material characterization of the graphite cathode material is shown in figure 1, and the powder X-ray result shows the phase purity of graphite; FIG. 2 is a field emission scanning electron micrograph showing the morphology of graphite as micron-sized particles; FIG. 3 shows the particle size distribution of graphite in the range of about 8 microns; the adsorption and desorption curves of the graphite in the 77K nitrogen condition of the graph shown in the figure 4 obtain the curve characteristic of no pore, and the results all accord with the intrinsic characteristic of the graphite.
(3) And (3) assembling the electrolyte obtained in the step (1), the positive electrode sheet obtained in the step (2) and the negative electrode metal zinc foil into a simple soft package battery. FIG. 10 is a graph of rate performance of an aqueous zinc-ion battery of an embodiment of the present invention at different concentrations of potassium bromide; the test voltage of the battery is 1.0V-2.0V, the working mode is constant current charging and discharging, and the result shows that the optimal performance is obtained when the concentration of the potassium bromide is 0.4M.
Example 3:
a preparation method of a high-energy density and high-voltage graphite-zinc-based ion battery based on an aqueous electrolyte comprises the following steps:
(1) Synthesis of electrolyte:
zinc chloride (81.78g, 0.6 mol) and potassium bromide (0.95g, 0.008mol) were dissolved in water (20 mL) to give an electrolyte containing potassium bromide (0.4 mol/L) and zinc chloride (30 mol/L).
(2) 850mg of artificial graphite positive electrode material, 50mg of super P conductive agent and 3.33g of 3% sodium carboxymethylcellulose aqueous solution were sufficiently stirred, and then film-coated by a wet film-forming method, and vacuum-dried at 60 ℃ for 12 hours to obtain a positive electrode sheet. The physical characterization of the used graphite cathode material is shown in figure 1, and the powder X-ray result shows the high purity of the graphite; FIG. 2 is a field emission scanning electron micrograph showing the morphology of graphite as micron-sized particles; FIG. 3 shows the particle size distribution of graphite in the range of about 8 microns; the adsorption and desorption curves of the graphite in the 77K nitrogen condition of the graphite in the figure 4 obtain the curve characteristics without holes, and the results all accord with the intrinsic characteristics of the graphite.
(3) And (3) assembling the electrolyte obtained in the step (1), the positive electrode sheet obtained in the step (2) and the negative electrode metal zinc foil into a simple soft package battery. Fig. 11 is a rate performance graph of the aqueous zinc ion battery added with the conductive additive in the embodiment of the invention, the test voltage of the battery is 1.0V-2.0V, the working mode is constant current charge and discharge, and the result shows that the discharge capacity is reduced when the conductive additive is added.
Example 4:
a preparation method of a high-energy density and high-voltage graphite-zinc-based ion battery based on an aqueous electrolyte comprises the following steps:
dissolving zinc chloride (81.78g, 0.6 mol) and potassium bromide (0.95g, 0.008mol) in water (20 mL) to obtain a solution containing potassium bromide (0.4 mol/L) and zinc chloride (30 mol/L); adding 10wt% of xanthan gum, heating at 80 ℃ for 2 hours, and naturally cooling to room temperature to obtain the gel-state electrolyte.
(2) 900mg of artificial graphite positive electrode material, 3.33g of a 3% sodium carboxymethylcellulose aqueous solution, was sufficiently stirred and then coated by a wet film-forming method, and was vacuum-dried at 80 ℃ for 10 hours to obtain a positive electrode sheet. The physical characterization of the used graphite cathode material is shown in figure 1, and the powder X-ray result shows the high purity of the graphite; FIG. 2 is a field emission scanning electron microscope image showing the morphology of graphite as micron-sized particles; FIG. 3 shows the particle size distribution of graphite in the range of about 8 microns; the adsorption and desorption curves of the graphite in the 77K nitrogen condition of the graph shown in the figure 4 obtain the curve characteristic of no pore, and the results all accord with the intrinsic characteristic of the graphite.
(3) And (3) assembling the electrolyte obtained in the step (1), the positive electrode sheet obtained in the step (2) and the negative electrode metal zinc foil into a simple soft package battery. Fig. 12 is a graph showing the cycle performance of the gel-state electrolyte of the aqueous zinc-ion battery in accordance with the example of the present invention. The test voltage of the battery is 1.0V-2.0V, the working mode is constant current charging and discharging, and the result shows that the gel electrolyte can inhibit the dissolution of halogen ions and stabilize the cycle performance.
The above description is intended to be illustrative of the preferred embodiments and not to limit the scope of the invention, and any substantially equivalent substitutions, process optimizations, modifications, and combinations of conditions are intended to be within the scope of the invention. A few terms are necessary in the description and illustration, nor are they intended to be limiting of the invention.

Claims (2)

1. A preparation method of a high-energy density and high-voltage graphite-zinc-based ion battery based on an aqueous electrolyte is characterized by comprising the following steps:
(1) Dissolving 0.001-1 equivalent of potassium bromide in a saturated zinc chloride solution to obtain a high-concentration electrolyte;
(2) Coating the artificial graphite positive electrode material by a wet film making method, and drying in vacuum at 60-100 ℃ for 6-12 hours to obtain a positive electrode piece;
(3) And (3) assembling the electrolyte obtained in the step (1), the positive pole piece obtained in the step (2) and the negative metal zinc foil into the simple soft package battery.
2. The method of claim 1, wherein the battery has a voltage window of 0.01V to 2.1V, and is operated by constant current charging and discharging with a current setting of 0.01 to 100ag -1 。
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CN111446508B (en) * 2020-05-01 2021-07-06 浙江大学 High-concentration solution and application and preparation method thereof
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CN113471550A (en) * 2021-07-06 2021-10-01 浙江恒威电池股份有限公司 Double-active-ion-enhanced chargeable and dischargeable hybrid zinc ion battery energy storage device
CN113644326B (en) * 2021-10-18 2022-01-04 北京金羽新能科技有限公司 Water-based zinc ion battery and formation method
CN116135788B (en) * 2023-03-13 2023-11-14 浙江师范大学 Preparation method, product and application of halogen intercalation vanadium pentoxide nanoflower

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