CN113936927A - High-voltage aqueous electrolyte and application thereof - Google Patents
High-voltage aqueous electrolyte and application thereof Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
- H01G11/62—Liquid electrolytes characterised by the solute, e.g. salts, anions or cations therein
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/54—Electrolytes
- H01G11/58—Liquid electrolytes
- H01G11/60—Liquid electrolytes characterised by the solvent
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02E60/13—Energy storage using capacitors
Abstract
The application provides a high-voltage aqueous electrolyte, which comprises an aqueous solvent and a chlorine salt solute. Additives can also be added to prepare the high-voltage aqueous gel electrolyte. The high-voltage aqueous electrolyte has a wide voltage window and high safety, and the preparation method is extremely simple and is suitable for the aqueous flexible planar micro supercapacitor with high voltage and high safety. In the application of the aqueous flexible planar micro supercapacitor, the high-voltage aqueous electrolyte improves the decomposition voltage of the aqueous electrolyte and widens Ti3C2TxThe working voltage window of the MXene electrode material further improves the electrochemical performance and the application range of the water system flexible planar micro supercapacitor, and lays a foundation for the popularization and the application of the water system flexible planar micro supercapacitor.
Description
Technical Field
The invention relates to a high-voltage aqueous electrolyte and application thereof, belonging to the technical field of electrolyte preparation and electrochemical energy storage.
Background
With the rapid development of modern technologies, the fields of intelligent wearable devices, self-powered microsystems and the like begin to permeate into the daily life of people, and the demand of the fields is gradually increasing. Since the prototype of the micro super capacitor is reported, the flexible planar micro super capacitor is increasingly favored as a novel micro energy storage device which can continuously supply power to the microelectronic device, and has the advantages of flexible design, space saving, high power density, long cycle life, maintenance-free property and the like, thereby becoming one of the most potential micro energy storage devices.
The energy density of the device is in direct proportion to the square of capacitance and voltage, the capacitance is enhanced mainly by regulating and controlling electrode materials, and the voltage is improved mainly in relation to the electrolyte used. At present, a novel two-dimensional transition metal layered Ti3C2TxThe MXene material has the advantages of high charge storage capacity, good conductivity, excellent flexibility and mechanical property, adjustable interlayer spacing, abundant electrochemical active sites and the like, and becomes an energy storage electrode material with great development prospect. Compared with organic electrolyte, the water system electrolyte has the advantages of no toxicity, no harm, no flammability, high ionic conductivity, high safety, low cost, environmental friendliness and the like. However, Ti is contained in the aqueous electrolyte3C2TxWhen MXene is used as an electrode material of a flexible planar micro supercapacitor, the MXene is easy to oxidize under high anode potential, so that the working voltage window is narrow, and the improvement of the energy density is seriously limited; limited by the thermodynamic decomposition voltage (1.23V) of water to make Ti3C2TxThe stable working voltage of the MXene water system flexible planar micro supercapacitor is difficult to break through 1V, so that Ti is increased3C2TxThe working voltage of the MXene water system flexible plane micro super capacitor becomes a difficult problem before a scientific interface.
Disclosure of Invention
The object of the present invention is to provide a Ti3C2TxThe high-voltage aqueous electrolyte for the MXene flexible planar micro supercapacitor has a wide voltage window and high safety, and is suitable for the high-voltage and high-safety aqueous planar micro supercapacitor.
A high-voltage aqueous electrolyte includes an aqueous solvent and a chlorine salt solute.
Optionally, the high voltage aqueous electrolyte is comprised of an aqueous solvent and a chloride solute.
Alternatively, the molar mass ratio of the chlorine salt solute to the water solvent is not less than 5 mol/Kg.
Optionally, the molar mass ratio of the chlorine salt solute to the water solvent is 5-20 mol/Kg.
Alternatively, the upper limit of the molar mass ratio of the chlorine salt solute to the water solvent is selected from 6mol/Kg, 8mol/Kg, 10mol/Kg, 12mol/Kg, 14mol/Kg, 16mol/Kg, 18mol/Kg, or 20 mol/Kg; the lower limit is selected from 5mol/Kg, 6mol/Kg, 8mol/Kg, 10mol/Kg, 12mol/Kg, 14mol/Kg, 16mol/Kg or 18 mol/Kg.
The chloride solute has a solubility limit in the aqueous solvent and the corresponding upper limit of its molar mass is the value corresponding to when it reaches its maximum solubility.
Optionally, the chloride solute is selected from at least one of lithium chloride, sodium chloride, potassium chloride, zinc chloride, magnesium chloride.
The high-voltage water system electrolyte comprises a water solvent and a chlorine salt solute, and has higher decomposition voltage than the existing water system electrolyte, so that an electrode material can work at higher voltage, and the energy density of an energy storage device is improved.
Optionally, the high-voltage aqueous electrolyte may further contain an additive;
the additive is at least one selected from silicon dioxide powder, polyvinyl alcohol and methylene bisacrylamide.
The additive is selected to enable the high-voltage water system electrolyte to form gel, so that the stability of the high-voltage water system electrolyte is improved, and the high-voltage water system electrolyte has higher safety when used for an energy storage device and is convenient for practical application.
Optionally, the amount of the additive is 1-30% of the mass of the solvent.
Preferably, the amount of the additive is 5-20% of the mass of the solvent.
Optionally, the additive is used in an amount such that the upper limit of the mass of the solvent is selected from 5%, 10%, 20%, 30%; the lower limit is selected from 1%, 5%, 10% or 20%.
Optionally, the electrochemical stability window of the high voltage aqueous electrolyte is greater than 2.5V.
According to another aspect of the present invention, there is provided a method for preparing the high voltage aqueous electrolyte, which is simple, safe and easy to operate.
A preparation method of a high-voltage water-based electrolyte is characterized in that a chlorine salt solute is fully dissolved in a water solvent to obtain the high-voltage water-based electrolyte.
Optionally, an additive may be further added to the high-voltage aqueous electrolyte.
In the application, the chlorine salt solute is added into the aqueous solvent and fully dissolved to obtain the high-voltage aqueous electrolyte. And adding an additive to obtain the high-voltage aqueous gel electrolyte.
According to another aspect of the application, the high-voltage aqueous electrolyte and the application of the high-voltage aqueous electrolyte prepared by the preparation method in an aqueous planar micro supercapacitor are provided.
According to still another aspect of the present application, there is provided the high-voltage aqueous electrolyte described above, the high-voltage aqueous electrolyte prepared by the above-described preparation method, and Ti3C2TxApplication in MXene flexible planar micro super capacitor.
As a specific implementation mode, Ti is filtered by a vacuum filtration method by using a mask plate3C2TxMXene is filtered on a filter membrane and then transferred on polyethylene terephthalate (PET) to obtain flexible Ti3C2TxMXene microelectrode, then coating the high-voltage aqueous electrolyte to assemble Ti3C2TxMXene flexible plane miniature ultracapacitor.
The beneficial effects that this application can produce include:
the high-voltage aqueous electrolyte provided by the application has a wide voltage window and high safety, and the preparation method is extremely simple, so that the high-voltage aqueous electrolyte is suitable for a high-voltage and high-safety aqueous planar micro supercapacitor. In the application of the aqueous flexible planar micro super capacitor, the high-voltage aqueous electrolysis of the application is adoptedLiquid, which improves the decomposition voltage of aqueous electrolytes and broadens Ti3C2TxThe working voltage window of the MXene electrode material further improves the electrochemical performance and the application range of the water system flexible planar micro supercapacitor, and lays a foundation for the popularization and the application of the water system flexible planar micro supercapacitor.
Drawings
Fig. 1 is a linear sweep voltammogram of a high-voltage aqueous electrolyte in examples 1, 3 and 4 of the present invention.
FIG. 2 is a linear sweep voltammogram of a high voltage aqueous electrolyte in examples 1 and 8 of the present invention.
FIG. 3 is a linear sweep voltammogram of an aqueous electrolyte of comparative example 1 of the present invention.
FIG. 4 shows the application of high-voltage aqueous electrolytes in examples 5, 6 and 7 of the present invention to Ti3C2TxElectrochemical cyclic voltammogram in MXene flexible planar micro-supercapacitors.
FIG. 5 shows the application of sample No. 9 in example 9 of the present invention to Ti3C2TxElectrochemical cyclic voltammogram in MXene flexible planar micro-supercapacitors.
FIG. 6 shows the application of the sulfuric acid aqueous gel electrolyte of comparative example 2 of the present invention to Ti3C2TxElectrochemical cyclic voltammogram in MXene flexible planar micro-supercapacitors.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the examples, the addition of the additive causes the high-voltage aqueous electrolyte to form a gel, and the resulting high-voltage aqueous electrolyte is referred to as a high-voltage aqueous gel electrolyte.
The analysis method in the examples of the present application is as follows:
the conductivity test analysis used a Mettler-Torledo S230-K conductivity meter.
The linear sweep voltammetry curve test and the electrochemical cyclic voltammetry curve test both adopt the Shanghai Chenghua electrochemical workstation.
Example 1
The high-voltage aqueous electrolyte of the present example specifically had the following composition: the solvent is water and the solute is lithium chloride. The preparation method comprises the following steps: according to the component ratio, 0.85 g of lithium chloride is added into each gram of water, namely 20mol/Kg, the lithium chloride is weighed and dissolved in the water by magnetic stirring to be fully dissolved, and the high-voltage aqueous electrolyte is obtained and is marked as a sample No. 1.
Example 2
The high-voltage aqueous electrolyte of the present example specifically had the following composition: the solvent is water and the solute is lithium chloride. The preparation method comprises the following steps: adding 0.425 g of lithium chloride into each gram of water according to the component ratio, namely 10mol/Kg, weighing the lithium chloride, dissolving the lithium chloride in the water, and stirring by magnetic force to fully dissolve the lithium chloride, thereby obtaining the high-voltage aqueous electrolyte of the embodiment, which is marked as sample No. 2.
Example 3
The high-voltage aqueous electrolyte of the present example specifically had the following composition: the solvent is water and the solute is sodium chloride. The preparation method comprises the following steps: adding 0.35g of sodium chloride into each gram of water according to the component ratio, namely 6mol/Kg, weighing the sodium chloride and dissolving the sodium chloride into the water to obtain the high-voltage water-based electrolyte of the embodiment, and marking as a sample No. 3.
Example 4
The high-voltage aqueous electrolyte of the present example specifically had the following composition: the solvent is water and the solute is potassium chloride. The preparation method comprises the following steps: adding 0.37g of potassium chloride into each gram of water according to the component proportion, namely 5mol/Kg, weighing the potassium chloride to dissolve in the water, namely obtaining the high-voltage water-based electrolyte of the embodiment, and marking as a sample No. 4.
Example 5
The high-voltage aqueous electrolyte of the present example specifically had the following composition: the solvent is water, the solute is lithium chloride, and the additive is silicon dioxide powder. The preparation method comprises the following steps: according to the component proportion, 0.85 g of lithium chloride is added into each gram of water, namely 20mol/Kg, the lithium chloride is weighed and dissolved in the water, then the silicon dioxide powder is added, the amount is 5 percent of the mass of the solvent, and the high-voltage aqueous gel electrolyte is obtained and recorded as sample No. 5.
Example 6
The high-voltage aqueous electrolyte of the present example specifically had the following composition: the solvent is water, the solute is sodium chloride, and the additive is silicon dioxide powder. The preparation method comprises the following steps: according to the component proportion, 0.35g of sodium chloride is added into each gram of water, namely 6mol/Kg, the sodium chloride is weighed and dissolved in the water, then the silicon dioxide powder is added, the amount of the silicon dioxide powder is 10 percent of the mass of the solvent, and the high-voltage aqueous gel electrolyte is obtained and is marked as sample No. 6.
Example 7
The high-voltage aqueous electrolyte of the present example specifically had the following composition: the solvent is water, the solute is potassium chloride, and the additive is silicon dioxide powder. The preparation method comprises the following steps: adding 0.37g of potassium chloride (5 mol/Kg) into water per gram according to the component ratio, weighing the potassium chloride to dissolve in the water, and then adding silicon dioxide powder, wherein the dosage is 10 percent of the mass of the solvent, so as to obtain the high-voltage aqueous gel electrolyte, and marking as a sample No. 7.
Example 8
The high-voltage aqueous electrolyte of the present example specifically had the following composition: the solvent is water and the solute is lithium chloride. The preparation method comprises the following steps: adding 0.0425 g of lithium chloride into each gram of water according to the component ratio, namely 1mol/Kg, weighing the lithium chloride, dissolving the lithium chloride in the water, and stirring by magnetic force to fully dissolve the lithium chloride, thereby obtaining the high-voltage aqueous electrolyte of the embodiment, which is marked as sample No. 8.
Example 9
The high-voltage aqueous electrolyte of the present example specifically had the following composition: the solvent is water and the solute is lithium chloride. The preparation method comprises the following steps: adding 0.0425 g of lithium chloride, namely 1mol/Kg, into each gram of water according to the component proportion, weighing the lithium chloride, dissolving the lithium chloride in the water by magnetic stirring, fully dissolving the lithium chloride, and then adding silicon dioxide powder, wherein the dosage is 20% of the mass of the solvent, so that the high-voltage aqueous gel electrolyte is obtained and is marked as sample No. 9.
Comparative example 1
The electrolyte of the example specifically consists of: the solvent is water and the solute is sulfuric acid. The preparation method comprises the following steps: 5.4 ml of analytically pure sulfuric acid is measured and prepared into 100 ml of solution with water to obtain 1mol/L sulfuric acid solution, namely the water-based electrolyte of the embodiment is obtained and is marked as D1 #.
Comparative example 2
The electrolyte of the example specifically consists of: the solvent is water and the solute is sulfuric acid. The preparation method comprises the following steps: measuring 5.4 ml of analytically pure sulfuric acid, preparing 100 ml of solution with water to obtain 1mol/L sulfuric acid solution, and adding polyvinyl alcohol with the amount being 10% of the mass of the solvent to obtain the water-based gel electrolyte, which is marked as D2 #.
Example 10
The samples prepared in the above examples were subjected to ion conductivity tests.
The ionic conductivity of sample # 1 was about 71mS/cm, the ionic conductivity of sample # 2 was about 158mS/cm, the ionic conductivity of sample # 3 was about 229mS/cm, the ionic conductivity of sample # 4 was about 351mS/cm, the ionic conductivity of sample # 5 was about 70mS/cm, the ionic conductivity of sample # 6 was about 213mS/cm, the ionic conductivity of sample # 7 was about 325mS/cm, and the ionic conductivity of sample # 8 was about 66 mS/cm.
Example 11
The samples prepared in the above examples and comparative examples were subjected to a linear sweep voltammogram test.
And (3) performing a linear sweep voltammetry curve test on the prepared high-voltage aqueous electrolyte by adopting a three-electrode system, wherein an Ag/AgCl electrode is taken as a reference electrode, activated carbon is taken as a counter electrode, and a titanium sheet is taken as a working electrode. The test results are shown in fig. 1, where LiCl represents the high voltage aqueous electrolyte of example 1, KCl represents the high voltage aqueous electrolyte of example 4, and NaCl represents the high voltage aqueous electrolyte of example 3, and it can be seen that the electrochemical stability window of the high voltage electrolyte was measured to be more than 2.5V. FIG. 2 is a result of a test of 20mol/Kg LiCl high voltage aqueous electrolyte of example 1 and 1mol/Kg LiCl high voltage aqueous electrolyte of example 8, and it can be seen that when the concentration of the electrolyte is decreased to 1mol/Kg, a slow hydrogen evolution reaction starts from about-0.5V, and the corresponding electrochemical stability window is also decreased; fig. 3 is a linear sweep voltammogram of the sulfuric acid water-based electrolyte in comparative example 1, and it can be seen that the electrochemical stability window of the sulfuric acid water-based electrolyte in comparative example 1 is less than 2V.
Example 12
The high-voltage aqueous electrolyte prepared in the above examples and the aqueous electrolyte prepared in the comparative example are used in the flexible planar micro supercapacitor, and the positive electrode and the negative electrode are both Ti3C2TxMXene nanosheet, and preparation of Ti by using a mask plate3C2TxMXene is filtered on a filter membrane and then transferred on polyethylene terephthalate (PET) to obtain flexible Ti3C2TxAnd the MXene microelectrode is coated with high-voltage aqueous electrolyte to form the flexible planar micro supercapacitor. And performing cyclic voltammetry test at 0-1.6V, wherein the scanning rate is 10 mV/s. FIG. 4 shows the application of high voltage aqueous electrolytes in example 5(LiCl), example 6(NaCl) and example 7(KCl) of the present invention to Ti3C2TxThe electrochemical cyclic voltammetry curve of the MXene flexible planar micro supercapacitor can show that Ti is contained3C2TxThe working voltage of the MXene planar micro super capacitor can reach 1.6V; FIG. 5 shows that when the concentration of LiCl is reduced to 1mol/Kg, the working voltage of the planar micro supercapacitor is lower than 1.6V; FIG. 6 shows the application of the sulfuric acid aqueous gel electrolyte of comparative example 2 to Ti3C2TxAn electrochemical cyclic voltammetry curve of the MXene flexible planar micro supercapacitor in sulfuric acid electrolyte shows that the working voltage of the planar micro supercapacitor is lower than 0.6V.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. A high-voltage aqueous electrolyte is characterized by comprising an aqueous solvent and a chlorine salt solute.
2. The high-voltage aqueous electrolyte according to claim 1, wherein the molar mass ratio of the chlorine salt solute to the water solvent is not less than 5 mol/Kg;
preferably, the molar mass ratio of the chlorine salt solute to the water solvent is 5-20 mol/Kg.
3. The high-voltage aqueous electrolyte according to claim 1, wherein the chlorine salt solute is at least one selected from the group consisting of lithium chloride, sodium chloride, potassium chloride, zinc chloride, and magnesium chloride.
4. The high-voltage aqueous electrolyte solution according to claim 1, further comprising an additive;
the additive is at least one selected from silicon dioxide powder, polyvinyl alcohol and methylene bisacrylamide.
5. The high-voltage aqueous electrolyte solution according to claim 4, wherein the amount of the additive is 1 to 30% by mass of the solvent;
preferably, the amount of the additive is 5-20% of the mass of the solvent.
6. The high-voltage aqueous electrolyte according to any one of claims 1 to 5, wherein the electrochemical stability window of the high-voltage aqueous electrolyte is greater than 2.5V.
7. The method for producing a high-voltage aqueous electrolyte solution according to any one of claims 1 to 5, wherein the high-voltage aqueous electrolyte solution is obtained by sufficiently dissolving a mixture containing a chlorine salt solute and an aqueous solvent.
8. The method for producing a high-voltage aqueous electrolyte according to claim 7, wherein an additive may be further added to the mixture.
9. Use of the high-voltage aqueous electrolyte according to any one of claims 1 to 5 or the high-voltage aqueous electrolyte prepared by the preparation method according to any one of claims 7 to 8 in an aqueous planar micro supercapacitor.
10. The high-voltage aqueous electrolyte according to any one of claims 1 to 5, the high-voltage aqueous electrolyte prepared by the method according to any one of claims 7 to 8, and the use thereof in Ti3C2TxApplication in MXene flexible planar micro super capacitor.
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