CN116779993A - Composite gel electrolyte of zinc ion battery, preparation method and application thereof - Google Patents

Composite gel electrolyte of zinc ion battery, preparation method and application thereof Download PDF

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Publication number
CN116779993A
CN116779993A CN202310865436.6A CN202310865436A CN116779993A CN 116779993 A CN116779993 A CN 116779993A CN 202310865436 A CN202310865436 A CN 202310865436A CN 116779993 A CN116779993 A CN 116779993A
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solution
gel electrolyte
ferricyanide
zinc
composite gel
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李维杰
郑晴睛
韩朝
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Central South University
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Central South 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
    • 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
    • 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
    • H01M2300/00—Electrolytes
    • H01M2300/0085—Immobilising or gelification of electrolyte

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  • Engineering & Computer Science (AREA)
  • Manufacturing & Machinery (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Primary Cells (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a composite gel electrolyte of a zinc ion battery, a preparation method and application thereof, wherein the preparation method comprises the following steps: dissolving potassium ferricyanide and sulfate containing metal ions in water to form a solution a and a solution b, slowly dripping the solution b into the solution a, stirring, reacting for a certain time, filtering, cleaning and drying to obtain ferricyanide; dissolving zinc trifluoromethane sulfonate in water to form a solution, filtering to obtain a zinc trifluoromethane sulfonate solution, dispersing ferricyanide in the zinc trifluoromethane sulfonate solution, and carrying out ultrasonic treatment to obtain a solution A; and dissolving polyvinyl alcohol in the solution A, heating and stirring, standing, and then freezing and thawing to obtain the composite gel electrolyte. According to the invention, ferricyanide is used as a filler to be added into the polyvinyl alcohol gel electrolyte, so that the electrolyte has higher room-temperature ionic conductivity and zinc ion migration number, and the zinc ion battery prepared based on the gel electrolyte has good cycle performance and high specific capacity.

Description

Composite gel electrolyte of zinc ion battery, preparation method and application thereof
Technical Field
The invention relates to the technical field of flexible zinc ion batteries, in particular to a composite gel electrolyte of a zinc ion battery, a preparation method and application thereof.
Background
With the development of big data, the real-time data acquisition requirement of various electronic devices is increasing, and in medical treatmentIn the fields of health care, automobiles, aviation, etc., there is also increasing interest in flexible and wearable electronics. Due to the high volume capacity of zinc metal (5855 mAh.cm -3 ) And ease of manufacturing processes, which are considered competing candidates for flexible devices. Meanwhile, the cost advantage of the water-based zinc ion battery is 25 dollars/kilowatt-hour, which is beneficial to the application of the water-based zinc ion battery in equipment of different scales. However, aqueous zinc ion batteries also face adverse water side reactions that cause zinc dendrite formation, thereby puncturing the separator and shorting. In addition, dissolution of the cathode material and formation of byproducts resulting in rapid capacity decay are also issues of concern.
Polymer hydrogel electrolytes, such as polyvinyl alcohol (PVA) and Polyacrylamide (PAM), play a key role in solving problems associated with zinc ion batteries. These electrolytes are capable of reducing the water content in the electrolyte. The solid-solid interface is introduced to replace the traditional solid-liquid interface, so that the growth of zinc dendrites can be effectively inhibited and the dissolution of the anode material can be prevented. The stable solid-solid interface can reduce side reactions caused by moisture at the interface in the charge and discharge process, thereby improving electrochemical stability.
However, the ionic conductivity in the polymer hydrogel electrolyte is about 10 -4 ～10 -1 S·cm -1 Lower than the aqueous electrolyte. Accordingly, there is a need to provide a gel electrolyte that increases room temperature ionic conductivity and flexibility.
Disclosure of Invention
In view of the above-mentioned shortcomings existing at present, the invention provides a composite gel electrolyte of zinc ion battery, preparation method and application thereof, the invention uses polyvinyl alcohol and zinc triflate as main raw materials, prussian blue analogue ferricyanide as filler, a gel electrolyte which shows excellent ionic conductivity and higher ionic migration number at room temperature is prepared, and the zinc ion battery using the gel electrolyte has excellent cycle performance and high specific capacity.
In order to achieve the above object, the present invention provides a method for preparing a composite gel electrolyte of a zinc ion battery, comprising the steps of:
step 1: dissolving potassium ferricyanide and sulfate containing metal ions in deionized water to form potassium ferricyanide solution and sulfate containing metal ions, slowly dripping the sulfate containing metal ions into the potassium ferricyanide solution, continuously stirring, reacting for a certain time, filtering, cleaning and drying to obtain ferricyanide;
step 2: dissolving zinc trifluoromethane sulfonate in deionized water to form a solution, filtering to obtain a zinc trifluoromethane sulfonate solution, dispersing ferricyanide in the zinc trifluoromethane sulfonate solution, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 3: and dissolving polyvinyl alcohol in the solution A, heating and stirring uniformly, standing to remove bubbles, and then freezing and thawing to obtain the composite gel electrolyte.
In accordance with one aspect of the invention, in step 1, the ferricyanide comprises one or more of iron ferricyanide, cobalt ferricyanide, nickel ferricyanide, manganese ferricyanide, copper ferricyanide, zinc ferricyanide.
According to one aspect of the invention, the concentration of the potassium ferricyanide solution is 0.05-0.2mol/L, and the concentration of the sulfate or chloride solution containing metal ions is 0.1-0.2mol/L; the concentration of the zinc trifluoromethane sulfonate solution is 1-4mol/L.
According to one aspect of the invention, in step 1, the reaction time is 4-6 hours; the cleaning is carried out by adopting deionized water; the drying temperature is 60-100 ℃ and the drying time is 12-15h.
According to one aspect of the invention, in step 3, the mass fraction of ferricyanide in the solution a is 0% to 25%, and the mass fraction of polyvinyl alcohol in the solution formed by dissolving the polyvinyl alcohol in the solution a is 10% to 30%.
According to one aspect of the invention, in step 3, the heating temperature is 60-100 ℃, the heating time is 3-5h, and the standing is normal temperature standing.
According to one aspect of the invention, in step 3, the freezing temperature is-30-10 ℃, and the freezing time is 13-20 hours; the thawing temperature is 20-30 ℃, and the thawing time is 20-30h.
Based on the same inventive concept, the invention also provides the composite gel electrolyte prepared by the preparation method.
Based on the same inventive concept, the invention also provides application of the composite gel electrolyte prepared by the En method in a zinc ion battery.
According to one aspect of the invention, the zinc ion battery comprises a gel electrolyte, a zinc metal negative electrode sheet, and a positive electrode sheet containing an active material; the active material is at least one selected from oxides, polyanions, prussian blue and organic positive electrode materials.
The invention has the beneficial effects that:
(1) The active filler is introduced as an ion conductive inorganic substance, so that the general function of the inert filler is maintained, and the ionic conduction process can be participated in by forming an additional path of zinc ion transport, thereby further improving the ion conductivity, obtaining a high ion migration number, and finally obtaining high specific capacity and stable cycle performance of the zinc ion battery;
(2) The ionic conductivity of the composite gel polymer electrolyte provided by the invention is up to 16.25 multiplied by 10 at room temperature - 3 S·cm -1 Higher than conventional PVA-based hydrogel electrolytes;
(3) The migration number of zinc ions of the composite gel polymer electrolyte provided by the invention is up to 0.62;
(4) The polymer gel electrolyte provided by the invention is applied to a zinc ion battery, and has high specific capacity, stable cycle performance and high coulombic efficiency at room temperature;
(5) The polymer gel electrolyte provided by the invention has the advantages of simple preparation process, simple filler preparation process and environmental friendliness, and can be applied to actual production.
Drawings
FIG. 1 is an XRD pattern of the filler prepared in example 1 of the present invention;
FIG. 2 is an SEM image of the filler prepared in example 1 of the invention;
FIG. 3a is an EIS pattern at room temperature after the composite gel electrolyte of example 1 of the present invention is assembled into a zinc metal-electrolyte-zinc metal battery; FIG. 3b is an EIS pattern at room temperature after the composite gel electrolyte of comparative example 1 of the present invention is assembled into a zinc metal-electrolyte-zinc metal battery;
FIG. 4a shows that the Zn HTO full cell composition of the composite gel electrolyte according to example 1 has a current density of 0.2A g at 25deg.C -1 A charge-discharge curve of the lower front 20 circles; FIG. 4b shows that the Zn HTO full cell composition based on comparative example 1 has a current density of 0.2A g at 25deg.C -1 A charge-discharge curve of the lower front 20 circles; FIG. 4c shows that the Zn HTO full cell composition based on comparative example 2 has a current density of 0.2Ag at 25deg.C -1 A charge-discharge curve of the lower front 20 circles;
fig. 5 is a cycle performance curve of a Zn HTO full cell of the composite gel electrolyte composition according to the present invention based on example 1 and comparative example 2.
Detailed Description
In order that the invention may be more readily understood, the invention will be further described with reference to the following examples. It should be understood that these examples are intended to illustrate the invention and not to limit the scope of the invention, and that the described embodiments are merely some, but not all, of the embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Unless defined otherwise, the terms of art used hereinafter are consistent with the meanings understood by those skilled in the art; unless otherwise indicated, all the materials and reagents referred to herein are commercially available or may be prepared by well-known methods.
Example 1
A method for preparing a gel electrolyte, comprising the steps of: preparation of filler: (1) Respectively dissolving 1-2g of potassium ferricyanide and zinc sulfate in deionized water to form potassium ferricyanide solution and zinc sulfate solution, slowly dripping the zinc sulfate solution into the potassium ferricyanide solution to form precipitated zinc ferricyanide, cleaning, and drying the obtained precipitate; preparation of gel electrolyte: (2) Preparing 5ML zinc trifluoromethane sulfonate solution, adding 15% of the filler obtained in step (1) into the solution, and uniformly dispersing the mixture by ultrasonic waves to obtain solution A; (3) 5% of polyvinyl alcohol was dissolved in the solution A, heated and stirred at 90℃for 4 hours, and left to stand for a suitable period of time to remove air bubbles. Then, after freezing at-18 ℃ for 15 hours, thawing at room temperature to obtain the composite gel electrolyte.
Example 2
This example differs from example 1 in that the polyvinyl alcohol content is 25% and the zinc ferricyanide filler content is 3%. Other parameters and conditions were consistent with example 1.
Example 3
This example differs from example 1 in that the polyvinyl alcohol content is 25% and the zinc ferricyanide filler content is 5%. Other parameters and conditions were consistent with example 1.
Example 3
This example differs from example 1 in that the polyvinyl alcohol content is 20% and the zinc ferricyanide filler content is 5%. Other parameters and conditions were consistent with example 1.
Example 4
This example differs from example 1 in that the polyvinyl alcohol content is 20% and the filler content is 10%. Other parameters and conditions were consistent with example 1.
Example 5
This example differs from example 1 in that the polyvinyl alcohol content is 15% and the zinc ferricyanide filler content is 20%. Other parameters and conditions were consistent with example 1.
Comparative example 1
A method for preparing a gel electrolyte, comprising the steps of: preparation of filler: (1) 1-2g of potassium ferricyanide and ferric trichloride are respectively dissolved in deionized water to form potassium ferricyanide solution and ferric trichloride solution, and the ferric trichloride solution is slowly dripped into the potassium ferricyanide solution to form precipitated ferric ferricyanide. Preparing a gel electrolyte; (2) Preparing 5ML zinc trifluoromethane sulfonate solution, adding 15% of the filler obtained in step (1) into the solution, and uniformly dispersing the mixture by ultrasonic waves to obtain solution A; (3) 15% of polyvinyl alcohol is dissolved in the solution A, heated and stirred for 4 hours at 90 ℃, and the solution is left to stand at room temperature for a period of time to remove bubbles. Then, after freezing at-18 ℃ for 15 hours, thawing at room temperature to obtain the gel electrolyte.
The comparative example differs from example 1 in that the polyvinyl alcohol content is 15% and the filler is iron ferricyanide and the content is 15%. Other parameters and conditions were consistent with example 1.
Comparative example 2
The comparative example differs from example 1 in that the content of polyvinyl alcohol is 15% and the content of zinc ferricyanide filler is 0%. Other parameters and conditions were consistent with example 1.
Performance inspection and result analysis:
as shown in FIG. 1, XRD was performed on the filler zinc ferricyanide prepared in example 1, and it is apparent from FIG. 1 that the XRD pattern of the filler prepared in example 1 is consistent with that of zinc ferricyanide (JCPLS: 38-0688), indicating that the crystallinity and purity of zinc ferricyanide prepared in example 1 are high. The result of scanning electron microscope analysis of the filler zinc iron cyanide prepared in example 1 is shown in fig. 2, and it is clear from fig. 2 that the filler zinc iron cyanide prepared in example 1 is in the form of particles.
The gel electrolytes prepared in examples 1 to 5 and comparative examples 1 to 2 were assembled into a stainless steel sheet-gel electrolyte-stainless steel sheet battery, and ac impedance was tested using an electrochemical workstation, and ion conductivity was calculated using the following equation 1.
sigma=l/RS equation 1
In formula 1, L is the thickness of the gel electrolyte, R is the cell resistance, and S is the area of the stainless steel sheet.
The test results of examples 1-5 and comparative examples 1-2 are shown in Table 1:
table 1:
as shown in table 1, the ionic conductivity of the polyvinyl alcohol gel electrolyte is improved with the increase of the addition amount of the zinc ferricyanide filler, because the active filler can not only provide zinc ions, but also reduce the crystallinity of the polymer and promote the dissociation of zinc salt, thereby constructing a new rapid ion transmission channel. As shown by EIS test, the polymer electrolyte with 15% polyvinyl alcohol and 15% zinc ferricyanide filler in example 1 has the highest ionic conductivity of 16.25S cm -1 。
The gel electrolytes prepared in example 1 and comparative example 1 were assembled into a zinc metal-electrolyte-zinc metal battery, and then subjected to EIS test at room temperature with an amplitude of 10mV, and the impedance R at this time was recorded 0 Then, a polarization voltage of 10mV is continuously applied, and an initial response current I is recorded 0 The polarization time was 2000s, when steady state current (I S ) Then stopping applying voltage, and then performing EIS test and recording impedance R at the moment S . The calculation formula is shown as 2:
in formula 2, I 0 For initially responding to current, R 0 Is the initial impedance, I S Is the steady state current and Rs is the impedance at which the steady state current is reached.
As shown in fig. 3, which shows EIS spectra at room temperature after the zinc metal-electrolyte-zinc metal batteries of example 1 and comparative example 1 are assembled, it is apparent from fig. 3 that the ion migration number of the polyvinyl alcohol gel electrolyte filled with zinc ferricyanide is higher than that of the gel electrolyte filled with iron ferricyanide, indicating that the active filler added with zinc ions further improves ion conductivity, which is favorable for migration of zinc ions.
The zinc ion migration number of the composite gel electrolyte prepared in example 1 was calculated to be 0.62 by equation 2 and fig. 3, and the zinc ion migration number of the composite gel electrolyte prepared in comparative example 1 was calculated to be 0.389.
Examples 1 andthe composite gel electrolytes of comparative examples 1-2 were assembled to be injected with the positive electrode active material H, respectively 2 Ti 3 O 7 ·xH 2 (HTO): binder polyvinylidene fluoride (PVDF): the conductive agent acetylene black comprises the following components in percentage by mass: 1:2, commercial zinc foil as a negative electrode, and glass fiber as a diaphragm, to obtain a Zn HTO full cell of the corresponding comparative example and example with a current density of 0.2A g at 25 ℃ -1 The charge-discharge curve for the first 20 lower turns is shown in fig. 4. As can be seen from fig. 4, the composite gel electrolyte of example 1 provides a specific capacity superior to that of the composite gel electrolytes of comparative examples 1 and 2. The results show that the zinc ferricyanide can provide more zinc ions as an active filler to promote the transmission of the zinc ions, so that the Zn HTO full battery has higher specific capacity. The Zn HTO full cell assembled from the composite gel electrolytes of example 1 and comparative example 2 had a current density of 0.2A g at 25 ℃ -1 The comparison graph of cycle stability and coulombic efficiency is shown in figure 5. As can be seen from fig. 5, the first week of example 1 has a significantly higher coulombic efficiency than comparative example 2 and a higher coulombic efficiency than comparative example 2 in 300 cycles, indicating that the specific capacity and coulombic efficiency can be improved by the introduction of zinc iron cyanide filler.
The foregoing is merely illustrative of the present invention, and the present invention is not limited thereto, and any changes or substitutions easily contemplated by those skilled in the art within the technical scope of the present invention should be included in the scope of the present invention. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.

Claims (10)

1. The preparation method of the composite gel electrolyte of the zinc ion battery is characterized by comprising the following steps of:
step 1: dissolving potassium ferricyanide and sulfate containing metal ions in deionized water to form potassium ferricyanide solution and sulfate containing metal ions, slowly dripping the sulfate containing metal ions into the potassium ferricyanide solution, continuously stirring, reacting for a certain time, filtering, cleaning and drying to obtain ferricyanide;
step 2: dissolving zinc trifluoromethane sulfonate in deionized water to form a solution, filtering to obtain a zinc trifluoromethane sulfonate solution, dispersing ferricyanide in the zinc trifluoromethane sulfonate solution, and uniformly dispersing by ultrasonic waves to obtain a solution A;
step 3: and dissolving polyvinyl alcohol in the solution A, heating and stirring uniformly, standing to remove bubbles, and then freezing and thawing to obtain the composite gel electrolyte.
2. The method of preparing a composite gel electrolyte for a zinc ion battery according to claim 1, wherein in step 1, the ferricyanide comprises one or more of iron ferricyanide, cobalt ferricyanide, nickel ferricyanide, manganese ferricyanide, copper ferricyanide, zinc ferricyanide.
3. The method for preparing a composite gel electrolyte according to claim 1, wherein the concentration of the potassium ferricyanide solution is 0.05-0.2mol/L, and the concentration of the sulfate or chloride solution containing metal ions is 0.1-0.2mol/L; the concentration of the zinc trifluoromethane sulfonate solution is 1-4mol/L.
4. The method for preparing a composite gel electrolyte according to claim 1, wherein in the step 1, the reaction time is 4 to 6 hours; the cleaning is carried out by adopting deionized water; the drying temperature is 60-100 ℃ and the drying time is 12-15h.
5. The method for producing a composite gel electrolyte according to claim 1, wherein in step 3, the mass fraction of ferricyanide in the solution a is 0% to 25%, and the mass fraction of polyvinyl alcohol in the solution formed by dissolving the polyvinyl alcohol in the solution a is 10% to 40%.
6. The method for preparing a composite gel electrolyte according to claim 1, wherein in the step 3, the heating temperature is 60 to 100 ℃ and the heating time is 3 to 5 hours, and the standing is normal temperature standing.
7. The method for preparing a composite gel electrolyte according to claim 1, wherein the freezing temperature is-30 to 10 ℃, and the freezing time is 13 to 20 hours; the thawing temperature is 20-30 ℃, and the thawing time is 20-30h.
8. A composite gel electrolyte obtained by the method for producing a composite gel electrolyte according to any one of claims 1 to 7.
9. Use of a composite gel electrolyte obtained by the method for producing a composite gel electrolyte according to any one of claims 1 to 7 or a composite gel electrolyte according to claim 8 in a zinc ion battery.
10. The use according to claim 9, wherein the zinc ion battery comprises a gel electrolyte, a zinc metal negative electrode sheet and a positive electrode sheet containing an active material; the active material is at least one selected from oxides, polyanions, prussian blue and organic positive electrode materials.
CN202310865436.6A 2023-07-14 2023-07-14 Composite gel electrolyte of zinc ion battery, preparation method and application thereof Pending CN116779993A (en)

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CN202310865436.6A CN116779993A (en) 2023-07-14 2023-07-14 Composite gel electrolyte of zinc ion battery, preparation method and application thereof

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