CN113745675B - Zinc electrode protected by negative framework hydrogel as modification layer and preparation method thereof - Google Patents

Zinc electrode protected by negative framework hydrogel as modification layer and preparation method thereof Download PDF

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CN113745675B
CN113745675B CN202111044954.9A CN202111044954A CN113745675B CN 113745675 B CN113745675 B CN 113745675B CN 202111044954 A CN202111044954 A CN 202111044954A CN 113745675 B CN113745675 B CN 113745675B
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zinc
hydrogel
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layer
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CN113745675A (en
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范红金
杨培华
杨金霖
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Sino Singapore International Joint Research Institute
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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
    • H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
    • H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
    • 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
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0402—Methods of deposition of the material
    • H01M4/0416—Methods of deposition of the material involving impregnation with a solution, dispersion, paste or dry powder
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/04—Processes of manufacture in general
    • H01M4/0471—Processes of manufacture in general involving thermal treatment, e.g. firing, sintering, backing particulate active material, thermal decomposition, pyrolysis
    • 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
    • Y02E60/10—Energy storage using batteries

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Abstract

The invention discloses a zinc electrode protected by negative framework hydrogel as a modification layer and a preparation method thereof. The zinc electrode consists of a zinc battery cathode, a connecting layer and negative framework hydrogel. The connecting layer effectively builds strong binding energy of hydrogel and zinc metal, improves free energy of an interface, further inhibits vertical growth of zinc deposition, and promotes lateral growth to avoid dendrite generation; meanwhile, the connecting layer always controls low-activity water molecules on the near surface of the negative electrode, prevents the peeling of the hydrogel layer, and improves the overall stability of the electrode surface structure. The negative skeleton hydrogel thin layer has strong zinc-philic characteristic, and is favorable for embedding zinc ions. Compared with the traditional zinc-philic oxide solid electrolyte membrane, the hydrogel modified layer has higher ionic conductivity, compact surface and few microcracks, and effectively limits hydrogen evolution reaction. The invention has the characteristics of low cost of materials, simple structure, reusability and the like, and can be used in the fields of stability and safety of batteries.

Description

Zinc electrode protected by negative framework hydrogel as modification layer and preparation method thereof
Technical Field
The invention relates to the technical field of batteries, in particular to a zinc electrode protected by using negative framework hydrogel as a modification layer and a preparation method thereof.
Background
High safety and high energy density aqueous zinc batteries are considered to be one of the most promising energy storage technologies for next generation electronics. In recent years, aqueous zinc batteries have been in a vigorous development due to the development of high-performance cathode materials and electrolytes. However, the zinc-based battery has short cycle life and low coulombic efficiency due to the severe zinc dendrite growth caused by uneven zinc dissolution and deposition in the battery cycle process, which severely restricts the industrial application of the water-based zinc battery.
In recent years, researchers have made great efforts to solve the above problems, and various methods have been proposed to inhibit dendrite growth. Wherein an additional layer with a lower metal affinity at the artificial solid electrolyte interface may act as a protective layer to limit dendrite growth. The various modification layers and protection layers of the modified zinc cathode are: metal compound (ZnO, tiO) 2 ZnS, etc.), polymers, metal organic framework compounds, etc. Chinese patent CN113097496a discloses a method for preparing a zinc negative electrode with a composite nanofiber protective layer, wherein the three-dimensional porous hollow structure of the composite nanofiber protective layer has a larger specific surface area, and can reduce the current density near the electrode, thereby slowing down dendrite growth. Chinese patent CN113005435a discloses a preparation method of zinc metal protective layer material, in which metal zinc is placed in metal ion solution to perform metal substitution reaction, so as to provide more active sites, adjust electric field distribution on the surface of electrode, inhibit dendrite growth, and endow the zinc negative electrode with low nucleation overpotential, low polarization voltage, high cycle stability and coulombic efficiency.
At present, most methods have the problems of complicated operation, harsh conditions, high cost and the like, and meanwhile, the conductivity of the protective layer self causes slow electrochemical dynamics so as to influence the zinc storage performance. Therefore, obtaining a zinc anode with high stability is a key technical problem to be solved in the application field at present.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a zinc electrode protected by using negative framework hydrogel as a modification layer and a preparation method thereof. The negative skeleton hydrogel can uniformly grow on the surface of a zinc electrode and has the characteristics of simple structure, safety, stability and the like.
The first object of the present invention can be achieved by adopting the following technical scheme:
a zinc electrode protected by negative skeleton hydrogel as a modification layer, wherein the zinc electrode sequentially comprises a zinc battery cathode, a connecting layer and the negative skeleton hydrogel from inside to outside;
wherein the negative skeleton hydrogel is hydrophilic porous hydrogel with negative skeleton charges;
the negative skeleton hydrogel is a thin layer with a zinc-philic characteristic, the thickness of the thin layer is 50 micrometers to 1 millimeter, and the zinc ion adsorption energy of the thin layer is greater than 1.2eV, so that the insertion of zinc ions is facilitated. Compared with the traditional zinc-philic oxide solid electrolyte membrane, the hydrogel modified layer has higher ionic conductivity, compact surface and few microcracks, and effectively limits hydrogen evolution reaction.
The connecting layer effectively builds strong binding energy of hydrogel and zinc sheet metal, improves free energy of an interface, further inhibits vertical growth of zinc deposition, and promotes lateral growth to avoid dendrite generation; meanwhile, the connecting layer always controls low-activity water molecules on the near surface of the negative electrode, prevents the peeling of the hydrogel layer, and improves the overall stability of the electrode surface structure.
According to the scheme, the connecting layer is a silane coupling agent such as 3- (methacryloyloxy) propyl trimethoxy silane; the coupling agent can enable the zinc electrode to be tightly and firmly connected with the subsequent hydrogel.
According to the scheme, the negative framework hydrogel is a framework negatively charged polymer such as polyacrylamide/acrylic acid-2-acrylamide-2-methylpropanesulfonic acid hydrogel, poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonate) or perfluorinated sulfonic acid hydrogel; the negative framework is beneficial to enhancing the adsorption of zinc ions in the electrolyte.
According to the scheme, the negative electrode of the zinc battery is a zinc sheet or a zinc foil.
The other object of the invention can be achieved by adopting the following technical scheme:
a preparation method of a zinc electrode protected by negative framework hydrogel as a modification layer comprises the following steps:
s1, cleaning a zinc battery cathode in oxygen plasma;
s2, soaking the negative electrode of the zinc battery in a silane coupling agent for 2-4 hours, growing a negative skeleton hydrogel thin layer with a zinc-philic characteristic on the negative electrode of the zinc battery, washing with ethanol and deionized water, and drying for later use;
wherein the negative skeleton hydrogel thin layer is used as an electrode protection layer.
The preparation process of the silane coupling agent is as follows:
3g of 3- (methacryloyloxy) propyltrimethoxysilane and 22. Mu.l of glacial acetic acid were added in succession to 150mL of water and stirred uniformly on a magnetic stirrer.
S3, placing the negative framework hydrogel into a mould filled with electrolyte solution for soaking for 2-4 hours;
s4, placing the die in a drying box, introducing nitrogen for 2-4 minutes, and curing for 3-5 hours by using an ultraviolet lamp to obtain the zinc electrode protected by using the negative framework hydrogel as the modification layer.
According to the scheme, the electrolyte solution is a zinc salt solution, and the zinc salt solution is one of a zinc chloride solution, a zinc acetate solution, a zinc triflate solution and a zinc sulfate solution.
According to the scheme, the concentration of the electrolyte solution is 1-6mol/L.
Compared with the prior art, the invention has the following advantages and effects:
1. the zinc battery cathode disclosed by the invention comprises a zinc sheet, a link layer and negative framework hydrogel, promotes zinc deposition to transversely grow, avoids dendrite formation, effectively limits hydrogen evolution reaction, and has the characteristics of simple structure, recycling, and the like.
2. Compared with the traditional zinc-philic oxide solid electrolyte membrane, the hydrogel modified layer has higher ionic conductivity, compact surface and few microcracks, and is beneficial to the intercalation of zinc ions, thereby effectively limiting hydrogen evolution reaction.
3. The preparation method of the zinc battery cathode disclosed by the invention has the advantages of low-cost and easily available raw materials, simple preparation process, good safety and easiness in industrialization.
Drawings
FIG. 1 is a schematic diagram of a zinc electrode protected by a negative skeleton hydrogel as a modification layer according to an embodiment of the present invention;
FIG. 2 is an area capacity in an embodiment of the invention1mAh cm – 2 Is 1mA cm – 2 A simulation schematic of zinc deposition and stripping at current density;
FIG. 3 is a graph showing the area capacity of 5mAh cm in an embodiment of the invention – 2 Is 10mA cm – 2 Schematic of zinc deposition and stripping simulation at current density.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the embodiments of the present invention more apparent, the technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments of the present 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.
Example 1
The embodiment provides a zinc electrode protected by negative framework hydrogel as a modification layer, wherein the zinc electrode sequentially comprises a zinc battery cathode, a connecting layer and the negative framework hydrogel from inside to outside.
Wherein the negative electrode of the zinc battery is a zinc sheet.
The hydrophilic porous hydrogel is polyacrylamide/acrylic acid-2-acrylamide-2-methylpropanesulfonic acid porous hydrogel (PAAm-) containing zinc chloride solution.
The connecting layer is 3- (methacryloxy) propyl trimethoxy silane (MPS).
Example two
The embodiment provides a preparation method of a zinc electrode protected by negative framework hydrogel serving as a modification layer, which comprises the following specific steps:
and T1, cleaning the negative electrode of the zinc battery in oxygen plasma, and treating the negative electrode in the oxygen plasma for 20 minutes.
T2, 3g of 3- (methacryloyloxy) propyltrimethoxysilane and 22. Mu.l of glacial acetic acid were added in succession to 150mL of water and stirred uniformly on a magnetic stirrer.
And T3, soaking the cathode of the zinc battery cleaned in the step T1 in the solution obtained in the step S2 for 3 hours, washing with ethanol and deionized water, and drying for later use.
T4, 8.53g of acrylamide, 24.87g of acrylic acid-2-acrylamide-2-methylpropanesulfonic acid, 0.0092g of N, N '-methylenebisacrylamide, 0.027g of 2-hydroxy-4' - (2-hydroxyethoxy) -2-methylpropaneketone were added sequentially to 60mL of deionized water. Stirring uniformly on a magnetic stirrer.
T5, pouring the solution obtained in the step T4 into a mould with the thickness of 20 multiplied by 0.1mm, putting the negative electrode of the zinc battery obtained in the step S3, putting the mould into a drying box, introducing nitrogen for 2 minutes, and using an ultraviolet lamp (365 nm, 4mW cm) -2 ) Curing for 4 hours to obtain the hydrogel-modified zinc electrode.
And T6, taking out the prepared zinc electrode, and preparing a wafer electrode with the diameter of 12 mm for standby (marked as Zn-MPS-PAAm-).
T7, handle 2M ZnSO 4 50 microliters of each electrolyte solution was dropped on the zinc electrode prepared in the two steps S6, and a button symmetric cell was assembled using a glass fiber separator. Zinc deposition and stripping tests were performed on a newware battery tester using constant current mode.
FIG. 2 shows an area capacity of 1mAh cm – 2 Is 1mA cm – 2 Zinc deposition and stripping at current density.
FIG. 3 shows an area capacity of 5mAh cm – 2 Is 10mA cm – 2 Zinc deposition and stripping at current density.
Area capacity 1mAh cm – 2 And 5mAh cm – 2 Respectively at a current density of 1mA cm – 2 And 10mA cm – 2 The results of the underlying zinc deposition and stripping show that the electrode without the modified hydrogel will short circuit within 100 hours due to zinc dendrite growth piercing the membrane; the modified zinc electrode exhibits excellent stability and can be subjected to zinc deposition and stripping for a long period of time.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.

Claims (4)

1. The zinc electrode is characterized by sequentially comprising a zinc battery cathode, a connecting layer and negative framework hydrogel from inside to outside;
wherein the negative skeleton hydrogel is hydrophilic porous hydrogel with negative skeleton charges;
the negative skeleton hydrogel is a thin layer with a zinc-philic characteristic, the thickness of the thin layer is 50 micrometers to 1 millimeter, and the zinc ion adsorption energy of the thin layer is greater than 1.2eV;
the connecting layer is used for constructing the strong binding energy of the negative framework hydrogel and the negative electrode of the zinc battery, improving the free energy of an interface, further inhibiting the vertical growth of zinc deposition and promoting the transverse growth of zinc deposition; meanwhile, the connecting layer always controls low-activity water molecules on the near surface of the negative electrode, so that the peeling of the hydrogel layer is prevented;
the negative framework hydrogel is polyacrylamide/acrylic acid-2-acrylamide-2-methylpropanesulfonic acid hydrogel; the connecting layer is a silane coupling agent and adopts 3- (methacryloyloxy) propyl trimethoxy silane; the negative electrode of the zinc battery is a zinc sheet or a zinc foil.
2. The method for preparing a zinc electrode protected by negative skeleton hydrogel as a finishing layer according to claim 1, comprising the steps of:
t1, cleaning a zinc battery cathode in oxygen plasma, and treating the zinc battery cathode in the oxygen plasma for 20 minutes;
t2, adding 3g of 3- (methacryloyloxy) propyl trimethoxysilane and 22 microliters of glacial acetic acid in 150mL of water in sequence, and uniformly stirring on a magnetic stirrer;
t3, soaking the cathode of the zinc battery cleaned in the step T1 in the solution obtained in the step S2 for 3 hours, washing with ethanol and deionized water, and drying for later use;
t4, 8.53g of acrylamide, 24.87g of acrylic acid-2-acrylamide-2-methylpropanesulfonic acid, 0.0092g of N, N '-methylenebisacrylamide and 0.027g of 2-hydroxy-4' - (2-hydroxyethoxy) -2-methylpropaneketone are sequentially added into 60mL of deionized water, and the mixture is uniformly stirred on a magnetic stirrer;
t5, pouring the solution obtained in the step T4 into a mould with the thickness of 20 multiplied by 0.1mm, putting the negative electrode of the zinc battery obtained in the step S3, putting the mould into a drying box, introducing nitrogen for 2 minutes, and using an ultraviolet lamp (365 nm, -4 mWcm) -2 ) Solidifying for 4 hours to obtain a hydrogel modified zinc electrode;
t6, taking out the prepared zinc electrode, and preparing a wafer electrode with the diameter of 12 mm for standby (marked as Zn-MPS-PAAm-);
t7, handle 2MZnSO 4 50 microliters of each electrolyte solution was dropped on the two zinc electrodes prepared in step S6, a button symmetric cell was assembled using a glass fiber membrane, and zinc deposition and stripping tests were performed on a newware cell tester using a constant current mode.
3. The method for preparing the zinc electrode protected by the negative skeleton hydrogel as a modification layer according to claim 2, wherein the electrolyte solution is a zinc salt solution, and the zinc salt solution is one of a zinc chloride solution, a zinc acetate solution, a zinc triflate solution and a zinc sulfate solution.
4. The method for producing a zinc electrode protected by a negative skeletal hydrogel as a finishing layer according to claim 2, wherein the concentration of the electrolyte solution is 1-6mol/L.
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CN114976055B (en) * 2022-06-14 2023-09-29 浙江大学 In-situ preparation method of silanol film for zinc-based flow battery
CN116387467A (en) * 2023-06-05 2023-07-04 武汉理工大学三亚科教创新园 Organic-inorganic interface as zinc negative electrode protective layer, zinc negative electrode, preparation method and battery

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