CN113725392B - Interface modified metal zinc cathode and preparation method thereof - Google Patents
Interface modified metal zinc cathode and preparation method thereof Download PDFInfo
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- CN113725392B CN113725392B CN202111053130.8A CN202111053130A CN113725392B CN 113725392 B CN113725392 B CN 113725392B CN 202111053130 A CN202111053130 A CN 202111053130A CN 113725392 B CN113725392 B CN 113725392B
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- H—ELECTRICITY
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- H—ELECTRICITY
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses an interface modified metal zinc cathode and a preparation method thereof, and aims to solve the technical problems that excessive zinc dendrites are generated on the surface of an electrode of a water-based zinc ion battery and side reactions occur. The surface of the metal zinc negative electrode is coated with a binder @ graphene oxide @ zinc oxide polymer composite film. The preparation method of the interface modified metal zinc cathode comprises the following steps: preparing a metal zinc negative plate; dissolving graphene oxide in a dispersing agent, adding zinc oxide after ultrasonic dispersion, and obtaining a solution A after ultrasonic dispersion again; dissolving a binder in a dispersing agent, stirring to obtain a jelly B, dissolving the jelly B in the solution A, and fully reacting to obtain a solution C; and (3) immersing the metal zinc negative plate into the solution C, taking out and drying to obtain the zinc negative plate. According to the invention, the surface of the zinc electrode sheet is modified, and the PVDF @ graphene oxide @ zinc oxide polymer composite membrane is coated, so that zinc dendrites with a small number are formed after the modified zinc electrode sheet is charged and discharged, and the service life of the battery is prolonged.
Description
Technical Field
The invention relates to the technical field of metal zinc cathodes of water-based zinc ion batteries, in particular to an interface-modified metal zinc cathode and a preparation method thereof.
Background
With the continuous development of society, fossil fuels face the problems of resource shortage, environmental pollution and the like, and people are promoted to continuously seek clean and replaceable novel energy sources. At present, a lithium ion battery is popularized and popularized on a large scale in the market as a new energy electrochemical energy storage device, but in the practical application process, because the metal lithium is insufficient in storage capacity and expensive in price, the organic electrolyte has potential safety hazards of flammability, toxicity and the like, and the development of the lithium battery in the fields of large-scale power grid energy storage systems, electric vehicles and the like is further limited.
Compared with the traditional organic electrolyte, the water-based electrolyte has the advantages of high ionic conductivity, safety, reliability, no toxicity, no harm and the like, so that people turn the research attention to the water-based ion battery. In addition, the metal zinc is unique among a plurality of metal ion battery materials by virtue of the characteristics of high theoretical capacity, high hydrogen evolution overpotential, abundant resources, low price and the like. Therefore, the water-based zinc ion battery is considered as one of the most promising water-based metal ion batteries, and is also a research hotspot in the field of energy storage nowadays.
However, when the metal zinc is used as the negative electrode of the battery, zinc dendrite is generated on the surface of the electrode in the charging and discharging processes, thereby reducing the coulomb efficiency of the battery and the utilization rate of the metal zinc, and the battery is likely to be short-circuited due to the piercing of the diaphragm caused by excessive dendrite generation. In addition, the surface of the electrode can generate hydrogen evolution reaction to cause electrode corrosion passivation, and the generation of hydrogen in a closed space can cause the volume expansion and even explosion of the battery, thereby seriously influencing the cycle stability and safety of the battery.
Disclosure of Invention
The invention aims to solve the technical problem of providing an interface modified metal zinc cathode and a preparation method thereof, and aims to solve the technical problems that excessive zinc dendrites are generated on the surface of an electrode of a water-based zinc ion battery and side reactions occur.
In order to solve the technical problems, the invention adopts the following technical scheme:
an interface modified metal zinc cathode is designed, and a binder @ graphene oxide @ zinc oxide polymer composite film is coated on the surface of the metal zinc cathode.
The oxidized graphene is different from the traditional graphene, after oxidation, the characteristics of the oxidized graphene are more active than those of the graphene due to the increase of oxygen-containing functional groups, the internal structure of the oxidized graphene exceeds the scale of the traditional chemical material, and the oxidized graphene serving as a soft material in a non-traditional form has the characteristics of colloid, a thin film, amphoteric molecules and the like. In addition, as an important derivative of graphene-based materials, graphene oxide is used as a precursor and a support carrier for synthesizing the graphene-based composite material, and is easy to functionalize, high in controllability and low in conductivity. In the process of compounding with metal, metal oxide, high molecular polymer and other materials, the material can be dispersed and attached effectively in large specific surface area to avoid agglomeration.
Preferably, the binder is PVDF, and the zinc oxide is nano zinc oxide.
Polyvinylidene Fluoride (PVDF) is mainly a vinylidene Fluoride homopolymer or a copolymer of vinylidene Fluoride and other small amounts of fluorine-containing vinyl monomers, has excellent characteristics such as strong oxidation resistance, easy dispersion, chemical corrosion resistance, high-temperature color change resistance, lyophilic property and the like, and is generally used as a binder in the field of batteries.
The nano zinc oxide presents spherical or white hexagonal system crystalline particles, and has extremely high chemical activity and excellent catalytic performance. The nano-grade zinc oxide has many chemical properties different from those of the traditional zinc oxide, and has the advantages of high chemical activity, large specific surface area, good hydrophilicity and the like.
Preferably, the binder @ graphene oxide @ zinc oxide polymer composite film is prepared from the following raw materials in parts by weight: 5-10 parts of adhesive, 1-3 parts of graphene oxide, 1-2 parts of zinc oxide and 1100-1200 parts of dispersant.
Preferably, the dispersant is NMP.
Preferably, the thickness of the binder @ graphene oxide @ zinc oxide polymer composite film is 10-15 microns.
The preparation method of the interface modified metal zinc cathode comprises the following steps:
(1) Preparing a metal zinc negative plate;
(2) Dissolving 1-3 parts of graphene oxide in 1000 parts of dispersing agent, adding 1-2 parts of zinc oxide after ultrasonic dispersion, and obtaining a dark brown solution A after ultrasonic dispersion again;
(3) Dissolving 50 parts of binder in 1000 parts of dispersant, and fully stirring to obtain a transparent jelly B;
(4) Dissolving 100-200 parts of the jelly B in the solution A, and after full reaction, obtaining a uniform bubble-free transparent solution C;
(5) And (3) protecting one surface of the metal zinc negative plate by using an adhesive tape, completely immersing the other surface of the metal zinc negative plate into the solution C, taking out the metal zinc negative plate and drying the metal zinc negative plate to obtain the zinc negative plate.
Preferably, the binder is PVDF, the zinc oxide is nano zinc oxide, and the dispersant is NMP.
Preferably, in the step (1), the metallic zinc negative electrode sheet is prepared by the following method: cutting a round zinc pole piece by using a zinc foil, adding ethanol to completely immerse the zinc pole piece, ultrasonically cleaning, and drying to obtain the zinc-plated electrode.
Preferably, in the step (2), the graphene oxide is 3 parts, and the nano zinc oxide is 2 parts.
Preferably, in the step (5), the drying step is: drying in an electric heating forced air drying oven for 10min, taking out, and vacuum drying at 100 deg.C for 24 hr.
Compared with the prior art, the invention has the beneficial technical effects that:
1. according to the invention, the surface of the zinc electrode sheet is modified, and the PVDF @ graphene oxide @ zinc oxide polymer composite membrane is coated, so that zinc dendrites with less number are formed on the modified zinc electrode sheet after charging and discharging, the result of battery short circuit caused by membrane piercing is avoided, the coulomb efficiency and the cycle performance are improved, and the service life of the battery is prolonged.
2. According to the invention, graphene oxide is dispersed and dissolved in NMP (N-methyl pyrrolidone), PVDF and nano zinc oxide particles are added, the mixture is coated on the surface of metal zinc and dried to form a coating, the side reaction of metal zinc and electrolyte is inhibited by utilizing the characteristics of close adhesion of a composite membrane, low conductivity of graphene oxide, hydrophilicity of nano zinc oxide and the like, zinc ions are guided to be uniformly deposited, so that the generation of zinc dendrites is reduced, and the cycle discharge life of the water system zinc ion battery is prolonged.
Drawings
FIG. 1 is a scanning electron microscope picture of the surface of metallic zinc after modification of PVDF @ graphene oxide @ zinc oxide polymer in test example 1;
FIG. 2 is a schematic diagram of the dimensions and thicknesses of a PVDF @ graphene oxide @ zinc oxide polymer composite membrane in test example 1;
FIG. 3 shows that the ratio of PVDF @ graphene oxide @ zinc oxide polymer modified zinc/zinc symmetric battery to unmodified pure zinc/zinc symmetric battery in test example 1 is 0.5A · g -1 Long cycle performance at current density is plotted;
FIG. 4 is a graph comparing the long cycle performance of PVDF @ graphene oxide @ zinc oxide polymer modified zinc/manganese dioxide full cells and unmodified pure zinc/manganese dioxide full cells under rate conditions in test example 1;
FIG. 5 is a scanning electron microscope image of the surface of a zinc plate after cycling of a PVDF @ graphene oxide @ zinc oxide polymer modified zinc/zinc symmetric cell in test example 1;
FIG. 6 is a scanning electron microscope image of the surface of a zinc plate after cycling of the pure zinc/zinc symmetric cell in test example 1.
Detailed Description
The following examples are intended to illustrate the present invention in detail and should not be construed as limiting the scope of the present invention in any way.
The instruments and devices referred to in the following examples are conventional instruments and devices unless otherwise specified; the related reagents and raw materials are all conventional reagents and raw materials sold in markets if the reagents and the raw materials are not particularly described; the related detection, test and preparation methods are all conventional methods if no special description is provided.
Example 1: the utility model provides an interface modification's metallic zinc negative pole, metallic zinc negative pole are diameter 12mm, the disk-shaped electrode slice of thickness 2mm, and the surface coating in metallic zinc negative pole has PVDF @ graphite oxide @ zinc oxide polymer composite membrane, and this polymer composite membrane comprises following preparation raw materials: 50mg of PVDF, 10mg of graphene oxide, 10mg of nano zinc oxide and 11 mL of NMP (N-methylpyrrolidone).
Example 2: the utility model provides an interface modification's metallic zinc negative pole, metallic zinc negative pole are diameter 12mm, the disk-shaped electrode slice of thickness 2mm, and the surface coating in metallic zinc negative pole has PVDF @ graphite oxide @ zinc oxide polymer composite membrane, and this polymer composite membrane comprises following preparation raw materials: 100mg of PVDF, 30 mg of graphene oxide, 20mg of nano zinc oxide and 12 mL of NMP (N-methylpyrrolidone). The thickness of PVDF @ graphene oxide @ zinc oxide polymer composite membrane is 10.83 microns.
Example 3: a preparation method of an interface modified metal zinc cathode comprises the following steps:
(1) Firstly, cutting a zinc foil into a plurality of disk-shaped electrode plates with the diameter of 12mm and the thickness of 2mm by using a button cell slicer, putting the disk-shaped electrode plates into a glass bottle, adding a proper amount of ethanol to ensure that the zinc electrode plates can be completely immersed in the disk-shaped electrode plates, putting the disk-shaped electrode plates into an ultrasonic cleaner for cleaning for 2 minutes, then putting the disk-shaped electrode plates into an electrothermal blowing drying box for drying, taking out the disk-shaped electrode plates after drying, and sticking an adhesive tape on one side of each electrode plate for protection for later use.
(2) 10mg of graphene oxide was weighed into a glass bottle using an analytical balance, 10 mL of NMP (N-methylpyrrolidone) was added using a dropper, graphene oxide was sufficiently dissolved in NMP by ultrasonic dispersion for half an hour, then 10mg of nano zinc oxide particles were further added by weighing and ultrasonic treatment again for half an hour, and a dark brown solution, called solution A, was obtained.
(3) 500 mg of PVDF (polyvinylidene fluoride) was weighed into a glass bottle, dissolved by adding 10 mL of NMP (N-methylpyrrolidone) to a dropper, and sufficiently stirred for 4 hours with a magnetic stirrer to form a transparent gum called solution B.
(4) Adding 1g of the solution B into the solution A, and fully stirring for 2 hours to ensure that the solution A and the solution B are mixed and then fully react to form a uniform bubble-free transparent solution, namely solution C.
(5) And clamping the electrode slice by using a pair of tweezers, dipping the electrode slice into the solution C, taking out the electrode slice after observing that the surface of one side which is not adhered with the adhesive tape is completely covered with liquid, and drying the electrode slice in an electric heating blowing drying oven for ten minutes. Taking out again and putting into a vacuum drying oven, setting the temperature to be 100 ℃ and the time to be 24 hours.
The surface of the zinc plate is observed to be covered with a dark brown film, which indicates that the electrode surface modification is finished.
Example 4: a preparation method of an interface modified metal zinc cathode comprises the following steps:
(1) Firstly, cutting a zinc foil into a plurality of disk-shaped electrode plates with the diameter of 12mm and the thickness of 2mm by using a button cell slicer, putting the disk-shaped electrode plates into a glass bottle, adding a proper amount of ethanol to ensure that the zinc electrode plates can be completely immersed in the disk-shaped electrode plates, putting the disk-shaped electrode plates into an ultrasonic cleaner for cleaning for 2 minutes, then putting the disk-shaped electrode plates into an electrothermal blowing drying box for drying, taking out the disk-shaped electrode plates after drying is finished, and sticking an adhesive tape on one side of each electrode plate for protection for later use.
(2) 30 mg of graphene oxide is weighed by an analytical balance into a glass bottle, 10 mL of NMP (N-methylpyrrolidone) is added by a dropper, the graphene oxide is fully dissolved in the NMP by ultrasonic dispersion for half an hour, and then 20mg of nano zinc oxide particles are weighed and added again by ultrasonic dispersion for half an hour to obtain a dark brown solution called solution A.
(3) 500 mg of PVDF (polyvinylidene fluoride) was weighed into a glass bottle, dissolved by adding 10 mL of NMP (N-methylpyrrolidone) to a dropper, and sufficiently stirred for 4 hours with a magnetic stirrer to form a transparent gum, which was called solution B.
(4) Adding 2 g of the solution B into the solution A, and fully stirring for 2 hours to ensure that the solution A and the solution B are mixed and then fully react to form a uniform bubble-free transparent solution, namely solution C.
(5) And clamping the electrode slice by using a pair of tweezers, dipping the electrode slice into the solution C, taking out the electrode slice after observing that the surface of one side which is not adhered with the adhesive tape is completely covered with liquid, and drying the electrode slice in an electric heating blowing drying oven for ten minutes. Taking out again and putting into a vacuum drying oven, setting the temperature to be 100 ℃ and the time to be 24 hours.
The surface of the zinc plate is observed to be covered with a dark brown film, which indicates that the electrode surface is modified completely.
Test example 1: the modified zinc cathode of the embodiment 4 is subjected to battery preparation and electrochemical performance test:
the prepared electrode plates are assembled into a CP2032 symmetric button cell, and compared with a CP2032 symmetric button cell assembled by pure zinc electrode plates, a Wuhan blue electricity CT 2001A system is used at 0.5mA cm -2 Constant current charge and discharge test under current density. In addition, the prepared modified zinc anode and unmodified pure zinc anode flakes are respectively mixed with MnO 2 And (4) assembling the positive electrode into a full battery, and performing performance test under the condition of multiplying power charge and discharge. Electrolyte is 2mol/L ZnSO 4 And the diaphragm is glass fiber filter paper.
As shown in fig. 1, the microstructure of the surface-modified zinc negative electrode obtained in example 4 is shown.
As shown in fig. 2, is the modified composite film thickness dimension prepared in example 4.
As shown in fig. 3, compared with the unmodified zinc/zinc symmetric battery, the modified zinc/zinc symmetric battery obtained in example 4 has better cycle performance, lower overpotential, and significantly improved charge-discharge cycle life.
As shown in fig. 4, the modified zinc/manganese dioxide full cell obtained for example 4 has more stable cycle performance and longer life span than the unmodified zinc/manganese dioxide full cell.
As shown in figure 5, the modified symmetrical battery cathode is taken out to observe the surface appearance of the modified symmetrical battery cathode, and the surface zinc dendrite number is found to be few, and a 'flat-lying' growth mode is presented, so that the short circuit of the battery caused by piercing a diaphragm is avoided, the cycle life of the battery is greatly prolonged, and the safety is improved.
As shown in fig. 6, the cathode of the short-circuited unmodified symmetric battery is taken out and observed for the microscopic morphology, and it is found that zinc dendrites which are dense and vertically grown are generated on the surface, which may cause the short circuit due to the piercing of the separator, and seriously affect the service life of the battery.
Test example 2: the modified zinc cathode of the embodiment 3 is subjected to battery preparation and electrochemical performance test:
the prepared electrode plates are assembled into a CP2032 symmetric button cell, and compared with a CP2032 symmetric button cell assembled by pure zinc electrode plates, a Wuhan blue electricity CT 2001A system is used at 0.5mA cm -2 And carrying out constant current charge and discharge test under the current density. In addition, the prepared modified zinc anode and unmodified pure zinc anode flakes are respectively mixed with MnO 2 And (4) assembling the positive electrode into a full battery, and performing performance test under the condition of multiplying power charge and discharge. The electrolyte is 2mol/L ZnSO 4 The diaphragm isGlass fiber filter paper.
The prepared zinc ion battery has better cycle performance and stronger stability, the zinc dendrite is obviously inhibited, and the service life of the water system zinc ion battery is greatly prolonged.
The invention is explained in detail above with reference to the drawings and the embodiments; however, those skilled in the art will understand that various changes and modifications to the specific parameters of the above embodiments, or equivalent substitutions of related parts and structures, may be made without departing from the spirit of the present invention, thereby forming various specific embodiments, which are all common variations of the present invention and are not described in detail.
Claims (5)
1. The interface-modified metal zinc cathode is characterized in that a binder @ graphene oxide @ zinc oxide polymer composite film is coated on the surface of the metal zinc cathode; the binder is PVDF, and the zinc oxide is nano zinc oxide; the preparation method of the metal zinc cathode comprises the following steps:
(1) Preparing a metal zinc negative plate;
(2) Dissolving 1-3 parts by weight of graphene oxide in 1000 parts by weight of dispersant, adding 1-2 parts by weight of zinc oxide after ultrasonic dispersion, and obtaining a dark brown solution A after ultrasonic dispersion again; the dispersing agent is NMP;
(3) Dissolving 50 parts of binder in 1000 parts of dispersant, and fully stirring to obtain a transparent jelly B;
(4) Dissolving 100-200 parts of the jelly B in the solution A, and after full reaction, obtaining a uniform bubble-free transparent solution C;
(5) And (3) protecting one surface of the metal zinc negative plate by using an adhesive tape, completely immersing the other surface of the metal zinc negative plate into the solution C, taking out the metal zinc negative plate and drying the metal zinc negative plate to obtain the zinc-containing negative plate.
2. The interface-modified metal zinc anode of claim 1, wherein the binder @ graphene oxide @ zinc oxide polymer composite film has a thickness of 10 to 15 μm.
3. The interface-modified metallic zinc negative electrode according to claim 1, wherein in the step (1), the metallic zinc negative electrode sheet is prepared by the following method: cutting a round zinc pole piece by using a zinc foil, adding ethanol to completely immerse the zinc pole piece, ultrasonically cleaning, and drying to obtain the zinc-plated electrode.
4. The interface modified metallic zinc anode of claim 1, wherein in step (2), the amount of graphene oxide is 3 parts and the amount of nano zinc oxide is 2 parts.
5. The interface-modified metallic zinc anode of claim 1, wherein in the step (5), the drying step is: drying in an electric heating forced air drying oven for 10min, taking out, and drying in a vacuum drying oven at 100 deg.C for 24 hr.
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