CN111769276A - Water-containing leaf-shaped lamellar structure nano material, preparation method thereof and lithium ion energy storage application - Google Patents
Water-containing leaf-shaped lamellar structure nano material, preparation method thereof and lithium ion energy storage application Download PDFInfo
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- CN111769276A CN111769276A CN202010483566.XA CN202010483566A CN111769276A CN 111769276 A CN111769276 A CN 111769276A CN 202010483566 A CN202010483566 A CN 202010483566A CN 111769276 A CN111769276 A CN 111769276A
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- H—ELECTRICITY
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- H—ELECTRICITY
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- 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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
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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
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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 belongs to the technical field of chemical materials, and particularly relates to a water-containing leaf-shaped lamellar structure nanocrystal material, a preparation method thereof and lithium ion energy storage application. The method comprises the following steps: the water-containing type lamellar structure nanosheet material can be prepared by a simple one-step solvothermal method, and the crystal powder is obtained by washing and drying. The obtained leaf-shaped lamellar crystal has length of 2-5 μm, thickness of 10-20nm, and chemical formula of CoSeO3·H2And O. The invention has simple and convenient process and high repeatability, and the lithium ion battery assembled by taking the leaf-shaped lamellar crystal prepared by the invention as the cathode electrochemical active material has higher specific capacity and high rate performance. In sodium ion batteries, lithium ion batteries, zinc ion batteries and super-electricityThe method has great application prospect in the fields of containers and the like.
Description
Technical Field
The invention belongs to the technical field of chemical material synthesis, and particularly relates to a water-containing leaf-shaped layered structure nanocrystal material, a preparation method thereof, and application in a rechargeable lithium ion battery.
Background
As the speed of social development has accelerated, the demand and dependence of people on batteries has increased. Batteries are closely related to the life of people, are widely used in various small portable electronic devices, and become a central link in large-scale devices such as electric vehicles and clean power storage devices along with the remarkable power shortage and environmental pollution problems. Among the numerous battery systems, lithium ion batteries are the key components for the transition from internal combustion engines to electrically driven vehicles, and rechargeable lithium ion batteries with excellent performance still face great challenges. The application of the graphite material which is traditionally used as the negative electrode material is greatly limited due to the limited theoretical capacity, and the synthesis of the high-capacity negative electrode material is the best way for realizing the power conversion. Over the past few decades, various types of negative electrode materials, including intercalated graphene, alloyed silicon, and converted metal oxygen/sulfur/selenium/nitride have been extensively studied and developed. The storage capacity of lithium ion batteries is thus greatly increased. However, none of these materials simultaneously exhibits satisfactory high-rate energy and long-cycle stability, and cannot meet the material requirements of high-power batteries.
The poor lithium ion cycling performance is mainly attributed to the significant volume change and cyclic electrochemical stress of the electrode during lithiation and delithiation during charge and discharge. Of which elemental silicon is considered one of the most promising high energy anode materials because of its ultra-high theoretical capacity. But the material generates large volume change and obvious cathode polarization phenomenon during the process of lithium ion insertion and extraction, thereby leading to rapid capacity decay and very low power density. This year. Researches on adding multi-grain boundary nano materials into various carbon-based materials and shortening lithium ion diffusion paths are considered to be very effective solutions for solving fission problems caused by deformation and improving cycle stability. However, these complex designs often correspond to complex manufacturing steps, thereby resulting in high production costs, further preventing their widespread use and industrial production. Therefore, it is very urgent and necessary to design a simple and low-cost cathode material with high performance.
Good rate performance of lithium ion batteries has been found in studies of two-dimensional double metal hydroxides and metal oxides/sulfides, and from the characteristics of these materials we conclude that a high rate performance lithium ion anode accompanied by long cycle stability can be achieved essentially by the structural design of the materials: the most common of them is the tunable two-dimensional structure, and the appropriate interlayer spacing between the two-dimensional nanosheets facilitates the storage of a large amount of lithium ions and the rapid transfer of lithium ions between the electrolyte and the electrode. And simultaneously, the volume change in the charge and discharge process can be reduced to the maximum extent. However, it remains a challenge to obtain high performance lithium ion anode materials because most inorganic compounds are not layered structure materials or spontaneously form methods that design reaction methods and conditions. Since water materials have been a contraindication for lithium ion battery materials for a long time, water-containing materials have been rarely studied as lithium ion battery materials. Researchers at North Carolina State University (NCSU) published a paper entitled "transition phenomena from batteries to pseudocapacitors in tungsten oxide batteries via structured water" and found that the energy storage rate of layered transition metal oxides could be improved by the addition of structured water. The basic principle of this technology is: the battery with unit volume can store more energy, ions can diffuse in the energy storage material more quickly, and meanwhile, the charge transfer is faster. To investigate this technique, researchers have focused on tungsten oxide crystals (WO)3) And hydrated tungsten oxide crystals (WO)3·2H2O) (both are the same material, but the tungsten oxide hydrate crystal is a layered material having an aqueous layer). The results show that the charge/discharge rate of tungsten oxide hydrate is significantly improved compared to conventional tungsten oxide crystals.
The invention provides the aqueous leaf-shaped nano lamellar structure CoSeO with simple and convenient process and good repeatability3·H2The length and size of the flaky structure of the O nano-sheet preparation method are 2-5 mu m, the thickness is about 10-20nm, and the layered structure is obvious. The nano-sheets with the leaf-shaped layer-by-layer structure are adopted as the negative active materialThe assembled water system lithium ion battery shows high specific capacity and excellent rate capability of lithium ion storage. Has great application prospect in the fields of lithium ion batteries, zinc ion batteries, super capacitors and the like.
Disclosure of Invention
The invention provides a water-containing tree leaf lamellar structure nanocrystal material which is simple and convenient to operate, safe and environment-friendly, and a preparation method thereof, and application of the water-containing tree leaf lamellar structure nanocrystal material in a water-based lithium ion battery, aiming at the difficulty in synthesis of the water-containing lamellar structure nanocrystal.
The invention provides a preparation method of a water-containing leaf-shaped lamellar structure nanocrystal material, which comprises the following specific steps:
(1) preparing a layered unstable crystal by adopting a hydrothermal synthesis process: 70ml of a mixed solution of water and ethanol (volume ratio of ethanol to deionized water: 1) was prepared, and 0.75g of Co (Ac) was weighed2·4H2O (3.0mmol) and 0.33g SeO2(3.0mmol) was added to the above 70ml of mixed solvent, stirred well for 1 and transferred to a 100ml inner container of polytetrafluoroethylene. Sealing in a stainless steel reaction kettle, standing in a forced air oven, and reacting at 150 deg.C for 15 h. After the reaction is finished, the reaction product is naturally cooled to room temperature. Taking out, alternately centrifuging and washing with deionized water and ethanol for several times, finally washing with ethanol, placing in an evaporation dish, drying in a vacuum oven at 70 ℃ for 24h, and drying for later use.
(2) Washing and drying to obtain the layered water-containing nanocrystalline powder material.
In the invention, the length of the layered water-containing nanocrystal is 2-5 mu m, and the thickness of the layered water-containing nanocrystal is 10-20 nm.
In the invention, the soluble cobalt salt is analytically pure hydrated Acetate Co (AC)2·4H2O，SeO2And polyvinylidene fluoride PVDF (binder) is analytical grade (AR), the ethanol is commercial grade absolute ethanol, the mass fraction is more than or equal to 99.8%, and all reagents are directly used without purification. Graphene (size: 0.2-1 μm, thickness: 0.8nm, monolayer rate: 90%), all water used was deionized water.
(3) The preparation method of the leaf-shaped nano lamellar structure crystal material is characterized in that,
a. the solvent for the solvent thermal reaction is a mixed solution of water and ethanol, and the volume ratio is 1: 1.
b. in order to fully dissolve the cobalt salt and the selenium dioxide, the solvothermal precursor solution needs to be fully stirred for 1 hour (the stirring mode is magnetic stirring).
c. The washing treatment is to transfer a product obtained after solvent heating into a centrifuge tube, centrifuge the product for 5mins at the rotating speed of 7000rpm, pour out supernatant liquid, re-disperse the supernatant liquid with water and ethanol in sequence and centrifuge the supernatant liquid, and repeat the operation for 3-4 times; and the drying treatment is to transfer the product obtained by the washing treatment to an evaporating dish and dry the product in a vacuum oven at 70 ℃ for 24 hours.
d. And the drying treatment is to transfer the product subjected to the washing treatment by the absolute ethyl alcohol into an evaporating dish and dry the product in a vacuum oven at 70 ℃ for 24 hours.
The invention also provides a water-based lithium ion battery which mainly comprises a positive pole piece, a negative pole piece, a diaphragm and electrolyte, wherein the positive pole piece comprises a positive active material, a conductive agent acetylene black and a binder PVDF according to a mass ratio of 7:2:1, and the negative material of the water-based lithium ion battery adopts the leaf-shaped CoSeO3·H2O-nano wafer layer structure. Weighing CoSeO with the mass ratio of 8:23·H2O and single-layer graphene, and 60 times and nodular graphite material (CoSeO)3·H2Sum of O and single-layer graphene) was put into a sealed stainless steel ball mill pot with rotation speed and rotation speed of 600 and 400rpm for ball milling for 8 hours, respectively, with 5, 10 and 20 mm diameter steel balls in the mass ratio of 7:2:1 in order. And taking out the fully mixed materials in the tank after the ball milling is finished, weighing the nodular graphite materials, the conductive agent acetylene black and the binder PVDF in a mass ratio of 7:2:1, putting the materials into a mortar for fully grinding, dripping NMP while stirring to enable the viscosity to be proper, sealing, and then carrying out magnetic stirring for 8-12 hours. Coating the slurry on 304 stainless steel foil with thickness of 10 μm by using a coater, slightly drying, drying in a vacuum drying oven at 80 deg.C for 12h, cooling to room temperature, cutting into a circular positive electrode plate with diameter of 15mm, weighing the dried slurry and making the surface density of the slurry be 1-2mg/cm2。
The circular pole piece is taken as a positive pole piece, 10-micron metal lithium foil with the diameter of 15mm is taken as a negative pole piece, glass fiber with the diameter of 19mm is taken as a diaphragm, and 1.0mol/L LiPF6The ethylene carbonate and dimethyl carbonate (volume ratio is 1:1) solution is used as electrolyte to assemble 2032 coin cell.
Compared with the prior art, the invention has the technical effects that:
1. the one-step hydrothermal synthesis process adopted by the invention is simple and convenient in process and good in repeatability.
2. The size of the layered water-containing nano crystal obtained by the invention is 2-5 mu m, and the thickness is 10-20 nm. The appearance presents an obvious layered structure, and has huge application prospect in the fields of lithium ion batteries, zinc ion batteries, aluminum ion batteries, super capacitors and the like due to the size effect, the characteristics of high specific surface area, multiple active sites and the like.
3. The invention provides a water system lithium ion battery, which adopts the mixture of layered water-containing nano-crystals and graphene as a negative electrode material, shows excellent lithium ion storage performance such as high specific capacity and high rate performance, and has certain breakthrough in the aspects of electrochemical performance and selection of electric lithium ion negative electrode materials.
Drawings
FIG. 1 (left panel) shows a hydrous leaf-like layered structure CoSeO prepared by the method of the present invention3·H2The scanning electron microscope picture of the O nano crystal can show that the size of the crystal is 2-5 μm, and the appearance presents obvious lamellar structure. Fig. 1 (right drawing) shows a lateral flow charge-discharge curve of an aqueous lithium ion battery assembled by using the material as a negative electrode active material, and the cycle stability of the material can be seen from the graph.
FIG. 2 shows the aqueous leaf-shaped layered CoSeO prepared by the method of the present invention3·H2Atomic force microscopy scanning of O nanocrystals. From FIG. 2, CoSeO can be obtained3·H2The thickness of the O-sheet structure is about 10-20nm, and the thin-layer structure is clearly visible.
FIG. 3 is an aqueous solution prepared by the process of the present inventionLeaf-shaped layered structure nanocrystal CoSeO3·H2XRD spectrum of O crystal powder. The spectrum shows that the crystal product has good crystallinity, obvious tropism growth and obvious laminated structure.
FIG. 4 shows the aqueous leaf-shaped layered CoSeO prepared by the method of the present invention3·H2And the rate curve of the water-based lithium ion battery assembled by taking the O nanocrystals as the negative electrode active material. The excellent rate capability of the material can be seen from the figure.
FIG. 5 shows the layered aqueous leaf-shaped layered CoSeO prepared by the method of the present invention3·H2And the circulation curve of the water-based lithium ion battery assembled by taking the O nanocrystals as the negative active material. The figure shows that the negative electrode material still shows high specific capacity and excellent long-cycle stability under the high current density of 4A/g, and has high capacity, good stability and high developability.
Claims (6)
1. A preparation method of a water-containing leaf-shaped lamellar structure nanocrystal material is characterized by comprising the following specific steps:
(1) preparing the leaf-shaped lamellar structure nanocrystal material by adopting a solvothermal synthesis process: 70ml of a mixed solution of water and ethanol (volume ratio of ethanol to deionized water: 1) was prepared, and 0.75g of Co (Ac) was weighed2·4H2O (3.0mmol) and 0.33gSeO2(3.0mmol) is added into the above 70ml mixed solvent, and the mixture is transferred into a 100ml polytetrafluoroethylene liner after being fully stirred for 1 h. Sealing in a stainless steel reaction kettle, standing in a forced air oven, and reacting at 150 deg.C for 15 h. After the reaction is finished, the reaction product is naturally cooled to room temperature. Taking out, alternately centrifuging and washing with deionized water and ethanol for several times, finally washing with ethanol, placing in an evaporation dish, drying in a vacuum oven at 70 ℃ for 24h, and drying for later use.
(2) Washing and drying to obtain the water-containing leaf-shaped lamellar structure nanocrystal material.
2. The method for preparing the hydrous tree-leaf-like lamellar structure nanocrystal material according to claim 1The method is characterized in that the soluble cobalt salt adopts analytically pure hydrated Acetate Co (AC)2·4H2O，SeO2The ethanol is analytically pure (AR), the ethanol is commercial grade absolute ethanol, the mass fraction is more than or equal to 99.8%, and all reagents are directly used without purification. Graphene (size: 0.2-1 μm, thickness: 0.8nm, monolayer rate: 90%). All water used was deionized water.
3. The method for preparing an aqueous dendritic lamellar structure nanocrystal material according to claim 1, wherein,
(1) the solvent for the solvent thermal reaction is a mixed solution of water and ethanol, and the volume ratio is 1: 1.
(2) in order to fully dissolve the cobalt salt and the selenium dioxide, the solvothermal precursor solution needs to be fully stirred for 1 hour (the stirring mode is magnetic stirring).
(3) Transferring the product obtained after solvent heating into a centrifuge tube, centrifuging at 7000rpm for 5mins, pouring out supernatant liquid, sequentially re-dispersing with water and ethanol, centrifuging, and repeating the operation for 3-4 times; and the drying treatment is to transfer the product obtained by the washing treatment to a drying dish and dry the product in a vacuum oven at 70 ℃ for 24 hours.
4. An aqueous type leaf-like lamellar structure nanocrystal material obtained by the production method according to any one of claims 1 to 3.
5. The use of the aqueous dendritic lamellar nanocrystalline material of claim 4 as a negative electrode material in aqueous lithium ion batteries.
6. An aqueous lithium ion battery characterized in that the mixed material of the aqueous leaf-shaped lamellar structure nanocrystal material of claim 4 and graphene is used as a negative electrode active material of a negative electrode sheet.
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| CN114429866A (en) * | 2022-02-10 | 2022-05-03 | 杭州瑁昂科技有限公司 | Planar filtering electrochemical capacitor and preparation method thereof |
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| CN114429866A (en) * | 2022-02-10 | 2022-05-03 | 杭州瑁昂科技有限公司 | Planar filtering electrochemical capacitor and preparation method thereof |
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