CN110844946A - Metastable crystal material and preparation method thereof - Google Patents

Metastable crystal material and preparation method thereof Download PDF

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Publication number
CN110844946A
CN110844946A CN201911134843.XA CN201911134843A CN110844946A CN 110844946 A CN110844946 A CN 110844946A CN 201911134843 A CN201911134843 A CN 201911134843A CN 110844946 A CN110844946 A CN 110844946A
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layered
metastable
crystalline material
crystal
niseo
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陈吉锋
包万双
邵疆
刘兴辉
何桂港
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Shanghai Ji Feng Electronic Ltd By Share Ltd
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • 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
    • H01M4/36—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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
    • C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/40—Electric properties
    • 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

Abstract

Layered metastable crystal material and preparation method thereof, wherein the layered metastable crystal material is NiSeO3·H2The O micron crystal has great application prospect in the fields of lithium ion batteries, zinc ion batteries, super capacitors and the like. The water system ion battery assembled by the material of the invention shows the lithium ion storage performance with high specific capacity and excellent rate capability.

Description

Metastable crystal material and preparation method thereof
Technical Field
The present invention relates to a metastable crystal preparation method and the metastable crystal, and more particularly to a metastable crystal with a layered structure and a preparation method thereof.
Background
With the rapid development of social economy and scientific technology, the problems in the aspects of resource utilization and environmental pollution are increasingly prominent. The development and utilization of various new energy sources are becoming more and more urgent, and corresponding energy storage materials and energy storage equipment also become research hotspots. Lithium ion batteries are used as 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 conventional application of graphite as a negative electrode material is greatly limited due to the limited theoretical capacity, and the synthesis of a high-capacity negative electrode material is the best way for realizing the above dynamic transformation. Over the past few decades, a variety of negative electrode materials, including intercalated graphene, alloyed silicon, and converted metal oxide/sulfide/selenide/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/delithiation charging and discharging. Elemental silicon, for example, is considered one of the most promising high energy anode materials because of its ultra-high theoretical capacity (about 4200 mAh/g). But the material generates about 300% volume change and significant cathode polarization during the insertion and extraction of lithium ions, thus resulting in rapid capacity fade 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 two-dimensional oxyhydroxide and bimetallic oxide/sulfide studies, and from the characteristics of these materials we conclude that high rate performance of lithium ion anodes with long cycle stability can be achieved essentially by the following two routes:
the first method is a tunable two-dimensional structure, and the appropriate interlayer spacing between two-dimensional nanosheets facilitates the storage of large quantities of lithium ions and the rapid transfer of lithium ions between the electrolyte and the electrode.
The second method is amorphization: such as a metallic glassy material, is a disordered state at the atomic level, but exhibits good electronic conductivity, thermal stability and elastic modulus. The amorphous structure has isotropic stress and can reduce the risk of fracture during electrochemical cycling because the electrochemically active atoms are arranged in a disordered manner. Studies have shown that amorphous anode materials exhibit enhanced electrochemical performance compared to crystalline anode materials. Therefore, it is very attractive to synthesize an amorphous anode material that can minimize the volume change and electrochemical strain during charge and discharge.
The metastable crystal (metastable crystal form) not only changes the organization structure of the material, but also has great influence on the material performance, however, because most inorganic compounds spontaneously crystallize or the nanostructure grows into a bulk material, how to obtain the stable metastable crystal material which can be used as an anode material is still a challenge.
Disclosure of Invention
Aiming at the difficulty of synthesizing the lamellar metastable state crystal, the invention provides a lamellar metastable state crystal material which is simple and convenient to operate, safe and environment-friendly and a preparation method thereof.
In a first aspect of the present application, there is provided a method of preparing a layered metastable crystalline material, comprising: nickel salt, SeO2Adding solvent into a reaction vessel, and heating for reaction to generate NiSeO3(ii) a And cooling, washing and drying to obtain the layered metastable state crystal material.
In a preferred embodiment, the solvent is a solvent capable of dissolving nickel salt and SeO simultaneously2For example water.
In a preferred embodiment, the molar ratio of Ni to Se is preferably 1: 1.
In a preferred embodiment, the nickel salt is a nickel salt that is soluble in the solvent (preferably water), and may for example be selected from: nickel nitrate, nickel sulfate, nickel acetate, nickel chloride, and hydrates of any one or more of the nickel salts described above.
In a preferred embodiment, the inner wall of the reaction vessel is a fluoropolymer material.
More preferably, the fluoropolymer may be polytetrafluoroethylene, polyhexafluoropropylene, polychlorotrifluoroethylene, polyvinylidene fluoride, tetrafluoroethylene-hexafluoropropylene copolymer, tetrafluoroethylene-hexafluoropropylene-trifluoroethylene copolymer, tetrafluoroethylene-hexafluoroethylene-vinylidene fluoride copolymer, tetrafluoroethylene-perfluoroalkyl vinyl ether copolymer, polytetrafluoroethylene-ethylene copolymer, or the like.
In a preferred embodiment, the heating is preferably to 150 deg.C, more preferably 160 deg.C and 200 deg.C, more preferably 170 deg.C and 190 deg.C. More preferably 180-.
In a preferred embodiment, the heating is performed after the container is sealed.
In a preferred embodiment, the reaction vessel is placed in a forced air oven for the heating.
In a preferred embodiment, the reaction is preferably carried out for a reaction time of at least 10 hours, more preferably from 10 to 24 hours, more preferably from 12 to 20 hours, more preferably from 15 to 18 hours.
In a preferred embodiment, the washing is preferably an alternating wash with water and alcohol.
In a preferred embodiment, the washing is suction filtration washing, and more preferably, the product obtained by the heating reaction is transferred to a buchner funnel, the inside of the buchner funnel is covered with an organic microporous filter membrane, deionized water or ethanol is added to the precipitate in the funnel to fill the inner volume of the funnel, and the washing solution is suction filtered until the washing solution is completely removed.
In a preferred embodiment, the drying is carried out by transferring the washed product to an evaporating dish and drying it in a forced air oven.
In a preferred embodiment, the temperature of the drying is preferably at least 50 ℃, more preferably 50-100 ℃, more preferably 60-90 ℃, more preferably 70-80 ℃.
In a preferred embodiment, the drying time is preferably at least 8 hours, more preferably 12-24 hours.
In a second aspect of the present application, a layered metastable crystalline material is provided.
In a preferred embodiment, the layered metastable crystal material is NiSeO3·H2And (4) O micron crystal.
In a preferred embodiment, the layered metastable crystal material is prepared by a method according to the first aspect of the present application.
In a preferred embodiment, the NiSeO3·H2The O micron crystal size is distributed in the range of 20-30 μm.
The application provides the layered metastable NiSeO with simple and convenient process and certain universality3·H2The layered structure of the product is obvious by the preparation method of O. Has great application prospect in the fields of lithium ion batteries, zinc ion batteries, super capacitors and the like. The aqueous lithium ion battery assembled by adopting the layered structure material shows the lithium ion storage performance with high specific capacity and excellent rate performance.
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 and has certain universality.
2. The size of the layered metastable crystal obtained by the invention is 20-30 μm, the appearance presents an obvious layered structure, and the layered metastable crystal 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 and the characteristics of high specific surface area, multiple active sites and the like.
Drawings
FIGS. 1A and 1B are layered metastable crystal NiSeO prepared by the method of the present invention3·H2Scanning electron microscopy image of O.
FIG. 2 is a layered metastable crystal NiSeO prepared by the method of the present invention3·H2XRD spectrum of O.
FIG. 3 is a layered metastable crystal NiSeO prepared by the method of the present invention3·H2O selected area electron diffraction pattern.
FIG. 4 is a layered metastable crystal NiSeO prepared by the method of the present invention3·H2Magnification curve of O.
FIG. 5 is a constant current charge-discharge curve of an aqueous secondary zinc ion battery assembled by using the layered metastable crystal as a positive electrode material and prepared by the method of the invention.
Detailed Description
The invention is further illustrated by the following specific examples.
Example 1
Weigh 0.58g of Ni (Ac)2·6H2O (2.0mmol) and 0.222g SeO2(2.0mmol) is added into 70ml deionized water, stirred for 30min fully and then transferred into a 100ml small-sized reaction kettle polytetrafluoroethylene liner in a laboratory. Sealing and standing in a blowing oven at 180 ℃ for reaction for 15 h.
After the reaction is finished, the reaction product is naturally cooled to room temperature. Transferring the obtained product to a Buchner funnel, alternately filtering and washing with deionized water and ethanol for several times, and placing in a vacuum oven at 70 ℃ for 12-24 h to obtain NiSeO3·H2O micron-sized crystals with the particle size of 50-100 μm.
Example 2
Weighing Ni (NO)3)2·6H2O (2.0mmol) and SeO2(2.0mmol) is added into 70ml deionized water, stirred for 30min fully and then transferred into a 100ml small-sized reaction kettle polytetrafluoroethylene liner in a laboratory. Sealing and standing in a blowing oven at 180 ℃ for reaction for 15 h.
After the reaction is finished, the reaction product is naturally cooled to room temperature. Transferring the obtained product to a Buchner funnel, alternately filtering and washing with deionized water and ethanol for several times, and placing in a vacuum oven at 70 ℃ for 12-24 h to obtain NiSeO3·H2O micron-sized crystals with the particle size of 50-100 μm.
FIGS. 1A and 1B show layered metastable crystal NiSeO obtained in the above examples of the present application3·H2And O, as can be seen from the scanning electron microscope images with different magnifications in figures 1A and 1B, the size of the crystal is 20-30 mu m, and the appearance presents a distinct layered structure.
FIG. 2 shows layered metastable crystal NiSeO prepared in the above examples of the present application3·H2XRD spectrum of O. From fig. 2, the crystal crystallinity of the product is good, the growth orientation is obvious, and the layered structure is obvious.
FIG. 3 layered metastable crystal NiSeO prepared in the above examples of the present application3·H2O selected area electron diffraction pattern. The left image is NiSeO shot after rapid focusing3·H2O is an electron diffraction pattern, the highly ordered arrangement of atoms is obviously seen, the right image is the NiSeO in the same area after being irradiated by the electron beam for a short time of seconds3·H2O is taken as an electron diffraction pattern, and the appearance of diffraction rings illustrates the amorphous character of the tested material, i.e. the atoms constituting the material are in disordered arrangement. The comparison of the two figures can judge that the atoms of the lamellar structure crystal are transformed from a highly ordered state to a completely disordered state through short-term electron beam irradiation, and the lamellar structure crystal shows obvious metastable state characteristics.
Example 3
Weighing NiSeO at a mass ratio of 8: 23·H2O-micron crystal and single-layer graphene, and 60 times and nodular graphite material (NiSeO)3·H2Sum of O-micron crystals and single-layer graphene) mass of abrasive (steel balls with diameters of 5, 10 and 20 mm in the order of mass ratio of 7: 2: 1) was placed in a sealed stainless steel ball milling jar and ball milled at a rotational speed and a spin speed of 700 and 600rpm, respectively, for 6 h.
And (3) 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, dropwise adding NMP while stirring to enable the viscosity to be proper, sealing, and then carrying out magnetic stirring for 8-12 hours to obtain the slurry.
Coating the slurry on 304L stainless steel foil with a 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, and cutting into a circular positive electrode piece with a diameter of 15mmThe dried slurry was weighed to have a areal density of about 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 solution of ethylene carbonate and dimethyl carbonate (volume ratio is 1: 1) is used as electrolyte to assemble 2032 coin cell.
FIG. 4 shows layered metastable crystal NiSeO prepared in the above examples of the present application3·H2Magnification curve of O. As can be seen from the figure, the layered metastable crystal NiSeO3·H2O has excellent rate performance.
Fig. 5 is a constant current charge and discharge curve of an aqueous secondary zinc ion battery assembled by using the layered metastable crystal as a positive electrode material, prepared in the above example of the present application. I.e. lamellar metastable crystal NiSeO3·H2And a cycle curve of the aqueous lithium ion battery, wherein the cycle curve is formed by using a mixed material of O and graphene spheroidal graphite as a positive electrode material. It can be seen from the figure that under the condition of a large current density of 3A/g, after 500 cycles, the coulombic efficiency is still kept at 100%, and the specific capacity is still kept above 600mAh/g, which indicates that the positive electrode material still shows high specific capacity and excellent long cycle stability under the large current density of 3A/g, and has large capacity, good stability and high developability.
The embodiments of the present invention have been described in detail, but the embodiments are merely examples, and the present invention is not limited to the embodiments described above. Any equivalent modifications and substitutions to those skilled in the art are also within the scope of the present invention. Accordingly, equivalent changes and modifications made without departing from the spirit and scope of the present invention should be covered by the present invention.

Claims (10)

1. A method of preparing a layered metastable crystalline material, comprising:
nickel salt, SeO2Adding solvent into a reaction vessel, and heating for reaction to generate NiSeO3；
And cooling, washing and drying to obtain the layered metastable state crystal material.
2. The method of claim 1, wherein the nickel salt, SeO, is2In such an amount that the molar ratio of Ni to Se is preferably 1: 1.
3. The method for preparing a layered metastable crystalline material according to claim 1, characterized in that the solvent is a solvent capable of dissolving nickel salt, SeO simultaneously2The solvent of (1).
4. The method for preparing a layered metastable crystalline material according to claim 1, characterized in that the nickel salt is selected from: nickel nitrate, nickel sulfate, nickel acetate, nickel chloride, and hydrates of any one or more of the nickel salts described above.
5. The method of preparing a layered metastable crystalline material according to claim 1, characterized in that said heating is performed after said reaction vessel is sealed.
6. The method for preparing a layered, metastable crystalline material according to claim 5, characterized in that said reaction vessel is placed in a forced air oven for said heating.
7. The method for preparing a layered metastable crystalline material according to claim 6, characterized in that the heating is heating to 150 ℃ or more; the reaction time of the reaction is at least 10 hours.
8. The method for preparing a layered metastable crystalline material according to claim 1, characterized in that the temperature for drying is at least 50 ℃; the drying time is at least 8 hours.
9. A lamellar metastable crystal material, characterized in that said lamellar metastable crystal materialThe crystalline material is NiSeO3·H2And (4) O micron crystal.
10. The layered metastable crystalline material of claim 9, characterized in that said NiSeO3·H2The O micron crystal size is distributed in the range of 20-30 μm.
CN201911134843.XA 2019-11-19 2019-11-19 Metastable crystal material and preparation method thereof Pending CN110844946A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3538162A (en) * 1967-10-20 1970-11-03 Uniroyal Inc Reductive alkylation of aromatic amino and nitro compounds utilizing base metal selenides and tellurides as catalysts
CN109603859A (en) * 2018-12-18 2019-04-12 山东大学 It is a kind of with the selenous acid nickel cobalt elctro-catalyst of nano net three-dimensional structure and its application

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3538162A (en) * 1967-10-20 1970-11-03 Uniroyal Inc Reductive alkylation of aromatic amino and nitro compounds utilizing base metal selenides and tellurides as catalysts
CN109603859A (en) * 2018-12-18 2019-04-12 山东大学 It is a kind of with the selenous acid nickel cobalt elctro-catalyst of nano net three-dimensional structure and its application

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* Cited by examiner, † Cited by third party
Title
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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
CN114429866B (en) * 2022-02-10 2023-07-28 杭州瑁昂科技有限公司 Planar filter electrochemical capacitor and preparation method thereof

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