CN109301231B - MoO (MoO)3Composite carbon dot lithium ion battery anode material and preparation method thereof - Google Patents

MoO (MoO)3Composite carbon dot lithium ion battery anode material and preparation method thereof Download PDF

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CN109301231B
CN109301231B CN201811351656.2A CN201811351656A CN109301231B CN 109301231 B CN109301231 B CN 109301231B CN 201811351656 A CN201811351656 A CN 201811351656A CN 109301231 B CN109301231 B CN 109301231B
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moo
lithium ion
ion battery
carbon dot
battery anode
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CN109301231A (en
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许占位
赵怡星
黄剑锋
曹丽云
贺菊菊
王天
杨军
沈学涛
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Shaanxi Coal And Chemical Technology Research Institute Co Ltd
Shaanxi University of Science and Technology
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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
    • H01M4/362—Composites
    • 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
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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

The invention discloses a MoO3The composite carbon dot lithium ion battery anode material and the preparation method thereof are characterized in that ammonium molybdate is used as a raw material, the composite carbon dot is used as a high-performance lithium ion battery cathode material, performic acid is used as an oxide to strip coal tar pitch to prepare the carbon dot, then the ammonium molybdate is used as a raw material, and the carbon dot is utilized to induce molybdenum trioxide to grow in an oriented manner by a hydrothermal method to form MoO with a sea urchin structure3Compounding carbon dot lithium ion battery anode materials; the method has the characteristics of simple preparation process, short period, low energy consumption, good repeatability, high yield and the like, and the MoO prepared by the method3The composite material can relieve volume expansion and increase the ion activation surface area, thereby improving the specific capacity and the cycling stability of the lithium ion battery.

Description

MoO (MoO)3Composite carbon dot lithium ion battery anode material and preparation method thereof
Technical Field
The invention relates to the technical field of lithium ion batteries, in particular to a MoO3A composite carbon dot lithium ion battery anode material and a preparation method thereof.
Background
Lithium ion batteries are more and more widely applied, but as the negative electrode of commercial lithium ion batteries, graphite can only transmit 372mAh g -1And the requirements of some electronic equipment such as electric automobiles which need large capacity cannot be met. [ Liu, J., P.J.Lu, S.Liang, J.Liu, W.Wang, M.Lei, S.Tang and Q.Yang, Ultrathin Li 3VO 4 nanobubon/graphene sandwich-like nanostructures with ultrahigh lithium ion storage properties.Nano Energy,2015.12:p.709-724.][Yan,J.,J.Zhang,Y.C. Su,X.G.Zhang and B.J.Xia,A novel perspective on the formation of the solid electrolyte interphase on the graphite electrode for lithium-ion batteries. Electrochimica Acta,2010.55(5):p.1785-1794.]MoO3As one member of transition metal oxide, the transition metal oxide has multiple valence states, higher thermodynamic chemical stability and rich mineral storage capacity, and can adapt to the development of the fields of hybrid electric vehicles, aerospace and the like. MoO3Having three crystal phases, i.e. thermodynamically stable orthorhombic alpha-MoO3(the specific capacity is up to 1117mAh g-1) Metastable monoclinic beta-MoO3And h-MoO of hexagonal stable phase3. In h-MoO3In, [ MoO ]6]The octahedron forms a z-shaped chain structure connected along the C-axis direction, and because molybdenum ions have good laminar flow structures and multiple valence states, a special tunnel structure caused by molybdenum vacancies is favorable for smaller ion embedding.
However, bulk MoO due to lower conductivity and poor lithium ion transport kinetics3Generally exhibit poor cycle performance as a negative electrode material for lithium ion batteries. Zhao, g., n.zhang and k.sun, Electrochemical prediction of pore MoO3film with a high a rate performance as an anode for Materials Chemistry A,2012.1(2): p.221- 3Has been synthesized and shows better electrochemical performance when applied to the cathode material of the lithium ion battery. Or it is compounded with a carbon material to improve its conductivity. The carbon dots refer to carbon particles having a particle size of less than 10nm and a fluorescent characteristic. The carbon dots have electrochemical luminescence property, up-conversion effect, certain catalytic action and good electrical conductivity. [ Meng, X., Q. Chang, C.Xue, J.Yang and S.Hu, Full-color carbon dots: from energy-efficiency synthesis to concentration-dependent phosphor properties, 2017.53(21): p.3074.][Wei,J.S.,H.Ding,P.Zhang,Y.F.Song,J. Chen,Y.G.Wang and H.M.Xiong,Carbon Dots/NiCo2O4Nanocomposites with Various Morphologies for High Performance Supercapacitors.Small,2016.12(43):p. 5927-5934.]。
Disclosure of Invention
The invention aims to provide a MoO3The method has the characteristics of simple preparation process, short period, low energy consumption, good repeatability, high yield and the like, and the prepared MoO3The composite material increases the ion activation surface area, and improves the specific capacity and the cycling stability of the lithium ion battery.
In order to achieve the above object, the present invention adopts the following technical solutions.
MoO (MoO)3A preparation method of a composite carbon point lithium ion battery anode material comprises the steps of fully mixing Ammonium Molybdate (AMB) and carbon points, adding the mixture into a hydrothermal kettle lining for hydrothermal reaction, and utilizing the carbon points to induce molybdenum trioxide to grow in an oriented manner in the decomposition process of the Ammonium Molybdate (AMB) to form hexagonal phase h-MoO similar to a sea urchin structure 3Obtaining MoO3The composite carbon dot lithium ion battery anode material.
Further, the method comprises the following steps:
1) adding performic acid serving as an oxide into the coal pitch, stirring and centrifuging, and taking supernate as a carbon dot solution with performic acid serving as a solvent;
2) putting 0.325-0.65 g of analytically pure ammonium molybdate into a beaker, adding 10ml of deionized water, and performing ultrasonic treatment to completely dissolve and uniformly disperse the ammonium molybdate;
3) adding 15-50 ml of carbon dot solution into the solution, fully mixing uniformly, putting into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 120-180 ℃ for 6-24 hours;
4) after the hydrothermal kettle is naturally cooled to room temperature, the hydrothermal kettle is washed for multiple times by deionized water and absolute ethyl alcohol respectively and then is dried in vacuum, and MoO is prepared3The composite carbon dot lithium ion battery cathode material.
Further, performic acid is added into the coal pitch in the step 1), the mixture is stirred for 24 hours and then centrifuged, and the supernatant is taken as a carbon dot solution of which the solvent is performic acid.
Further, deionized water is respectively used in the step 4)Washing with absolute ethyl alcohol for more than three times, and vacuum drying for 12-36 h to obtain MoO3The composite carbon dot lithium ion battery cathode material.
MoO (MoO)3The composite carbon dot lithium ion battery anode material is a hexagonal phase h-MoO similar to a sea urchin structure 3And (5) structure.
MoO of the invention3The preparation method of the composite carbon point lithium ion battery anode material comprises the steps of taking ammonium molybdate as a raw material, taking the composite carbon point as a high-performance lithium ion battery cathode material, taking performic acid as an oxide to strip coal pitch to prepare the carbon point, taking ammonium molybdate as a raw material, and utilizing the carbon point to induce molybdenum trioxide to grow in an oriented manner to form MoO with a sea urchin structure by a hydrothermal method3Compounding carbon dot lithium ion battery anode materials; the method has the characteristics of simple preparation process, short period, low energy consumption, good repeatability, high yield and the like, and the MoO prepared by the method3The composite material can relieve volume expansion and increase the ion activation surface area, thereby improving the specific capacity and the cycling stability of the lithium ion battery.
MoO prepared by the method of the invention3The product has high purity, shows excellent conductivity, cycling stability and high specific discharge capacity when used in a lithium ion battery, improves the capacity and rate capability of the lithium ion battery, and can be used as a lithium ion battery cathode material in the aspect of higher capacity.
Drawings
FIG. 1 is an XRD spectrum of the prepared composite material
FIG. 2 is an SEM micrograph of a composite material
FIG. 3 is a cycle performance map of a composite material
Detailed Description
The present invention will be described in further detail with reference to the following examples, which are not intended to limit the invention thereto.
Example 1
1) Adding performic acid serving as an oxide into the coal pitch, stirring for 24 hours, centrifuging, and taking supernatant, wherein the supernatant is a carbon dot solution with performic acid serving as a solvent;
2) 0.325g of analytically pure molybdic acid was takenAmmonium ((NH)4)Mo7O24·4H2O) putting the mixture into a beaker, adding 10ml of deionized water, and carrying out ultrasonic treatment for 10min to ensure that ammonium molybdate is completely dissolved and uniformly dispersed;
3) adding 15ml of carbon dot solution into the solution, fully and uniformly mixing, putting into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 180 ℃ for 6 hours;
4) after the hydrothermal kettle is naturally cooled to room temperature, washing the hydrothermal kettle with deionized water and absolute ethyl alcohol for more than three times respectively, and performing vacuum drying for 12 hours to obtain MoO3The composite carbon dot lithium ion battery cathode material.
Example 2
1) Adding performic acid serving as an oxide into the coal pitch, stirring for 24 hours, centrifuging, and taking supernatant, wherein the supernatant is a carbon dot solution with performic acid serving as a solvent;
2) 0.45g of analytically pure ammonium molybdate ((NH) was taken4)Mo7O24·4H2O) putting the mixture into a beaker, adding 10ml of deionized water, and carrying out ultrasonic treatment for 10min to ensure that ammonium molybdate is completely dissolved and uniformly dispersed;
3) Adding 30ml of carbon dot solution into the solution, fully and uniformly mixing, putting into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 120 ℃ for 24 hours;
4) after the hydrothermal kettle is naturally cooled to room temperature, washing the hydrothermal kettle with deionized water and absolute ethyl alcohol for more than three times respectively, and performing vacuum drying for 20 hours to obtain MoO3The composite carbon dot lithium ion battery cathode material.
Example 3
1) Adding performic acid serving as an oxide into the coal pitch, stirring for 24 hours, centrifuging, and taking supernatant, wherein the supernatant is a carbon dot solution with performic acid serving as a solvent;
2) 0.55g of analytically pure ammonium molybdate ((NH) was taken4)Mo7O24·4H2O) putting the mixture into a beaker, adding 10ml of deionized water, and carrying out ultrasonic treatment for 10min to ensure that ammonium molybdate is completely dissolved and uniformly dispersed;
3) adding 45ml of carbon dot solution into the solution, fully and uniformly mixing, putting into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 150 ℃ for 15 hours;
4) after the hydrothermal kettle is naturally cooled to room temperature, washing the hydrothermal kettle with deionized water and absolute ethyl alcohol for more than three times respectively, and performing vacuum drying for 24 hours to obtain MoO3The composite carbon dot lithium ion battery cathode material.
Referring to FIG. 1, it can be seen that the product prepared is h-MoO3When the method is compared with a standard PDF card (No.21-0569), the peak position is basically completely matched, and other impurity peaks are not found, which shows that the h-MoO prepared by the method 3The crystalline phase has a better purity.
Referring to fig. 2, an SEM image of the composite material, it is evident that molybdenum trioxide is a large narrow sheet material with carbon dots attached to its surface that serves to connect two micron sheets of molybdenum trioxide.
Example 4
1) Adding performic acid serving as an oxide into the coal pitch, stirring for 24 hours, centrifuging, and taking supernatant, wherein the supernatant is a carbon dot solution with performic acid serving as a solvent;
2) 0.65g of analytically pure ammonium molybdate ((NH) was taken4)Mo7O24·4H2O) putting the mixture into a beaker, adding 10ml of deionized water, and carrying out ultrasonic treatment for 10min to ensure that ammonium molybdate is completely dissolved and uniformly dispersed;
3) adding 50ml of carbon dot solution into the solution, fully and uniformly mixing, putting into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 170 ℃ for 14 hours;
4) and after the hydrothermal kettle is naturally cooled to room temperature, washing the hydrothermal kettle with deionized water and absolute ethyl alcohol for more than three times respectively, and performing vacuum drying for 36 hours to obtain MoO3The composite carbon dot lithium ion battery cathode material.
Referring to fig. 3, when the composite material prepared by the invention is applied to a lithium ion battery cathode material, excellent electrochemical stability is shown. I.e. when the current density is 100mA g-1In time, the product can maintain 1000mAh g after circulating for 30 circles -1The capacity of (c). Exhibit MoO3The composite carbon dots have higher specific capacity and better cycling stability.
In conclusion, the method of the invention has novel design idea and simple and convenient operation. The preparation method of the invention has the advantages of simple preparation method of Ammonium Molybdate (AMB) and carbon, easy control of the process, short preparation period, high repeatability of the product, good uniformity and contribution to large-scale production.
Molybdenum trioxide directly generated in one step by a hydrothermal method is used as a bulk material, and when the bulk material is applied to a lithium ion battery cathode material, a bulk structure is easily collapsed in a charging and discharging process, so that the capacity of the material is reduced and the cycling stability is poor. The invention can not only expand the application of the waste residue coal pitch after coal carbonization, but also improve the specific capacity of the lithium ion battery. In addition, the preparation process is simple and easy to control, the energy consumption is low, the repeatability of the product is good, and the large-scale production is facilitated.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting the same, and although the present invention is described in detail with reference to the above embodiments, those of ordinary skill in the art should understand that: modifications and equivalents may be made to the embodiments of the invention without departing from the spirit and scope of the invention, which is to be covered by the claims.

Claims (4)

1. MoO (MoO)3The preparation method of the composite carbon dot lithium ion battery anode material is characterized by comprising the following steps of: fully mixing Ammonium Molybdate (AMB) and carbon points, adding the mixture into a lining of a hydrothermal kettle for hydrothermal reaction, and inducing oriented growth of molybdenum trioxide by using the carbon points in the decomposition process of the Ammonium Molybdate (AMB) to form hexagonal phase h-MoO similar to sea urchin structure3Obtaining MoO3Compounding carbon dot lithium ion battery anode materials;
the preparation method specifically comprises the following steps:
1) adding performic acid serving as an oxide into the coal pitch, stirring and centrifuging, and taking supernate as a carbon dot solution with performic acid serving as a solvent;
2) putting 0.325-0.65 g of analytically pure ammonium molybdate into a beaker, adding 10ml of deionized water, and performing ultrasonic treatment to completely dissolve and uniformly disperse the ammonium molybdate;
3) adding 15-50 ml of the carbon dot solution prepared in the step 1) into the solution obtained in the step 2), fully mixing uniformly, putting into a polytetrafluoroethylene lining of a hydrothermal kettle, and carrying out hydrothermal reaction at 120-180 ℃ for 6-24 hours;
4) after the hydrothermal kettle is naturally cooled to room temperature, washing the reaction product with deionized water and absolute ethyl alcohol for multiple times respectively, and then drying in vacuum to prepare the MoO3The composite carbon dot lithium ion battery anode material.
2. The method of claim 1, wherein: adding performic acid into the coal pitch in the step 1), stirring for 24 hours, centrifuging, and taking supernate as a carbon point solution with performic acid as a solvent.
3. The method of claim 1, wherein: washing with deionized water and absolute ethyl alcohol respectively in the step 4) for more than three times, and vacuum drying for 12-36 h to obtain MoO3The composite carbon dot lithium ion battery anode material.
4. MoO prepared based on the method of any one of claims 1-33Composite carbon dot lithium ion battery anode material, wherein MoO3Is hexagonal phase h-MoO similar to sea urchin structure3。
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CN109888253A (en) * 2019-03-29 2019-06-14 华南理工大学 A kind of coated by titanium dioxide molybdenum trioxide material and the preparation method and application thereof
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