CN109449424B - Cobalt molybdate composite carbon dot lithium ion battery anode material and preparation method thereof - Google Patents

Cobalt molybdate composite carbon dot lithium ion battery anode material and preparation method thereof Download PDF

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CN109449424B
CN109449424B CN201811351659.6A CN201811351659A CN109449424B CN 109449424 B CN109449424 B CN 109449424B CN 201811351659 A CN201811351659 A CN 201811351659A CN 109449424 B CN109449424 B CN 109449424B
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cobalt molybdate
lithium ion
cobalt
ion battery
carbon dot
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CN109449424A (en
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许占位
赵怡星
王天
孔硌
沈学涛
杨军
黄剑锋
曹丽云
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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
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
    • 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
    • H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
    • 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
    • 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 cobalt molybdate composite carbon dot lithium ion battery anode material and a preparation method thereof, wherein ammonium molybdate and cobalt chloride hexahydrate are used as raw materials to be sintered to generate a cobalt molybdate precursor, and then a carbon dot is used for inducing cobalt molybdate to grow in an oriented manner by a hydrothermal method to form a protruding nanoparticle structure, so that the cobalt molybdate composite carbon dot lithium ion battery anode material is obtained; the method has the characteristics of simple preparation process, short period, low energy consumption, good repeatability, high yield and the like, the cobalt molybdate composite material prepared by the method can relieve volume expansion and increase the ion activation surface area, and a certain pseudo capacitance can be generated due to the existence of carbon points, so that the specific volume and the energy density of the material are improved.

Description

Cobalt molybdate composite 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 cobalt molybdate composite carbon dot lithium ion battery anode material and a preparation method thereof.
Background
Lithium ion batteries are mainly applied to the electronic and electrical industry, and energy-saving and environment-friendly lithium ion battery automobiles which are newly introduced have the defects of poor endurance stability, low capacity and the like, so that people are prompted to search for electrode materials with higher capacity. Intercalation reactionThe conversion reaction and the alloying reaction are three major mechanisms of the reaction of the lithium ion battery and influence the theoretical capacity of the material. For materials possessing conversion reactions, the first lithium insertion is accompanied by Li2The oxide is changed into a metal simple substance by the generation of O, a plurality of electrons participate in the reaction, and the material has higher reversible specific capacity and energy density. Cobalt molybdate, having up to 980mAh g-1Has been widely studied. [ Sandhya, C.P., John, B., Gouri, C, Sreemololanadhan, H.,&Manwatkar,S.K.Promising anode material for lithium-ion cells based on cobalt oxide synthesized by microwave heating.Ionics,2017.1-9.][Wang,B.,Li,S.,Wu,X.,Liu,J.,Tian,W.,&Chen,J.Self-assembly of ultrathin mesoporous CoMoO4nanosheet networks on flexible carbon fabric as a binder-free anode for lithium-ion batteries.New Journal of Chemistry,2016.40(3),2259-2267.]during charge and discharge, the material undergoes volume expansion due to intercalation and deintercalation of lithium ions, resulting in capacity fade and cycle life reduction. Different preparation processes are designed to prepare the cobalt molybdate composite electrode material so as to improve the capacity and stability of the battery. [ Xu, J., Gu, S., Fan, L., Xu, P.,&Lu,B..Electrospun lotus root-like CoMoO4@graphene nanofibers as high-performance anode for lithium ion batteries.Electrochimica Acta,2016.196,125-130.]carbon dots, one of the new pets for carbon materials, have a size of less than 10 nm. It is popular among researchers because of its non-toxicity, excellent conductivity, photocatalytic properties and photoluminescence properties. [ Meng, X., Chang, Q., Xue, C., Yang, J.,&Hu,S.Full-colour carbon dots:from energy-efficient synthesis to concentration-dependent photoluminescence properties.Chemical Communications,2017.53(21),3074.].
disclosure of Invention
The invention aims to provide a cobalt molybdate composite carbon dot lithium ion battery anode material and a preparation method thereof.
The surface area of the activated ions is increased, and the specific capacity and the cycling stability of the lithium ion battery are improved.
In order to achieve the above object, the present invention adopts the following technical solutions.
A preparation method of a cobalt molybdate composite carbon dot lithium ion battery anode material comprises the steps of taking ammonium molybdate and cobalt chloride hexahydrate as raw materials, and sintering by a solid phase method to generate a cobalt molybdate raw material; and then, inducing cobalt molybdate to grow bulges along different crystal faces by using the carbon points through a hydrothermal method, and synthesizing the cobalt molybdate composite carbon point nano structure with small bulges to obtain the cobalt molybdate composite carbon point 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 supernatant as a carbon dot solution;
2) putting 0.15-1.15 g of analytically pure ammonium molybdate into a mortar, adding 0.35-1.85 mg of cobalt chloride hexahydrate, fully grinding, putting into a crucible, sintering in a muffle furnace, heating the muffle furnace at the speed of 5-10 ℃/min, heating to 80-120 ℃ from room temperature, and preserving heat for 1-3 hours; (ii) a Heating to 300-450 ℃ at the speed of 1-5 ℃/min, and preserving heat for 1-3 h;
3) naturally cooling to room temperature, respectively carrying out suction filtration and washing on the prepared product by adopting water and ethanol for multiple times, and drying to obtain precursor cobalt molybdate powder; the mixture is filtered and cleaned for a plurality of times,
4) obtaining cobalt molybdate powder and 5-45 ml of the carbon dot solution prepared in the step 1), uniformly mixing, adding 10ml of deionized water, putting into a hydrothermal reaction kettle, heating to 120-180 ℃, and preserving heat for 6-12 hours;
5) after the heat preservation reaction is finished, cooling to room temperature, adding deionized water, standing for precipitation, pouring out supernatant, adding deionized water, and repeating the steps for multiple times; and then, carrying out suction filtration on the obtained product for multiple times by using ethanol and deionized water, and drying in vacuum to obtain the cobalt molybdate composite carbon dot lithium ion battery anode material.
Further, in the step 1), performic acid is added into the coal pitch, the mixture is stirred for 24 hours and then centrifuged, and the supernatant is taken to be a carbon point solution.
Further, in the step 3), the prepared product is filtered and cleaned by adopting filter paper with the aperture of 0.224 mu m, and is dried for 24 hours at the temperature of 60-80 ℃ to obtain precursor cobalt molybdate powder.
Further, after the heat preservation reaction in the step 5) is finished, cooling to room temperature, adding 10-50 ml of deionized water, standing for one day, pouring out supernatant, adding 10-50 ml of deionized water, and repeating the steps for three times; and (3) carrying out suction filtration on the obtained product for 3-5 times by using ethanol and deionized water, and drying in a vacuum oven to obtain the cobalt molybdate composite carbon dot lithium ion battery anode material.
A cobalt molybdate composite carbon dot lithium ion battery anode material is a nano structure with small bulges along different crystal faces.
According to the preparation method of the cobalt molybdate composite carbon dot lithium ion battery anode material, ammonium molybdate and cobalt chloride hexahydrate are used as raw materials and sintered to generate a cobalt molybdate precursor, and then a carbon dot is used for inducing cobalt molybdate to grow in an oriented manner by a hydrothermal method to form a protruding nanoparticle structure, so that the cobalt molybdate composite carbon dot lithium ion battery anode material is obtained; the method has the characteristics of simple preparation process, short period, low energy consumption, good repeatability, high yield and the like, the cobalt molybdate composite material prepared by the method can relieve volume expansion and increase the ion activation surface area, and a certain pseudo capacitance can be generated due to the existence of carbon points, so that the specific volume and the energy density of the material are improved.
The preparation method is simple, the process is easy to control, the preparation period is short, the repeatability of the product is high, the uniformity is good, and the large-scale production is facilitated. The cobalt molybdate prepared by the method has high purity, shows excellent conductivity, cycling stability and high specific discharge capacity when being used in a lithium ion battery, and can be applied to the aspect of high-capacity lithium ion battery cathode materials.
Drawings
FIG. 1 is a TEM photograph of the prepared carbon dots
FIG. 2 is an XRD spectrum of the prepared composite material
FIG. 3 is an SEM image of the prepared 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 taking performic acid as a solvent;
2) 0.35g of analytically pure ammonium molybdate ((NH) was taken4)Mo7O24·4H2O) was placed in a mortar, and 0.45mg of cobalt chloride hexahydrate (CoCl) was added2·6H2O) grinding, and fully grinding for half an hour; putting the ground mixture into a crucible and sintering in a muffle furnace; heating to 120 ℃ at the heating rate of 5 ℃/min, and keeping the temperature for one hour; then the temperature is raised to 450 ℃ at the temperature rise speed of 1 ℃/min, and the temperature is kept for two hours;
3) naturally cooling to room temperature, performing suction filtration on the prepared product by using filter paper with the aperture of 0.224 mu m, using water and ethanol, washing for 3-6 times, and drying in a vacuum drying oven at 70 ℃ for 24 hours;
4) adding the dried product into 30ml of deionized water, fully and uniformly mixing, putting into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 180 ℃ for 12 hours;
5) after the hydrothermal kettle is naturally cooled to the room temperature, 10-50 ml of deionized water is added, the mixture is kept stand for one day, supernatant liquid of the upper layer is poured off, 10-50 ml of deionized water is added, and the steps are repeated for three times; and (3) carrying out suction filtration on the obtained product for 3-5 times by using ethanol and deionized water, and drying in a vacuum oven to obtain the cobalt molybdate composite carbon dot lithium ion battery anode material.
Fig. 1 is a transmission diagram of a carbon quantum dot, and it can be seen from fig. 1 that the prepared carbon dot solution is relatively uniform in size and distribution.
FIG. 2 is an XRD pattern of the composite material, and the composite material prepared is a monoclinic phase of cobalt molybdate as can be seen in the corresponding pdf cards 21-0868.
FIG. 3 is a scanned graph of composite material, and it can be seen that the particle size of the material prepared by the present invention is below nanometer level, which is helpful for improving electrochemical performance of the 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 taking performic acid as a solvent;
2) 0.15g of analytically pure ammonium molybdate ((NH) was taken4)Mo7O24·4H2O) was placed in a mortar, and 0.35mg of cobalt chloride hexahydrate (CoCl) was added2·6H2O) grinding, and fully grinding for half an hour; putting the ground mixture into a crucible and sintering in a muffle furnace; heating to 100 ℃ at a heating rate of 10 ℃/min, and keeping the temperature for 3 hours; then heating to 350 ℃ at the heating rate of 3 ℃/min, and preserving the heat for 3 hours;
3) naturally cooling to room temperature, performing suction filtration on the prepared product by using water and ethanol, cleaning for 3-6 times, and drying for 24 hours at 60 ℃ in a vacuum drying oven;
4) adding the dried product into 5ml of carbon point solution, fully and uniformly mixing, putting into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 150 ℃ for 10 hours;
5) after the hydrothermal kettle is naturally cooled to the room temperature, 10-50 ml of deionized water is added, the mixture is kept stand for one day, supernatant liquid of the upper layer is poured off, 10-50 ml of deionized water is added, and the steps are repeated for three times; and (3) carrying out suction filtration on the obtained product for 3-5 times by using ethanol and deionized water, and drying in a vacuum oven to obtain the cobalt molybdate composite carbon dot lithium ion battery anode 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 taking performic acid as a solvent;
2) 0.65g of analytically pure ammonium molybdate ((NH) was taken4)Mo7O24·4H2O) was placed in a mortar, and 0.85mg of cobalt chloride hexahydrate (CoCl) was added2·6H2O) grinding, and fully grinding for half an hour; putting the ground mixture into a crucible and sintering in a muffle furnace; heating to 80 ℃ at the heating rate of 8 ℃/min, and keeping the temperature for 2 hours; then the temperature is raised to 3 ℃ at the temperature rise rate of 5 ℃/minPreserving the heat for 2 hours at 00 ℃;
3) naturally cooling to room temperature, carrying out suction filtration on the prepared product by using water and ethanol, cleaning for 3-6 times, and drying for 24 hours in a vacuum drying oven at 80 ℃;
4) adding the dried product into 30ml of carbon point solution, fully and uniformly mixing, putting into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 180 ℃ for 6 hours;
5) after the hydrothermal kettle is naturally cooled to the room temperature, 10-50 ml of deionized water is added, the mixture is kept stand for one day, supernatant liquid of the upper layer is poured off, 10-50 ml of deionized water is added, and the steps are repeated for three times; and (3) carrying out suction filtration on the obtained product for 3-5 times by using ethanol and deionized water, and drying in a vacuum oven to obtain the cobalt molybdate composite carbon dot lithium ion battery anode material.
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 taking performic acid as a solvent;
2) 1.15g of analytically pure ammonium molybdate ((NH) was taken4)Mo7O24·4H2O) was placed in a mortar, and 1.85mg of cobalt chloride hexahydrate (CoCl) was added2·6H2O) grinding, and fully grinding for half an hour; placing the ground mixture into a crucible in a muffle furnace; heating to 120 ℃ at the heating rate of 2 ℃/min, and keeping the temperature for 2 hours; then heating to 400 ℃ at the heating rate of 2 ℃/min, and preserving the heat for 1 hour;
3) naturally cooling to room temperature, performing suction filtration on the prepared product by using water and ethanol, cleaning for 3-6 times, and drying for 24 hours at 60 ℃ in a vacuum drying oven;
4) adding the dried product into 45ml of carbon point solution, fully and uniformly mixing, putting into a polytetrafluoroethylene lining, and carrying out hydrothermal reaction at 120 ℃ for 12 hours;
5) after the hydrothermal kettle is naturally cooled to the room temperature, 10-50 ml of deionized water is added, the mixture is kept stand for one day, supernatant liquid of the upper layer is poured off, 10-50 ml of deionized water is added, and the steps are repeated for three times; and (3) carrying out suction filtration on the obtained product for 3-5 times by using ethanol and deionized water, and drying in a vacuum oven to obtain the cobalt molybdate composite carbon dot lithium ion battery anode material.
The method takes ammonium molybdate and cobalt chloride hexahydrate as raw materials, and the raw materials of the cobalt molybdate are firstly generated by sintering through a solid phase method; and then, a hydrothermal method is utilized to induce cobalt molybdate to grow bulges along different crystal faces by using carbon dots, and the synthetic substance and the synthetic process of the method synthesize the special structure of the cobalt molybdate with small bulges, so that the capacity and the rate capability of the lithium ion battery can be further improved.
In conclusion, the method of the invention has novel design idea and simple and convenient operation. 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 body structure is easily collapsed in the charging and discharging process, so that the capacity of the material is reduced and the cycle 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 (6)

1. A preparation method of a cobalt molybdate composite carbon dot lithium ion battery anode material is characterized by comprising the following steps: ammonium molybdate and cobalt chloride hexahydrate are used as raw materials, and a cobalt molybdate raw material is generated by sintering through a solid phase method; and inducing cobalt molybdate to grow bulges along different crystal faces by using carbon points prepared by using formic acid as a solvent through a hydrothermal method, and synthesizing a cobalt molybdate composite carbon point nano structure with small bulges to obtain the cobalt molybdate composite carbon point lithium ion battery anode material.
2. The method of claim 1, comprising the steps of:
1) adding performic acid serving as an oxide into the coal pitch, stirring and centrifuging, and taking supernatant as a carbon dot solution;
2) putting 0.15-1.15 g of analytically pure ammonium molybdate into a mortar, adding 0.35-1.85 mg of cobalt chloride hexahydrate, fully grinding, putting into a crucible, sintering in a muffle furnace, heating the muffle furnace at the speed of 5-10 ℃/min, heating to 80-120 ℃ from room temperature, and preserving heat for 1-3 hours; heating to 300-450 ℃ at the speed of 1-5 ℃/min, and preserving heat for 1-3 h;
3) naturally cooling to room temperature, respectively carrying out suction filtration and washing on the prepared product by adopting water and ethanol for multiple times, and drying to obtain precursor cobalt molybdate powder;
4) obtaining cobalt molybdate powder and 5-45 mL of the carbon dot solution prepared in the step 1), uniformly mixing, adding 10mL of deionized water, putting into a hydrothermal reaction kettle, heating to 120-180 ℃, and preserving heat for 6-12 hours;
5) after the heat preservation reaction is finished, cooling to room temperature, adding deionized water, standing for precipitation, pouring out supernatant, adding deionized water, and repeating the steps for multiple times; and then, carrying out suction filtration on the obtained product for multiple times by using ethanol and deionized water, and drying in vacuum to obtain the cobalt molybdate composite carbon dot lithium ion battery anode material.
3. The method of claim 2, wherein: adding performic acid into the coal pitch in the step 1), stirring for 24 hours, centrifuging, and taking supernatant as carbon dot solution.
4. The method of claim 2, wherein: and in the step 3), the prepared product is filtered and cleaned by adopting filter paper with the aperture of 0.224 mu m, and is dried for 24 hours at the temperature of 60-80 ℃ to obtain precursor cobalt molybdate powder.
5. The method of claim 2, wherein: after the heat preservation reaction in the step 5) is finished, cooling to room temperature, adding 10-50 mL of deionized water, standing for one day, pouring out supernatant, adding 10-50 mL of deionized water, and repeating the steps for three times; and (3) carrying out suction filtration on the obtained product for 3-5 times by using ethanol and deionized water, and drying in a vacuum oven to obtain the cobalt molybdate composite carbon dot lithium ion battery anode material.
6. The cobalt molybdate composite carbon dot lithium ion battery anode material prepared based on the method of any one of claims 1 to 5 is a nano structure with small bulges along different crystal planes.
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