CN109638237A - A kind of compound anode material for lithium-ion batteries and preparation method thereof - Google Patents
A kind of compound anode material for lithium-ion batteries and preparation method thereof Download PDFInfo
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- CN109638237A CN109638237A CN201811416057.4A CN201811416057A CN109638237A CN 109638237 A CN109638237 A CN 109638237A CN 201811416057 A CN201811416057 A CN 201811416057A CN 109638237 A CN109638237 A CN 109638237A
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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
- H01M4/364—Composites as mixtures
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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
- 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
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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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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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
- H01M4/58—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
- H01M4/582—Halogenides
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- 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 belongs to field of lithium ion battery material, a kind of compound anode material for lithium-ion batteries and preparation method thereof is disclosed.The compound anode material for lithium-ion batteries is made of lithium fluoride, vanadium trioxide and conductive carbon.Preparation method are as follows: by V2O3Powder, LiF powder and conductive carbon pass through ball milling mixing, drying；Or be add to deionized water ammonium metavanadate and carbohydrate, it is stirred in sol form and takes out drying, 500~800 DEG C of heat treatment, obtains V under reducing atmosphere or inert atmosphere2O3- C, then by V2O3By ball milling mixing, drying obtains compound anode material for lithium-ion batteries for-C and LiF powder.Preparation method of the invention is simple, easy to operate, and the compound anode material for lithium-ion batteries charging and discharging capacity of gained is high, has a good application prospect.
Description
Technical field
The invention belongs to field of lithium ion battery material, and in particular to a kind of compound anode material for lithium-ion batteries and its
Preparation method.
Background technique
Since the commercialization of nineteen ninety lithium secondary battery, lithium ion battery technology has affected human lives' dearly
Every aspect.Can the high energy density cells of charge and discharge popularize various portable electronic products, also make long course continuation mileage
Electric car and smart grid energy storage become possibility.Why lithium ion battery technology can obtain immense success, very greatly
Cobalt acid lithium (LiCoO should be attributed to the fact that in degree2) positive electrode invention and commercialization, so that lithium battery is no longer needed dangerous metal
Lithium is as negative electrode material.The limitation of lithium cell cathode material has been decontroled, different types of novel anode material emerges in large numbers in succession, including
Embedded type negative electrode material (such as graphite, transition metal oxide of early stage etc.), alloy-type negative electrodes material (such as silicon etc.) and turn
Change type negative electrode material (such as transition metal oxide nano particle).Although current negative electrode material has different reaction mechanisms,
But embedded type compound is still the first choice of anode material for lithium-ion batteries.In numerous embedded type positive electrodes, stratiform gold
Belong to oxide and polyanionic compound is still important component part, most of positive electrode is all in main structure
It is inside reversibly embedded in and deviates from lithium ion, the redox reaction of transition metal in simultaneous structure.But positive electrode
The biggish weight of main structure, limits the specific capacity of positive electrode and the energy density of battery.Metal based on conversion reaction
Fluoride positive electrode, although showing excellent cycle performance near output voltage 3V, since the positive electrode is free of
Lithium ion, it is necessary to by cathode as lithium source, seriously limit the selection of negative electrode material, the use of lithium anode will also drop
The safety of low battery.
The positive electrode being commercialized at present is mainly the transistion metal compound containing lithium, is usually had one-dimensional, two-dimentional or three
The lithium ion tunnel of dimension and open crystal structure, such as transition metal phosphate (LiMPO4, M is transition metal), stratiform
Oxide (LiMO2) or spinel type compound (LiM2O4).However, these materials only have redox active numerous
Transistion metal compound in occupy seldom quantity.There are many transition metal oxides, sulfide, phosphate for nature
And nitrate, wherein having may much have the electrochemistry for being suitable as positive electrode to lithium potential, but they often all can
Because being free of lithium or ignored without lithium ion tunnel.If decontroling these limitations, it is new that searching can be provided to us
The anode material for lithium-ion batteries of type provides new chance.By taking transition metal oxide as an example, past research is limited only to
It is used as negative electrode material, shows it relative to Li using conversion reaction+Oxidation-reduction potential of/the Li lower than~1V.But
It is, if it is compound with the lithium-containing compound of small-molecular-weight, conductive carbon, to be expected to as a kind of compound lithium ion battery just
Pole material, and export and be higher than traditional lithium-ion battery positive electrode (LiCoO2, LiMn2O4, LiFePO4) specific capacity, make lithium from
Sub- battery has higher energy density.
Summary of the invention
In place of the above shortcoming and defect of the existing technology, the primary purpose of the present invention is that providing a kind of compound
Type anode material for lithium-ion batteries.
Another object of the present invention is to provide the preparation methods of above-mentioned compound anode material for lithium-ion batteries.
The object of the invention is achieved through the following technical solutions:
A kind of compound anode material for lithium-ion batteries, by lithium fluoride (LiF), vanadium trioxide (V2O3) and conductive carbon (C)
Form (LiF-V2O3-C)。
Preferably, the conductive carbon refers at least one in graphite, acetylene black, conductive black, carbon nanotubes and graphene
Kind.
Preferably, the molar ratio LiF:V of the lithium fluoride, vanadium trioxide and conductive carbon2O3: C=4:1:0.2.
The preparation method of above-mentioned compound anode material for lithium-ion batteries, including following preparation step:
By V2O3Powder, LiF powder and conductive carbon obtain compound lithium ion cell positive material by ball milling mixing, drying
Expect (LiF-V2O3-C)。
Preferably, the condition of the ball milling mixing are as follows: 300~600rpm of rotational speed of ball-mill, 24~96h of Ball-milling Time.
Preferably, the V2O3Powder is prepared via a method which: taking vanadic anhydride (V2O5) powder, in reproducibility gas
500~800 DEG C of 5~36h of heat treatment, obtain V under atmosphere2O3Powder.
Preferably, the reducing atmosphere refers to Ar-H2Gaseous mixture atmosphere, N2-H2Gaseous mixture atmosphere, hydrogen atmosphere or ammonia
Gas atmosphere.
The preparation method of above-mentioned compound anode material for lithium-ion batteries, including following preparation step:
(1) by ammonium metavanadate (NH4VO3) and carbohydrate be add to deionized water, be stirred in sol form and take
It dries out, 500~800 DEG C of heat treatment, obtains V under reducing atmosphere or inert atmosphere2O3With conductive carbon composite (V2O3-
C)；
(2) by V2O3By ball milling mixing, drying obtains compound anode material for lithium-ion batteries for-C and LiF powder
(LiF-V2O3-C)。
Preferably, the carbohydrate refers at least one of glucose, sucrose, citric acid, cellulose and starch.
Preferably, the reducing atmosphere refers to Ar-H2Gaseous mixture atmosphere, N2-H2Gaseous mixture atmosphere, hydrogen atmosphere or
Ammonia atmosphere；The inert atmosphere refers to Ar, N2、CO2Or He atmosphere.
Preferably, the heat treatment time is 5~36h.
Preferably, the condition of the ball milling mixing are as follows: 300~600rpm of rotational speed of ball-mill, 24~96h of Ball-milling Time.
Compound anode material for lithium-ion batteries of the invention and preparation method have the following advantages that and the utility model has the advantages that
(1)V2O3Middle vanadium is+trivalent, and the highest valence state of vanadium is+5 valences, and the vanadium of+5 valences be it is stable, be common in five oxidations
Two vanadium (V2O5) and lithium vanadate (Li3VO4).Therefore, V is utilized2O3Bielectron reaction (being oxidized to+5 valences from+trivalent), while by
LiF provides lithium ion, and conductive carbon improves the electric conductivity of material, and when charging can make V2O3It aoxidizes and deviates from lithium ion from LiF, because
This composite L iF-V of the invention2O3- C can be used as a kind of novel anode material for lithium-ion batteries.
(2) due to V2O3Bielectron reaction can be carried out, in molar ratio LiF:V2O3: C=4:1:0.2 is compound, and gained is compound
The theoretical specific capacity of type positive electrode is 418mAh/g, much higher than commercialization positive electrode (LiCoO2, LiMn2O4, LiFePO4)
Specific capacity.The composite material is used as positive electrode, the energy density of lithium ion battery can be greatly improved, is expected to meet dynamic
The energy density of power battery reaches the requirement of 400Wh/kg.
(3) present invention synthesis V2O3After powder, is mixed using simple high-energy ball milling, a kind of compound lithium can be obtained
Ion battery anode material LiF-V2O3- C, the preparation method is simple, easy to operate, and particle size, pattern are easy to control, have compared with
High industrialization prospect.
Detailed description of the invention
Fig. 1 is compound anode material for lithium-ion batteries LiF-V in the embodiment of the present invention 12O3The scanning electron microscope of-C
(SEM) figure and element M apping figure.
Fig. 2 is compound anode material for lithium-ion batteries LiF-V in the embodiment of the present invention 22O3- C and with LiF and V2O3's
The X-ray diffractogram that normal data compares.
Fig. 3 is compound anode material for lithium-ion batteries LiF-V in the embodiment of the present invention 32O3- C is in 1.5~4.8V voltage
Charging and discharging curve figure in range.
Specific embodiment
Present invention will now be described in further detail with reference to the embodiments and the accompanying drawings, but embodiments of the present invention are unlimited
In this.
Embodiment 1
A kind of preparation method of compound anode material for lithium-ion batteries of the present embodiment, specific preparation process is as follows:
(1) vanadic anhydride (V of 5g is taken2O5) powder, under reducing atmosphere 600 DEG C heat treatment 24 hours after, can get
V2O3Powder.
(2) by V2O3, LiF powder and graphite be in molar ratio V2O3: LiF:C=1:4:0.2 is put into ceramic ball grinder, with
Behind revolving speed mixing and ball milling 24 hours of 400rpm, low temperature drying after taking-up obtains compound anode material for lithium-ion batteries (LiF-
V2O3-C)。
Scanning electron microscope (SEM) figure and element M apping figure of the present embodiment products therefrom are shown in Fig. 1, as seen from the figure,
C in product, O, V, F Elemental redistribution are uniform, it was demonstrated that LiF, V2O3It has been adequately mixed with three kinds of substances of graphite.
Embodiment 2
A kind of preparation method of compound anode material for lithium-ion batteries of the present embodiment, specific preparation process is as follows:
(1) vanadic anhydride (V of 5g is taken2O5) powder, under reducing atmosphere 800 DEG C heat treatment 20 hours after, can get
V2O3Powder.
(2) by V2O3, LiF powder and acetylene black be in molar ratio V2O3: LiF:C=1:4:0.2 is put into ceramic ball grinder,
After revolving speed mixing and ball milling 48 hours of 500rpm, low temperature drying after taking-up obtains compound anode material for lithium-ion batteries
(LiF-V2O3-C)。
The present embodiment products therefrom and with LiF and V2O3X-ray diffraction (XRD) map for comparing of normal data see
Fig. 2, as seen from the figure, the XRD spectrum of product is LiF, V after ball milling2O3The superposition of the two, unbodied conductive carbon cannot be by X-rays
It is detected, is not generated other new object phases.
Embodiment 3
A kind of preparation method of compound anode material for lithium-ion batteries of the present embodiment, specific preparation process is as follows:
(1) by 1.5g ammonium metavanadate (NH4VO3) and 2.7g citric acid, it is added in the deionized water of 70mL, stirs 3 hours
Afterwards in sol form taking-up put baking oven drying, under reducing atmosphere or inert atmosphere 700 DEG C heat treatment 28 hours after, can get
V2O3With conductive carbon composite V2O3-C。
(2) by the V of 3g2O3- C and 2.2g LiF powder are put into ceramic ball grinder, small with the revolving speed mixing and ball milling 48 of 600rpm
Shi Hou, low temperature drying after taking-up obtain compound anode material for lithium-ion batteries (LiF-V2O3-C)。
Charging and discharging curve of the positive electrode obtained by the present embodiment in 1.5~4.8V voltage range is as shown in Figure 3.By in figure
It is found that compound anode material for lithium-ion batteries LiF-V2O3- C initial charge specific capacity is 405mAh/g, first discharge specific capacity
For 339mAh/g, it is much higher than commercialization positive electrode (LiCoO2, LiMn2O4, LiFePO4) specific capacity.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (10)
1. a kind of compound anode material for lithium-ion batteries, it is characterised in that: the compound anode material for lithium-ion batteries by
Lithium fluoride, vanadium trioxide and conductive carbon composition.
2. a kind of compound anode material for lithium-ion batteries according to claim 1, it is characterised in that: the conductive carbon is
Refer at least one of graphite, acetylene black, conductive black, carbon nanotubes and graphene.
3. a kind of compound anode material for lithium-ion batteries according to claim 1, it is characterised in that: the lithium fluoride,
The molar ratio LiF:V of vanadium trioxide and conductive carbon2O3: C=4:1:0.2.
4. a kind of described in any item preparation methods of compound anode material for lithium-ion batteries of claims 1 to 3, feature exist
In including following preparation step:
By V2O3Powder, LiF powder and conductive carbon obtain compound anode material for lithium-ion batteries by ball milling mixing, drying.
5. a kind of preparation method of compound anode material for lithium-ion batteries according to claim 4, it is characterised in that institute
State the condition of ball milling mixing are as follows: 300~600rpm of rotational speed of ball-mill, 24~96h of Ball-milling Time.
6. a kind of preparation method of compound anode material for lithium-ion batteries according to claim 4, it is characterised in that institute
State V2O3Powder is prepared via a method which: taking V2O5Powder, 500~800 DEG C of 5~36h of heat treatment, obtain under reducing atmosphere
To V2O3Powder；The reducing atmosphere refers to Ar-H2Gaseous mixture atmosphere, N2-H2Gaseous mixture atmosphere, hydrogen atmosphere or ammonia gas
Atmosphere.
7. a kind of described in any item preparation methods of compound anode material for lithium-ion batteries of claims 1 to 3, feature exist
In including following preparation step:
(1) ammonium metavanadate and carbohydrate are add to deionized water, are stirred in sol form and take out drying, also
500~800 DEG C of heat treatment, obtains V under originality atmosphere or inert atmosphere2O3With conductive carbon composite V2O3-C；
(2) by V2O3By ball milling mixing, drying obtains compound anode material for lithium-ion batteries for-C and LiF powder.
8. a kind of preparation method of compound anode material for lithium-ion batteries according to claim 7, it is characterised in that: institute
It states carbohydrate and refers at least one of glucose, sucrose, citric acid, cellulose and starch.
9. a kind of preparation method of compound anode material for lithium-ion batteries according to claim 7, it is characterised in that: institute
The reducing atmosphere stated refers to Ar-H2Gaseous mixture atmosphere, N2-H2Gaseous mixture atmosphere, hydrogen atmosphere or ammonia atmosphere；Described is lazy
Property atmosphere refers to Ar, N2、CO2Or He atmosphere；The heat treatment time is 5~36h.
10. a kind of preparation method of compound anode material for lithium-ion batteries according to claim 7, it is characterised in that institute
State the condition of ball milling mixing are as follows: 300~600rpm of rotational speed of ball-mill, 24~96h of Ball-milling Time.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112850683A (en) * | 2019-11-27 | 2021-05-28 | 中国科学院大连化学物理研究所 | Preparation method and application of vanadium-based polyanion compound |
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| CN112850683A (en) * | 2019-11-27 | 2021-05-28 | 中国科学院大连化学物理研究所 | Preparation method and application of vanadium-based polyanion compound |
| CN112850683B (en) * | 2019-11-27 | 2022-11-08 | 中国科学院大连化学物理研究所 | Preparation method and application of vanadium-based polyanion compound |
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