CN109167027A - A kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method - Google Patents
A kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method Download PDFInfo
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- CN109167027A CN109167027A CN201810947675.5A CN201810947675A CN109167027A CN 109167027 A CN109167027 A CN 109167027A CN 201810947675 A CN201810947675 A CN 201810947675A CN 109167027 A CN109167027 A CN 109167027A
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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
- H01M4/366—Composites as layered products
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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
- H01M4/58—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
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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
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
- H01M4/587—Carbonaceous material, e.g. graphite-intercalation compounds or CFx for inserting or intercalating light metals
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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 present invention relates to a kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation methods, comprising the following steps: expanded graphite is prepared graphene oxide dispersion by Hummers method；Ascorbic acid, lithium carbonate and ferric phosphate are sequentially added in graphene oxide dispersion, is sufficiently mixed grinding, are spray-dried, are obtained mixed powder；Mixed powder is subjected to step-up temperature sintering in the tube-type atmosphere furnace for being connected with inert gas, obtains redox graphene/carbon coating/composite ferric lithium phosphate material；The method of the present invention is simple, and sintering feed can be applied to lithium ion battery directly as positive electrode, and graphene oxide is directly heat reduced to redox graphene by high temperature during the sintering process, without adding reducing agent；(3C specific discharge capacity reaches 151 mAh g to redox graphene/carbon coating/composite ferric lithium phosphate material conductivity with higher, lithium ion diffusion rate and the excellent high rate performance of the method for the present invention preparation‑1)。
Description
Technical field
The present invention relates to technical field of lithium ion, especially a kind of redox graphene/carbon coating/LiFePO4
The preparation method of composite material.
Background technique
Gradually deficient and its caused environment of the progress of development and science and technology although as society, fossil fuel is dirty
Dye problem is got worse.Therefore, in order to seek safe and healthy, sustainable development, energy storage matched with its for new energy
The exploitation of facility is risen therewith.
Wherein, lithium ion battery due to high-energy density, high efficiency and it is light the advantages that become most important one storage
One of energy device.And the performance and cost of electrode material of lithium battery a possibility that directly affecting its business application.Science and technology
Be constantly progressive need electrode material have better rate charge-discharge performance, better cyclical stability, lower cost.
Olivine-type LiFePO4 is due to its high open-circuit voltage (3.45V vs. Li+/ Li), high theoretical capacity (170
mAh g-1), low cost, stable structure, the advantages such as safety and environmental protection be considered as most promising anode material of lithium battery
One of.However, capacity and short charging time when being more importantly safety, high-power output in practical application.In this side
Face, the low conductivity (10 that olivine-type LiFePO4 is shown-10-10-9 S cm-1) and lesser lithium ion diffusion rate (10-16-10-14 cm2 s-1) largely limit its application in terms of anode material for lithium-ion batteries.Low conductivity be by
Lead to the shortage of mixed valence in the low solubility of LiFePO4 and ferric phosphate.And low Li+Diffusion rate is due to Li+Only edge
[010] face forms the shared LiO in side6Octahedron results in Li+It one-dimensional can only spread.Therefore, it is next to seek a kind of reasonable method
Improve its low conductance and low lithium ion diffuses into for the research direction of current mainstream.
Graphene is due to its unique carbon atom sp2The cellular hexagon two-dimensional structure of hybridized orbit composition, makes its tool
There are theoretical specific surface area (2630 m of superelevation2 g-1) and carrier mobility high at room temperature (~ 10 000 cm2 V-1 s-1)。
Currently, having had quite a few research shows that graphene and the compound material of LiFePO4 are for improving LiFePO4
There is positive effect in terms of low conductivity and low lithium ion diffusion rate, and improve energy-storage property and stability.But directly
Inevitably there is a problem of that mixing is uneven and later period finished product is easy to reunite using graphene mixing.
Summary of the invention
It is an object of the invention to overcome the deficiencies of the prior art and provide a kind of redox graphene/carbon coating/phosphoric acid
The preparation method of iron lithium composite material solves current graphene and LiFePO4 mixing is uneven and later period agglomeration traits, preparation have
There is the composite material of higher energy storage and stability, can be used for making anode material for lithium-ion batteries.
To achieve the above object, the invention adopts the following technical scheme:
A kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method, comprising the following steps:
S1, expanded graphite is prepared into graphene oxide dispersion by Hummers method；
S2, ascorbic acid, lithium carbonate and ferric phosphate are sequentially added in graphene oxide dispersion, be sufficiently mixed grinding, it is spraying
It is dry, obtain mixed powder；
S3, mixed powder is subjected in the tube-type atmosphere furnace for being connected with inert gas step-up temperature sintering, obtains oxygen reduction fossil
Black alkene/carbon coating/composite ferric lithium phosphate material.
Further, the graphene oxide in dispersion liquid shared mass fraction be 1-10 ‰, the ascorbic acid,
Mass fraction shared in total mixed liquor is respectively 2-8%, 5-15% and 25%-45% respectively for lithium carbonate and ferric phosphate.
Further, the heating rate of the tube-type atmosphere furnace is 2-10 DEG C/min, and the step-up temperature was divided into for three stages, the
One stage from room temperature to 150 DEG C, kept the temperature 30min；Second stage is warming up to 300 DEG C from 150 DEG C, keeps the temperature 30min；Third
Stage is warming up to 600-1100 DEG C, after the completion of phase III heating from 300 DEG C, Isothermal sinter 5-15 h.
Further, the inert gas that the tube-type atmosphere furnace is passed through is one of nitrogen, helium or argon gas, inert gas
Flow velocity be 50-100 ml/min.
Beneficial effects of the present invention are as follows: the present invention is based on industrial processes, simple to operation, and sintering feed can be direct
It is used as positive electrode, directly applies to lithium ion battery.Redox graphene/carbon coating/composite ferric lithium phosphate material,
Make remaining several object by the oxygen-containing functional group and the bigger serface of itself of surface of graphene oxide functionalization abundant
Material can be with uniform adsorption, so as to avoid mixing unevenness and later period agglomeration traits；Improved using graphene oxide dispersibility and
Interaction between enhancing other raw materials, then directly avoid addition reducing agent by thermal reduction and restore, by graphite oxide
Without destroying the structure of material while alkene is reduced to redox graphene, solves the problems, such as graphene reunion, enhance
Electrical conductance and lithium ion transport rate.Redox graphene/carbon coating/LiFePO4 composite wood made from the method for the present invention
Material has high rate performance outstanding, and 3C specific discharge capacity is up to 151 mAh g-1, for promoting the forthright again of lithium ion battery
It can be of great significance with cyclical stability.
Detailed description of the invention
Fig. 1 is that the TEM for the graphene oxide that the embodiment of the present invention 1 is prepared by Hummers method schemes, it can be seen that system in figure
The graphene oxide layer obtained is thin, and granularity is micron level；
Fig. 2 and Fig. 3 is redox graphene/carbon coating/composite ferric lithium phosphate material SEM prepared by the embodiment of the present invention 1
Figure, it can be seen that redox graphene and carbon-coated LiFePO 4 for lithium ion batteries success are compound from scanning electron microscope (SEM) photograph；
Fig. 4 is redox graphene/carbon coating/composite ferric lithium phosphate material high rate performance prepared by the embodiment of the present invention 1
Figure, as can be seen from the figure composite material of the invention efficiency for charge-discharge under the conditions of 3C is higher than 98%, and table first goes out good multiplying power
Charge-discharge performance；
Fig. 5 is redox graphene/carbon coating/composite ferric lithium phosphate material of the preparation of the embodiment of the present invention 1 in different multiplying
Under charging and discharging curve figure；The composite material under the conditions of 0.2C gram volume more than 160 mAh g-1, gram volume under the conditions of 3C
Performance still reaches 148 mAh g-1, show high capacity and play.
Specific embodiment
The present invention will be further described With reference to embodiment:
Embodiment 1
A kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method, comprising the following steps:
S1, by expanded graphite by Hummers method: pre-oxidation, oxidation, removing after, centrifugation dispel unstripped graphite, then lead to
It crosses dilute hydrochloric acid and remaining foreign ion is removed in deionized water washing, and wash to neutrality, deionized water is added according to the solid content measured
Dilution, is configured to the graphene oxide dispersion that graphene oxide mass fraction is 5 ‰, and the TEM of graphene oxide schemes such as Fig. 1 institute
Show.
S2, ascorbic acid, lithium carbonate and ferric phosphate are sequentially added in 5 ‰ graphene oxide dispersion, be sufficiently mixed
Grinding.Wherein, it is 3%, 6%, 25% that ascorbic acid, lithium carbonate and ferric phosphate account for the mass fraction of total mixed liquor respectively, spraying dry
It is dry, obtain mixed powder.
S3, mixed powder is subjected to step-up temperature sintering in the tube-type atmosphere furnace of nitrogen atmosphere, wherein the temperature rise period point
For three phases, the first stage from room temperature to 150 DEG C, keeps the temperature 30 min；Second stage is from 150 DEG C to 300 DEG C, heat preservation 30
min；Phase III is warming up to 800 DEG C, Isothermal sinter 8h from 300 DEG C, obtains redox graphene/carbon coating/ferric phosphate
Lithium composite material (it characterizes as shown in Figures 2 and 3).The heating rate in each stage of tube-type atmosphere furnace is 5 DEG C/min, is passed through
Nitrogen flow rate is 50mL/min.
Lithium ion battery is prepared using obtained composite material as positive electrode, the lithium ion battery of preparation carries out constant current and fills
Discharge test.
The production method of electrode are as follows: by electrode material, Ketjen black and polyvinylidene fluoride according to mass ratio 8:1:1 in
Mixed pulp in N-Methyl pyrrolidone, and by slurry be coated in aluminium foil on, drying, be sliced preparation work electrode, combination electrode
Material surface density is 1mg/cm2。
Test method are as follows: lithium piece selects the carbon of 1 M lithium hexafluoro phosphate as reference electrode, electrolyte in lithium ion half-cell
Vinyl acetate/dimethyl carbonate (mass ratio 1:1) mixed liquor；Battery charging and discharging is tested on Arbin BT-1 battery test system
Carry out, voltage range select 2.0-4.2V (vs. Li+/Li), charge-discharge magnification according to nanocomposite Mass Calculation.
Test result is referred to shown in Fig. 4-Fig. 5.
Embodiment 2
A kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method, comprising the following steps:
S1, by expanded graphite by Hummers method: pre-oxidation, oxidation, removing after, centrifugation dispel unstripped graphite, then lead to
It crosses dilute hydrochloric acid and remaining foreign ion is removed in deionized water washing, and wash to neutrality, deionized water is added according to the solid content measured
Dilution is configured to the graphene oxide dispersion that graphene oxide mass fraction is 8 ‰.
S2, ascorbic acid, lithium carbonate and ferric phosphate are sequentially added in 8 ‰ graphene oxide dispersion, be sufficiently mixed
Grinding.Wherein, it is 6%, 10%, 30% that ascorbic acid, lithium carbonate and ferric phosphate account for the mass fraction of total mixed liquor respectively, spraying dry
It is dry, obtain mixed powder.
S3, mixed powder is subjected to step-up temperature sintering in the tube-type atmosphere furnace of helium atmosphere, wherein the temperature rise period point
For three phases, the first stage from room temperature to 150 DEG C, keeps the temperature 30 min；Second stage is from 150 DEG C to 300 DEG C, heat preservation 30
min；Phase III is warming up to 900 DEG C, Isothermal sinter 10h from 300 DEG C, obtains redox graphene/carbon coating/ferric phosphate
Lithium composite material.The heating rate in each stage of tube-type atmosphere furnace is 7 DEG C/min, and being passed through helium flow velocity is 60mL/min.
Redox graphene prepared by embodiment 2/carbon coating/composite ferric lithium phosphate material electric performance test can join
Examine embodiment 1.
Embodiment 3
A kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method, comprising the following steps:
S1, by expanded graphite by Hummers method: pre-oxidation, oxidation, removing after, centrifugation dispel unstripped graphite, then lead to
It crosses dilute hydrochloric acid and remaining foreign ion is removed in deionized water washing, and wash to neutrality, deionized water is added according to the solid content measured
Dilution is configured to the graphene oxide dispersion that graphene oxide mass fraction is 1 ‰.
S2, ascorbic acid, lithium carbonate and ferric phosphate are sequentially added in 1 ‰ graphene oxide dispersion, be sufficiently mixed
Grinding.Wherein, it is 2%, 5%, 40% that ascorbic acid, lithium carbonate and ferric phosphate account for the mass fraction of total mixed liquor respectively, spraying dry
It is dry, obtain mixed powder.
S3, mixed powder is subjected to step-up temperature sintering in the tube-type atmosphere furnace of argon atmosphere, wherein the temperature rise period point
For three phases, the first stage from room temperature to 150 DEG C, keeps the temperature 30 min；Second stage is from 150 DEG C to 300 DEG C, heat preservation 30
min；Phase III is warming up to 600 DEG C, Isothermal sinter 15h from 300 DEG C, obtains redox graphene/carbon coating/ferric phosphate
Lithium composite material.The heating rate in each stage of tube-type atmosphere furnace is 2 DEG C/min, and being passed through argon gas flow velocity is 80mL/min.
Redox graphene prepared by embodiment 3/carbon coating/composite ferric lithium phosphate material electric performance test can join
Examine embodiment 1.
Embodiment 4
A kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method, comprising the following steps:
S1, by expanded graphite by Hummers method: pre-oxidation, oxidation, removing after, centrifugation dispel unstripped graphite, then lead to
It crosses dilute hydrochloric acid and remaining foreign ion is removed in deionized water washing, and wash to neutrality, deionized water is added according to the solid content measured
Dilution is configured to the graphene oxide dispersion that graphene oxide mass fraction is 10 ‰.
S2, ascorbic acid, lithium carbonate and ferric phosphate are sequentially added in 10 ‰ graphene oxide dispersion, be sufficiently mixed
Grinding.Wherein, it is 8%, 15%, 45% that ascorbic acid, lithium carbonate and ferric phosphate account for the mass fraction of total mixed liquor respectively, spraying dry
It is dry, obtain mixed powder.
S3, mixed powder is subjected to step-up temperature sintering in the tube-type atmosphere furnace of nitrogen atmosphere, wherein the temperature rise period point
For three phases, the first stage from room temperature to 150 DEG C, keeps the temperature 30 min；Second stage is from 150 DEG C to 300 DEG C, heat preservation 30
min；Phase III is warming up to 1100 DEG C, Isothermal sinter 5h from 300 DEG C, obtains redox graphene/carbon coating/ferric phosphate
Lithium composite material.The heating rate in each stage of tube-type atmosphere furnace is 10 DEG C/min, and being passed through nitrogen flow rate is 100mL/min.
Redox graphene prepared by embodiment 4/carbon coating/composite ferric lithium phosphate material electric performance test can join
Examine embodiment 1.
Embodiment described above only describe the preferred embodiments of the invention, not to model of the invention
It encloses and is defined, without departing from the spirit of the design of the present invention, those of ordinary skill in the art are to technical side of the invention
The various changes and improvements that case is made should all fall into the protection scope that claims of the present invention determines.
Claims (4)
1. a kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation method, which is characterized in that including with
Lower step:
S1, expanded graphite is prepared into graphene oxide dispersion by Hummers method；
S2, ascorbic acid, lithium carbonate and ferric phosphate are sequentially added in graphene oxide dispersion, be sufficiently mixed grinding, it is spraying
It is dry, obtain mixed powder；
S3, mixed powder is subjected in the tube-type atmosphere furnace for being connected with inert gas step-up temperature sintering, obtains oxygen reduction fossil
Black alkene/carbon coating/composite ferric lithium phosphate material.
2. a kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation side according to claim 1
Method, which is characterized in that the graphene oxide in dispersion liquid shared mass fraction be 1-10 ‰, the ascorbic acid,
Mass fraction shared in total mixed liquor is respectively 2-8%, 5-15% and 25%-45% respectively for lithium carbonate and ferric phosphate.
3. a kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation side according to claim 1
Method, which is characterized in that the heating rate of the tube-type atmosphere furnace is 2-10 DEG C/min, and the step-up temperature was divided into for three stages, the
One stage from room temperature to 150 DEG C, kept the temperature 30min；Second stage is warming up to 300 DEG C from 150 DEG C, keeps the temperature 30min；Third
Stage is warming up to 600-1100 DEG C, after the completion of phase III heating from 300 DEG C, Isothermal sinter 5-15 h.
4. a kind of redox graphene/carbon coating/composite ferric lithium phosphate material preparation side according to claim 1
Method, which is characterized in that the inert gas that the tube-type atmosphere furnace is passed through is one of nitrogen, helium or argon gas, inert gas
Flow velocity be 50-100 ml/min.
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Cited By (1)
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| CN110400919A (en) * | 2019-06-21 | 2019-11-01 | 南京信息职业技术学院 | A kind of preparation process preparing composite ferric lithium phosphate material based on chemical in situ sedimentation |
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