CN105406035B - A kind of preparation method of regular octahedron type ferric phosphate/graphene oxide presoma - Google Patents
A kind of preparation method of regular octahedron type ferric phosphate/graphene oxide presoma Download PDFInfo
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- CN105406035B CN105406035B CN201510727167.2A CN201510727167A CN105406035B CN 105406035 B CN105406035 B CN 105406035B CN 201510727167 A CN201510727167 A CN 201510727167A CN 105406035 B CN105406035 B CN 105406035B
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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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- 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
A kind of preparation method of regular octahedron type ferric phosphate/graphene oxide presoma of the present invention, graphene oxide is put into ultrasonic field ultrasonic, adds solution of ferrous chloride, the mass ratio of ferro element and graphene oxide is 1 ~ 2:12.5, deionized water and absolute ethyl alcohol are added in the case of stirring, H is added dropwise during concussion2O2, obtain being dispersed with the iron salt solutions of graphene oxide;Then it is added dropwise phosphate solution in ultrasound, Fe in reaction mixture:P mol ratio=1:2 ~ 2.5, by reaction mixture in ultrasonic field it is ultrasonic, be then loaded into bag filter, solution after the completion of dialysis is added into reactor, reacted in 150 ~ 200 DEG C of baking oven, then reaction product is subjected to freeze-drying process, obtain regular octahedron type ferric phosphate/graphene oxide presoma.The tap density for the composite positive pole that the method for the present invention obtains is higher, and specific capacity height, good cycle, high rate performance are excellent.
Description
Technical field
The invention belongs to materialogy field, is related to a kind of anode material for lithium-ion batteries, specifically a kind of positive octahedral
The preparation method of build ferric phosphate/graphene oxide presoma.
Background technology
Technological revolution and intelligent, mobile electronic equipment fast development with new energy field, people are for storage
Can and electronic product etc. battery research and development attention rate more and more higher.
At present, lithium ion battery is because high with voltage, and energy density is big, and good cycle, self discharge is small, memoryless effect
Should, the advantages that working range is wide and be widely used in the fields such as notebook computer, digital camera, electronic instrument, mobile phone;
In recent years, lithium ion battery is widely applied to the Large Copacity such as electric bicycle, electric automobile, Aero-Space energy storage device neck again
Domain.Wherein, LiFePO 4 material is used as current these Large Copacities electricity because having many advantages, such as that other positive electrodes do not possess
The preferred positive electrode in pond.Such as:Higher voltage platform(3.4-3.5V), higher theoretical capacity(For 170mAh/g), follow
Ring performance is good(The LiFePO synthesized under optimal conditions4It is recyclable more than 2000 times), stability is good, high-temperature behavior is good, security
Can it is good, building-up process is simple, environmentally friendly, the features such as nontoxic, abundant raw material.
The energy is the important substance basis that human society is depended on for existence and development.With economic and society continuous development,
The world is also being continuously increased to the demand of the energy.In the case where nowadays global warming and ecological environment constantly deteriorate,
Lithium ion battery is also just of increased attention as a kind of green energy resource.It is but only due to LiFePO4 structure
Characteristic has obstructed the conduction of electronics so that the electronic conductivity very low (10 of LiFePO4-9 S·cm -1), cause its electrochemistry
Can be poor.And graphene is a kind of new material of carbon family very popular in recent years, its thickness only has 0.335nm, graphene and
Its derivative graphene oxide has good physics and chemical property, has huge surface area and abundant functional group, tool
There are the properties such as excellent mechanics, electricity, optics, calorifics.Become good absorption, electrochemical material.So can be by stone
The excellent electric conductivity of the black alkene chemical property special with LiFePO4 combines.
The content of the invention
For above-mentioned technical problem of the prior art, the invention provides a kind of regular octahedron type ferric phosphate/oxidation stone
The preparation method of black alkene presoma, the preparation method solution of described this regular octahedron type ferric phosphate/graphene oxide presoma
Determined LiFePO4 of the prior art electronic conductivity it is low, cause the bad technical problem of its chemical property.
The invention provides a kind of preparation method of regular octahedron type ferric phosphate/graphene oxide presoma, including it is following
Step:
(1)One prepares the step of being dispersed with the iron salt solutions of graphene oxide;
Graphene oxide is put into ultrasound in ultrasonic field, the concentration of described graphene oxide is 3 ~ 8mg/ml, adds chlorine
Change ferrous iron solution, the concentration of described solution of ferrous chloride be 0.1 ~ 0.5g/ml, in the case of stirring add deionized water with
Absolute ethyl alcohol, graphene oxide, ferrous chloride aqueous solution, the material ratio of deionized water and absolute ethyl alcohol are 10ml:2-4ml:
40ml:52-54ml, concussion, the H that mass percent concentration is 20 ~ 40% is added dropwise during concussion2O2, ferro element and H2O2Rub
You are than being 1:1 ~ 2, obtain being dispersed with the iron salt solutions of graphene oxide;
(2)One the step of preparing regular octahedron type ferric phosphate/graphene oxide presoma;
By step(1)Phosphate solution is added dropwise in ultrasound for the iron salt solutions for being dispersed with graphene oxide of middle preparation, instead
Answer Fe in mixed liquor:P mol ratio=1:2 ~ 2.5, the pH value for adjusting reaction mixture is 3 ~ 5, by reaction mixture in ultrasonic field
Stood after middle ultrasound, be then loaded into bag filter, dialysed 3 ~ 5 days in deionized water, the solution after the completion of dialysis is added
Reactor, 150 ~ 200℃Baking oven in react 10 ~ 20h, then reaction product is subjected to freeze-drying process, obtain positive octahedral
Build ferric phosphate/graphene oxide presoma.
Further, described ultrasonic field will be kept under low-temperature condition, it is impossible to because it is ultrasonic the reason for cause water temperature to rise,
Because the inlet and outlet water-carrying capacity of ultrasonic instrument is difficult to control, it is possible to ice cube is added in ultrasonic field to limit in water temperature
Rise.
Further, described phosphate solution is biphosphate ammonia solution, the quality of described biphosphate ammonia solution
Percent concentration is 20 ~ 60%.
Further, concentration is used to adjust the pH value of solution for 25% ammonia spirit.
Further, described H2O2Rate of addition must be slow, and ceaselessly shakes solution.
Further, to strengthen dialysis-effect, magneton is added in the container equipped with deionized water on magnetic stirring apparatus
It is stirred continuously, and repeatedly changes deionized water.
Of the invention first using frerrous chloride, graphene oxide and hydrogen peroxide as raw material, ultrasonic side is slowly added dropwise normal temperature below
Ammonium dihydrogen phosphate, 180 after a couple of days of dialysing℃Lower hydro-thermal reaction 12hFreeze-drying process is carried out afterwards obtains the compound lithium of graphene
Ion battery composite positive pole ideal presoma FePO4。
The regular octahedron type nanoscale composite positive pole that this preparation method is prepared, fully by the excellent conduction of graphene
Performance applications are in the preferable presoma FePO of LiFePO 4 of anode material4Synthesis in, to solve existing positive pole material phosphoric acid iron
The preferable presoma FePO of lithium4The deficiency and lithium iron phosphate positive material poorly conductive of fabricating technology, poor circulation
Problem.
The present invention compares with prior art, and its technological progress is significant.Present invention process process is simple, strong operability,
Equipment investment is few, and production cost is low, and the tap density of gained graphene modified phosphate iron lithium/carbon composite material is higher, specific capacity
Height, good cycle, high rate performance are excellent, are suitable for electrokinetic cell application field.
Brief description of the drawings
Fig. 1 is the SEM figures of the composite positive pole of the embodiment of the present invention 1.
Fig. 2 is the SEM figures of the composite positive pole of the embodiment of the present invention 2.
Fig. 3 is the SEM figures of the composite positive pole of the embodiment of the present invention 3.
Embodiment
Technical scheme is further described with reference to specific embodiment, but the present invention is not limited to
Following embodiments.
Embodiment 1
The graphene oxide made from improved Hummers methods is put into 30 min of ultrasound in ultrasonic field, then added wherein
Enter a certain amount of solution of ferrous chloride prepared, deionized water and absolute ethyl alcohol are added in the case of stirring so that mass concentration
For 5mg ml-1Graphene oxide:Mass concentration is 0.2 g ml-1Ferrous chloride aqueous solution:Deionized water:Absolute ethyl alcohol
For 10ml:2-4ml:40ml:52-54ml ratio, is constantly shaken, and is slowly added dropwise during concussion slightly excessive
30%H2O2, ferro element and H2O2Mol ratio be 1:1 ~ 2, this has just obtained the iron salt solutions for being dispersed with graphene oxide, continues
The biphosphate ammonia solution prepared is added dropwise in ultrasound.Fe: P mol ratio=1 in its reaction mixture: 2, regulation reaction is mixed
The pH to 3 ~ 5 of liquid is closed, reaction mixture is stood into a period of time in normal temperature ultrasonic field after ultrasound, is then loaded into bag filter
Dialyse 5 days in deionized water, to strengthen dialysis-effect, magneton is added in the container equipped with deionized water in magnetic stirring apparatus
On be stirred continuously, and repeatedly change deionized water.Solution after the completion of dialysis is loaded into reactor, 150℃Condition
12 are reacted in baking ovenh, then reaction product is subjected to freeze-drying process, obtain the compound anode material for lithium-ion batteries of graphene
The preferable presoma regular octahedron type FePO of LiFePO44。
Embodiment 2
The graphene oxide made from improved Hummers methods is put into 30 min of ultrasound in ultrasonic field, then added wherein
Enter a certain amount of solution of ferrous chloride prepared, deionized water and absolute ethyl alcohol are added in the case of stirring so that mass concentration
For 5mg ml-1Graphene oxide:Mass concentration is 0.2 g ml-1Ferrous chloride aqueous solution:Deionized water:Absolute ethyl alcohol
For 10ml:2-4ml:40ml:52-54ml ratio, is constantly shaken, and is slowly added dropwise during concussion slightly excessive
30%H2O2, ferro element and H2O2Mol ratio be 1:1 ~ 2, this has just obtained the iron salt solutions for being dispersed with graphene oxide, continues
The biphosphate ammonia solution prepared is added dropwise in ultrasound.Fe: P mol ratio=1 in its reaction mixture: 2, regulation reaction is mixed
The pH to 3 ~ 5 of liquid is closed, reaction mixture is stood into a period of time in normal temperature ultrasonic field after ultrasound, is then loaded into bag filter
Dialyse 4 days in deionized water, to strengthen dialysis-effect, magneton is added in the container equipped with deionized water in magnetic stirring apparatus
On be stirred continuously, and repeatedly change deionized water.Solution after the completion of dialysis is loaded into reactor, 200℃Condition
12 are reacted in baking ovenh, then reaction product is subjected to freeze-drying process, obtain the compound anode material for lithium-ion batteries of graphene
The preferable presoma regular octahedron type FePO of LiFePO44。
Embodiment 3
The graphene oxide made from improved Hummers methods is put into 30 min of ultrasound in ultrasonic field, then added wherein
Enter a certain amount of solution of ferrous chloride prepared, deionized water and absolute ethyl alcohol are added in the case of stirring so that mass concentration
For 5mg ml-1Graphene oxide:Mass concentration is 0.2 g ml-1Ferrous chloride aqueous solution:Deionized water:Absolute ethyl alcohol
For 10ml:2-4ml:40ml:52-54ml ratio, is constantly shaken, and is slowly added dropwise during concussion slightly excessive
30%H2O2, ferro element and H2O2Mol ratio be 1:1 ~ 2, this has just obtained the iron salt solutions for being dispersed with graphene oxide, continues
The biphosphate ammonia solution prepared is added dropwise in ultrasound.Fe: P mol ratio=1 in its reaction mixture: 2.5, regulation reaction
The pH of mixed liquor to 3 ~ 5, reaction mixture is stood into a period of time in normal temperature ultrasonic field after ultrasound, is then loaded into dialysis
Bag is dialysed 3 days in deionized water, and to strengthen dialysis-effect, magneton is added in the container equipped with deionized water in magnetic agitation
It is stirred continuously on device, and repeatedly changes deionized water.Solution after the completion of dialysis is loaded into reactor, 180℃Condition
Baking oven in react 12h, then reaction product is subjected to freeze-drying process, obtain the compound lithium ion cell positive material of graphene
Expect the preferable presoma regular octahedron type FePO of LiFePO44。
Claims (3)
1. a kind of preparation method of regular octahedron type ferric phosphate/graphene oxide presoma, it is characterised in that comprise the following steps:
(1)One prepares the step of being dispersed with the iron salt solutions of graphene oxide;
Graphene oxide is put into ultrasound in ultrasonic field, the concentration of described graphene oxide is 3 ~ 8mg/ml, adds protochloride
Ferrous solution, the concentration of described solution of ferrous chloride is 0.1 ~ 0.5g/ml, and deionized water and anhydrous is added in the case of stirring
Ethanol, graphene oxide, ferrous chloride aqueous solution, the material ratio of deionized water and absolute ethyl alcohol are 10ml:2-4ml:40ml:
52-54ml, concussion, the H that mass percent concentration is 20 ~ 40% is added dropwise during concussion2O2, ferro element and H2O2Mol ratio be
1:1 ~ 2, obtain being dispersed with the iron salt solutions of graphene oxide;
(2)One the step of preparing regular octahedron type ferric phosphate/graphene oxide presoma;
By step(1)Phosphate solution is added dropwise in ultrasound for the iron salt solutions for being dispersed with graphene oxide of middle preparation, and reaction is mixed
Close Fe in liquid:P mol ratio=1:2 ~ 2.5, the pH value for adjusting reaction mixture is 3 ~ 5, and reaction mixture is surpassed in ultrasonic field
Stood after sound, be then loaded into bag filter, dialysed 3 ~ 5 days in deionized water, the solution after the completion of dialysis is added into reaction
Kettle, 10 ~ 20h is reacted in 150 ~ 200 DEG C of baking oven, then reaction product is subjected to freeze-drying process, obtain regular octahedron type
Ferric phosphate/graphene oxide presoma.
2. a kind of preparation method of regular octahedron type ferric phosphate/graphene oxide presoma according to claim 1, it is special
Sign is:Described phosphate solution is ammonium dihydrogen phosphate, the mass percent concentration of described ammonium dihydrogen phosphate
For 20 ~ 60%.
3. a kind of preparation method of regular octahedron type ferric phosphate/graphene oxide presoma according to claim 1, it is special
Sign is:During dialysis, the deionized water of 2 ~ 5 times is at least changed.
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CN109037616A (en) * | 2018-07-10 | 2018-12-18 | 桂林理工大学 | Change the method for preparing high performance LiFePO4/three-dimensional graphene composite material by the morphology and size of ferric phosphate |
CN113851618B (en) * | 2021-08-10 | 2023-06-23 | 桂林理工大学 | Method for preparing high-performance ferric phosphate/graphene composite anode material by utilizing hydrochloric acid leaching solution of iron vitriol slag and application of high-performance ferric phosphate/graphene composite anode material |
CN115520845B (en) * | 2022-09-02 | 2023-12-26 | 衢州华友钴新材料有限公司 | Regular octahedron ferric phosphate and preparation method thereof, lithium iron phosphate positive electrode material and lithium iron phosphate battery |
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CN102148371A (en) * | 2011-03-03 | 2011-08-10 | 上海大学 | Graphene/phosphoric acid iron-lithium composite material with sandwich structure and preparation method thereof |
CN102403501A (en) * | 2011-11-24 | 2012-04-04 | 上海电力学院 | Method for preparation of cathode material spherical FePO4 of lithium-ion battery |
CN102683697A (en) * | 2012-05-14 | 2012-09-19 | 中南大学 | Preparation method of graphene-based LiFePO4/C composite material |
CN103311543A (en) * | 2012-12-10 | 2013-09-18 | 上海电力学院 | Anode material hydroxyl iron phosphate for lithium ion batteries and preparation method thereof |
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Publication number | Priority date | Publication date | Assignee | Title |
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CN102148371A (en) * | 2011-03-03 | 2011-08-10 | 上海大学 | Graphene/phosphoric acid iron-lithium composite material with sandwich structure and preparation method thereof |
CN102403501A (en) * | 2011-11-24 | 2012-04-04 | 上海电力学院 | Method for preparation of cathode material spherical FePO4 of lithium-ion battery |
CN102683697A (en) * | 2012-05-14 | 2012-09-19 | 中南大学 | Preparation method of graphene-based LiFePO4/C composite material |
CN103311543A (en) * | 2012-12-10 | 2013-09-18 | 上海电力学院 | Anode material hydroxyl iron phosphate for lithium ion batteries and preparation method thereof |
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