CN109256547A - A kind of preparation method of porous graphene-lithium iron phosphate positive material - Google Patents
A kind of preparation method of porous graphene-lithium iron phosphate positive material Download PDFInfo
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- CN109256547A CN109256547A CN201811034040.2A CN201811034040A CN109256547A CN 109256547 A CN109256547 A CN 109256547A CN 201811034040 A CN201811034040 A CN 201811034040A CN 109256547 A CN109256547 A CN 109256547A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H—ELECTRICITY
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- 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
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- 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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- 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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Abstract
The invention discloses a kind of preparation methods of porous graphene-lithium iron phosphate positive material, first by crystalline flake graphite through Hummers method oxidation after, dry, grind and be put into again expansion process in high temperature process furnances, then it is removed through polyvinylpyrrolidonesolution solution ultrasound, porous graphene solution obtained is sufficiently mixed grinding with suitable glucose, lithium carbonate, ferric phosphate, dries again, obtain powder object, final powder object heats up sintering under an inert atmosphere to get porous graphene-lithium iron phosphate positive material.Operation of the present invention is simple, easy to industrialized production, directly applies to lithium ion battery for moulding material prepared by the present invention as positive electrode, specific discharge capacity is high, and has excellent high rate performance.
Description
Technical field
The present invention relates to technical field of lithium ion, specifically a kind of porous graphene-lithium iron phosphate positive material
Preparation method.
Background technique
Since petroleum resources are increasingly depleted, environmental pollution is serious, and the requirement for controlling CO2 emissions is higher and higher, seeks
Energy substitution fossil fuel of looking for novelty is applied to automobile and causes extensive concern, such as using lithium ion battery with high energy density
Mixed power electric car and pure electric automobile are considered as the suitable replacements of substitute fossil fuels automobile.Positive electrode is more
Pursuit be height ratio capacity and excellent high rate performance, and LiFePO4 is being applied to height as the lithium ion battery of positive electrode
Electric tool, hybrid power and the pure electric automobile of power have excellent security performance, high capacity (170 mAhg-1), therefore
It is considered to have the positive electrode of development prospect.However low conductivity (10-9 S cm-1) and lithium ion diffusion rate (10-15–10-12 cm2 s-1) seriously hinder the development of LiFePO4.
Graphene is a kind of planar material being made of carbon atom with sp2 hybridized orbit, with excellent physico
Performance is learned, research finds the composite positive pole that LiFePO4 and graphene are formed, greatly improves the conductivity of electrode material,
And the graphene of porous structure and LiFePO4 are compound, can not only improve material electric conductivity also and can satisfy lithium ion and quickly move
The needs of shifting, therefore porous graphene/composite ferric lithium phosphate material is steady to the circulation for improving battery as lithium ion anode material
It is qualitative and forthright again have highly important effect.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation sides of porous graphene-lithium iron phosphate positive material
Method, the porous graphene-lithium iron phosphate positive material being prepared has excellent high rate performance, and specific discharge capacity is high.
The technical solution of the present invention is as follows:
A kind of preparation method of porous graphene-lithium iron phosphate positive material, has specifically included following steps:
(1), a certain amount of crystalline flake graphite is added suitable potassium hydroxide solution and dries progress again after the oxidation of Hummers method
After grinding, be put into expansion process in high temperature process furnances, then it is washed after, suitable polyvinylpyrrolidonesolution solution ultrasound is added
Porous graphene solution is made in removing；
(2), porous graphene solution made from step (1) is sufficiently mixed with suitable glucose, lithium carbonate, ferric phosphate and is ground
Mill is dried again, obtains powder object, and final powder object heats up under an inert atmosphere to be sintered to get porous graphene-LiFePO4 just
Pole material.
The concentration of the potassium hydroxide solution is 0.1-1mol/L；Temperature in the high temperature process furnances is set as
700-1000℃；The concentration of the polyvinylpyrrolidonesolution solution is 0.01-1mol/L.
The mass fraction that the glucose accounts for porous graphene solution is 1-10%, and the lithium carbonate accounts for porous graphite
The mass fraction of alkene solution is 5-20%, and the mass fraction that the ferric phosphate accounts for porous graphene solution is 10-50%.
The parameter of the sintering that heats up under an inert atmosphere is: heating rate 2-10oC/min, sintering temperature is in 500-
1000oC, sintering time 2-15 hours；The inert atmosphere is at least one of nitrogen, helium, argon gas.
The concentration of the potassium hydroxide solution is 0.1mol/L；Temperature in the high temperature process furnances is set as 700
℃；The concentration of the polyvinylpyrrolidonesolution solution is 0.1mol/L.
The mass fraction that the glucose accounts for porous graphene solution is 2.3%, and the lithium carbonate accounts for porous graphene
The mass fraction of solution is 5%, and the mass fraction that the ferric phosphate accounts for porous graphene solution is 20%.
The parameter of the sintering that heats up under an inert atmosphere is: heating rate 5oC/min, sintering temperature is 700oC is burnt
The knot time 12 hours.
Advantages of the present invention:
Operation of the present invention is simple, easy to industrialized production, directly applies using moulding material prepared by the present invention as positive electrode
In lithium ion battery, 3C specific discharge capacity is high, and has excellent high rate performance.
Detailed description of the invention
Fig. 1 is TEM figure of the crystalline flake graphite after the oxidation of Hummers method in the embodiment of the present invention 2;
Fig. 2 is SEM of the porous graphene-lithium iron phosphate positive material that is prepared of the embodiment of the present invention 2 under 1 μm of scale
Figure;
Fig. 3 is SEM of the porous graphene-lithium iron phosphate positive material that is prepared of the embodiment of the present invention 2 under 200nm scale
Figure;
Fig. 4 is porous graphene-lithium iron phosphate positive material high rate performance figure that the embodiment of the present invention 2 is prepared.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
A kind of preparation method of porous graphene-lithium iron phosphate positive material, has specifically included following steps:
(1), the potassium hydroxide solution of appropriate 0.5mol/L is added again after the oxidation of Hummers method in the crystalline flake graphite of 0.25kg
After drying is ground, it is put into expansion process in 1000 DEG C of high temperature process furnances, then after deionized water is washed, is added appropriate
Polyvinylpyrrolidone (PVP) the solution ultrasound of 0.05mol/L is removed, and porous graphene solution is made；
(2), porous graphene solution made from step (1) is sufficiently mixed with suitable glucose, lithium carbonate, ferric phosphate and is ground
Mill is dried again, obtains powder object, and final powder object heat up sintering under 700 DEG C of nitrogen atmospheres, wherein heating rate for 5 DEG C/
Min is sintered 12h, obtains porous graphene/lithium iron phosphate positive material；Wherein, glucose accounts for the quality of porous graphene solution
Score is 2.3%, and the mass fraction that lithium carbonate accounts for porous graphene solution is 5%, and ferric phosphate accounts for the quality of porous graphene solution
Score is 20%.
Porous graphene/lithium iron phosphate positive material made from embodiment 1 is distinguished in 1C, 2C, 3C multiplying power discharge capacity
It is 155mAh/g, 150mAh/g, 145.2mAh/g.
Embodiment 2
A kind of preparation method of porous graphene-lithium iron phosphate positive material, has specifically included following steps:
(1), the potassium hydroxide solution of appropriate 0.1mol/L is added again after the oxidation of Hummers method in the crystalline flake graphite of 0.25kg
After drying is ground, it is put into expansion process in 800 DEG C of high temperature process furnances, then after deionized water is washed, is added appropriate
Polyvinylpyrrolidone (PVP) the solution ultrasound of 0.1mol/L is removed, and porous graphene solution is made；
(2), porous graphene solution made from step (1) is sufficiently mixed with suitable glucose, lithium carbonate, ferric phosphate and is ground
Mill is dried again, obtains powder object, and final powder object heat up sintering under 700 DEG C of nitrogen atmospheres, wherein heating rate for 5 DEG C/
Min is sintered 12h, obtains porous graphene/lithium iron phosphate positive material；Wherein, glucose accounts for the quality of porous graphene solution
Score is 2.3%, and the mass fraction that lithium carbonate accounts for porous graphene solution is 5%, and ferric phosphate accounts for the quality of porous graphene solution
Score is 20%.
Porous graphene solution prepared by embodiment 2 carries out TEM characterization (see figure 1), porous graphene/LiFePO4 lithium
Ion positive electrode carries out SEM characterization (see Fig. 2 and Fig. 3) and high rate performance characterizes (see figure 4).The system that embodiment 2 is prepared
Standby obtained porous graphene/lithium iron phosphate positive material 1C, 2C, 3C multiplying power discharge capacity be respectively 159.2mAh/g,
154.7mAh/g, 150mAh/g, the specific discharge capacity under 1C multiplying power under charging, 3C multiplying power after electric discharge, 100 circulations are
145.8mAh/g。
Embodiment 3
A kind of preparation method of porous graphene-lithium iron phosphate positive material, has specifically included following steps:
(1), the potassium hydroxide solution of appropriate 0.1mol/L is added again after the oxidation of Hummers method in the crystalline flake graphite of 0.25kg
After drying is ground, it is put into expansion process in 1000 DEG C of high temperature process furnances, then after deionized water is washed, is added appropriate
Polyvinylpyrrolidone (PVP) the solution ultrasound of 0.1mol/L is removed, and porous graphene solution is made；
(2), porous graphene solution made from step (1) is sufficiently mixed with suitable glucose, lithium carbonate, ferric phosphate and is ground
Mill is dried again, obtains powder object, and final powder object heat up sintering under 900 DEG C of nitrogen atmospheres, wherein heating rate for 5 DEG C/
Min is sintered 12h, obtains porous graphene/lithium iron phosphate positive material；Wherein, glucose accounts for the quality of porous graphene solution
Score is 2.3%, and the mass fraction that lithium carbonate accounts for porous graphene solution is 5%, and ferric phosphate accounts for the quality of porous graphene solution
Score is 20%.
Porous graphene/lithium iron phosphate positive material made from embodiment 3 is distinguished in 1C, 2C, 3C multiplying power discharge capacity
It is 140mAh/g, 135.4mAh/g, 116.2mAh/g.
Embodiment 4
A kind of preparation method of porous graphene-lithium iron phosphate positive material, has specifically included following steps:
(1), the potassium hydroxide solution of appropriate 0.1mol/L is added again after the oxidation of Hummers method in the crystalline flake graphite of 0.25kg
After drying is ground, it is put into expansion process in 800 DEG C of high temperature process furnances, then after deionized water is washed, is added appropriate
Polyvinylpyrrolidone (PVP) the solution ultrasound of 0.1mol/L is removed, and porous graphene solution is made；
(2), porous graphene solution made from step (1) is sufficiently mixed with suitable glucose, lithium carbonate, ferric phosphate and is ground
Mill is dried again, obtains powder object, and final powder object heat up sintering under 700 DEG C of nitrogen atmospheres, wherein heating rate for 5 DEG C/
Min is sintered 12h, obtains porous graphene/lithium iron phosphate positive material；Wherein, glucose accounts for the quality of porous graphene solution
Score is 5%, and the mass fraction that lithium carbonate accounts for porous graphene solution is 15%, and ferric phosphate accounts for the quality point of porous graphene solution
Number is 35%.
Porous graphene/lithium iron phosphate positive material made from embodiment 4 is distinguished in 1C, 2C, 3C multiplying power discharge capacity
It is 110.3mAh/g, 101.4mAh/g, 87.9mAh/g.
Embodiment 5
A kind of preparation method of porous graphene-lithium iron phosphate positive material, has specifically included following steps:
(1), the potassium hydroxide solution of appropriate 0.1mol/L is added again after the oxidation of Hummers method in the crystalline flake graphite of 0.25kg
After drying is ground, it is put into expansion process in 800 DEG C of high temperature process furnances, then after deionized water is washed, is added appropriate
Polyvinylpyrrolidone (PVP) the solution ultrasound of 0.1mol/L is removed, and porous graphene solution is made；
(2), porous graphene solution made from step (1) is sufficiently mixed with suitable glucose, lithium carbonate, ferric phosphate and is ground
Mill is dried again, obtains powder object, and final powder object heat up sintering under 700 DEG C of nitrogen atmospheres, wherein heating rate for 5 DEG C/
Min is sintered 4h, obtains porous graphene/lithium iron phosphate positive material；Wherein, glucose accounts for the quality of porous graphene solution
Score is 2.3%, and the mass fraction that lithium carbonate accounts for porous graphene solution is 5%, and ferric phosphate accounts for the quality of porous graphene solution
Score is 20%.
Porous graphene/lithium iron phosphate positive material made from embodiment 5 is distinguished in 1C, 2C, 3C multiplying power discharge capacity
It is 100.6mAh/g, 85.1mAh/g, 60mAh/g.
Embodiment 6
A kind of preparation method of porous graphene-lithium iron phosphate positive material, has specifically included following steps:
(1), the potassium hydroxide solution of appropriate 0.1mol/L is added again after the oxidation of Hummers method in the crystalline flake graphite of 0.25kg
After drying is ground, it is put into expansion process in 800 DEG C of high temperature process furnances, then after deionized water is washed, is added appropriate
Polyvinylpyrrolidone (PVP) the solution ultrasound of 0.1mol/L is removed, and porous graphene solution is made；
(2), porous graphene solution made from step (1) is sufficiently mixed with suitable glucose, lithium carbonate, ferric phosphate and is ground
Mill is dried again, obtains powder object, and final powder object heat up sintering under 700 DEG C of nitrogen atmospheres, wherein heating rate for 10 DEG C/
Min is sintered 4h, obtains porous graphene/lithium iron phosphate positive material；Wherein, glucose accounts for the quality of porous graphene solution
Score is 2.3%, and the mass fraction that lithium carbonate accounts for porous graphene solution is 5%, and ferric phosphate accounts for the quality of porous graphene solution
Score is 20%.
Porous graphene/lithium iron phosphate positive material made from embodiment 5 is distinguished in 1C, 2C, 3C multiplying power discharge capacity
It is 105.6mAh/g, 80.4mAh/g, 57.9mAh/g.
It although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of variations, modification, replacement can be carried out to these embodiments without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (7)
1. a kind of preparation method of porous graphene-lithium iron phosphate positive material, it is characterised in that: specifically included following step
It is rapid:
(1), a certain amount of crystalline flake graphite is added suitable potassium hydroxide solution and dries progress again after the oxidation of Hummers method
After grinding, be put into expansion process in high temperature process furnances, then it is washed after, suitable polyvinylpyrrolidonesolution solution ultrasound is added
Porous graphene solution is made in removing；
(2), porous graphene solution made from step (1) is sufficiently mixed with suitable glucose, lithium carbonate, ferric phosphate and is ground
Mill is dried again, obtains powder object, and final powder object heats up under an inert atmosphere to be sintered to get porous graphene-LiFePO4 just
Pole material.
2. a kind of preparation method of porous graphene-lithium iron phosphate positive material according to claim 1, feature exist
In: the concentration of the potassium hydroxide solution is 0.1-1mol/L；Temperature in the high temperature process furnances is set as 700-
1000℃；The concentration of the polyvinylpyrrolidonesolution solution is 0.01-1mol/L.
3. a kind of preparation method of porous graphene-lithium iron phosphate positive material according to claim 1, feature exist
In: the mass fraction that the glucose accounts for porous graphene solution is 1-10%, and the lithium carbonate accounts for porous graphene solution
Mass fraction be 5-20%, the ferric phosphate account for porous graphene solution mass fraction be 10-50%.
4. a kind of preparation method of porous graphene-lithium iron phosphate positive material according to claim 1, feature exist
In: the parameter of the sintering that heats up under an inert atmosphere is: heating rate 2-10oC/min, sintering temperature is in 500-1000oC,
Sintering time 2-15 hours；The inert atmosphere is at least one of nitrogen, helium, argon gas.
5. a kind of preparation method of porous graphene-lithium iron phosphate positive material according to claim 2, feature exist
In: the concentration of the potassium hydroxide solution is 0.1mol/L；Temperature in the high temperature process furnances is set as 700 DEG C；Institute
The concentration for the polyvinylpyrrolidonesolution solution stated is 0.1mol/L.
6. a kind of preparation method of porous graphene-lithium iron phosphate positive material according to claim 3, feature exist
In: the mass fraction that the glucose accounts for porous graphene solution is 2.3%, and the lithium carbonate accounts for porous graphene solution
Mass fraction be 5%, the ferric phosphate account for porous graphene solution mass fraction be 20%.
7. a kind of preparation method of porous graphene-lithium iron phosphate positive material according to claim 4, feature exist
In: the parameter of the sintering that heats up under an inert atmosphere is: heating rate 5oC/min, sintering temperature is 700oC, sintering time
12 hours.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111799446A (en) * | 2020-05-27 | 2020-10-20 | 广西华政新能源科技有限公司 | Fast-charging type explosion-proof lithium ion battery |
| CN115579463A (en) * | 2022-08-17 | 2023-01-06 | 厦门海辰储能科技股份有限公司 | Graphene lithium iron phosphate composite material, preparation method thereof, pole piece and secondary battery |
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| US20180145328A1 (en) * | 2015-08-07 | 2018-05-24 | Board Of Regents, The University Of Texas System | Graphene oxide-polymer aerogels and electrodes |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111799446A (en) * | 2020-05-27 | 2020-10-20 | 广西华政新能源科技有限公司 | Fast-charging type explosion-proof lithium ion battery |
| CN111799446B (en) * | 2020-05-27 | 2021-08-10 | 广西华政新能源科技有限公司 | Fast-charging type explosion-proof lithium ion battery |
| CN115579463A (en) * | 2022-08-17 | 2023-01-06 | 厦门海辰储能科技股份有限公司 | Graphene lithium iron phosphate composite material, preparation method thereof, pole piece and secondary battery |
| CN115579463B (en) * | 2022-08-17 | 2024-01-23 | 厦门海辰储能科技股份有限公司 | Graphene lithium iron phosphate composite material, preparation method thereof, pole piece and secondary battery |
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Application publication date: 20190122 |