CN107834044A - A kind of graphene-based composite ferric lithium phosphate material and application - Google Patents
A kind of graphene-based composite ferric lithium phosphate material and application Download PDFInfo
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- H01M10/05—Accumulators with non-aqueous electrolyte
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- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- 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
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Abstract
The present invention relates to a kind of graphene-based composite ferric lithium phosphate material and application.The preparation method of the composite is：Lithium compound, phosphate, molysite, graphite, intercalator are mixed with water, prepare graphene slurry；Hydrogen peroxide, nitrogen source mixing are added into graphene slurry, prepares precursor pulp；Precursor pulp is subjected to hydro-thermal reaction, obtains hydrogel；Hydrogel is soaked in organic carbon source solution, separated, then is sintered under reducing atmosphere, is produced.In the composite, nitrogen source plays a part of doping vario-property, can form C N keys with graphene and improve the electric conductivity of composite；Pass through the water sorption of hydrogel, composite inner and adsorption organic carbon source can be made, porous charcoal is formed after sintered, have the function that to improve conductance and imbibition liquid-keeping property, the comprehensive function of above material makes the composite have the characteristics of conductance is good, tap density is high, and the high rate performance and gram volume for significantly improving composite ferric lithium phosphate material play.
Description
Technical field
The invention belongs to lithium ion battery electrode material field, and in particular to a kind of graphene-based composite ferric lithium phosphate material
And application.
Background technology
LiFePO 4 material with its security performance it is high, it is environment-friendly, have extended cycle life the advantages that and turn into lithium ion battery
Staple material, but there is the shortcomings of relatively low gram volume, high rate performance and poorly conductive in the material, limit in itself
Its application in high-energy-density density, fast charge field of lithium ion battery.LiFePO 4 material is coated and is modified so as to carry
The gram volume of high material plays and electronics conduction velocity, turns into one of direction for improving LiFePO 4 material.
Application publication number is that CN106602006A patent discloses a kind of grapheme lithium iron phosphate composite, and this is compound
Material sinters through ultrasonic disperse, drying, reduction using ferric lithium phosphate precursor and graphene as raw material, prepares LiFePO4 and bag
Overlay on the graphene on LiFePO4 surface.The graphene layer and LiFePO4 of the grapheme lithium iron phosphate composite pass through absorption
Effect is combined together, and still suffers from the defects of conductance is poor, tap density is relatively low, causes high rate performance, the gram volume hair of material
Wave and need further to be improved.
The content of the invention
It is an object of the invention to provide a kind of graphene-based composite ferric lithium phosphate material, so as to solve existing LiFePO4
The problem of high rate performance is poor, gram volume is relatively low be present in composite.
Second object of the present invention is to provide above-mentioned graphene-based composite ferric lithium phosphate material as lithium ion battery
The application of positive electrode.
To achieve the above object, the technical solution adopted in the present invention is：
A kind of graphene-based composite ferric lithium phosphate material, is prepared by the method comprised the following steps：
1) lithium compound, phosphate, molysite, graphite, intercalator and water are mixed, prepares graphene slurry；
2) hydrogen peroxide, nitrogen source mixing are added into graphene slurry, prepares precursor pulp；
3) precursor pulp is subjected to hydro-thermal reaction, obtains hydrogel；
4) hydrogel is soaked in organic carbon source solution, separation of solid and liquid, then solid phase is sintered under reducing atmosphere, i.e.,
.
Graphene-based composite ferric lithium phosphate material provided by the invention, add hydrogen peroxide into graphene slurry, nitrogen source is entered
Water-filling thermal response, hydrogen peroxide have weak oxide effect, can be that grapheme material surface introducing hydroxyl, carboxyl etc. can reactive groups
Group, after hydro-thermal reaction, grapheme material can reactive group with phosphate cation formed with chemical bond company answering
Fit hydrogel, the high-density graphite alkenyl phosphoric acid iron lithium presoma with nano aperture is formed after drying, then through in reducing atmosphere
Under sintering, prepare graphene-based composite ferric lithium phosphate material.
In the composite, nitrogen source plays a part of doping vario-property, can form C-N keys with graphene and improve composite wood
The electric conductivity of material；By the suction-operated of hydrogel, composite inner and adsorption organic carbon source, sintered rear shape can be made
Into porous charcoal, have the function that to improve conductance and imbibition liquid-keeping property, the comprehensive function of above material has the composite
There is the characteristics of conductance is good, tap density is high, the high rate performance and gram volume for significantly improving composite ferric lithium phosphate material play.
In step 1), lithium compound, phosphate, molysite, intercalator, the mol ratio of graphite are (1~1.5)：1：1：(0.1
~3)：(1~10).In the step, for ease of being well mixed, lithium compound, molysite, phosphate can be dissolved in water and prepare mixed liquor
A；Mixed by graphite, intercalator and water mixed preparing mixed liquid B, then by mixed liquor A, mixed liquid B, ultrasonic disperse, prepare graphite
Alkene slurry.
The lithium compound is lithium carbonate and/or lithium hydroxide.The phosphate is M3PO4、M2HPO4、MH2PO4In extremely
Few one kind, M is sodium, potassium or ammonium.The graphite is preferably crystalline flake graphite.The intercalator is sodium hypochlorite.
In step 2), graphite raw material and hydrogen peroxide, the mass ratio of nitrogen source are (4~12) in graphene slurry：(0.01~
0.3)：(0.08~0.6), the mass concentration of hydrogen peroxide is 1~30%.
In step 2), the nitrogen source is pyrroles, ammoniacal liquor, aniline, urea, at least one of melamine, the ammoniacal liquor
Mass concentration be 1~30%.
In step 3), the hydro-thermal reaction is to react 2~6h at 150~200 DEG C.
In step 4), the organic carbon source is at least one of phenolic resin, glucose sugar, sucrose, starch, citric acid.
The mass concentration of the organic carbon source solution is 1%~5%.The time of the immersion is 6~24h.Water-setting is isolated after immersion
Glue, in 40~60 DEG C of dry 24~72h, xerogel is obtained, the xerogel is sintered under reducing atmosphere.
In step 4), the reducing atmosphere is hydrogen atmosphere.The sintering is to be incubated 6~12h at 600~900 DEG C.
Using above-mentioned graphene-based composite ferric lithium phosphate material as anode material for lithium-ion batteries, have high conductivity,
The characteristics of high-tap density, the high rate performance and gram volume that can significantly improve LiFePO 4 material play.
Brief description of the drawings
Fig. 1 is the SEM figures of the graphene-based composite ferric lithium phosphate material prepared by the present embodiment 1.
Embodiment
Embodiments of the present invention are described further with reference to specific embodiment.
Embodiment 1
The graphene-based composite ferric lithium phosphate material of the present embodiment, is prepared using following steps：
1) by 8.88g (0.12mol) lithium carbonate, 27.8g (0.1mol) FeSO4·7H2O, 11.5g (0.1mol) di(2-ethylhexyl)phosphate
Hydrogen ammonium is dissolved in 500ml water, prepares mixed liquor A；
4.8g crystalline flake graphites, 14.8g (0.2mol) sodium hypochlorite intercalators and 500ml water are mixed, prepare mixed liquid B；
After mixed liquor A and mixed liquid B are mixed, ultrasonic disperse 12h, floating impurity is centrifuged off, obtains lower layer graphene
Slurry；
2) into graphene slurry, addition 0.11ml hydrogen peroxide (mass concentration 10%), 0.22g pyrroles are stirred, so
After be transferred in autoclave, 180 DEG C carry out hydro-thermal reaction 4h, isolated hydrogel；
3) hydrogel is placed in the glucose solution that 176ml concentration is 1% and soaks 12h, again in 50 DEG C of dryings after separation
48h, obtain xerogel；
4) xerogel is transferred in tube furnace, in a hydrogen atmosphere, sinters 8h in 800 DEG C, be cooled to room temperature, then through powder
It is broken, grind and produce graphene-based lithium iron phosphate positive material.
Embodiment 2
The graphene-based composite ferric lithium phosphate material of the present embodiment, is prepared using following steps：
1) by 2.4g (0.1mol) lithium hydroxide, 14.3g (0.1mol) ferrous oxalate, 13.2g (0.1mol) Diammonium phosphate (DAP)
500ml water is dissolved in, prepares mixed liquor A；
12g crystalline flake graphites, 0.74g (0.01mol) sodium hypochlorite intercalators and 500ml water are mixed, prepare mixed liquid B；
After mixed liquor A and mixed liquid B are mixed, ultrasonic disperse 24h, floating impurity is centrifuged off, obtains lower layer graphene
Slurry；
2) into graphene slurry, addition 0.016g hydrogen peroxide (mass concentration 1%), 0.08g urea are stirred, so
After be transferred in autoclave, 150 DEG C carry out hydro-thermal reaction 6h, isolated hydrogel；
3) hydrogel is placed in the starch solution that 80ml concentration is 1% and soaks 24h, again in 40 DEG C of dry 72h after separation,
Obtain xerogel；
4) xerogel is transferred in tube furnace, in a hydrogen atmosphere, sinters 12h in 600 DEG C, be cooled to room temperature, then pass through
Crush, grind and produce graphene-based lithium iron phosphate positive material.
Embodiment 3
The graphene-based composite ferric lithium phosphate material of the present embodiment, is prepared using following steps：
1) by 11.1g (0.15mol) lithium carbonate, 27.8g (0.1mol) FeSO4·7H2O, 20.3g (0.1mol) ammonium phosphate
500ml water is dissolved in, prepares mixed liquor A；
6g crystalline flake graphites, 22.2g (0.3mol) sodium hypochlorite intercalators and 500ml water are mixed, prepare mixed liquid B；
After mixed liquor A and mixed liquid B are mixed, ultrasonic disperse 48h, floating impurity is centrifuged off, obtains lower layer graphene
Slurry；
2) 0.31g hydrogen peroxide (mass concentration 30%) is added into graphene slurry, (mass concentration is 0.62g ammoniacal liquor
10%) it is stirred, is then transferred into autoclave, hydro-thermal reaction 2h, isolated hydrogel is carried out at 200 DEG C；
3) hydrogel is placed in the phenol resin solution that 31ml concentration is 1% and soaks 24h, again in 60 DEG C of dryings after separation
24h, obtain xerogel；
4) xerogel is transferred in tube furnace, in a hydrogen atmosphere, sinters 6h in 900 DEG C, be cooled to room temperature, then through powder
It is broken, grind and produce graphene-based lithium iron phosphate positive material.
, can be according to the technique of embodiment 1 in the other embodiment of the graphene-based lithium iron phosphate positive material of the present invention
Step and dosage, nitrogen source equivalent is replaced with into aniline, melamine, organic carbon source replaces with sucrose, citric acid, can obtain and real
Apply the suitable product of the performance of example 1.
Comparative example
The graphene-based lithium iron phosphate positive material of comparative example is prepared using following methods：By 11.1g lithium carbonates,
27.8g FeSO4·7H2O, 20.3g ammonium phosphate is added in 500ml redistilled waters with 0.31g graphenes, and ultrasonic disperse is uniform
Afterwards, filter, dry, be then transferred into tube furnace, in a hydrogen atmosphere, calcine 8h at 750 DEG C, Temperature fall to room temperature,
Through crushing, being classified, produce.
Test example 1
This test example is observed the surface topography of the graphene-based lithium iron phosphate positive material of embodiment 1, its SEM figures
As shown in figure 1, as seen from the figure, graphene-based lithium iron phosphate positive material surface irregularity, there is abundant pore structure,
It is expected that with stronger imbibition ability.
Test example 2
This test example carries out chemical property survey to the graphene-based lithium iron phosphate positive material of each embodiment and comparative example
Examination.
2.1 button cells are tested
Weigh respectively the lithium iron phosphate positive material of 2.0g embodiments 1~3 and comparative example, 0.1g conductive blacks,
0.1gPVDF is mixed, and is added 2.5g 1-METHYLPYRROLIDONEs and is mixed, obtains positive electrode slurry.Positive electrode slurry is applied
It is overlying on aluminium foil (coating thickness is 140 μm), in 120 DEG C of vacuum drying 2h, 5mm disk is broken into using card punch, is reused
Tablet press machine 120 DEG C of vacuum heat-preserving 12h, weighs positive pole sheet weight in 10Mpa lower sheetings.Assembled in the glove box of argon gas protection
Into button cell, wherein, negative pole is metal lithium sheet, and electrolyte is the LiPF that concentration is 1mol/L6(solvent is by volume ratio 1 for solution:
1 EC, DEC is mixed), barrier film is Celgard2400 microporous polyethylene films.
The button cell assembled is tested into electrical property on blue electric tester, in 2.75V~4.25V voltage ranges,
With 0.2C constant current charge/discharge, electric discharge capacity and first efficiency, as a result as shown in table 1.
1 each embodiment of table and comparative example buckle electrical test results
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 | Comparative example |
| Discharge capacity (mAh/g) first | 162.2 | 161.3 | 160.3 | 153.5 |
| Efficiency (%) first | 97.9 | 96.9 | 95.3 | 93.4 |
The discharge capacity and efficiency first of composite ferric lithium phosphate material prepared by embodiment it can be seen from the result of table 1
Apparently higher than comparative example, its reason is that the presence of N doping, graphene network and carbon source can effectively improve the conductance of material, from
And the gram volume for being advantageous to improve positive electrode plays and the raising of efficiency first.
2.2 imbibition liquid-keeping properties are tested
The imbibition liquid-keeping property of each embodiment and comparative example is investigated, as a result as shown in table 2.
The imbibition liquid-keeping property of 2 each embodiment of table and comparative example contrasts
The imbibition liquid-keeping property of each embodiment is significantly stronger than comparative example it can be seen from the result of table 2, and its reason is reality
The lithium iron phosphate positive material for applying example has higher specific surface area, and the immersion of hydrogel, drying process can form abundant
Nano aperture, help further to improve the imbibition liquid-keeping property of material.
2.3 soft-package batteries are tested
The composite ferric lithium phosphate material prepared respectively using embodiment 1~3 and comparative example is positive electrode, using graphite as negative pole
Material, the LiPF using concentration as 1mol/L6(solvent is by volume ratio 1 for solution:1 EC, DEC is mixed) it is electrolyte,
The films of Celgard 2400 are barrier film, prepare 5Ah soft-package batteries, detect high rate performance and cycle performance, as a result as shown in table 3.
The chemical property of 3 each embodiment of table and comparative example contrasts
As shown in Table 3, the high rate performance of the lithium ion battery of embodiment and cycle performance are much better than comparative example, former
Because effectively improving the conductance of electronics in charge and discharge process in the graphene-based lithium iron phosphate positive material, hydrogel is through leaching
Bubble, drying process can form abundant hole, Stability Analysis of Structures, and have stronger imbibition ability, so as to effectively improve
The cycle performance and high rate charge-discharge performance of the lithium ion battery of preparation.
Claims (10)
1. a kind of graphene-based composite ferric lithium phosphate material, it is characterised in that be prepared by the method comprised the following steps：
1) lithium compound, phosphate, molysite, graphite, intercalator and water are mixed, prepares graphene slurry；
2) hydrogen peroxide, nitrogen source mixing are added into graphene slurry, prepares precursor pulp；
3) precursor pulp is subjected to hydro-thermal reaction, obtains hydrogel；
4) hydrogel is soaked in organic carbon source solution, separation of solid and liquid, then solid phase is sintered under reducing atmosphere, produced.
2. graphene-based composite ferric lithium phosphate material as claimed in claim 1, it is characterised in that in step 1), lithium compound,
Phosphate, molysite, intercalator, the mol ratio of graphite are (1~1.5)：1：1：(0.1~3)：(1~10).
3. graphene-based composite ferric lithium phosphate material as claimed in claim 1 or 2, it is characterised in that the lithium compound is
Lithium carbonate and/or lithium hydroxide.
4. graphene-based composite ferric lithium phosphate material as claimed in claim 1 or 2, it is characterised in that the phosphate is
M3PO4、M2HPO4、MH2PO4At least one of, M is sodium, potassium or ammonium.
5. graphene-based composite ferric lithium phosphate material as claimed in claim 1 or 2, it is characterised in that the intercalator is secondary
Sodium chlorate.
6. graphene-based composite ferric lithium phosphate material as claimed in claim 1, it is characterised in that in step 2), graphene slurry
Graphite raw material and hydrogen peroxide, the mass ratio of nitrogen source are (4~12) in material：(0.01~0.3)：(0.08~0.6), the matter of hydrogen peroxide
It is 1~30% to measure concentration.
7. the graphene-based composite ferric lithium phosphate material as described in claim 1 or 6, it is characterised in that in step 2), the nitrogen
Source is at least one of pyrroles, ammoniacal liquor, aniline, urea, melamine, and the mass concentration of the ammoniacal liquor is 1~30%.
8. graphene-based composite ferric lithium phosphate material as claimed in claim 1, it is characterised in that in step 3), the hydro-thermal
Reaction is to react 2~6h at 150~200 DEG C.
9. graphene-based composite ferric lithium phosphate material as claimed in claim 1, it is characterised in that in step 4), the sintering
It is to be incubated 6~12h at 600~900 DEG C.
10. a kind of graphene-based composite ferric lithium phosphate material as claimed in claim 1 is as anode material for lithium-ion batteries
Using.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110233284A (en) * | 2019-07-17 | 2019-09-13 | 江西省汇亿新能源有限公司 | A kind of low form high-energy density long circulating ferric phosphate lithium cell |
| CN111081994A (en) * | 2019-10-30 | 2020-04-28 | 广东工业大学 | Surface-modified lithium-rich layered transition metal oxide and preparation method and application thereof |
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| CN101800310A (en) * | 2010-04-02 | 2010-08-11 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing graphene-doped anode material for lithium-ion batteries |
| CN102169986A (en) * | 2011-04-02 | 2011-08-31 | 江苏乐能电池股份有限公司 | Preparation method of lithium ferric phosphate / grapheme composite positive electrode material |
| CN102447110A (en) * | 2011-12-14 | 2012-05-09 | 哈尔滨工业大学 | Preparation method of carbon nanomaterial-doped spherical iron phosphate and preparation method of carbon nanomaterial-doped lithium iron phosphate |
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2017
- 2017-11-02 CN CN201711064492.0A patent/CN107834044B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101800310A (en) * | 2010-04-02 | 2010-08-11 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing graphene-doped anode material for lithium-ion batteries |
| CN102169986A (en) * | 2011-04-02 | 2011-08-31 | 江苏乐能电池股份有限公司 | Preparation method of lithium ferric phosphate / grapheme composite positive electrode material |
| CN102447110A (en) * | 2011-12-14 | 2012-05-09 | 哈尔滨工业大学 | Preparation method of carbon nanomaterial-doped spherical iron phosphate and preparation method of carbon nanomaterial-doped lithium iron phosphate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110233284A (en) * | 2019-07-17 | 2019-09-13 | 江西省汇亿新能源有限公司 | A kind of low form high-energy density long circulating ferric phosphate lithium cell |
| CN111081994A (en) * | 2019-10-30 | 2020-04-28 | 广东工业大学 | Surface-modified lithium-rich layered transition metal oxide and preparation method and application thereof |
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