CN107394130A - The LFP raw powder's production technologies that a kind of three-dimensional porous graphene is modified - Google Patents
The LFP raw powder's production technologies that a kind of three-dimensional porous graphene is modified Download PDFInfo
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- CN107394130A CN107394130A CN201710478313.1A CN201710478313A CN107394130A CN 107394130 A CN107394130 A CN 107394130A CN 201710478313 A CN201710478313 A CN 201710478313A CN 107394130 A CN107394130 A CN 107394130A
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Abstract
The invention discloses the LiFePO that a kind of three-dimensional porous graphene is modified4(LFP) method for preparing anode material; first by the source of iron of selection, lithium source, phosphorus source; ball milling is carried out according to a certain percentage; using acetone as medium, glucose is made and graphene is carbon source, and batch (-type) ball milling is carried out using planetary ball mill; vacuum constant temperature is dried; afterwards, the high temperature sintering under protective atmosphere, you can obtain the tiny C@LFP/G composites of grain graininess.Gained C@LFP/G composites of the invention have the crystal phase structure same with phase pure material, have excellent chemical property, and the technological operation is simple, is adapted to industrial mass production.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, and in particular to a kind of three-dimensional porous graphene
Modified LFP raw powder's production technologies.
Background technology
In past 20 years, due to lithium ion battery（LIB）It is lightly portable to wait spy with high-energy-density, high efficiency
Point, in electric car（EV）, plug-in hybrid electric automobile（HEV）Occur with the application aspect of large-scale energy storage revolutionary
Change.However, these new applications need LIB to possess the electrode material of higher energy and more power ability, meanwhile, the electrode
Material must possess the features such as cost is low and environment-friendly.In general, the performance of electrode material directly affects lithium ion battery
Performance, its cost also directly determines the cost of battery.Therefore, can be by using with height in order to meet this demand
High rate performance, excellent cyclical stability, inexpensive and environmentally friendly new electrode materials are forthright to improve LIB times
Energy.Due to olivine-type LFP, cost is low, abundant raw materials, and security is good, Stability Analysis of Structures and environment-friendly, high voltage platform
（3.45V vs. Li / Li+）, high theoretical specific capacity（〜170 mA h / g）, it is considered to be most promising positive pole material
One of material.However, during electrokinetic cell practical application, olivine LFP shows low conductivity（10-9 ~ 10-10S /
cm）, low lithium ion diffusion coefficient（10-14To 10-16cm2/ s）.Therefore, the method for raising LFP chemical properties is sought still
The height of right investigation of materials person is pursued.
At present, domestic and international researcher is to solve the above problems to have paid huge effort, including reduces grain diameter,
Xenogenesis ion and coated with carbon or other conductive layers are adulterated, wherein carbon coating is most efficient method.These methods mainly collect
In improving LFP inherent characteristics in itself.Three-dimensional porous structure can be formed from suitable carbon source material cladding LFP particles,
Shorten Li+Diffusion path, so as to improve Li+Diffusion rate, can also effectively reduce the pair that electrode material and electrolyte occur
Reaction, improve the reversible capacity and cyclical stability of electrode material.Therefore it is also a kind of to prepare three-dimensional porous C@LFP composites
Up-and-coming technology.
Recently, graphene shows huge potentiality in lithium ion battery applications.When some metals or metal oxide
Anode material is modified by graphene, and cyclical stability and high rate performance are all improved.These are mainly due to graphene film
Excellent electric conductivity and structural flexibility, these characteristics may also rise important in the chemical property for improving LFP positive electrodes
Effect.
For LFP electrodes, battery performance is not only relevant with LFP characteristics, and relevant with electrode performance, such as loose structure.
Introducing Process During High Energy Ball Milling can be in LFP particle internal build pore structure, and this is primarily due to, Process During High Energy Ball Milling one side energy
Carbon nanoparticle is enough made, it is used as " sacrifice " masterplate, can be in particle internal structure hole, on the other hand, refinement and optimization
The granular size and Elemental redistribution of presoma, efficiently reduce the particle size of product particle.
At present, LFP raw powder's production technologies mainly have high temperature solid-state method, carbothermic method, sol-gal process, Hydrothermal Synthesiss
Method and microwave sintering method etc..Sol-gal process, hydrothermal synthesis method and microwave sintering method are because cost is high, technical difficulty is big, yield
Low shortcoming, therefore realize that industrialization is highly difficult.High temperature solid-state method and carbothermic method are the more works of current commercial application
Process, two methods are first to be well mixed raw material, then synthesize LFP at high temperature.But due to high temperature solid-state method
Larger and mixing is uneven with the material granule of carbothermic method preparation, causes the carbon coating of final products uneven, and product
Purity is not high.Can solve that carbon coating is uneven to ask well using softening-Rheological Phase Method synthesis C@LFP/G composites
Topic.
The content of the invention
A kind of softening-the Rheological Phase Method for the LFP powders being modified it is an object of the invention to provide three-dimensional porous graphene
Preparation method.The present invention mainly solves the problems, such as that the big high rate performance of LFP/C composites that is prepared in conventional solid-state method is low,
It can be prepared under the conditions of big multiplying power by softening-Rheological Phase Method, there is the C@LFP/G composites of high rate capability.
Technical scheme is as follows：
The LFP raw powder's production technologies that a kind of three-dimensional porous graphene is modified, including following preparation process：
(1) by raw material FeC2O4·2H2O、NH4H2PO4、LiCO33.6g is pressed with acetone:2.3g:0.74g:（20~45）G ratio,
Appropriate carbon source and graphene are added, is scattered in acetone, by the use of dodecyl sodium sulfate as dispersant, ultrasound a period of time,
Intermittent high-speed ball milling is carried out in high energy ball mill, forms rheology phase mixture；
(2) by step（1）In obtained by rheology phase mixture acetone is waved under the conditions of certain temperature in air dry oven
Send out, form solid precursor；
(3) by step（2）In obtained by solid precursor be put into vacuum drying chamber, temperature is set to 50 ~ 80 DEG C, vacuum drying
5 ~ 40h, room temperature taking-up is naturally cooled to, obtains sheet and the uniform solid precursor of composition；
(4) by step（3）In obtained by sheet and the uniform solid precursor of composition be put into agate mortar and be ground, it
Afterwards, 500 mesh sieve are crossed, obtain yellow powdery solid presoma；
(5) by step（4）In obtained by pulverulent solids presoma put into atmosphere protection stove and be warming up to 1 ~ 10 DEG C/min
350 DEG C, 2 ~ 4h is incubated, is then warming up to 600 ~ 700 DEG C with 1 ~ 10 DEG C/min, 5 ~ 24h is incubated, obtains modified three-dimensional porous stone
The LFP powders that black alkene is modified；
(6) by step（5）The LFP powders that the three-dimensional porous graphene of middle acquisition is modified, which are put into agate mortar, somewhat gently to be carried out
Grinding, afterwards, 500 mesh sieve are crossed, obtain the active material for the LFP powders that the thinner three-dimensional porous graphene of particle is modified.
Further, the LFP raw powder's production technologies that above-mentioned three-dimensional porous graphene is modified, preparation process（1）In
FeC2O4·2H2O can use Fe (Ac)2Instead of.
Further, the LFP raw powder's production technologies that above-mentioned three-dimensional porous graphene is modified, preparation process（1）In
NH4H2PO4(NH can be used4)2HPO4Substitute.
Further, the LFP raw powder's production technologies that above-mentioned three-dimensional porous graphene is modified, preparation process（1）Li2CO3
In can use LiOHH2O, LiNO3, LiAc replacements.
Further, the LFP raw powder's production technologies that above-mentioned three-dimensional porous graphene is modified, preparation process（1）Acetone
It can be substituted with absolute ethyl alcohol.
Further, the LFP raw powder's production technologies that above-mentioned three-dimensional porous graphene is modified, preparation process（1）Carbon source
To be any in laurate, glucose, sucrose, starch, citric acid or oxalic acid, the addition of the carbon source is the theoretical generations of LFP
The 1% ~ 20% of amount.
Further, the LFP raw powder's production technologies that above-mentioned three-dimensional porous graphene is modified, preparation process (1) high energy
Ball mill batch (-type) ball milling, 10 ~ 20min is often run, stops 1 ~ 5min, then invert 10 ~ 20min, Ceramics ball grinder, pellet
For Φ 5mm agate ball, ratio of grinding media to material（3~5）：（1~10）, it is 400 ~ 800r/min, 0 ~ 15h of time to control rotating speed.
Further, the LFP raw powder's production technologies that above-mentioned three-dimensional porous graphene is modified, preparation process (1) are described
Graphene addition is the 1% ~ 10% of LFP theory growing amounts.
Further, the LFP raw powder's production technologies that above-mentioned three-dimensional porous graphene is modified, preparation process (2) are described
Certain temperature is 25 ~ 40 DEG C, ensures that ferrous ion is not oxidized.
Further, the LFP raw powder's production technologies that above-mentioned three-dimensional porous graphene is modified, preparation process (5) are described
Protective atmosphere is H2、H2/Ar、N2Or any one in Ar atmosphere.
The solution have the advantages that：Due to being in rheology state in mix stages using raw material during this method, thus it is mixed
Close it is highly uniform, meanwhile, using dispersant of the effumability organic solvent as high-energy ball milling wet-milling process, to synthesizing C LFP/
G composites carbon content the introducing of carbon source, is coated on LFP particle surfaces, forms meso-hole structure, can limit LFP without influence
The undue growth of grain, shorten Li+Diffusion path, so as to improve Li+Diffusion rate, electrode material can also be effectively reduced
The side reaction occurred with electrolyte, the reversible capacity and cyclical stability of electrode material are improved, LFP/C active material granularities are made
100-300 nm are concentrated in distribution.The LFP powder composite materials that the three-dimensional porous graphene of gained is modified do not change pure phase LFP crystalline phase
Structure, good chemical property is presented during electrochemical property test.
Brief description of the drawings
Fig. 1 is the products C@LFP/G and PDF # 81-1173 of embodiment 1 X ray diffracting data figure.
Fig. 2 is the products C@LFP/G of embodiment 1 transmission electron microscope picture.
Fig. 3 is the products C@LFP/G of embodiment 1 electrochemistry high rate performance figure.
Fig. 4 is the products C@LFP/G and PDF # 81-1173 of embodiment 2 X ray diffracting data figure.
Fig. 5 is the products C@LFP/G of embodiment 2 transmission electron microscope picture.
Fig. 6 is the products C@LFP/G of embodiment 2 electrochemistry high rate performance figure.
Embodiment
Technical scheme is further elaborated with below by embodiment.
Embodiment 1：A kind of preparation method of C@LFP/G (1% G), step are as follows：
A. by raw material FeC2O4·2H2O、NH4H2PO4、LiCO33.6g is pressed with acetone：2.3g：0.74g:40g ratio, add
0.63g glucose, 0.063g graphene is added, intermittent high-speed ball milling is carried out in high energy ball mill, often runs 10
Min, 30 s of interval, then inverts 10 min, Ceramics ball grinder, and pellet is the mm agate balls of Φ 5, ratio of grinding media to material 3:10, control
Rotating speed processed is 600 r/min, and the H-shaped of time 6 is into rheology phase mixture；
B. the rheology phase mixture obtained by step (a) at 50 DEG C is volatilized away acetone in air dry oven, shape
Into solid precursor；
C. solid precursor resulting in step (b) is put into vacuum drying chamber, temperature is set to 80 DEG C, vacuum drying 20
H, room temperature is naturally cooled to, obtain sheet and the uniform solid precursor of composition；
D. the uniform solid precursor of sheet and composition resulting in step (c) is put into agate mortar and be ground, it
Afterwards, 500 mesh sieve are crossed, obtain yellow powdery solid presoma；
E. pulverulent solids presoma resulting in step (d) is put into high-purity argon gas atmosphere protection stove with 1 DEG C/min liters
Temperature is incubated 4h to 350 DEG C, is then warming up to 700 DEG C with 5 DEG C/min, is incubated 10h, obtains C@LFP/G active materials；
F. by step（i）Middle acquisition C@LFP/G active materials, which are put into agate mortar, to be somewhat gently ground, and afterwards, crosses 500
Mesh sieve, obtain the thinner C@LFP/G active materials of particle.
The present embodiment products C@LFP/G and PDF # 81-1173 X ray diffracting data is shown in Fig. 1.
The present embodiment products C@LFP/G transmission electron microscope is shown in Fig. 2.
The present embodiment products C@LFP/G electrochemistry high rate performance is shown in Fig. 3.
Embodiment 2：A kind of preparation method of C@LFP/G (3% G) composite, step are as follows：
A. by raw material FeC2O4·2H2O、NH4H2PO4、LiCO33.6g is pressed with acetone：2.3g：0.74g:40g ratio, add
0.63g glucose, 0.19g graphene carry out intermittent high-speed ball milling in high energy ball mill, often run 10 min, interval
30 s, then invert 10 min, Ceramics ball grinder, and pellet is the mm agate balls of Φ 5, ratio of grinding media to material 3:10, control the rotating speed to be
600 r/min, the H-shaped of time 6 is into rheology phase mixture；
B. the rheology phase mixture obtained by step (a) at 50 DEG C is volatilized away acetone in air dry oven, shape
Into solid precursor；
C. solid precursor resulting in step (b) is put into vacuum drying chamber, temperature is set to 80 DEG C, vacuum drying 20
H, room temperature is naturally cooled to, obtain sheet and the uniform solid precursor of composition；
D. the uniform solid precursor of sheet and composition resulting in step (c) is put into agate mortar and be ground, it
Afterwards, 500 mesh sieve are crossed, obtain pulverulent solids presoma；
E. pulverulent solids presoma resulting in step (d) is put into high-purity argon gas atmosphere protection stove with 1 DEG C/min liters
Temperature is incubated 4h to 350 DEG C, is then warming up to 700 DEG C with 5 DEG C/min, is incubated 10h, obtains C@LFP/G active materials；
F. by step（i）Middle acquisition C@LFP/G active materials, which are put into agate mortar, to be somewhat gently ground, and afterwards, crosses 500
Mesh sieve, obtain the thinner C@LFP/G active materials of particle.
The present embodiment products C@LFP/G and PDF # 81-1173 X ray diffracting data is shown in Fig. 4.
The present embodiment products C@LFP/G transmission electron microscope is shown in Fig. 5.
The present embodiment products C@LFP/G electrochemistry high rate performance is shown in Fig. 6.
Claims (10)
1. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene is modified, it is characterised in that comprise the following steps：
By raw material FeC2O4·2H2O、NH4H2PO4、LiCO33.6g is pressed with acetone:2.3g:0.74g:（20~45）G ratio, add
Appropriate carbon source and graphene, are scattered in acetone, and dispersant, ultrasound a period of time, in height are used as by the use of dodecyl sodium sulfate
Intermittent high-speed ball milling can be carried out in ball mill, form rheology phase mixture；
By step（1）In obtained by rheology phase mixture acetone is volatilized under the conditions of certain temperature in air dry oven
Go, form solid precursor；
By step（2）In obtained by solid precursor be put into vacuum drying chamber, temperature is set to 50 ~ 80 DEG C, vacuum drying 5 ~
40h, room temperature taking-up is naturally cooled to, obtains sheet and the uniform solid precursor of composition；
By step（3）In obtained by sheet and the uniform solid precursor of composition be put into agate mortar and be ground, afterwards,
500 mesh sieve are crossed, obtain yellow powdery solid presoma；
By step（4）In obtained by pulverulent solids presoma put into atmosphere protection stove and be warming up to 350 with 1 ~ 10 DEG C/min
DEG C, 2 ~ 4h is incubated, is then warming up to 600 ~ 700 DEG C with 1 ~ 10 DEG C/min, is incubated 5 ~ 24h, three-dimensional porous graphene is obtained and is modified
LiFePO 4 powder；
By step（5）The LFP powders that the three-dimensional porous graphene of middle acquisition is modified, which are put into agate mortar, somewhat gently to be ground
Mill, afterwards, 500 mesh sieve are crossed, obtain the LiFePO 4 powder that the thinner three-dimensional porous graphene of particle is modified.
2. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene as claimed in claim 1 is modified, it is characterised in that
Preparation process（1）Middle FeC2O4·2H2O can use Fe (Ac)2Instead of.
3. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene as claimed in claim 1 is modified, it is characterised in that
Preparation process（1）Middle NH4H2PO4(NH can be used4)2HPO4Substitute.
4. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene as claimed in claim 1 is modified, it is characterised in that
Preparation process（1）Li2CO3In can use LiOHH2O, LiNO3, LiAc replacements.
5. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene as claimed in claim 1 is modified, it is characterised in that
Preparation process（1）Acetone can be substituted with absolute ethyl alcohol.
6. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene as claimed in claim 1 is modified, it is characterised in that
Preparation process（1）Carbon source is any, addition of the carbon source in laurate, glucose, sucrose, starch, citric acid or oxalic acid
Measure as the 1% ~ 20% of LFP theory growing amounts.
7. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene as claimed in claim 1 is modified, it is characterised in that system
Standby step (1) high energy ball mill batch (-type) ball milling, often runs 10 ~ 20min, stops 1 ~ 5min, 10 ~ 20min is then inverted, from pottery
Porcelain ball grinder, pellet be Φ 5mm agate ball, ratio of grinding media to material（3~5）：（1~10）, it is 400 ~ 800r/min to control rotating speed, the time 0 ~
15h。
8. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene as claimed in claim 1 is modified, it is characterised in that
Preparation process (1) the graphene addition is the 1% ~ 10% of LFP theory growing amounts, and agate jar is selected in wet-milling, and pellet is
Agate ball, ratio of grinding media to material（3~5）：（1~10）, it is 400 ~ 800r/min, 0 ~ 15h of time to control rotating speed.
9. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene as claimed in claim 1 is modified, it is characterised in that system
Standby step (2) described certain temperature is 25 ~ 40 DEG C, ensures that ferrous ion is not oxidized.
10. the LFP raw powder's production technologies that a kind of three-dimensional porous graphene as claimed in claim 1 is modified, it is characterised in that
Preparation process (5) described protective atmosphere is H2、H2/Ar、N2Or any one in Ar atmosphere.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108390041A (en) * | 2018-02-28 | 2018-08-10 | 石河子大学 | Foamed nickel current collector LiFePO4/graphene composite material electrode slice and preparation method thereof |
| CN109192955A (en) * | 2018-09-10 | 2019-01-11 | 成都紫苑华光新材料科技有限公司 | A kind of preparation method of LiFePO4/graphene in-situ composite |
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| CN101673824A (en) * | 2009-09-23 | 2010-03-17 | 上海电力学院 | Preparation method of LiFePO4/C composite materials |
| CN102306783A (en) * | 2011-09-14 | 2012-01-04 | 哈尔滨工业大学 | Multi-layer graphene/lithium iron phosphate intercalated composite material, preparation method thereof, and lithium ion battery adopting multi-layer grapheme/lithium iron phosphate intercalated composite material as anode material |
| CN105762343A (en) * | 2016-04-17 | 2016-07-13 | 郑叶芳 | Preparation method of LiFePO4/C anode material by rheological phase method |
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2017
- 2017-06-22 CN CN201710478313.1A patent/CN107394130A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101673824A (en) * | 2009-09-23 | 2010-03-17 | 上海电力学院 | Preparation method of LiFePO4/C composite materials |
| CN102306783A (en) * | 2011-09-14 | 2012-01-04 | 哈尔滨工业大学 | Multi-layer graphene/lithium iron phosphate intercalated composite material, preparation method thereof, and lithium ion battery adopting multi-layer grapheme/lithium iron phosphate intercalated composite material as anode material |
| CN105762343A (en) * | 2016-04-17 | 2016-07-13 | 郑叶芳 | Preparation method of LiFePO4/C anode material by rheological phase method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108390041A (en) * | 2018-02-28 | 2018-08-10 | 石河子大学 | Foamed nickel current collector LiFePO4/graphene composite material electrode slice and preparation method thereof |
| CN109192955A (en) * | 2018-09-10 | 2019-01-11 | 成都紫苑华光新材料科技有限公司 | A kind of preparation method of LiFePO4/graphene in-situ composite |
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Application publication date: 20171124 |