CN110048113A - A kind of carbon/ferric metasilicate lithium/composite ferric lithium phosphate material and preparation method thereof - Google Patents
A kind of carbon/ferric metasilicate lithium/composite ferric lithium phosphate material and preparation method thereof Download PDFInfo
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- CN110048113A CN110048113A CN201910358483.5A CN201910358483A CN110048113A CN 110048113 A CN110048113 A CN 110048113A CN 201910358483 A CN201910358483 A CN 201910358483A CN 110048113 A CN110048113 A CN 110048113A
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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
- H01M4/362—Composites
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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
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- 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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- H01M4/62—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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- H—ELECTRICITY
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- 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 provides a kind of carbon/ferric metasilicate lithium/composite ferric lithium phosphate material and preparation method thereof, belongs to anode material for lithium-ion batteries technical field.Described method includes following steps: carbon/ferric metasilicate lithium being mixed addition deionized water with carbon/LiFePO4 and is prepared into slurry; it is sprayed in spray dryer; obtain mixture; by this mixture high temperature sintering under inert gas protection; after isothermal holding; spherical structure carbon/ferric metasilicate lithium/composite ferric lithium phosphate material can be obtained in cooled to room temperature.Preparation method low cost of raw materials of the invention, technical process are simple, economic and environment-friendly, are suitble to scale industrialization production and application, promote the development of electric car.The present invention prepares resulting spherical structure carbon/ferric metasilicate lithium/composite ferric lithium phosphate material good cycle, and good rate capability, discharge curve is ramped, realizes the target that can accurately calculate the SOC of ferric phosphate lithium ion battery by simply measuring voltage.
Description
[technical field]
The present invention relates to anode material for lithium-ion batteries, and in particular to a kind of spherical structure carbon/ferric metasilicate lithium/LiFePO4
Composite material and preparation method.
[background technique]
Lithium-ion battery monomer is made of the part such as positive and negative electrode, electrolyte, diaphragm and shell, and wherein positive electrode is to lithium
The performance of ion battery has large effect, is one of critical material of lithium ion battery.Anode material for lithium-ion batteries has
Multiple choices, currently, there are three types of positive electrode for power lithium-ion battery is common, i.e. LiMn2O4, ternary material and phosphorus
Sour iron lithium.
Wherein, olivine-type LiFePO4Positive electrode theoretical capacity is 170mAh/g, generally performance 150mAh/g.In recent years
Come, due to its excellent security performance, it is environmental-friendly, have extended cycle life the advantages that, be widely used in electric car and mixing
In power vehicle.But due to the influence of self structure, typical carbon/ferric phosphate lithium cell charging and discharging curve phase after discharge
The very high vertical line of verticality declined by the very high horizontal line of levelness and suddenly is constituted, and voltage is in nonlinear dependence between capacity
System, this feature cause to be difficult to directly calculate LiFePO by simply measuring cell voltage4Battery remaining capacity (SOC,
State of Charge), the SOC that battery is accurately calculated to battery management system brings difficulty.
Li2FeSiO4Equally can reversible deintercalate lithium ions, can be as the positive electrode of lithium ion battery.Li2FeSiO4Tool
Have the advantages that abundant raw material resources, cheap, no hygroscopicity, nontoxic, environmental-friendly, thermal stability be good and lithium-ion electric
The research and development focus of pond positive electrode.Wherein, Li2FeSiO4The ramped degree of the charging and discharging curve of material is very high, and most of
In 3V hereinafter, this is exactly LiFePO4Needed for the part below the ramped 3.4V of material charging and discharging curve.
Currently, the scholar of lot of domestic and foreign is in order to solve LiFePO4The problem of lithium ion battery SOC accurately calculates is carried out
Deep work, achieves serial achievement.But they are started with from improvement mathematical model and raising equipment measuring accuracy
Conduct a research work, as a result, mathematical model is more complicated, measuring device is more complicated, using being restricted, therefore finds one
The ramped LiFePO of kind simple process, high-volume, low cost, discharge curve4The preparation method of material is that a urgent need solves
The problem of.In this regard, the present invention is proposed using increase Li2FeSiO4 phase, optimization composition and adjusted and controlled method, construct novel
Carbon/ferric metasilicate lithium/iron phosphate compound anode material of lithium realizes the ramped of lithium iron phosphate positive material charging and discharging curve, from material
Material is started with, and solves the problems, such as that power lithium-ion battery SOC accurately calculates.
[summary of the invention]
Goal of the invention of the invention is: in view of the above problems, provide a kind of spherical structure carbon/ferric metasilicate lithium/
Composite ferric lithium phosphate material and preparation method thereof, preparation method low cost of raw materials of the invention, technical process are simple, pass through
Ji environmental protection is suitble to scale industrialization production and application, promotes the development of electric car.The present invention prepares resulting spherical structure
Carbon/ferric metasilicate lithium/composite ferric lithium phosphate material good cycle, good rate capability, discharge curve is ramped, realizes by simple
Ground measurement voltage can accurately calculate the target of the SOC of ferric phosphate lithium ion battery.
To achieve the goals above, The technical solution adopted by the invention is as follows:
A kind of carbon/ferric metasilicate lithium/composite ferric lithium phosphate material preparation method, includes the following steps: carbon/ferric metasilicate lithium
Addition deionized water is mixed with carbon/LiFePO4 and is prepared into slurry, is sprayed in spray dryer, obtains mixture, it will
This mixture high temperature sintering under inert gas protection, after isothermal holding, spherical structure is can be obtained in cooled to room temperature
Carbon/ferric metasilicate lithium/composite ferric lithium phosphate material.
Specifically, carbon of the invention/ferric metasilicate lithium/composite ferric lithium phosphate material preparation method includes the steps that are as follows:
(1) carbon/ferric metasilicate lithium and carbon/LiFePO4 are dispersed by weight for 0.5%:99.5%~10%:90%
In deionized water, being adjusted to solid content is 5%~40% slurry, and the machine in the case where speed of agitator is 70~150 revs/min of speed
Tool stirs 3~8h, is uniformly mixed slurry；
(2) spray dryer parameter is set, parameter includes: that inlet air temperature is 120~300 DEG C, and leaving air temp is 90~
150 DEG C, atomizer rotating speed is 200~300 revs/min, and wriggling pump speed is 300~1500ml/h；
(3) slurry of the step (1) is pumped into spray dryer under agitation and is sprayed, obtain forerunner
Body；
(4) under inert gas protection by obtained presoma, sintering temperature is burnt under conditions of being 300~800 DEG C
Knot, soaking time are 8h~for 24 hours, and after heat preservation, spherical structure carbon/ferric metasilicate lithium/phosphorus is can be obtained in cooled to room temperature
Sour iron lithium composite material.
It is above-mentioned to prepare resulting spherical structure carbon/ferric metasilicate lithium/composite ferric lithium phosphate material and can be used as lithium ion battery just
Pole material.
In conclusion by adopting the above-described technical solution, the beneficial effects of the present invention are:
1, carbon/ferric metasilicate lithium/composite ferric lithium phosphate material prepared by the present invention has spherical structure, is keeping preferably following
Under the premise of ring performance, high rate performance, also have the characteristics that ramped discharge curve, capacity and voltage linear relationship, uses
The composite material does the anode of lithium battery, can greatly reduce SOC's by simply measuring cell voltage direct measuring SOC
Calculate difficulty, calculate cost, to prevent lithium ion battery overcharging or overdischarging, guarantees the normal use of battery, extend battery
Service life provide data basis.
2, low raw-material cost, technical process used in preparation method of the invention be simple, economical and energy saving, non-generation environment
Pollution is suitble to scale industrialization production and application, can push the scale application of lithium iron phosphate positive material, promotes electric car
Development.
[Detailed description of the invention]
Fig. 1 is spherical carbon/ferric metasilicate lithium prepared by the embodiment of the present invention 1/composite ferric lithium phosphate material SEM figure.
Fig. 2 is spherical carbon/ferric metasilicate lithium/composite ferric lithium phosphate material chemical property prepared by the embodiment of the present invention 1
Figure.
Fig. 3 is that spherical carbon/ferric metasilicate lithium/composite ferric lithium phosphate material prepared by the embodiment of the present invention 1 discharges song for the first time
Line chart.
Fig. 4 is spherical carbon/ferric metasilicate lithium prepared by the embodiment of the present invention 1/part composite ferric lithium phosphate material SOC-OCV
Amplified curve figure.
[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.
A kind of carbon/ferric metasilicate lithium/composite ferric lithium phosphate material preparation method of the invention, include the following steps: by carbon/
Ferric metasilicate lithium mixes addition deionized water with carbon/LiFePO4 and is prepared into slurry, is sprayed, is mixed in spray dryer
Object is closed, by this mixture high temperature sintering under inert gas protection, after isothermal holding, ball is can be obtained in cooled to room temperature
Shape structural carbon/ferric metasilicate lithium/composite ferric lithium phosphate material.
In some embodiments of the invention, deionized water is added in described mix carbon/ferric metasilicate lithium with carbon/LiFePO4
The specific practice for being prepared into slurry is, by carbon/ferric metasilicate lithium and carbon/LiFePO4 by weight for 0.5%:99.5%~
10%:90% is scattered in deionized water, and being adjusted to solid content is 5%~40% slurry, and carries out 3~8h of mechanical stirring, is made
Slurry is uniformly mixed.
In some embodiments of the invention, when described spraying, the parameter of the spray dryer of setting are as follows: inlet air temperature is
120~300 DEG C, leaving air temp is 90~150 DEG C, and atomizer rotating speed is 200~300 revs/min, and wriggling pump speed is 300-
1500ml/h。
In some embodiments of the invention, the specific practice of the high temperature sintering is under inert gas protection, to be sintered
Temperature is sintered under conditions of being 300~800 DEG C, and soaking time is 8h~for 24 hours, after heat preservation, cooled to room temperature,
Spherical structure carbon/ferric metasilicate lithium/composite ferric lithium phosphate material can be obtained.
In following embodiment of the invention, the carbon/ferric metasilicate lithium and carbon/LiFePO4 are prepared by the following method
Arrive: the carbon/ferric metasilicate lithium is by solid phase method using ferrous oxalate, and silica, lithium carbonate, glucose is raw material wherein iron
Source: lithium source: silicon source: carbon source=1:2:1:0.75 (molar ratio) adds the raw material into agate pot and 15mL acetone conduct is added
Agate pot is then placed in setting speed 300rpm on planetary ball mill instrument by dispersing agent, time 2h, obtained slurry in an oven 80
DEG C dry 12h, then grinding is broken goes to burning boat, is warming up to 700 DEG C of heat preservation 12h with 2 DEG C/min, obtains target after natural cooling
Product；Carbon/LiFePO4 is commercially produced product, is purchased from Shenzhen City Beiterui New Energy Materials Co., Ltd, it is characterized in that
200~400nm of primary particle, 0.8 ± 0.2g/cm of tap density3, granularity D50=1.1 ± 0.5 μm, specific surface be 12.0 ±
2.0m2/g。
Embodiment 1
Dispersing carbon/ferric metasilicate lithium of 1g and 99g carbon/LiFePO4 in deionized water and adjusting solid content is 10%,
The mechanical stirring 5h in the case where revolving speed is 80 revs/min of speed, sets spray dryer parameter: inlet air temperature is 180 DEG C, leaving air temp
Be 100 DEG C, atomizer rotating speed be 200 revs/min, wriggling pump speed be 1000ml/h, be spray-dried to obtain presoma, will before
Driving body, 700 DEG C of sintering, heat preservation 12h processing, cooled to room temperature after heat preservation obtain product under inert gas protection.
(1) shape characteristic:
Obtained carbon/ferric metasilicate lithium/composite ferric lithium phosphate material is observed into its pattern, gained using scanning electron microscope analysis
SEM figure is as shown in Figure 1.Show that composite material is spherical structure as shown in figure 1, partial size is 5 microns, and spherical structure is conducive to mention
High battery multiplying power and cycle performance.
(2) electric performance test
Test group: using the obtained carbon/ferric metasilicate lithium/composite ferric lithium phosphate material of the present embodiment as positive electrode with lead
Electric carbon black, Kynoar are mixed with beating according to the mass ratio of 8:1:1, and solvent is N-Methyl pyrrolidone, beating time 8h,
The slurry accomplished fluently uniformly is coated on aluminium foil, 80 DEG C of vacuum drying 12h, then roll-in strikes piece and obtains positive plate, with lithium piece
For to electrode, electrolyte is EC:DEC:DMC=1:1:1 (V/V), the polyethene microporous membrane that diaphragm is 2400 is assembled into button mould
Quasi- battery, is tested after standing 12h.
Contrast groups: the composite material in test group is replaced using carbon/LiFePO4, is fabricated to button simulated battery, is stood
It is tested after 12h.
Under 0.1C, 0.5C, 1C, 2C, 3C different multiplying, sample charge and discharge electrical measurement is carried out in the voltage range of 1.5-4.2V
Examination, and it is as shown in Figure 2 a to obtain chemical property figure, as being shown under 0.1C, 0.5C, 1C, 2C, 3C different multiplying in Fig. 2 a
Specific discharge capacity is 162.1mAh/g, 157.4mAh/g, 153.2mAh/g, 146.6mAh/g, 141.5mAh/g, 162.7mAh/
G, it is more preferable than contrast groups performance, Fig. 2 b is shown in recycled 100 times under 0.1C after capacity retention ratio still have 97.3%, it is shown that the ball
Shape structural carbon/ferric metasilicate lithium/composite ferric lithium phosphate material has excellent high rate performance and cycle performance.
Fig. 3 is that test group and contrast groups test resulting discharge curve for the first time, it can be seen that in specific discharge capacity
In this segment limit of 120mAh/g~150mAh/g, spherical structure carbon/ferric metasilicate lithium/composite ferric lithium phosphate material discharge curve tool
There is ramped feature, and contrast groups are horizontal linear in this section.
Fig. 4 is the SOC-OCV partial enlargement curve graph of test group and contrast groups, it can be seen that spherical structure carbon/ferrosilite
Lithium/composite ferric lithium phosphate material is an inclined curve in remaining capacity 10%-20%, to the curve carry out linear fit its
Degree of fitting is up to 0.9872, show it is in a linear relationship between voltage and specific capacity, can simply by measurement cell voltage it is accurate
Calculate battery SOC, measuring method is, according to the relational expression y=a+b*x of Fig. 4, wherein a=7.74939, b=-0.03925, y generation
Table cell voltage, x represent remaining capacity, and the percentage of remaining capacity can be then calculated after testing to cell voltage.
Embodiment 2
It disperses carbon/ferric metasilicate lithium of 1.5g in deionized water with 98.5g carbon/LiFePO4 and adjusts solid content and be
10%, the mechanical stirring 8h in the case where revolving speed is 100 revs/min of speed, set spray dryer parameter: inlet air temperature is 180 DEG C, out
Air temperature is 100 DEG C, and wriggling pump speed is 300ml/h, and atomizer rotating speed is 250 revs/min, is spray-dried to obtain forerunner
Body, by presoma, 650 DEG C of sintering, heat preservation 12h processing, cooled to room temperature after heat preservation are obtained under inert gas protection
To product.
Embodiment 3
It disperses carbon/ferric metasilicate lithium of 0.5g in deionized water with 99.5g carbon/LiFePO4 and adjusts solid content and be
5%, the mechanical stirring 3h in the case where magnetic agitation rotating speed is 120 revs/min of speed, set spray dryer parameter: inlet air temperature as
180 DEG C, leaving air temp is 100 DEG C, and wriggling pump speed is 1500ml/h, and atomizer rotating speed is 300 revs/min, is spray-dried
Presoma is obtained, presoma 600 DEG C of sintering, heat preservation 8h processing under inert gas protection naturally cool to after heat preservation
Room temperature obtains product.
Embodiment 4
Dispersing carbon/ferric metasilicate lithium of 5g and 95g carbon/LiFePO4 in deionized water and adjusting solid content is 30%,
The mechanical stirring 5h in the case where magnetic agitation rotating speed is 70 revs/min of speed, sets spray dryer parameter: inlet air temperature as 120 DEG C,
Leaving air temp is 90 DEG C, and wriggling pump speed is 800ml/h, and atomizer rotating speed is 200 revs/min, is spray-dried to obtain forerunner
Body, by presoma, 300 DEG C of sintering, heat preservation 12h processing, cooled to room temperature after heat preservation are obtained under inert gas protection
To product.
Embodiment 5
Dispersing carbon/ferric metasilicate lithium of 10g and 90g carbon/LiFePO4 in deionized water and adjusting solid content is 40%,
The mechanical stirring 8h in the case where magnetic agitation rotating speed is 150 revs/min of speed, sets spray dryer parameter: inlet air temperature 300
DEG C, leaving air temp is 150 DEG C, and wriggling pump speed is 1000ml/h, and atomizer rotating speed is 220 revs/min, is spray-dried to obtain
Presoma, by presoma, 800 DEG C of sintering, heat preservation are handled for 24 hours under inert gas protection, and room is naturally cooled to after heat preservation
Temperature obtains product.
Embodiment 2-5 products therefrom is scanned electron microscope analysis and observes its pattern and progress electric performance test, result
Display composite material is spherical structure；Electrical property and carbon/lithium iron phosphate electrode material are excellent on an equal basis, and SOC-OCV is in remaining electricity
Measuring 10%-20% is an inclined curve, carries out linear fit degree of fitting between 0.9610-0.9891 to curve, can use
Battery SOC is accurately calculated in passing through measurement cell voltage.
Above description is the detailed description for the present invention preferably possible embodiments, but embodiment is not limited to this hair
Bright patent claim, it is all the present invention suggested by technical spirit under completed same changes or modifications change, should all belong to
In the covered the scope of the patents of the present invention.
Claims (6)
1. a kind of carbon/ferric metasilicate lithium/composite ferric lithium phosphate material preparation method, it is characterised in that: the method includes as follows
Step: carbon/ferric metasilicate lithium is mixed into addition deionized water with carbon/LiFePO4 and is prepared into slurry, is carried out in spray dryer
It is spraying, mixture is obtained, by this mixture high temperature sintering under inert gas protection, after isothermal holding, cooled to room temperature,
Spherical structure carbon/ferric metasilicate lithium/composite ferric lithium phosphate material can be obtained.
2. carbon according to claim 1/ferric metasilicate lithium/composite ferric lithium phosphate material preparation method, it is characterised in that: institute
It states carbon/ferric metasilicate lithium to mix deionized water is added to be prepared into the specific practice of slurry with carbon/LiFePO4 and is, by carbon/silicic acid
Iron lithium and carbon/LiFePO4 are scattered in deionized water by weight for 0.5%:99.5%~10%:90%, are adjusted to solid
Content is 5%~40% slurry, and low whipping speed is 70~150 revs/min of lower 3~8h of mechanical stirring, is uniformly mixed slurry.
3. carbon according to claim 1/ferric metasilicate lithium/composite ferric lithium phosphate material preparation method, it is characterised in that: institute
When stating spraying, the parameter of the spray dryer of setting are as follows: inlet air temperature is 120~300 DEG C, and leaving air temp is 90~150 DEG C, compacted
Dynamic pump speed is 300~1500ml/h, and atomizer rotating speed is 200~300 revs/min.
4. carbon according to claim 1/ferric metasilicate lithium/composite ferric lithium phosphate material preparation method, it is characterised in that: institute
The specific practice for stating high temperature sintering is that under inert gas protection, sintering temperature is sintered under conditions of being 300~800 DEG C,
Soaking time is 8h~for 24 hours, and after heat preservation, spherical structure carbon/ferric metasilicate lithium/phosphoric acid is can be obtained in cooled to room temperature
Iron lithium composite material.
5. carbon according to claim 1/ferric metasilicate lithium/composite ferric lithium phosphate material preparation method, it is characterised in that: packet
The step of including are as follows:
(1) it disperses carbon/ferric metasilicate lithium and carbon/LiFePO4 in by weight for 0.5%:99.5%~10%:90%
In ionized water, being adjusted to solid content is 5%~40% slurry, and low whipping speed be 70~150 revs/min of lower mechanical stirrings 3~
8h is uniformly mixed slurry；
(2) spray dryer parameter is set, parameter includes: that inlet air temperature is 120~300 DEG C, and leaving air temp is 90~150
DEG C, wriggling pump speed is 300~1500ml/h, and atomizer rotating speed is 200~300 revs/min；
(3) slurry of the step (1) is pumped into spray dryer under agitation and is sprayed, obtain presoma；
(4) under inert gas protection by obtained presoma, sintering temperature is sintered for 300~800 DEG C, and soaking time is
8h~for 24 hours, after heat preservation, spherical structure carbon/ferric metasilicate lithium/LiFePO4 composite wood is can be obtained in cooled to room temperature
Material.
6. preparing resulting carbon/ferric metasilicate lithium/composite ferric lithium phosphate material by any one of claim 1-5.
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| CN115084514A (en) * | 2022-08-09 | 2022-09-20 | 松山湖材料实验室 | Lithium-added polyanion cathode material for lithium battery, preparation method of cathode material and lithium battery |
| CN115084514B (en) * | 2022-08-09 | 2024-05-03 | 松山湖材料实验室 | Lithium battery lithium-added polyanion positive electrode material, preparation method thereof and lithium battery |
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Application publication date: 20190723 |