CN109755518A - The preparation method of carbon-coated LiFePO 4 for lithium ion batteries material - Google Patents
The preparation method of carbon-coated LiFePO 4 for lithium ion batteries material Download PDFInfo
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Abstract
The present invention provides a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries material, including slurrying dispersion steps plus lithium step, grinding steps, drying-granulating step and sintering step.Slurrying dispersion steps include that FeOOH, inorganic acid, phosphoric acid and carbon source are added in solvent to be mixed into slurry and disperse, and react 1h-20h, the additional amount of carbon source is so that the mass percent 1%-7% of carbon is counted in carbon-coated LiFePO 4 for lithium ion batteries material；Adding lithium step includes that lithium source is added in the slurry of dispersion；Grinding steps include the slurry after grinding plus lithium step, grind 0.5h-10h；Drying-granulating step includes that slurry is dried by the method being spray-dried, is granulated and obtains powder；And sintering step includes being sintered powder in inert gas, obtains carbon-coated LiFePO 4 for lithium ion batteries material.
Description
Technical field
The present invention relates to lithium ion anode material technical field, especially a kind of preparation side of carbon-coated LiFePO 4 for lithium ion batteries material
Method.
Background technique
Operating voltage is high, specific capacity is high, self discharge is small, cyclicity is good, long service life, weight because having for lithium ion battery
Gently, outstanding advantages of small in size and the optimization power supply for becoming the portable electronic devices such as mobile phone, laptop.In recent years
Come, the traffic discharged with being on the rise for environmental problem, lithium ion battery in low exhaust gas such as electric car, hybrid vehicles
Application on tool is more and more concerned, and to the safety of lithium ion battery, power and service life, more stringent requirements are proposed for this.
As the important component of lithium ion battery, the research of positive electrode is the research emphasis of people all the time.
Early in 1997, just it has been found that the LiFePO4 with olivine structural can be used as the positive electrode of lithium ion battery.Together
When, LiFePO4 has that stable structure, raw material sources are abundant, safety is good, can use at high temperature, is environmentally friendly, is suitable
Voltage class and higher specific capacity the advantages that, receive the favor of vast scientific research institution and commercial company.But ferric phosphate
The fatal defects that lithium is determined there are one by its lattice structure, that is, extremely low electronic conductivity and ion diffusion rates, greatly
Capacity attenuation is rapid when current charging and discharging, and high rate capability is poor.
Currently, the preparation method of nano-grade lithium iron phosphate mainly has high temperature solid-state method, template synthesis method, hydro-thermal method, co-precipitation
Method, sol-gal process etc..Wherein, high temperature solid-state method is the method for being easiest to realize industrialization, and LiFePO4 industry at present
The main stream approach of change.The preparation process conventional method of high temperature solid-state method is that source of iron, lithium source and P source compound are passed through dispersion, ball
Mill, then lithium iron phosphate positive material is obtained by high temperature sintering.The source of iron of high temperature solid-state method mainly has ferric phosphate, iron oxide, grass
Sour iron is referred to as phosphoric acid iron process, oxidation iron process, oxalic acid iron process.Wherein, ironworker is aoxidized with the water system of water as solvent
Skill, during the sintering process due to iron oxide and phosphorus source, carbon source, lithium source, reaction process are complicated, and the structure of matter changes greatly, lead to crystalline substance
Body structure is poor.Moreover, carbon-coating cladding is difficult, carbon-coating is frangible, and crystal grain is easy to grow up, and can further result in resistivity height, charge and discharge
Performance, high rate performance and poor circulation.
Summary of the invention
The object of the present invention is to provide that can prepare, resistance rate is low, the carbon packet of charge-discharge performance, high rate performance and good cycle
Cover the preparation method of LiFePO 4 material.
In order to solve the above technical problem, the present invention provides a kind of preparation methods of carbon-coated LiFePO 4 for lithium ion batteries material, including
Slurrying dispersion steps plus lithium step, grinding steps, drying-granulating step and sintering step.Slurrying dispersion steps include by hydroxyl
Iron oxide, inorganic acid, phosphoric acid and carbon source, which are added in solvent, to be mixed into slurry and disperses, and 1h-20h, the addition of carbon source are reacted
It measures so that the mass percent 1%-7% of carbon is counted in carbon-coated LiFePO 4 for lithium ion batteries material；Adding lithium step includes being added to lithium source point
In scattered slurry；Grinding steps include the slurry after grinding plus lithium step, grind 0.5h-10h；Drying-granulating step includes that will grind
Slurry after mill is dried by the method being spray-dried, is granulated and is obtained powder；And sintering step includes by powder in inertia
It is sintered in gas, obtains carbon-coated LiFePO 4 for lithium ion batteries material.
Optionally, according to n (Fe): n (PO4)=(0.96~1.01): FeOOH and phosphoric acid is added in 1 molar ratio,
The molar ratio of the lithium in iron and lithium source in FeOOH is n (Fe): n (Li)=(0.96~1.02): (0.98~1.04),
In inorganic acid in ionizable hydrogen ion and FeOOH iron mole ratio be n (H+): n (Fe)=(0.1~0.5):
1, the solid content of slurry is 20%-50%.
Optionally, before drying-granulating step, stabilization aid is added to the stability that slurry is improved in slurry, surely
The additive amount of auxiliary agent is determined for the 0.1%-2% of the gross mass of slurry, and stabilization aid is water solubility copolymer.
Optionally, stabilization aid includes that polyene alcohols water solubility copolymer, polyene acids water-soluble polymer and diluted acid are total
Any one or more in polymers class water-soluble polymer.
Optionally, inorganic acid is one of hydrochloric acid, nitric acid, sulfuric acid, hydrobromic acid, hydroiodic acid and chloric acid or a variety of.
Optionally, carbon source includes organic carbon source, any one or more in inorganic carbon source, organic carbon source be glucose,
One of sucrose, starch, cyclodextrin and polyethylene glycol are a variety of, and inorganic carbon source is superconductive carbon black (Super P), Ketjen black
And one of acetylene black or a variety of.
Optionally, lithium source is one or both of lithium carbonate and lithium hydroxide.
Optionally, it is spray-dried in drying-granulating step using spray dryer, spray dryer is pressure injection
Any one or more in formula spray dryer, rotary and centrifugal type spray dryer and two-phase streaming spray dryer.
Optionally, the inlet temperature range of drying-granulating step is 200 DEG C -300 DEG C, the exit of drying-granulating step
Temperature range is 60 DEG C -150 DEG C.
Optionally, the mode of the sintering in sintering step is in one-part form sintering, two-part sintering and three-stage sintering
Any one；The holding temperature of one-part form sintering is 600 DEG C -750 DEG C, and soaking time is -10 hours 1 hour；Two-part sintering
Including first segment sintering and second segment sintering, first segment sintering holding temperature be 300 DEG C -500 DEG C, soaking time be 1 hour -
5 hours, the holding temperature of second segment sintering was 600 DEG C -750 DEG C, and soaking time is -10 hours 1 hour；Three-stage is sintered
First segment sintering, second segment sintering and three-stage sintering, the holding temperature of first segment sintering are 200 DEG C -300 DEG C, soaking time
It is -5 hours 1 hour, the holding temperature of second segment sintering is 450 DEG C -550 DEG C, and soaking time is -3 hours 1 hour, third section
The holding temperature of sintering is 650 DEG C -750 DEG C, and soaking time is -5 hours 1 hour.
As further preferred technical solution or feature, inorganic acid is preferably any in nitric acid, hydrochloric acid and sulfuric acid
It is one or more.
As further preferred technical solution or feature, the reaction time of slurrying dispersion steps is preferably 1h-5h.
As further preferred technical solution or feature, the time of grinding steps is preferably 1h-6h.
As further preferred technical solution or feature, spray dryer be preferably rotary and centrifugal type spray dryer or
Two-phase streaming spray dryer.
As further preferred technical solution or feature, the inlet temperature range of spray drying step is 230 DEG C-
280 DEG C, the outlet temperature range of spray drying step is 80 DEG C -130 DEG C.
As further preferred technical solution or feature, the mode of the sintering in sintering step is preferably that two-part is burnt
Knot, still more preferably for first segment sintering holding temperature be 350 DEG C -500 DEG C, soaking time be -5 hours 2 hours, second
The holding temperature of section sintering is 675 DEG C -725 DEG C, soaking time be -5 hours 1 hour as further preferred technical solution or
Feature, water-soluble polymer are preferably polyvinyl alcohol.
To sum up, the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material of the invention is with phosphoric acid using FeOOH as source of iron
Phosphorus source increases reacting to each other for FeOOH using inorganic acid is added.In liquid phase mixed process, just make FeOOH
Certain reaction occurs with phosphoric acid, generates certain presoma, reduces the side reaction effect of dried feed during the sintering process, thus
Improve electric conductivity, charge-discharge performance, the high rate performance etc. of product.Also, the acidic environment that inorganic acid provides can help carbon
The carbon of the process of cladding, cladding is not easily broken.
Secondly, stabilization aid and presoma have synergistic effect, stability is further increased, the generation of side effect is reduced.
Specific embodiment
With reference to embodiment, the embodiment of the present invention is furthur described in detail.Following instance is for saying
The bright present invention, but be not intended to limit the scope of the invention.
Range mentioned in the present invention includes endpoint value.Fe, PO that the present invention mentions4And H+Respectively refer to iron atom, phosphoric acid
Radical ion and hydrogen ion, and n refers to the amount of substance.Although the solvent in the embodiment of the present invention is deionized water,
The present invention does not do any restriction to the type of solvent, and solvent can also be tap water, industrial water or other organic solvents.
Embodiment 1
(1) by FeOOH, phosphoric acid n (Fe): n (PO in molar ratio4)=0.98:1 and hydrogen ion and FeOOH
Middle iron mole ratio be n (H+): the sulfuric acid of n (Fe)=0.15:1 ratio, and the Portugal calculated by theoretical carbon content for 3%
Grape sugar is add to deionized water, and is mixed into the slurry that solid content is 30%, dispersion, reaction 120min.
(2) lithium carbonate of n (Li): n (Fe)=1.01:1 is added in obtained slurry in step (1), continues to disperse
30min。
(3) obtained slurry in step (2) is added in sand mill and grinds 60min.
(4) gained slurry in step (3) is passed through into two-phase streaming spray dryer, with 235 DEG C of entrance, 90 DEG C of outlet is set
Surely it is dried, is granulated.
(5) by powder obtained in step (4), under nitrogen protection, it is small 3 to be kept the temperature within heat preservation 3 hours, 680 DEG C according to 350 DEG C
When system sintering, obtain the carbon coating phosphoric acid of 0.1C average discharge capacity 154mAh/g, 1C average discharge capacity 138mAh/g
Iron lithium material product.
Embodiment 2
1) by FeOOH, phosphoric acid n (Fe): n (PO in molar ratio4In)=0.96:1 and hydrogen ion and FeOOH
Iron mole ratio be n (H+): n (Fe)=0.3:1 ratio nitric acid, and the cyclodextrin calculated by theoretical carbon content for 2%
It is add to deionized water, is mixed into the slurry that solid content is 25%, dispersion, reaction 60min.
2) lithium carbonate of n (Li): n (Fe)=1.01:1 is added in obtained slurry in step (1), continues to disperse
30min。
(3) obtained slurry in step (2) is added in ball mill and grinds 90min.
(4) gained slurry in step (3) is passed through into rotary and centrifugal type spray dryer, with 255 DEG C of entrance, exports 100 DEG C
Be set for it is dry, be granulated.
(5) by powder obtained in step (4), under nitrogen protection, 2.5 hours, 690 DEG C of heat preservations 3 are kept the temperature according to 410 DEG C
The system sintering of hour, obtains the carbon coating phosphorus of 0.1C average discharge capacity 151mAh/g, 1C average discharge capacity 132mAh/g
Sour iron lithium material product.
Embodiment 3
(1) by FeOOH, phosphoric acid n (Fe): n (PO in molar ratio4)=0.98:1 and hydrogen ion and FeOOH
Middle iron mole ratio be n (H+): the hydrochloric acid of n (Fe)=0.35:1 ratio, and the shallow lake calculated by theoretical carbon content for 5%
Powder is add to deionized water, and is mixed into the slurry that solid content is 20%, dispersion, reaction 90min.
(2) lithium carbonate of n (Li): n (Fe)=1.01:1 is added in obtained slurry in step (1), continues to disperse
30min。
(3) obtained slurry in step (2) is added in sand mill and grinds 90min.
(4) gained slurry in step (3) is passed through into rotary and centrifugal type spray dryer, with 265 DEG C of entrance, exports 105 DEG C
Be set for it is dry, be granulated.
(5) by powder obtained in step (4), under nitrogen protection, it is small 4 to be kept the temperature within heat preservation 2 hours, 675 DEG C according to 500 DEG C
When system sintering, obtain the carbon coating phosphoric acid of 0.1C average discharge capacity 149mAh/g, 1C average discharge capacity 129mAh/g
Iron lithium material product.
Embodiment 4
On the basis of embodiment 1, PVA is added into slurry, detailed process is as follows:
(1) by FeOOH, phosphoric acid n (Fe): n (PO in molar ratio4)=0.98:1 and hydrogen ion and FeOOH
Middle iron mole ratio be n (H+): the sulfuric acid of n (Fe)=0.15:1 ratio, and the Portugal calculated by theoretical carbon content for 3%
Grape sugar is add to deionized water, and is mixed into the slurry that solid content is 30%, the 0.5% of the quality of slurry is added into slurry
PVA, dispersion, reaction 120min.
(2) lithium carbonate of n (Li): n (Fe)=1.01:1 is added in obtained slurry in step (1), continues to disperse
30min。
(3) obtained slurry in step (2) is added in sand mill and grinds 60min.
(4) gained slurry in step (3) is passed through into two-phase streaming spray dryer, with 235 DEG C of entrance, 90 DEG C of outlet is set
Surely it is dried, is granulated.
(5) by powder obtained in step (4), under nitrogen protection, it is small 3 to be kept the temperature within heat preservation 3 hours, 680 DEG C according to 350 DEG C
When system sintering, obtain the carbon coating phosphoric acid of 0.1C average discharge capacity 158mAh/g, 1C average discharge capacity 142mAh/g
Iron lithium material product.
Comparative example 1
(1) by FeOOH, phosphoric acid n (Fe): n (PO in molar ratio4)=0.98:1 and by theoretical carbon content be 3% based on
The glucose of calculation is add to deionized water, and is mixed into the slurry that solid content is 30%, dispersion, reaction 120min.
(2) lithium carbonate of n (Li): n (Fe)=1.01:1 is added in obtained slurry in step (1), continues to disperse
30min。
(3) obtained slurry in step (2) is added in sand mill and grinds 60min.
(4) gained slurry in step (3) is passed through into two-phase streaming spray dryer, with 235 DEG C of entrance, 90 DEG C of outlet is set
Surely it is dried, is granulated.
(5) by powder obtained in step (4), under nitrogen protection, it is small 3 to be kept the temperature within heat preservation 3 hours, 680 DEG C according to 350 DEG C
When system sintering, obtain the carbon coating phosphoric acid of 0.1C average discharge capacity 144mAh/g, 1C average discharge capacity 113mAh/g
Iron lithium material product.
Comparative example 2
(1) by FeOOH, phosphoric acid n (Fe): n (PO in molar ratio4)=0.96:1 and by theoretical carbon content be 2% based on
The cyclodextrin of calculation is add to deionized water, and is mixed into the slurry that solid content is 25%, dispersion, reaction 60min.
(2) lithium carbonate of n (Li): n (Fe)=1.01:1 is added in obtained slurry in step (1), continues to disperse
30min。
(3) obtained slurry in step (2) is added in ball mill and grinds 90min.
(4) gained slurry in step (3) is passed through into rotary and centrifugal type spray dryer, with 255 DEG C of entrance, exports 100 DEG C
Be set for it is dry, be granulated.
(5) by powder obtained in step (4), under nitrogen protection, 2.5 hours, 690 DEG C of heat preservations 3 are kept the temperature according to 410 DEG C
The system sintering of hour, obtains the carbon coating phosphorus of 0.1C average discharge capacity 139mAh/g, 1C average discharge capacity 106mAh/g
Sour iron lithium material product.
Comparative example 3
(1) by FeOOH, phosphoric acid n (Fe): n (PO in molar ratio4)=0.98:1 and by theoretical carbon content be 5% based on
The starch of calculation is add to deionized water, and is mixed into the slurry that solid content is 20%, dispersion, reaction 90min.
(2) lithium carbonate of n (Li): n (Fe)=1.01:1 is added in obtained slurry in step (1), continues to disperse
30min。
(3) obtained slurry in step (2) is added in sand mill and grinds 90min.
(4) gained slurry in step (3) is passed through into rotary and centrifugal type spray dryer, with 265 DEG C of entrance, exports 105 DEG C
Be set for it is dry, be granulated.
(5) by powder obtained in step (4), under nitrogen protection, it is small 4 to be kept the temperature within heat preservation 2 hours, 675 DEG C according to 500 DEG C
When system sintering, obtain the carbon coating phosphoric acid of 0.1C average discharge capacity 141mAh/g, 1C average discharge capacity 102mAh/g
Iron lithium material product.
Carbon-coated LiFePO 4 for lithium ion batteries material product made from the above embodiment of the present invention 1-4 and comparative example 1-3 carries out electrochemistry
Performance test, as a result as shown in table 1 below.
The electrochemical property test result of table 1 embodiment 1-4 and comparative example 1-3
As can be seen from the above data, when not adding inorganic acid, its 1C of carbon-coated LiFePO 4 for lithium ion batteries material product is flat
Equal discharge capacity and 5C average discharge capacity are very low, and chemical property is obvious undesirable.With ionizable hydrogen from
The concentration of son is continuously increased, and 1C average discharge capacity and 5C average discharge capacity are also continuously improved, and the chemical property the more next
Better.And by the addition of stabilization aid, chemical property, which has, further to be significantly improved.
The preparation method of carbon-coated LiFePO 4 for lithium ion batteries material of the invention, using FeOOH as source of iron, using phosphoric acid as phosphorus source,
Increase reacting to each other for FeOOH using inorganic acid is added.In liquid phase mixed process, just make FeOOH and phosphorus
Certain reaction occurs for acid, generates certain presoma, the side reaction effect of dried feed during the sintering process is reduced, to improve
Electric conductivity, charge-discharge performance, high rate performance of product etc..Also, the acidic environment that inorganic acid provides can help carbon coating
Process, the carbon of cladding is not easily broken.
Secondly, stabilization aid and presoma have synergistic effect, stability is further increased, the generation of side effect is reduced.
The preparation method of carbon-coated LiFePO 4 for lithium ion batteries material of the invention, preparation process is simple, easy to accomplish, and preparation efficiency is high, industrialization
It is high to produce adaptability.
Although the present invention is disclosed above by preferred embodiment, however, it is not intended to limit the invention, this any known skill
Skill person can make some changes and embellishment without departing from the spirit and scope of the present invention, therefore protection scope of the present invention is worked as
Subject to claims range claimed.
Claims (10)
1. a kind of preparation method of carbon-coated LiFePO 4 for lithium ion batteries material characterized by comprising
Slurrying dispersion steps: FeOOH, inorganic acid, phosphoric acid and carbon source are added in solvent and is mixed into slurry and divides
Dissipate, react 1h-20h, the additional amount of the carbon source so that in the carbon-coated LiFePO 4 for lithium ion batteries material carbon mass percent 1%-
7% meter；
Add lithium step: lithium source is added in the slurry of dispersion；
Grinding steps: the slurry after grinding plus lithium step grinds 0.5h-10h；
Drying-granulating step: the slurry after grinding is dried by the method being spray-dried, is granulated and obtains powder；And
Sintering step: the powder is sintered in inert gas, obtains the carbon-coated LiFePO 4 for lithium ion batteries material.
2. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material as described in claim 1, which is characterized in that according to n (Fe): n
(PO4)=(0.96~1.01): the FeOOH and phosphoric acid is added in 1 molar ratio, iron in the FeOOH and
The molar ratio of lithium in the lithium source is n (Fe): n (Li)=(0.96~1.02): (0.98~1.04), in the inorganic acid
In ionizable hydrogen ion and the FeOOH iron mole ratio be n (H+): n (Fe)=(0.1~0.5): 1, it is described
The solid content of slurry is 20%-50%.
3. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material as described in claim 1, which is characterized in that in the drying-granulating
Before step, stabilization aid is added to the stability that the slurry is improved in slurry, the additive amount of the stabilization aid is
The 0.1%-2% of the gross mass of the slurry, the stabilization aid are water solubility copolymer.
4. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material as claimed in claim 3, which is characterized in that the stabilization aid packet
It includes any in polyene alcohols water solubility copolymer, polyene acids water-soluble polymer and diluted acid copolymer analog water-soluble polymer
It is one or more.
5. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material as described in claim 1, which is characterized in that the inorganic acid is
One of hydrochloric acid, nitric acid, sulfuric acid, hydrobromic acid, hydroiodic acid and chloric acid are a variety of.
6. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material as described in claim 1, which is characterized in that the carbon source includes
Any one or more in machine carbon source, inorganic carbon source, the organic carbon source are glucose, sucrose, starch, cyclodextrin and poly- second
One of glycol is a variety of, and the inorganic carbon source is superconductive carbon black, one of Ketjen black and acetylene black or a variety of.
7. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material as described in claim 1, which is characterized in that the lithium source is carbonic acid
One or both of lithium and lithium hydroxide.
8. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material as described in claim 1, which is characterized in that the drying-granulating step
It is spray-dried in rapid using spray dryer, the spray dryer is injection bowl spray dryer, rotating centrifugal
Any one or more in formula spray dryer and two-phase streaming spray dryer.
9. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material as claimed in claim 8, which is characterized in that the drying-granulating step
Rapid inlet temperature range is 200 DEG C -300 DEG C, and the outlet temperature range of the drying-granulating step is 60 DEG C -150 DEG C.
10. the preparation method of carbon-coated LiFePO 4 for lithium ion batteries material as described in claim 1, which is characterized in that the sintering step
In sintering mode be one-part form sintering, two-part sintering and three-stage sintering in any one；The one-part form sintering
Holding temperature be 600 DEG C -750 DEG C, soaking time be -10 hours 1 hour；Two-part sintering include first segment sintering and
Second segment sintering, the holding temperature of first segment sintering are 300 DEG C -500 DEG C, and soaking time is -5 hours 1 hour, second segment sintering
Holding temperature be 600 DEG C -750 DEG C, soaking time be -10 hours 1 hour；Three-stage sintering include first segment sintering,
Second segment sintering and three-stage sintering, the holding temperature of first segment sintering are 200 DEG C -300 DEG C, and soaking time is 1 hour -5 small
When, the holding temperature of second segment sintering is 450 DEG C -550 DEG C, and soaking time is -3 hours 1 hour, the heat preservation temperature of three-stage sintering
Degree is 650 DEG C -750 DEG C, and soaking time is -5 hours 1 hour.
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| CN111081319B (en) * | 2019-11-01 | 2023-07-25 | 力神（青岛）新能源有限公司 | Modeling method for carbon content of positive electrode material |
| CN116354326A (en) * | 2023-02-28 | 2023-06-30 | 中南大学 | Preparation method of lithium ion battery anode material lithium iron phosphate |
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