CN108539174A - A kind of preparation method of ferrous phosphate lithium/carbon composite material - Google Patents
A kind of preparation method of ferrous phosphate lithium/carbon composite material Download PDFInfo
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- CN108539174A CN108539174A CN201810361573.5A CN201810361573A CN108539174A CN 108539174 A CN108539174 A CN 108539174A CN 201810361573 A CN201810361573 A CN 201810361573A CN 108539174 A CN108539174 A CN 108539174A
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- 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 preparation methods of nano-lithium iron phosphate/carbon composite of coated with carbon, and iron powder is dissolved with phosphoric acid, Orqanics Monomer is dissolved in the water, and then mix two kinds of solution of above-mentioned gained, are slowly added to oxidant reaction.Again the nano ferric phosphate presoma of polymer overmold is obtained after filter, washing, drying；The regular hour will be handled with certain heat treatment temperature in mixed atmosphere after the nano ferric phosphate presoma of obtained polymer overmold and the uniform ball milling mixing of lithium source, obtains nano-lithium iron phosphate/carbon composite.Synthesis technology of the present invention is simple, and the nano ferric phosphate presoma of polymer overmold is obtained by one-step oxidation process, and process conditions are easily controllable, and source of iron is of low cost, and phosphoric acid can be recycled, and is not necessarily to Additional carbon sources, and production cost is low.
Description
Technical field
The present invention relates to a kind of preparation method of anode material for lithium-ion batteries, more particularly to a kind of ferrous phosphate lithium/carbon
The preparation method of composite material.
Background technology
LiFePO 4 (the LiFePO of olivine structural4) positive electrode is abundant with raw material resources, cheap, heat
Stability and chemical stability are good, have extended cycle life, it is safe the advantages that paid close attention to by numerous researchers.But in reality
There is also some shortcomings, electron conductions poor (10 in the production and application on border-10~10-9S/cm), and due to lithium ion only
It can be along [010] one-dimensional channel transfer, lithium ion diffusion velocity low (about 10-14cm2/ s), make to polarize in charge and discharge process
Seriously.Currently, mainly material is modified using the methods of conductive material cladding, nanosizing, pattern control and element doping,
Improve the chemical property of material.Wherein nanosizing can shorten Li+With time of the electronics needed for from bulk diffusion to electrolyte,
Improve Li+Diffusion rate；Surface cladding can improve transmission of the electronics between material interface.It is received at present about carbon coating preparation
The research of rice LiFePO4 is more, the method that Patent CN101944601A is disclosed use the obtained grain size of phase crystallisation for 20~
The ferric lithium phosphate precursor of 100nm, then be sufficiently mixed in the solution with nanoscale charcoal, sintering obtains the nanometer phosphorus of uniform charcoal cladding
Sour iron lithium.This carbon coating belongs to the cladding after synthesis, increases preparation section.Patent CN103367722A prepares charcoal cladding phosphorus
Amphipathic Carbon Materials and ethylene glycol are configured to suspension by the method for sour iron lithium composite material, and it includes hydrogen to be added in suspension
The source of iron of the lithium source of lithia and phosphorus source and ferrous sulfate including phosphoric acid is stirred reaction, then is placed in pyroreaction kettle
Solvent thermal reaction is carried out, is placed in retort and is heat-treated, the charcoal that particle size is 30~100nm is obtained and coats ferric phosphate
Lithium composite material.It needs to carry out solvent thermal reaction using autoclave in building-up process, technological process is complicated, and equipment requirement is high.
Invention content
The present invention is intended to provide a kind of preparation method of ferrous phosphate lithium/carbon composite material, can be prepared carbon-coated
The composite material of nano-lithium iron phosphate/carbon, the high rate performance and cycle performance of material are preferable.The present invention passes through following scheme reality
It is existing.
A kind of preparation method of ferrous phosphate lithium/carbon composite material, includes the following steps：
(I) it is added in phosphoric acid or/and phosphoric acid solution 1 metal iron powder to form solution A to being completely dissolved in 25~100 DEG C,
The polymerizable Orqanics Monomer dissolving that is added to the water for forming conjugated chain is formed into solution B, the mass concentration of Orqanics Monomer is
0.1%~50%；The amount ratio of the substance of metal iron powder and phosphoric acid is (0.1~2):1；
(II) at 25~100 DEG C, oxidant water will be added thereto in two kinds of solution mixed processes of A, B obtained by step (I)
The mass concentration of solution, oxidant is 0.1%~50%；Reaction 0.5~for 24 hours；Product after reaction obtains solid-state after separation
Polymer overmold nano ferric phosphate presoma and phosphoric acid solution 2；The oxidant is selected from per-type oxidizer, alkali gold
Belong to persulfide, over cure ammonium, alkali metal hydracid salt compounds, hydracid ammonium, alkali metal hypohalite, hypohalogenous acids ammonium, peroxide
Change one or more mixtures in benzoyl, perbenzoic acid, peroxidating diethyl propyl benzene；
(III) by the nano ferric phosphate presoma of the solid polymer overmold obtained by step (II) and lithium source ball milling mixing
Afterwards, wherein the amount ratio of the substance of the nano ferric phosphate presoma and lithium source of polymer overmold is 1:(0.9~1.1), containing also
It being heat-treated under conditions of Primordial Qi atmosphere, temperature is 500~800 DEG C, the time 1~for 24 hours.
To reduce the impurity of intermediate reaction product, keep product quality more excellent, the solid polymer packet obtained by (II)
After the nano ferric phosphate presoma that covers is washed-dry, it is used further to (III) step.
In view of environmental protection need, the phosphoric acid solution 1 in (I) step may be used will described (II) step reaction after through point
From phosphoric acid solution 2 mixed with phosphoric acid by the amount of the substance of the phosphoric acid needed for (I) step after the solution that is prepared.
The Orqanics Monomer of polymerizable formation conjugated chain in (I) step is selected from dopamine, Dopamine hydrochloride, inclined fluorine second
Any one or a few mixing in alkene, thiophene, pyrroles, benzene sulfonic acid, aniline, penylene, phenylene ethylene and double alkynes etc., these can
Conductive polymer subclass compound is formed after polymerizeing the aggregated reaction of organic compound for forming conjugated chain.
The reducing atmosphere of (III) step is that reducing atmosphere is reducing gas, reducing gas and nitrogen or/and inert gas
Mixed atmosphere or the mixing atmosphere that can be analyzed to include reducing gas (such as ammonia) in heat treatment temperature, reducing gas is hydrogen
Or/and carbon monoxide.
Compared with existing preparation method, preparation method of the invention has the following advantages：
1, preparation method of the invention can aoxidize the presoma that polymer overmold be prepared with a step, thus with after synthesis
Carbon coating compare, simplified process, process conditions are easily controllable.
2, the present invention directly uses iron powder as source of iron, of low cost.
3, the phosphoric acid of one of raw material of the invention can be recycled, and reduce production cost.
4, nano-lithium iron phosphate/carbon composite obtained by the present invention, 1~6nm of carbon layers having thicknesses of composite material,
Particle size be 10~80nm, carbon coating uniformly, good crystallinity, have preferable high rate performance and cycle performance,
Description of the drawings
1 nano-grade lithium iron phosphate of Fig. 1 embodiments/carbon composite makes lithium ion battery high rate performance test result
1 nano-grade lithium iron phosphate of Fig. 2 embodiments/carbon composite makes cycle performance of lithium ion battery test result
Specific implementation mode
Embodiment 1
By the iron powder of 9g, temperature be 40 DEG C, 500r/min under conditions of stirring and dissolving in 85mL mass concentrations be 20%
Phosphoric acid solution in, 6g aniline is dissolved in heating stirring in 65mL distilled water.Then two kinds of solution of above-mentioned gained are mixed simultaneously
It is placed in the speed high-speed stirred with 800r/min in reactor, the mistake that 30mL mass fractions are 10% is slowly added dropwise in whipping process
Hydrogen oxide reacts 1h.Mixed solution obtains the nano ferric phosphate presoma of polymer overmold after filtration, washing and drying.By hydrogen
Lithia is 1 with nano ferric phosphate presoma molar ratio:1, by lithium hydroxide and the uniform ball milling mixing of nano ferric phosphate presoma
Afterwards, in hydrogen atmosphere, 700 DEG C are warming up to the heating rate of 2 DEG C/min, keeps the temperature 6h, after Temperature fall, obtains carbon layers having thicknesses
For the nano-grade lithium iron phosphate composite material for the coated with carbon that 2~4nm, particle size are 50nm.
The nano-grade lithium iron phosphate prepared using the method for the present invention/carbon composite makes lithium ion battery, and to test it forthright again
Can, the results are shown in Figure 1.The result shows that the material, in 1C charge and discharge, the capacity of battery is still up to 140mAhg-1, lithium ion
Battery has good high rate performance.
The nano-grade lithium iron phosphate prepared using the method for the present invention/carbon composite is made lithium ion battery and tests its cyclicity
Can, the results are shown in Figure 2.The result shows that under 5C multiplying powers, recycled by 160 times, capacity retention ratio is more than 98%, lithium ion
Battery has good cycle performance.
Embodiment 2
The concentrated phosphoric acid of 40mL 85% is taken, 96mL distilled water is added and is diluted to 25%, 15g iron powders are then added, are in temperature
30 DEG C, stirring and dissolving under conditions of 400r/min, meanwhile, 13g thiophene is dissolved in heating stirring in 200mL distilled water.Then
Two kinds of solution of above-mentioned gained are mixed into the speed high-speed stirred being placed in reactor with 750r/min, are slowly added in whipping process
Enter the hydrogen peroxide that 20mL mass fractions are 30%, reacts 3h.Mixed solution obtains polymer packet after filtration, washing and drying
The nano ferric phosphate covered.
By the molar ratio 1 of lithium carbonate and nano ferric phosphate:1 weighs, by lithium carbonate and the uniform ball milling mixing of nano ferric phosphate
Afterwards, in the argon hydrogen mixed atmosphere (H containing volume ratio 5%2) in the heating rate of 5 DEG C/min be warming up to 750 DEG C, keep the temperature 10h, from
So after cooling, the nano-grade lithium iron phosphate for obtaining the surface coating decoration that carbon layers having thicknesses are 1~3nm, particle size is 35nm is compound
Material.
Embodiment 3
The concentrated phosphoric acid of 68.4mL 85% is taken, 513mL distilled water is added and is diluted to 10%, 17g iron powders are then added, normal
Stirring and dissolving under conditions of temperature, 1000r/min, meanwhile, 8g pyrroles is dissolved in heating stirring in 300mL distilled water.Then will
The two kinds of solution mixing of above-mentioned gained are placed in the speed high-speed stirred in reactor with 2000r/min, slowly add in whipping process
Enter the sodium hypochlorite that 5mL mass fractions are 1.0%, reacts 3h.Mixed solution obtains polymer packet after filtration, washing and drying
The nano ferric phosphate covered.
By the molar ratio 1 of lithium carbonate and nano ferric phosphate:1 weighs, after lithium carbonate and the uniform ball milling mixing of nano ferric phosphate,
650 DEG C are warming up to the heating rate of 2 DEG C/min in the mixed atmosphere of carbon monoxide and nitrogen (CO containing volume ratio 5%),
8h is kept the temperature, after Temperature fall, obtains the nanometer phosphoric acid for the surface coating decoration that carbon layers having thicknesses are 3~5nm, particle size is 70nm
Iron lithium composite material.
Embodiment 4
Take the concentrated phosphoric acid of 40mL 85%, 96mL distilled water be added and is diluted to 25%, 15g iron powders are then added, room temperature,
Stirring and dissolving under conditions of 1000r/min, meanwhile, 10g pyrroles is dissolved in heating stirring in 100mL distilled water.It then will be upper
It states two kinds of solution of gained and mixes the speed high-speed stirred being placed in reactor with 1500r/min, be slowly added in whipping process
The peroxidating diethyl propyl benzene that 8mL mass fractions are 1.0% reacts 1h.Mixed solution is polymerize after filtration, washing and drying
The nano ferric phosphate of object cladding.
By the molar ratio 1.05 of lithium hydroxide and nano ferric phosphate:1 weighs, lithium hydroxide and the uniform ball milling of nano ferric phosphate
After mixing, in nitrogen and the hydrogen mixed gas (H for being 10% containing volume ratio2) be warming up to the heating rate of 2 DEG C/min in atmosphere
700 DEG C, 8h is kept the temperature, after Temperature fall, obtains receiving for the surface coating decoration that carbon layers having thicknesses are 2~5nm, particle size is 40nm
Rice composite ferric lithium phosphate material.
Embodiment 5
Take the concentrated phosphoric acid of 20mL85%, 65mL distilled water be added and is diluted to 20%, 9g iron powders are then added, 50 DEG C,
Stirring and dissolving under conditions of 750r/min, meanwhile, 12g dopamines are dissolved in heating stirring in 300mL distilled water.It then will be upper
It states two kinds of solution of gained and mixes the speed high-speed stirred being placed in reactor with 1000r/min, be slowly added in whipping process
The bromic acid nak response 3h that 10mL mass fractions are 30%.Mixed solution obtains receiving for polymer overmold after filtration, washing and drying
Rice ferric phosphate.
By the molar ratio 1 of lithium carbonate and nano ferric phosphate:1 weighs, after lithium carbonate and the uniform ball milling mixing of nano ferric phosphate,
In argon gas and the hydrocarbon gaseous mixture of hydrogenation (CO for being 8% containing a volume ratio) atmosphere 650 are warming up to the heating rate of 3 DEG C/min
DEG C, 5h is kept the temperature, after Temperature fall, obtains the nanometer for the surface coating decoration that carbon layers having thicknesses are 1~3nm, particle size is 60nm
Composite ferric lithium phosphate material.
Embodiment 6
Take the concentrated phosphoric acid of 50mL 85%, 233mL distilled water be added and is diluted to 15%, 30g iron powders are then added, 40 DEG C,
Stirring and dissolving under conditions of 1000r/min, meanwhile, 15g dopamines are dissolved in heating stirring in 350mL distilled water.Then will
The two kinds of solution mixing of above-mentioned gained are placed in the speed high-speed stirred in reactor with 2000r/min, slowly add in whipping process
Enter the sodium peroxydisulfate that 8mL mass fractions are 1.0%, reacts 2h.Mixed solution obtains polymer packet after filtration, washing and drying
The nano ferric phosphate covered.
By the molar ratio 1 of lithium carbonate and nano ferric phosphate:1 weighs, after lithium carbonate and the uniform ball milling mixing of nano ferric phosphate,
Ammonia is passed through in device, in the heating rate of 3 DEG C/min be warming up to 800 DEG C, keep the temperature 12h, after Temperature fall, obtain carbon-coating thickness
The nano-grade lithium iron phosphate composite material for the surface coating decoration that degree is 1~2nm, particle size is 35nm.
Embodiment 7
Take the concentrated phosphoric acid of 20mL85%, 65mL distilled water be added and is diluted to 20%, 10g iron powders are then added, 60 DEG C,
Stirring and dissolving under conditions of 1500r/min, meanwhile, 12g dopamines are dissolved in heating stirring in 300mL distilled water.Then will
The two kinds of solution mixing of above-mentioned gained are placed in the speed high-speed stirred in reactor with 1500r/min, slowly add in whipping process
It is 1.0% perbenzoic acid to enter 8mL mass fractions, reacts 6h.Mixed solution obtains polymer after filtration, washing and drying
The nano ferric phosphate of cladding, separated phosphoric acid solution are prepared 20% phosphoric acid solution, are used for down after being mixed with concentrated phosphoric acid
Primary dissolving iron powder.
By the molar ratio 1.1 of lithium carbonate and nano ferric phosphate:1 weighs, lithium carbonate and the uniform ball milling mixing of nano ferric phosphate
Afterwards, with the liter of 5 DEG C/min in the mixed atmosphere of hydrogen, carbon monoxide and nitrogen (CO, 5% H2 that are 8% containing volume ratio)
Warm speed is warming up to 1000 DEG C, keeps the temperature 8h, after Temperature fall, obtains the table that carbon layers having thicknesses are 1~3nm, particle size is 20nm
The nano-grade lithium iron phosphate composite material of face coating decoration.
Embodiment 8
The concentrated phosphoric acid of 68.4mL 85% is taken, 513mL distilled water is added and is diluted to 10%, 17g iron powders are then added, 50
DEG C, stirring and dissolving under conditions of 500r/min, meanwhile, 10g vinylidenes are dissolved in heating stirring in 200mL distilled water.With
Two kinds of solution of above-mentioned gained are mixed into the speed high-speed stirred being placed in reactor with 1500r/min afterwards, are delayed in whipping process
The slow hypochlorous acid ammonium that 10mL mass fractions are added and are 1.0%, reacts 5h.Mixed solution is polymerize after filtration, washing and drying
The nano ferric phosphate of object cladding.10% phosphoric acid solution is prepared in separated phosphoric acid solution after being mixed with concentrated phosphoric acid, be used for
Dissolving iron powder next time.
By the molar ratio 1 of lithium hydroxide and nano ferric phosphate:1 weighs, and lithium hydroxide and the uniform ball milling of nano ferric phosphate are mixed
After conjunction, 850 DEG C are warming up to the heating rate of 2 DEG C/min in carbon monoxide atmosphere, keep the temperature 10h, after Temperature fall, obtain carbon
The nano-grade lithium iron phosphate composite material for the surface coating decoration that layer thickness is 3~4nm, particle size is 35nm.
It is further to note that specific technical features described in the above specific embodiments, in not lance
In the case of shield, can be combined by any suitable means, in order to avoid unnecessary repetition, the present invention to it is various can
The combination of energy no longer separately illustrates.
In addition, various embodiments of the present invention can be combined randomly, as long as it is without prejudice to originally
The thought of invention, it should also be regarded as the disclosure of the present invention.
Claims (6)
1. a kind of preparation method of ferrous phosphate lithium/carbon composite material, it is characterised in that：Include the following steps, (I) is by metallic iron
Powder is added in phosphoric acid or/and phosphoric acid solution 1 to form solution A to being completely dissolved in 25~100 DEG C, by polymerizable formation conjugated chain
The Orqanics Monomer dissolving that is added to the water forms solution B, and the mass concentration of Orqanics Monomer is 0.1%~50%；Metal iron powder
Amount ratio with the substance of phosphoric acid is (0.1~2):1；
(II) at 25~100 DEG C, aqueous oxidizing agent solution will be added thereto in two kinds of solution mixed processes of A, B obtained by step (I),
The mass concentration of oxidant is 0.1%~50%；Reaction 0.5~for 24 hours；Product after reaction obtains solid polymerization after separation
The nano ferric phosphate presoma and phosphoric acid solution 2 of object cladding；The oxidant is selected from per-type oxidizer, alkali metal over cure
Compound, over cure ammonium, alkali metal hydracid salt compounds, hydracid ammonium, alkali metal hypohalite, hypohalogenous acids ammonium, benzoyl peroxide first
One or more mixtures in acyl, perbenzoic acid, peroxidating diethyl propyl benzene；
(III) by after the nano ferric phosphate presoma of the solid polymer overmold obtained by step (II) and lithium source ball milling mixing,
The amount ratio of the nano ferric phosphate presoma of middle polymer overmold and the substance of lithium source is 1:(0.9~1.1) is containing reducing atmosphere
Under conditions of be heat-treated, temperature is 500~800 DEG C, time 1~for 24 hours.
2. a kind of preparation method of ferrous phosphate lithium/carbon composite material as described in claim 1, it is characterised in that：Described
(II) after the nano ferric phosphate presoma of the solid polymer overmold obtained by is washed-dry, it is used for (III) step.
3. a kind of preparation method of ferrous phosphate lithium/carbon composite material as described in claim 1, it is characterised in that：Described
Phosphoric acid solution 1 in (I) step is the phosphorus that separated phosphoric acid solution 2 presses needed for (I) step after reacting described (II) step
The amount of the substance of acid is prepared after being mixed with phosphoric acid.
4. a kind of preparation method of ferrous phosphate lithium/carbon composite material as described in claim 1, it is characterised in that：Described
(I) Orqanics Monomer of the polymerizable formation conjugated chain in step is selected from dopamine, Dopamine hydrochloride, vinylidene, thiophene, pyrrole
It coughs up, any one or a few the mixing in benzene sulfonic acid, aniline, penylene, phenylene ethylene and double alkynes etc..
5. a kind of preparation method of ferrous phosphate lithium/carbon composite material as described in claim 1, it is characterised in that：Described
(III) reducing atmosphere of step is the mixed atmosphere of reducing gas, reducing gas and nitrogen or/and inert gas or is being heat-treated temperature
It can be analyzed to include the mixed atmosphere of reducing gas when spending.
6. a kind of preparation method of ferrous phosphate lithium/carbon composite material as claimed in claim 5, it is characterised in that：Described
(III) reducing gas of the reducing atmosphere of step is hydrogen or/and carbon monoxide.
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| CN201810361573.5A CN108539174A (en) | 2018-04-20 | 2018-04-20 | A kind of preparation method of ferrous phosphate lithium/carbon composite material |
| PCT/CN2019/078880 WO2019201050A1 (en) | 2018-04-20 | 2019-03-20 | Method for preparing lithium iron phosphate/carbon composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019201050A1 (en) * | 2018-04-20 | 2019-10-24 | 中南大学 | Method for preparing lithium iron phosphate/carbon composite material |
| CN111740113A (en) * | 2020-07-01 | 2020-10-02 | 中南大学 | Preparation method of lithium iron phosphate/carbon nanotube composite positive electrode material |
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| CN113285071B (en) * | 2021-05-14 | 2022-04-26 | 合肥国轩高科动力能源有限公司 | Lithium iron phosphate and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102683695A (en) * | 2011-12-30 | 2012-09-19 | 南昌大学 | Process for preparing LiFePO4/C composite cathode material by precursor in-situ polymerization-carbothermic process |
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| JP5196555B2 (en) * | 2008-08-06 | 2013-05-15 | 独立行政法人産業技術総合研究所 | Method for producing electrode material precursor and method for producing electrode material using the obtained electrode material precursor |
| CN108539174A (en) * | 2018-04-20 | 2018-09-14 | 中南大学 | A kind of preparation method of ferrous phosphate lithium/carbon composite material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102683695A (en) * | 2011-12-30 | 2012-09-19 | 南昌大学 | Process for preparing LiFePO4/C composite cathode material by precursor in-situ polymerization-carbothermic process |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2019201050A1 (en) * | 2018-04-20 | 2019-10-24 | 中南大学 | Method for preparing lithium iron phosphate/carbon composite material |
| CN111740113A (en) * | 2020-07-01 | 2020-10-02 | 中南大学 | Preparation method of lithium iron phosphate/carbon nanotube composite positive electrode material |
| CN111740113B (en) * | 2020-07-01 | 2021-07-16 | 中南大学 | Preparation method of lithium iron phosphate/carbon nanotube composite positive electrode material |
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Application publication date: 20180914 |