CN105977456A - Solid-phase synthesis method for preparing LiMn1-xFexPO4/C composite material - Google Patents
Solid-phase synthesis method for preparing LiMn1-xFexPO4/C composite material Download PDFInfo
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Abstract
The invention relates to a solid-phase synthesis method for preparing a LiMn1-xFexPO4/C composite material. The preparation process comprises the following steps: amphiphilic organic matter (such as oleylamine, oleic acid, etc.) which is used as a surfactant is dissolved in a certain amount of a non-polar organic solvent (such as acetone, carbon tetrachloride, cyclohexane, etc.) to form a solution 1; the solution 1 is mixed with lithium salt, divalent manganese salt, ferrous salt, phosphate and a carbon source material at a certain stoichiometric ratio to obtain a mixture; and the mixture successively undergoes wet ball-milling, drying, pre-sintering and calcination so as to obtain the nanoscaleLiMn1-xFexPO4/C composite cathode material for a lithium ion battery. According to the preparation method, the amphiphilic surfactant and the non-polar organic solvent are introduced on the basis of a traditional soilid-phase synthesis method so as to prepare the LiMn1-xFexPO4/C composite material with the particle size of 5-60 nm. The invention provides a feasible scheme for large-scale preparation of the nanoscale lithium ferromanganese phosphate material.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, particularly relate to a kind of lithium ion battery positive pole
LiMn1-xFexPO4The synthetic method of/C composite.
Background technology
Anode material for lithium-ion batteries is the maximum bottleneck of limiting lithium ion cell development.The iron phosphate lithium positive pole material of olivine-type
Material has Stability Analysis of Structures, good cycle, low cost, the advantage such as safe and environment-friendly, is to study the deepest widest lithium ion
One of cell positive material.But its relatively low embedding de-lithium current potential (3.4Vvs.Li/Li+) cause its energy density low.It is all
The lithium manganese phosphate material of olivine-type structure, its theoretical specific capacity identical with LiFePO4 (170mAh/g), but lithium manganese phosphate
Embedding de-lithium current potential be 4.1Vvs.Li/Li+, therefore the theoretical energy density of lithium manganese phosphate is LiFePO4 theoretical energy density
1.2 again.But the electronic conductivity of lithium manganese phosphate and lithium ion diffusion coefficient are far below LiFePO4, cause pure phosphoric acid manganese lithium
The chemical property extreme difference of material, limits its actual application.Recent research result indicate that and part manganese in lithium manganese phosphate is used
After ferrum replaces, the iron manganese phosphate lithium material of formation, not only there is high theoretical energy density but also there is preferable chemical property,
Substitution material as LiFePO4 has huge using value.
Currently the preparation modification approach of iron manganese phosphate lithium material mainly being had two kinds, one is by effective bag carbon to improve material
The electronic conductivity of material, one is by iron manganese phosphate for lithium granule nanorize, to shorten effective the evolving path of lithium ion, improves
The chemical property of material.Although having been reported that the methods such as employing solvent-thermal method, liquid phase co-electrodeposition method, hydro-thermal method obtain nanometer
The iron manganese phosphate lithium material of size, but these preparation methoies are relatively costly, and preparation flow is complicated, is difficult to large-scale production.High
Temperature solid phase method have simple to operate, condition is easy to get, low cost, the advantage such as industrialized production that is suitable for, but traditional solid state reaction
The iron manganese phosphate lithium material primary particle that method obtains is bigger, it is more difficult to obtain the iron manganese phosphate for lithium of nano-scale.
Summary of the invention
The method of the present invention introduces amphiphilic surfactant and non-polar organic solvent on the basis of conventional solid synthetic method
Prepare the LiMn that particle diameter is 5-60nm1-xFexPO4/ C composite, it is provided that one prepares nano-scale phosphorus on a large scale
The feasible scheme of acid ferromanganese lithium material.
The method of the present invention uses amphipathic Organic substance (such as oleyl amine, oleic acid etc.) as surfactant, surfactant pole
Property group one end adsorb in surface of active material, the other end nonpolar long-chain hydrocarbon chain is stretched in non-polar solven, formed glue
Binding structure.This micellar structure and carbon source can effectively prevent growing up and reuniting of crystal grain, in burn-in process surfactant and
The gas such as carbon dioxide, carbon monoxide is released in carbon source pyrolysis, can be internally generated substantial amounts of pore at material, in last calcining
During pyrolysis after surfactant and carbon source carbonization, formed carbon-coating be coated on iron manganese phosphate for lithium primary particle, improve material
The electronic conductivity of material.
Use LiMn prepared by the inventive method1-xFexPO4/ C composite specific surface area is 20-90m2/ g, primary particle
Particle diameter is 5-60nm, and the average pore size of composite inner hole is that in 3-80nm, and this composite, carbon element content is
1-20wt%, the composition formula of this composite is LiMn1-xFexPO4/C(0≤x≤1)。
A kind of LiMn that the present invention provides1-xFexPO4The solid phase synthesis process of/C composite, the method includes following preparation
Step:
Step 1: join amphipathic surfactant in nonpolar organic solvent and stir formation mixed solution；
Step 2: that lithium salts, manganous salt, ferrous salt, phosphate, carbon source and the step 1 of certain stoichiometric proportion are prepared is mixed
Close solution and obtain mixed slurry by dispersing modes such as ball milling, high-energy ball milling or sand millings, be dried acquisition precursors；
Step 3: by the presoma of step 2 gained in protective atmosphere, carries out pre-burning at 300-450 DEG C, the process time of pre-burning
For 3-6 hour, carbon source and unnecessary surfactant being pyrolyzed, then make annealing treatment, the material after annealing is ground
Process；
Step 4: by the material that processes through step 3 in protective atmosphere, calcining at 600-750 DEG C, calcination time is 6-12
Hour, then make annealing treatment.
Compared with prior art, advantages of the present invention has:
(1) described LiMn1-xFexPO4In/C composite, the particle diameter of the primary particle of iron manganese phosphate for lithium is at Nano grade, and
Composite inner has substantial amounts of nano aperture, when as anode material for lithium-ion batteries, shows good electrochemistry
Energy.
(2) described LiMn1-xFexPO4/ C composite uses the preparation method of high temperature solid-state, and this preparation method has operation letter
List, condition are easy to get, low cost, the advantage of applicable large-scale industrial production.
Accompanying drawing explanation
Fig. 1 is the LiMn of preparation in embodiment 10.8Fe0.2PO4The XRD figure spectrum of/C composite.
Fig. 2 is the LiMn of preparation in embodiment 10.8Fe0.2PO4Scanning electron microscope (SEM) photo of/C composite.
Fig. 3 is the LiMn of preparation in embodiment 20.8Fe0.2PO4Scanning electron microscope (SEM) photo of/C/CNT composite.
Fig. 4 is the LiMn of preparation in embodiment 10.8Fe0.2PO4Isothermal nitrogen adsorption desorption (BET) curve of/C composite.
Fig. 5 is the LiMn of preparation in embodiment 10.8Fe0.2PO4/ C composite is as the head of anode material for lithium-ion batteries 0.05C
Secondary charging and discharging curve.
Fig. 6 is the LiMn of preparation in embodiment 10.8Fe0.2PO4/ C composite is as the circulation of anode material for lithium-ion batteries 1C
Performance.
Detailed description of the invention
In order to be able to further appreciate that technical scheme, below in conjunction with specific embodiment, the present invention is done the most in detail
Describe.It is understood that specific embodiment described herein is only in order to further illustrate inventive feature, and need not
In limiting the present invention.
Embodiment 1
Taking 6mL oleic acid to be dissolved in 60mL acetone soln, stirring is configured to uniform solution S O1, takes
2.041gCH3COOLi·2H2O、3.921g(CH3COO)2Mn·4H2O、0.720gFeC2O4·2H2O、2.301g
NH4H2PO4, 1.0g sucrose adds in ball grinder, with the rotating speed ball milling 20h of 550rpm together with solution S O1.First ball
In mixture after mill is placed on fume hood, ventilation process 12h tentatively removes the acetone soln in mixture, then does in 65 DEG C of vacuum
It is dried 12h under conditions of dry, obtains the block persursor material being dried.This presoma is placed in tube furnace, at argon-hydrogen
The protective atmosphere of gaseous mixture (volume fraction of hydrogen is 8%) is warming up to 400 DEG C with the programming rate of 5 DEG C/min, 400 DEG C
Constant temperature 5 hours, then in the protective atmosphere of argon-hydrogen gaseous mixture (volume fraction of hydrogen is 8%) Temperature fall to room
Temperature, is next ground material processing.Material after grinding is placed in tube furnace, at argon-hydrogen gaseous mixture (hydrogen
Volume fraction be 8%) protective atmosphere is warming up to 600 DEG C with the programming rate of 5 DEG C/min, 600 DEG C of constant temperature 10h,
In argon-hydrogen gaseous mixture (volume fraction of hydrogen is 8%) protective atmosphere, Temperature fall is to room temperature, i.e. obtains
LiMn0.8Fe0.2PO4/ C composite.
XRD test result (Fig. 1) shows, XRD spectral line is consistent with PDF card #74-0375, illustrates had
There is the LiMn of olivine structural0.8Fe0.2PO4Material.This is can be seen that from the stereoscan photograph (Fig. 2) of this material
LiMn0.8Fe0.2PO4The primary particle particle diameter of/C composite is at about 40nm.Inhale de-from the BET isothermal nitrogen of this material
Attached curve (Fig. 4) can be seen that this LiMn0.8Fe0.2PO4The specific surface area of/C composite is about 56.3m2/ g, in material
There is substantial amounts of pore space structure in portion, and the average pore size of hole is 6nm.With the LiMn synthesized0.8Fe0.2PO4/ C composite is
Positive pole, with lithium metal as negative pole, is assembled into fastening lithium ionic cell, carries out electrochemical property test.Record at room temperature condition
Under, under 0.05C multiplying power, LiMn0.8Fe0.2PO4/ C composite first discharge specific capacity is 157mAh/g (Fig. 5),
LiMn0.8Fe0.2PO4/ C composite 1C circulation 50 circle still has the specific discharge capacity (Fig. 6) of 113mAh/g.
Embodiment 2
Taking 6mL oleic acid to be dissolved in 60mL acetone soln, stirring is configured to uniform solution S O2, takes
2.041gCH3COOLi·2H2O、3.921g(CH3COO)2Mn·4H2O、0.720gFeC2O4·2H2O、2.301g
NH4H2PO4, 1.0g sucrose, 0.065g CNT (CNT) add in ball grinder, with 550rpm together with solution S O2
Rotating speed ball milling 20h.In first the mixture after ball milling being placed on fume hood, ventilation process 12h tentatively removes third in mixture
Ketone solution, then under conditions of 65 DEG C of vacuum drying, it is dried 12h, obtain the block persursor material being dried.By this presoma
It is placed in tube furnace, with the liter of 5 DEG C/min in the protective atmosphere of argon-hydrogen gaseous mixture (volume fraction of hydrogen is 8%)
Temperature speed is warming up to 400 DEG C, and 400 DEG C of constant temperature 5 hours, then argon-hydrogen gaseous mixture (volume fraction of hydrogen is 8%)
Protective atmosphere in Temperature fall to room temperature, next material is ground process.Material after grinding is placed in tube furnace
In, it is warming up to the programming rate of 5 DEG C/min in argon-hydrogen gaseous mixture (volume fraction of hydrogen is 8%) protective atmosphere
600 DEG C, 600 DEG C of constant temperature 10h, in argon-hydrogen gaseous mixture (volume fraction of hydrogen is 8%) protective atmosphere, Temperature fall arrives
Room temperature, i.e. obtains LiMn0.8Fe0.2PO4/ C/CNT composite.
Embodiment 3
Taking 6mL oleyl amine to be dissolved in 60mL tetrachloromethane solution, stirring is configured to uniform solution S O3, takes
2.041gCH3COOLi·2H2O、2.941g(CH3COO)2Mn·4H2O、1.439gFeC2O4·2H2O、2.301g
NH4H2PO4, 1.4g glucose add in high-energy ball milling tank together with solution S O3, ball milling 1 hour.Mixing after ball milling
Compound is placed on the tetrachloromethane solution that ventilation process 24h in fume hood tentatively removes in mixture, more vacuum drying at 80 DEG C
Under the conditions of be dried 12h, obtain the block persursor material being dried.This presoma is placed in tube furnace, in argon-hydrogen mixing
Gas (volume fraction of hydrogen is 5%) protective atmosphere is warming up to 450 DEG C with the programming rate of 5 DEG C/min, 450 DEG C of constant temperature
3 hours, then in argon-hydrogen gaseous mixture (volume fraction of hydrogen is 5%) protective atmosphere, Temperature fall, to room temperature, connect down
It is ground material processing.Material after grinding is placed in tube furnace, at argon-hydrogen gaseous mixture (volume integral of hydrogen
Number is 5%) protective atmosphere is warming up to 600 DEG C with the programming rate of 5 DEG C/min, 600 DEG C of constant temperature 8h, in argon-hydrogen mixing
In gas (volume fraction of hydrogen is 5%) protective atmosphere, Temperature fall is to room temperature, i.e. obtains LiMn0.6Fe0.4PO4/ C is combined
Material.
Embodiment 4
Taking 6mL oleyl amine to be dissolved in 60mL acetone soln, stirring is configured to uniform solution S O4, takes
2.041gCH3COOLi·2H2O、3.43g(CH3COO)2Mn·4H2O、1.08gFeC2O4·2H2O、2.301gNH4H2PO4、
1.0g citric acid adds in ball grinder together with solution S O4, with the rotating speed ball milling 16h of 600rpm.The mixing after ball milling
Thing is placed on the tetrachloromethane solution that ventilation process 12h in fume hood tentatively removes in mixture, then at 70 DEG C of vacuum drying bars
It is dried 12h under part, obtains the block persursor material being dried.This presoma is placed in tube furnace, at argon-hydrogen gaseous mixture
(volume fraction of hydrogen is 8%) protective atmosphere is warming up to 400 DEG C with the programming rate of 5 DEG C/min, 400 DEG C of constant temperature 5
Hour, then in argon-hydrogen gaseous mixture (volume fraction of hydrogen is 8%) protective atmosphere, Temperature fall, to room temperature, connects down
It is ground material processing.Material after grinding is placed in tube furnace, at argon-hydrogen gaseous mixture (volume integral of hydrogen
Number is 8%) protective atmosphere is warming up to 650 DEG C with the programming rate of 5 DEG C/min, 650 DEG C of constant temperature 7h, in argon-hydrogen mixing
In gas (volume fraction of hydrogen is 8%) protective atmosphere, Temperature fall is to room temperature, i.e. obtains LiMn0.7Fe0.3PO4/ C is combined
Material.
Embodiment described above is only the description of the several embodiments of the present invention, can not therefore be interpreted as the present invention special
The restriction of profit scope.It should be pointed out that, protected without departing from the claims in the present invention for those of ordinary skill in the art
Under the scope protected, it is also possible to make some deformation and improvement, within these broadly fall into protection scope of the present invention.
Claims (9)
1. prepare LiMn for one kind1-xFexPO4The solid phase synthesis process of/C (0≤x≤1) composite, it is special
Levy and be, including following preparation process:
Step 1: join amphipathic surfactant in nonpolar organic solvent and stir shape
Become mixed solution；
Step 2: by the lithium salts of certain stoichiometric proportion, manganous salt, ferrous salt, phosphate, carbon source and
The mixed solution of step 1 preparation obtains mixing slurry by dispersing modes such as ball milling, high-energy ball milling or sand millings
Material, is dried acquisition precursors；
Step 3: by the presoma of step 2 gained in protective atmosphere, carries out pre-burning at 300-450 DEG C,
The process time of pre-burning is 3-6 hour, carbon source and unnecessary surfactant is pyrolyzed, then carries out
Annealing, the material after annealing is ground processing；
Step 4: by the material that processes through step 3 in protective atmosphere, calcine at 600-750 DEG C,
Calcination time is 6-12 hour, then makes annealing treatment.
Preparation method the most according to claim 1, it is characterised in that live in the surface in described step 1
Property agent one end is polar group, i.e. hydroxyl, carboxyl or amido, the other end be nonpolar have 8～
The long-chain hydrocarbon chain of 20 carbon atoms, these surfactants are oleic acid or oleyl amine.
Preparation method the most according to claim 1, it is characterised in that nonpolar in described step 1
Organic solvent is acetone, carbon tetrachloride, oxolane or hexamethylene.
Preparation method the most according to claim 1, it is characterised in that the lithium salts in step 2 be lithium acetate,
Lithium carbonate, Lithium hydrate or lithium dihydrogen phosphate.
Preparation method the most according to claim 1, it is characterised in that the manganous salt in step 2 be manganese acetate,
Manganese chloride, manganese sulfate or manganese nitrate.
Preparation method the most according to claim 1, it is characterised in that the ferrous salt in step 2 be Ferrox.,
Ferrous chloride, ferrous sulfate or Ferrous acetate.
Preparation method the most according to claim 1, it is characterised in that the phosphate in step 2 is biphosphate
Ammonium, diammonium phosphate or ammonium phosphate.
Preparation method the most according to claim 1, it is characterised in that the carbon source described in step 2 include sucrose,
The mixture of one or more in glucose, lactose, citric acid, CNT, graphene oxide.
Preparation method the most according to claim 1, it is characterised in that the protection described in step 3 and step 4
Property atmosphere is nitrogen, argon or argon-hydrogen mixed gas.
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Cited By (6)
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| CN107623142A (en) * | 2017-09-07 | 2018-01-23 | 山东鸿正电池材料科技有限公司 | A kind of high power lithium ion power battery |
| CN107623112A (en) * | 2017-08-18 | 2018-01-23 | 宁波知能新材料有限公司 | Mix carbon coating lithium iron manganese phosphate anode material of lithium boron phosphate modification and preparation method thereof |
| CN107732176A (en) * | 2017-09-26 | 2018-02-23 | 深圳市德方纳米科技股份有限公司 | The preparation method of nano-scale lithium ion battery anode material |
| CN109417162A (en) * | 2018-09-28 | 2019-03-01 | 宁波致良新能源有限公司 | Anode additive and preparation method thereof, anode and preparation method thereof and lithium ion battery |
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| CN115636402A (en) * | 2022-10-28 | 2023-01-24 | 深圳市德方纳米科技股份有限公司 | Lithium manganese iron phosphate material and preparation method and application thereof |
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| CN107623112B (en) * | 2017-08-18 | 2020-11-13 | 宁波致良新能源有限公司 | Lithium-doped boron phosphate modified carbon-coated lithium manganese iron phosphate cathode material and preparation method thereof |
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| CN109417162A (en) * | 2018-09-28 | 2019-03-01 | 宁波致良新能源有限公司 | Anode additive and preparation method thereof, anode and preparation method thereof and lithium ion battery |
| WO2020062046A1 (en) * | 2018-09-28 | 2020-04-02 | 宁波致良新能源有限公司 | Positive electrode additive and preparation method therefor, positive electrode and preparation method therefor, and lithium ion battery |
| CN109417162B (en) * | 2018-09-28 | 2021-09-21 | 宁波致良新能源有限公司 | Positive electrode additive and preparation method thereof, positive electrode and preparation method thereof, and lithium ion battery |
| JP2022502830A (en) * | 2018-09-28 | 2022-01-11 | 寧波致良新能源有限公司Ningbo Zhiliang New Energy Co., Ltd. | Positive electrode additive and its manufacturing method, positive electrode and its manufacturing method, and lithium ion battery |
| JP7158595B2 (en) | 2018-09-28 | 2022-10-21 | 寧波致良新能源有限公司 | Positive electrode additive and manufacturing method thereof, positive electrode and manufacturing method thereof, and lithium ion battery |
| CN111564622A (en) * | 2020-07-14 | 2020-08-21 | 天能帅福得能源股份有限公司 | Lithium manganese iron phosphate cathode material and preparation method thereof |
| CN115636402A (en) * | 2022-10-28 | 2023-01-24 | 深圳市德方纳米科技股份有限公司 | Lithium manganese iron phosphate material and preparation method and application thereof |
| CN115636402B (en) * | 2022-10-28 | 2024-04-16 | 深圳市德方纳米科技股份有限公司 | Lithium iron manganese phosphate material and preparation method and application thereof |
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