CN105070912A - Preparation method of spherical lithium ion battery cathode material lithium manganese phosphate - Google Patents

Preparation method of spherical lithium ion battery cathode material lithium manganese phosphate Download PDF

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Publication number
CN105070912A
CN105070912A CN201510436183.6A CN201510436183A CN105070912A CN 105070912 A CN105070912 A CN 105070912A CN 201510436183 A CN201510436183 A CN 201510436183A CN 105070912 A CN105070912 A CN 105070912A
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preparation
manganese phosphate
solution
ion battery
ball
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罗绍华
郭克石
王志远
张俊
包硕
吕方
刘东芳
杨悦
孙梅竹
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Northeastern University China
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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
    • 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
    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/139—Processes of manufacture
    • H01M4/1397—Processes of manufacture of electrodes based on inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy
    • 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
    • H01M4/58—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
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • 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 invention discloses a preparation method of a spherical lithium ion battery cathode material lithium manganese phosphate belonging to the technical scope of preparation of novel energy materials. The method comprises the following steps: by a coprecipitation method, with LiOH.H2O and H3PO4 as raw materials, reacting, precipitating and calcining the raw materials to obtain Li3PO4; by a polyhydric alcohol-assisted hydrothermal process, taking MnSO4.H2O and the Li3PO4 for reaction in a PEG400-H2O mixed solution, and centrifuging, drying and sieving the product to obtain LiMnPO4; and carrying out ball-mill mixing and calcining on the LiMnPO4 and ascorbic acid, and finally obtaining the LiMnPO4/C composite material. The LiMnPO4/C composite material prepared by the method is spherical; and the particle sizes are 0.3-2 microns. Compared with an existing preparation method, the product prepared by the method is better in particle size control and inherits the morphology of a precursor; the process is easy to control; the cost is low; the productivity is high; and a novel method is provided for preparation of the lithium manganese phosphate cathode material.

Description

A kind of preparation method of ball-shaped lithium-ion battery anode material lithium manganese phosphate
Technical field
The invention belongs to new energy materials technology of preparing scope, particularly a kind of preparation method of ball-shaped lithium-ion battery anode material lithium manganese phosphate.
Background technology
Lithium ion battery is widely used in portable electronic products field because of features such as its good cycle performance, higher energy density and higher fail safes, and be just progressively developed to the car battery of electric motor car, hybrid electric vehicle, prospect is very wide.In lithium ion battery, positive electrode is most important part, is also the key determining performance of lithium ion battery.Manganese-lithium phosphate anode material has the high voltage of 4.1V, stable in air, fail safe is good, environmental friendliness, and the features such as raw material sources are extensive, have prospect, become the emphasis of current research.
At present, the method and approach preparing lithium manganese phosphate is more, is wherein the most commonly still solid phase method, and as emerging in Central South University Wang Zhi etc., adopt solid phase method to obtain the lithium manganese phosphate of pure phase, but the method Granularity Distribution is uneven, power consumption greatly.In recent years a lot of new method has also been emerged in large numbers, if patent of invention publication number is CN102427131A, name is called the Chinese patent of " lithium manganese phosphate/carbon preparation method of anode material for lithium-ion batteries metal magnesium-doped ", adopt the synthesis path of batch mixing, ball milling, roasting, the lithium manganese phosphate uniform particle sizes obtained, but product fails to inherit the regular morphology of presoma.Patent of invention publication number is CN103050693A, name is called the Chinese patent of " a kind of method preparing spherical LiMnPO 4 anode material ", describes method lithium source, manganese source and phosphorus source being obtained spherical lithium manganese phosphate according to spray pyrolysis after certain ratio batch mixing, microwave sintering.It is even that the program obtains particle size, but higher to equipment requirement.
Summary of the invention
The object of this invention is to provide a kind of preparation method of ball-shaped lithium-ion battery anode material lithium manganese phosphate, it is characterized in that, described method comprises the steps:
1) coprecipitation prepares Li 3pO 4, its concrete preparation process is: be the LiOHH of 0.5 ~ 2.2mol/L by concentration 2after O solution is heated with stirring to 25 ~ 80 DEG C, by the H of 0.5 ~ 2mol/L 3pO 4dropwise joins LiOHH 2in O solution.After dropwising, by solution left standstill, be precipitated product; Above-mentioned precipitated product is washed, and vacuumize, to sieve, at 300 DEG C ~ 400 DEG C, calcine 2 ~ 4h afterwards, obtain canescence Li 3pO 4powder;
2) polyalcohol assisting alcohol-hydrothermal method prepares LiMnPO 4; Its concrete preparation process is: get MnSO 4h 2o and above-mentioned steps 1) Li that synthesizes 3pO 4powder is with Li +: Mn 2+the mol ratio of=1:0.9 ~ 1:1.1 is dissolved in the PEG400-H of equal-volume ratio 2in O mixed solution, vigorous stirring 15min, is transferred in reactor by the mixed solution of gained, after reacting 8 ~ 12h, is cooled to room temperature in homogeneous reactor at 150 ~ 200 DEG C.Product through washing, and vacuumize, to sieve, and obtains LiMnPO 4;
3) LiMnPO is prepared in high-temperature calcination 4/ C composite.By LiMnPO 4fully mix in a little absolute ethyl alcohol with the mass ratio of 8:1 ~ 4:1 with ascorbic acid, ball milling 3 ~ 6h, at 50 DEG C, dry 6 ~ 12h obtains mixed-powder afterwards.Above-mentioned mixed-powder is placed in tube furnace, and under argon atmosphere, 500 ~ 650 DEG C of calcining 3 ~ 6h, obtain spherical LiMnPO after cooling naturally 4/ C composite.
Described step 1) middle LiOHH 2o solution concentration is 0.5 ~ 2.2mol/L, described H 3pO 4solution concentration is 0.5 ~ 2mol/L, and reaction temperature is 25 ~ 80 DEG C.
Described step 1) middle H 3pO 4solution adds LiOHH 2the mode of O solution is for dropwise to add.
In described step 1) through washing, dry, sieve after precipitated product, its calcining heat is 300 ~ 400 DEG C, and calcination time is 2 ~ 4h.
Described step 2) middle MnSO 4h 2o and Li 3pO 4powder is with Li +: Mn 2+the mol ratio of=1:0.9 ~ 1:1.1 is dissolved in the PEG400-H of equal-volume ratio 2in O mixed solution, mixing time is 15min.
Described step 2) mixed solution, the reaction temperature in homogeneous reactor is 150 ~ 200 DEG C, and the reaction time is 8 ~ 12h.
Described step 3) middle LiMnPO 4be 8:1 ~ 4:1 with ascorbic acid mixed proportion, mixing method is ball milling 3 ~ 6h, dry 6 ~ 12h at 50 DEG C after ball milling.
Described step 3) mixed-powder is placed in tube furnace, calcination atmosphere is argon gas, and calcining heat is 500 ~ 650 DEG C, and the time is 3 ~ 6h, and the type of cooling is nature cooling.
The invention has the beneficial effects as follows that synthesis path has that technique is simple, process is easily controlled, cost is low, productive rate advantages of higher, compared with other lithium manganese phosphates preparation method, end product microscopic appearance is better, evenly spherical, inheriting its presoma shape characteristic, providing new method for preparing spherical lithium manganese phosphate.
Accompanying drawing explanation
Fig. 1 is spherical LiMnPO in embodiment 1 4the XRD figure of/C composite positive pole.
Fig. 2 is spherical LiMnPO in embodiment 1 4the SEM figure of/C composite positive pole.
Fig. 3 is spherical LiMnPO in embodiment 2 4the XRD figure of/C composite positive pole.
Fig. 4 is spherical LiMnPO in embodiment 2 4the SEM figure of/C composite positive pole.
Embodiment
The invention provides a kind of preparation method of ball-shaped lithium-ion battery anode material lithium manganese phosphate, below in conjunction with accompanying drawing Fig. 1-Fig. 4 and embodiment 1-5, the present invention is further described.
embodiment 1
Be the LiOHH of 0.5mol/L by concentration 2after O solution 200mL is heated with stirring to 80 DEG C, by the H of 0.5mol/L 3pO 4solution 50mL dropwise joins in above-mentioned LiOH solution.After dropwising, by solution left standstill, be precipitated product.This precipitated product is washed, and vacuumize, to sieve, at 300 DEG C, calcine 2h afterwards, obtain canescence Li 3pO 4powder.
By MnSO 4h 2the Li that O and above-mentioned steps are synthesized 3pO 4powder is with Li +: Mn 2+the mol ratio of=1:0.9 is dissolved in the PEG400-H of 36mL equal-volume ratio 2in O mixed solution, vigorous stirring 15min; Be transferred in reactor by the mixed solution of gained, after reacting 8h, be cooled to room temperature in homogeneous reactor at 150 DEG C, product through washing, and vacuumize, to sieve, and obtains LiMnPO 4.
By above-mentioned LiMnPO 4fully mix in a little absolute ethyl alcohol with the mass ratio of 8:1 with ascorbic acid, ball milling 3h, at 50 DEG C, dry 6h obtains mixed-powder.Above-mentioned mixed-powder is placed in tube furnace, and under ar gas environment, 500 DEG C of calcining 3h, obtain spherical LiMnPO after cooling naturally 4/ C composite positive pole.
embodiment 2
Be the LiOHH of 1.0mol/L by concentration 2after O solution 200mL is heated with stirring to 70 DEG C, by the H of 1.0mol/L 3pO 4solution 50mL dropwise joins in above-mentioned LiOH solution.After dropwising, by solution left standstill, be precipitated product.This precipitated product is washed, and vacuumize, to sieve, at 325 DEG C, calcine 2.5h afterwards, obtain canescence Li 3pO 4powder.
By MnSO 4h 2the Li that O and above-mentioned steps are synthesized 3pO 4powder is with Li +: Mn 2+the mol ratio of=1:0.95 is dissolved in the PEG400-H of 36mL equal-volume ratio 2in O mixed solution, vigorous stirring 15min; Be transferred in reactor by the mixed solution of gained, after reacting 9h, be cooled to room temperature in homogeneous reactor at 160 DEG C, product through washing, and vacuumize, to sieve, and obtains LiMnPO 4.
By above-mentioned LiMnPO 4fully mix in a little absolute ethyl alcohol with the mass ratio of 8:1 with ascorbic acid, ball milling 3.5h, at 50 DEG C, dry 7h obtains mixed-powder.Above-mentioned mixed-powder is placed in tube furnace, and under ar gas environment, 550 DEG C of calcining 4h, obtain spherical LiMnPO after cooling naturally 4/ C composite positive pole.
embodiment 3
Be the LiOHH of 1.7mol/L by concentration 2after O solution 200mL is heated with stirring to 50 DEG C, by the H of 1.5mol/L 3pO 4solution 50mL dropwise joins in above-mentioned LiOH solution.After dropwising, by solution left standstill, be precipitated product.This precipitated product is washed, and vacuumize, to sieve, at 350 DEG C, calcine 3h afterwards, obtain canescence Li 3pO 4powder.
By MnSO 4h 2the Li that O and above-mentioned steps are synthesized 3pO 4powder is with Li +: Mn 2+the mol ratio of=1:1 is dissolved in the PEG400-H of 36mL equal-volume ratio 2in O mixed solution, vigorous stirring 15min; Be transferred in reactor by the mixed solution of gained, after reacting 10h, be cooled to room temperature in homogeneous reactor at 170 DEG C, product through washing, and vacuumize, to sieve, and obtains LiMnPO 4.
By above-mentioned LiMnPO 4fully mix in a little absolute ethyl alcohol with the mass ratio of 16:3 with ascorbic acid, ball milling 5h, at 50 DEG C, dry 10h obtains mixed-powder.Above-mentioned mixed-powder is placed in tube furnace, and under ar gas environment, 600 DEG C of calcining 5h, obtain spherical LiMnPO after cooling naturally 4/ C composite positive pole.
embodiment 4
Be the LiOHH of 2.0mol/L by concentration 2after O solution 200mL is heated with stirring to 35 DEG C, by the H of 1.8mol/L 3pO 4solution 50mL dropwise joins in above-mentioned LiOH solution.After dropwising, by solution left standstill, be precipitated product.This precipitated product is washed, and vacuumize, to sieve, at 375 DEG C, calcine 3.5h afterwards, obtain canescence Li 3pO 4powder.
By MnSO 4h 2the Li that O and above-mentioned steps are synthesized 3pO 4powder is with Li +: Mn 2+the mol ratio of=1:1.05 is dissolved in the PEG400-H of 36mL equal-volume ratio 2in O mixed solution, vigorous stirring 15min; Be transferred in reactor by the mixed solution of gained, after reacting 11h, be cooled to room temperature in homogeneous reactor at 180 DEG C, product through washing, and vacuumize, to sieve, and obtains LiMnPO 4.
By above-mentioned LiMnPO 4fully mix in a little absolute ethyl alcohol with the mass ratio of 4:1 with ascorbic acid, ball milling 4h, at 50 DEG C, dry 7h obtains mixed-powder.Above-mentioned mixed-powder is placed in tube furnace, and under ar gas environment, 550 DEG C of calcining 5h, obtain spherical LiMnPO after cooling naturally 4/ C composite positive pole.
embodiment 5
Be the LiOHH of 2.2mol/L by concentration 2after O solution 200mL is heated with stirring to 25 DEG C, by the H of 2.0mol/L 3pO 4solution 50mL dropwise joins in above-mentioned LiOH solution.After dropwising, by solution left standstill, be precipitated product.This precipitated product is washed, and vacuumize, to sieve, at 400 DEG C, calcine 4h afterwards, obtain canescence Li 3pO 4powder.
By MnSO 4h 2the Li that O and above-mentioned steps are synthesized 3pO 4powder 96 is with Li +: Mn 2+the mol ratio of=1:1.1 is dissolved in the PEG400-H of 36mL equal-volume ratio 2in O mixed solution, vigorous stirring 15min; Be transferred in reactor by the mixed solution of gained, after reacting 12h, be cooled to room temperature in homogeneous reactor at 200 DEG C, product through washing, and vacuumize, to sieve, and obtains LiMnPO 4.
By above-mentioned LiMnPO 4fully mix in a little absolute ethyl alcohol with the mass ratio of 4:1 with ascorbic acid, ball milling 6h, at 50 DEG C, dry 12h obtains mixed-powder.Above-mentioned mixed-powder is placed in tube furnace, and under ar gas environment, 650 DEG C of calcining 6h, obtain spherical LiMnPO after cooling naturally 4/ C composite positive pole.

Claims (8)

1. a preparation method for ball-shaped lithium-ion battery anode material lithium manganese phosphate, is characterized in that, described method comprises the steps:
1) coprecipitation prepares Li 3pO 4, its concrete preparation process is: be the LiOHH of 0.5 ~ 2.2mol/L by concentration 2after O solution is heated with stirring to 25 ~ 80 DEG C, by the H of 0.5 ~ 2mol/L 3pO 4dropwise joins LiOHH 2in O solution, after dropwising, by solution left standstill, be precipitated product, above-mentioned precipitated product is washed, and vacuumize, to sieve, at 300 DEG C ~ 400 DEG C, calcine 2 ~ 4h afterwards, obtain canescence Li 3pO 4powder;
2) polyalcohol assisting alcohol-hydrothermal method prepares LiMnPO 4; Its concrete preparation process is: get MnSO 4h 2o and above-mentioned steps 1) Li that synthesizes 3pO 4powder is with Li +: Mn 2+the mol ratio of=1:0.9 ~ 1:1.1 is dissolved in the PEG400-H of equal-volume ratio 2in O mixed solution, vigorous stirring 15min, is transferred in reactor by the mixed solution of gained, reacts after 8 ~ 12h, be cooled to room temperature in homogeneous reactor at 150 ~ 200 DEG C, and product through washing, and vacuumize, to sieve, and obtains LiMnPO 4;
3) LiMnPO is prepared in high-temperature calcination 4/ C composite, by LiMnPO 4fully mix in a little absolute ethyl alcohol with the mass ratio of 8:1 ~ 4:1 with ascorbic acid, ball milling 3 ~ 6h, at 50 DEG C, dry 6 ~ 12h obtains mixed-powder afterwards; above-mentioned mixed-powder is placed in tube furnace; under argon atmosphere, 500 ~ 650 DEG C of calcining 3 ~ 6h, obtain spherical LiMnPO after cooling naturally 4/ C composite.
2. the preparation method of a kind of ball-shaped lithium-ion battery anode material lithium manganese phosphate according to claim 1, is characterized in that, step 1) described LiOHH 2o solution concentration is 0.5 ~ 2.2mol/L, described H 3pO 4solution concentration is 0.5 ~ 2mol/L, and reaction temperature is 25 ~ 80 DEG C.
3. the preparation method of a kind of ball-shaped lithium-ion battery anode material lithium manganese phosphate according to claim 1, is characterized in that, step 1) described H 3pO 4solution adds LiOHH 2the mode of O solution is for dropwise to add.
4. the preparation method of a kind of ball-shaped lithium-ion battery anode material lithium manganese phosphate according to claim 1, is characterized in that, step 1) described through washing, dry, sieve after precipitated product, its calcining heat is 300 ~ 400 DEG C, and calcination time is 2 ~ 4h.
5. the preparation method of a kind of ball-shaped lithium-ion battery anode material lithium manganese phosphate according to claim 1, is characterized in that, step 2) described MnSO 4h 2o and Li 3pO 4powder is with Li +: Mn 2+the mol ratio of=1:0.9 ~ 1:1.1 is dissolved in the PEG400-H of equal-volume ratio 2in O mixed solution, mixing time is 15min.
6. the preparation method of a kind of ball-shaped lithium-ion battery anode material lithium manganese phosphate according to claim 1, is characterized in that, step 2) described mixed solution, the reaction temperature in homogeneous reactor is 150 ~ 200 DEG C, and the reaction time is 8 ~ 12h.
7. the preparation method of a kind of ball-shaped lithium-ion battery anode material lithium manganese phosphate according to claim 1, is characterized in that, step 3) described LiMnPO 4be 8:1 ~ 4:1 with ascorbic acid mixed proportion, mixing method is ball milling 3 ~ 6h, dry 6 ~ 12h at 50 DEG C after ball milling.
8. the preparation method of a kind of ball-shaped lithium-ion battery anode material lithium manganese phosphate according to claim 1, is characterized in that, step 3) described mixed-powder is placed in tube furnace, calcination atmosphere is argon gas, calcining heat is 500 ~ 650 DEG C, and the time is 3 ~ 6h, and the type of cooling is nature cooling.
CN201510436183.6A 2015-07-23 2015-07-23 Preparation method of spherical lithium ion battery cathode material lithium manganese phosphate Pending CN105070912A (en)

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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106957049A (en) * 2017-05-09 2017-07-18 东北大学 A kind of method for preparing nanoscale lithium manganese phosphate
CN106981648A (en) * 2017-06-05 2017-07-25 东北大学秦皇岛分校 Composite positive pole, its preparation method and the lithium ion battery comprising the composite positive pole
CN112018364A (en) * 2020-09-05 2020-12-01 河南科技学院 Equimolar hydrothermal method for preparing LiMnPO4Method for preparing composite material and application of composite material in lithium battery
CN112456464A (en) * 2020-11-25 2021-03-09 安徽工业大学 Method for preparing electrode material by using eutectic salt

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103258994A (en) * 2013-05-06 2013-08-21 天津巴莫科技股份有限公司 Positive material for lithium ion battery, preparation method of material, and lithium ion battery
CN104577123A (en) * 2015-02-02 2015-04-29 哈尔滨工业大学 Preparation method of cathode material for lithium ion cell
CN104701539A (en) * 2013-12-07 2015-06-10 天津赫维科技有限公司 Method for preparing lithium-manganese phosphate positive material by adopting wet-chemical method

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103258994A (en) * 2013-05-06 2013-08-21 天津巴莫科技股份有限公司 Positive material for lithium ion battery, preparation method of material, and lithium ion battery
CN104701539A (en) * 2013-12-07 2015-06-10 天津赫维科技有限公司 Method for preparing lithium-manganese phosphate positive material by adopting wet-chemical method
CN104577123A (en) * 2015-02-02 2015-04-29 哈尔滨工业大学 Preparation method of cathode material for lithium ion cell

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106957049A (en) * 2017-05-09 2017-07-18 东北大学 A kind of method for preparing nanoscale lithium manganese phosphate
CN106981648A (en) * 2017-06-05 2017-07-25 东北大学秦皇岛分校 Composite positive pole, its preparation method and the lithium ion battery comprising the composite positive pole
CN112018364A (en) * 2020-09-05 2020-12-01 河南科技学院 Equimolar hydrothermal method for preparing LiMnPO4Method for preparing composite material and application of composite material in lithium battery
CN112456464A (en) * 2020-11-25 2021-03-09 安徽工业大学 Method for preparing electrode material by using eutectic salt

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Application publication date: 20151118