CN109004212A - A kind of big multiplying power manganate cathode material for lithium and preparation method thereof - Google Patents
A kind of big multiplying power manganate cathode material for lithium and preparation method thereof Download PDFInfo
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- CN109004212A CN109004212A CN201810647107.3A CN201810647107A CN109004212A CN 109004212 A CN109004212 A CN 109004212A CN 201810647107 A CN201810647107 A CN 201810647107A CN 109004212 A CN109004212 A CN 109004212A
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
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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
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Abstract
The present invention provides a kind of big multiplying power manganate cathode material for lithium and preparation method thereof, and the positive electrode is by spinel lithium manganate and is coated between its primary particle and the solid electrolyte on second particle surface forms, and is porous microsphere shape.The preparation method is that: lithium source, manganese source are subjected to high-energy ball milling first, obtain spinel lithium manganate after subsequently heat-treated.Then the cladding for carrying out solid electrolyte is heat-treated after carrying out high-energy ball milling with solid electrolyte.By the LiMn2O4 after cladding and after high molecular polymer aqueous solution stirs and to form uniform sizing material, it is spray-dried, and be heat-treated and remove macromolecule to pore-creating, obtains the big multiplying power manganate cathode material for lithium.Solubility of the manganese in organic bath can be effectively reduced in the positive electrode, improve lithium ion conducting rate, have big circulation performance.
Description
Technical field
The invention belongs to technical field of lithium ion, and in particular to a kind of big multiplying power manganate cathode material for lithium and its preparation
Method.
Background technique
Spinel lithium manganate LiMn2O4Positive electrode resourceful, low in cost, stable structure, safety with raw material manganese source
The advantages that property is high, is one of the anode material for lithium-ion batteries by favor.But the Mn due to LiMn2O4 on electric discharge latter stage surface3+
The high easily disproportionation of concentration generates the Mn for dissolving in electrolyte2+And electrolyte lithium salt LiPF6The a small amount of HF generated can corrode LiMn2O4
The loss for causing manganese element, so that capacity attenuation is very fast.In addition, the conductivity of LiMn2O4 is relatively low.The two is unfavorable for LiMn2O4
Big circulation.It is thus not applied for applying the lithium ion battery on electric car with fast charge at present for strategy.
There is research to coat spinel lithium manganate, the material coated has silica, aluminium oxide etc., so can be with
Inhibit the loss of manganese element, but the electric conductivity of these covering materials is poor, cannot provide good conductive environment.In recent years,
Solid electrolyte has obtained very big research.Some solid state electrolysis confrontation water oxygens are insensitive, can long-term existence in air, and
Lithium ion conducting rate is also considerable, also there is wider electrochemical window, provides new thinking to prepare electrode material.In
It is that people begin trying to coat one layer of solid electrolyte by sol-gal process on spinel lithium manganate；But colloidal sol is used merely
Gel method cladding solid electrolyte still has that energy density is not high.Meanwhile using merely using sol-gal process into
Row cladding, there is also certain problems when industrially applying.
Summary of the invention
The present invention is in view of the deficiencies of the prior art；A kind of manganate cathode material for lithium of big multiplying power porous microsphere shape is devised,
And a set of matched preparation method is devised simultaneously.
A kind of big multiplying power manganate cathode material for lithium of the present invention；The big multiplying power manganate cathode material for lithium is by spinel lithium manganate
LiMn2O4It is formed with solid electrolyte；The spinel lithium manganate LiMn2O4Primary particle between and second particle surface deposit
There is solid electrolyte, and is being porous microsphere shape.
In a kind of big multiplying power manganate cathode material for lithium of the invention, the mass fraction of solid electrolyte is 1%~6%.
A kind of big multiplying power manganate cathode material for lithium of the present invention；It is described by spinel lithium manganate LiMn2O4With solid state electrolysis texture
At porous microsphere partial size be 10-15 microns；Preferably 11.5-12.5 microns.
A kind of big multiplying power manganate cathode material for lithium of the present invention；The big multiplying power manganate cathode material for lithium is made with graphite
The Soft Roll of 3200mAh tests the discharge capacity of its 30C；Its discharge capacity is 2985mAh-3130mAh.Significantly larger than existing skill
Product in art.
A kind of preparation method of big multiplying power manganate cathode material for lithium of the present invention；The following steps are included:
Step 1
Ball milling cladding is carried out with solid state electrolysis confrontation spinel lithium manganate；It is heat-treated after ball milling；After being coated
Spinel lithium manganate；
Step 2
Spinel lithium manganate after cladding obtained by step 1 is mixed with high molecular polymer aqueous solution, slurrying；So
After be spray-dried, and be heat-treated and remove high molecular polymer to pore-creating, obtain the big multiplying power lithium manganate cathode material
Material.
A kind of preparation method of big multiplying power manganate cathode material for lithium of the present invention；The preparation method of the spinel lithium manganate
Are as follows: lithium source, manganese source are subjected to high-energy ball milling, obtain spinel lithium manganate after subsequently heat-treated.The revolving speed of the high-energy ball milling is
100~600rpm, Ball-milling Time are 12~28h.The heat treatment are as follows: under an oxygen-containing atmosphere, preferably under air atmosphere, in
400~1000 DEG C of 2~12h of calcining.Preferably, lithium source and manganese source press LiMn2O4Stoichiometric ratio ingredient.As into
The preferred embodiment of one step, the lithium source in the lithium compounds such as lithium hydroxide, lithium acetate, lithium carbonate, lithium nitrate at least one
Kind, manganese source uses manganese dioxide, manganese carbonate or manganese sesquioxide managnic oxide etc.,
A kind of preparation method of big multiplying power manganate cathode material for lithium of the present invention；In step 1, the solid electrolyte is selected from
La-Li-Ti-O system solid electrolyte (such as Li0.3La0.56TiO3), Li-Al-Ti-P-O system solid electrolyte (such as
Li1.3Ti1.7Al0.3(PO4)3), Li-La-Ta-O system solid electrolyte (such as Li5La3Ta2O12), Li-B-O system solid state electrolysis
Matter (such as 3Li2O-B2O3), Li-Ti-Zr-P-O system solid electrolyte (such as LiTi0.5Zr1.5(PO4)3) etc. stable in the air deposit
Oxide and at least one of phosphate system.
A kind of preparation method of big multiplying power manganate cathode material for lithium of the present invention；In step 1, when ball milling coats, ball milling is controlled
Revolving speed is 100~600rpm, and Ball-milling Time is 12~28h.
A kind of preparation method of big multiplying power manganate cathode material for lithium of the present invention；In step 1, after ball milling cladding, oxygenous
Under atmosphere, preferably under air atmosphere, in 400~1000 DEG C of 2~12h of calcining.Heat treatment i.e. after ball milling cladding are as follows: oxygenous
Under atmosphere, preferably under air atmosphere, in 400~1000 DEG C, preferably 700~850 DEG C of 2~12h of calcining.
A kind of preparation method of big multiplying power manganate cathode material for lithium of the present invention；In step 2, the high molecular polymer choosing
From at least one of water soluble polymers such as polyvinylpyrrolidone, carboxymethyl cellulose.
Preferably, in the aqueous solution of high molecular polymer described in step 2, the mass fraction of high molecular polymer is
0.05%~3%.
Preferably, by solid-liquid mass ratio, the ratio of 1:1.5-3, preferably 1:2 will coat obtained by step 1 in step 2
Spinel lithium manganate afterwards mixed with high molecular polymer aqueous solution, slurrying.
Preferably, the inlet temperature of spray drying is 200~350 DEG C in step 2, outlet temperature is 85~130 DEG C.
A kind of preparation method of big multiplying power manganate cathode material for lithium of the present invention；In step 2, the heat treatment are as follows: oxygen-containing
Under atmosphere, preferably under air atmosphere, in 400~1000 DEG C, preferably 700~850 DEG C of 2~12h of calcining.
Principle and advantage
The present invention devises a kind of manganate cathode material for lithium of big multiplying power porous microsphere shape for the first time；The big multiplying power LiMn2O4
Positive electrode is by spinel lithium manganate LiMn2O4It is formed with solid electrolyte；The spinel lithium manganate LiMn2O4Primary
There are solid electrolytes with second particle surface between grain, and are porous microsphere shape.
The present invention uses ball milling cladding for the first time and has prepared with high molecular polymer drying process with atomizing and has excellent performance
Product.It is realized between the primary particle of spinel lithium manganate using ball milling, spray drying and second particle surface coats
Solid electrolyte, and be porous microsphere shape.Solve the problems, such as that manganese element is lost in cyclic process, and improve lithium from
Subconductivity enhances big high rate performance.Preparation method is simple for this, is suitble to industrialization.Meanwhile it is optimized after, by each
The synergistic effect of preparation parameter, the discharge capacity for realizing 30C are up to 2985mAh-3130mAh, preferably 3000-3130mAh.
Product significantly larger than in the prior art.
Detailed description of the invention
Attached drawing 1 is embodiment 1-4 and comparative example 1, the discharge capacity of 2 products obtained therefrom 30C of comparative example detection figure.
Specific embodiment
Present invention ball-milling method and spray drying process prepare big multiplying power manganate cathode material for lithium.Below by specific implementation case
Example further illustrates.
Embodiment 1:
Firstly, lithium carbonate and manganese dioxide are pressed LiMn2O4Stoichiometric ratio weigh, then will be each with high speed ball mill
Raw material is mixed, ball milling speed 400rpm, Ball-milling Time 18h.Material after ball milling is put into crucible, in 500 DEG C
Keep the temperature 8h, natural cooling in furnace.Obtain spinel lithium manganate.
Further according to LiMn2O4Quality 5% weigh solid electrolyte Li0.3La0.56TiO3.By Li0.3La0.56TiO3With manganese
Sour lithium mixing, is mixed each raw material with high speed ball mill, ball milling speed 400rpm, Ball-milling Time 18h.After ball milling
Material be put into crucible, in natural cooling in 500 DEG C of heat preservation 4h, furnace.Obtain Li0.3La0.56TiO3The spinel manganese of cladding
Sour lithium.
By the Li of 500g0.3La0.56TiO3The carboxylic first that the spinel lithium manganate of cladding and the mass fraction of 1000g are 1.5%
Base cellulose aqueous solution mixes, by stirring to get uniform sizing material.Uniformly mixed slurry is subjected to spray drying treatment, is entered
Mouth temperature is 350 DEG C, and outlet temperature is 120 DEG C.By above-mentioned presoma in 800 DEG C of calcining 4h with remove carboxymethyl cellulose to
Pore-creating.Obtain Li0.3La0.56TiO3The spinel lithium manganate porous microsphere of cladding.3200mAh is made in institute's prepared material and graphite
Soft Roll, test the discharge capacity of its 30C, discharge capacity 3126.9mAh.
Embodiment 2:
Firstly, lithium carbonate and manganese dioxide are pressed LiMn2O4Stoichiometric ratio weigh, then will be each with high speed ball mill
Raw material is mixed, ball milling speed 100rpm, Ball-milling Time 28h.Material after ball milling is put into crucible, in 1000 DEG C
Keep the temperature 8h, natural cooling in furnace.Obtain spinel lithium manganate.
Further according to LiMn2O4Quality 1% weigh solid electrolyte Li0.3La0.56TiO3.By Li0.3La0.56TiO3With manganese
Sour lithium mixing, is mixed each raw material with high speed ball mill, ball milling speed 100rpm, Ball-milling Time 12h.After ball milling
Material be put into crucible, in natural cooling in 400 DEG C of heat preservation 12h, furnace.Obtain Li0.3La0.56TiO3The spinel manganese of cladding
Sour lithium.
By the Li of 500g0.3La0.56TiO3The carboxylic first that the spinel lithium manganate of cladding and the mass fraction of 1000g are 0.05%
Base cellulose aqueous solution mixes, by stirring to get uniform sizing material.Uniformly mixed slurry is subjected to spray drying treatment, is entered
Mouth temperature is 200 DEG C, and outlet temperature is 85 DEG C.By above-mentioned presoma in 400 DEG C of calcining 12h with remove carboxymethyl cellulose to
Pore-creating.Obtain Li0.3La0.56TiO3The spinel lithium manganate porous microsphere of cladding.3200mAh is made in institute's prepared material and graphite
Soft Roll, test the discharge capacity of its 30C, discharge capacity 2987.6mAh.
Embodiment 3:
Firstly, lithium carbonate and manganese dioxide are pressed LiMn2O4Stoichiometric ratio weigh, then will be each with high speed ball mill
Raw material is mixed, ball milling speed 600rpm, Ball-milling Time 12h.Material after ball milling is put into crucible, in 400 DEG C
Keep the temperature 4h, natural cooling in furnace.Obtain spinel lithium manganate.
Further according to LiMn2O4Quality 6% weigh solid electrolyte Li0.3La0.56TiO3.By Li0.3La0.56TiO3With manganese
Sour lithium mixing, is mixed each raw material with high speed ball mill, ball milling speed 600rpm, Ball-milling Time 28h.After ball milling
Material be put into crucible, in natural cooling in 1000 DEG C of heat preservation 3h, furnace.Obtain Li0.3La0.56TiO3The spinel manganese of cladding
Sour lithium.
By the Li of 500g0.3La0.56TiO3The carboxymethyl that the spinel lithium manganate of cladding and the mass fraction of 1000g are 3%
Cellulose aqueous solution mixes, by stirring to get uniform sizing material.Uniformly mixed slurry is subjected to spray drying treatment, entrance
Temperature is 350 DEG C, and outlet temperature is 130 DEG C.By above-mentioned presoma in 1000 DEG C of calcining 2h with remove carboxymethyl cellulose to
Pore-creating.Obtain Li0.3La0.56TiO3The spinel lithium manganate porous microsphere of cladding.3200mAh is made in institute's prepared material and graphite
Soft Roll, test the discharge capacity of its 30C, discharge capacity 2988.6mAh.
Embodiment 4:
Firstly, lithium carbonate and manganese dioxide are pressed LiMn2O4Stoichiometric ratio weigh, then will be each with high speed ball mill
Raw material is mixed, ball milling speed 400rpm, Ball-milling Time 20h.Material after ball milling is put into crucible, in 700 DEG C
Keep the temperature 7h, natural cooling in furnace.Obtain spinel lithium manganate.
Further according to LiMn2O4Quality 3.5% weigh solid electrolyte Li0.3La0.56TiO3.By Li0.3La0.56TiO3With
LiMn2O4 mixing, is mixed each raw material with high speed ball mill, ball milling speed 400rpm, Ball-milling Time 20h.By ball milling
Material afterwards is put into crucible, in natural cooling in 700 DEG C of heat preservation 7h, furnace.Obtain Li0.3La0.56TiO3The spinelle of cladding
LiMn2O4.
By the Li of 500g0.3La0.56TiO3The carboxylic first that the spinel lithium manganate of cladding and the mass fraction of 1000g are 1.5%
Base cellulose aqueous solution mixes, by stirring to get uniform sizing material.Uniformly mixed slurry is subjected to spray drying treatment, is entered
Mouth temperature is 275 DEG C, and outlet temperature is 108 DEG C.By above-mentioned presoma in 700 DEG C of calcining 7h with remove carboxymethyl cellulose to
Pore-creating.Obtain Li0.3La0.56TiO3The spinel lithium manganate porous microsphere of cladding.3200mAh is made in institute's prepared material and graphite
Soft Roll, test the discharge capacity of its 30C, discharge capacity 3078.4mAh.
Comparative example 1:
Lithium carbonate and manganese dioxide are pressed into LiMn2O4Stoichiometric ratio weigh, then with high speed ball mill by each raw material into
Row mixing, ball milling speed 400rpm, Ball-milling Time 20h.Material after ball milling is put into crucible, in 700 DEG C of heat preservation 7h,
Natural cooling in furnace.Obtain spinel lithium manganate.Institute's prepared material and graphite are made to the Soft Roll of 3200mAh, test its 30C's
Discharge capacity, discharge capacity 783.7mAh.
Comparative example 2
Lithium carbonate and manganese dioxide are pressed into LiMn2O4Stoichiometric ratio weigh, then with high speed ball mill by each raw material into
Row mixing, ball milling speed 400rpm, Ball-milling Time 20h.Material after ball milling is put into crucible, in 700 DEG C of heat preservation 7h,
Natural cooling in furnace.Obtain spinel lithium manganate.
Further according to LiMn2O4Quality 5% weigh solid electrolyte Li0.3La0.56TiO3.By Li0.3La0.56TiO3With manganese
Sour lithium mixing, is mixed each raw material with high speed ball mill, ball milling speed 400rpm, Ball-milling Time 18h.After ball milling
Material be put into crucible, in natural cooling in 500 DEG C of heat preservation 4h, furnace.Obtain Li0.3La0.56TiO3The spinel manganese of cladding
Sour lithium.
Institute's prepared material and graphite are made to the Soft Roll of 3200mAh, test the discharge capacity of its 30C, discharge capacity is only
1770.7mAh。
Claims (10)
1. a kind of big multiplying power manganate cathode material for lithium；It is characterized by: the big multiplying power manganate cathode material for lithium is by spinel manganese
Sour lithium LiMn2O4It is formed with solid electrolyte；The spinel lithium manganate LiMn2O4Primary particle between and second particle table
There are solid electrolytes in face, and are porous microsphere shape.
2. a kind of big multiplying power manganate cathode material for lithium according to claim 1, it is characterised in that: the big multiplying power LiMn2O4
The mass fraction of solid electrolyte is 1%~6% in positive electrode.
3. a kind of big multiplying power manganate cathode material for lithium according to claim 1, it is characterised in that: described by spinelle mangaic acid
Lithium LiMn2O4The partial size of the porous microsphere constituted with solid electrolyte is 10-15 microns.
4. a kind of big multiplying power manganate cathode material for lithium according to claim 1, it is characterised in that: by the big multiplying power mangaic acid
The Soft Roll of 3200mAh is made in lithium anode material and graphite, tests the discharge capacity of its 30C；Its discharge capacity is 2985mAh-
3130mAh。
5. a kind of preparation method of big multiplying power manganate cathode material for lithium described in -4 any one according to claim 1；Its feature exists
In；The following steps are included:
Step 1
Ball milling cladding is carried out with solid state electrolysis confrontation spinel lithium manganate；It is heat-treated after ball milling；Point after being coated is brilliant
Stone LiMn2O4；
Step 2
Spinel lithium manganate after cladding obtained by step 1 is mixed with high molecular polymer aqueous solution, slurrying；Then into
Row spray drying, and be heat-treated and remove high molecular polymer to pore-creating, obtain the big multiplying power manganate cathode material for lithium.
6. a kind of preparation method of big multiplying power manganate cathode material for lithium according to claim 5；It is characterized by: the point
Spar LiMn2O4 the preparation method comprises the following steps: by lithium source, manganese source carry out high-energy ball milling, obtain spinel lithium manganate after subsequently heat-treated；
The revolving speed of the high-energy ball milling is 100~600rpm, and Ball-milling Time is 12~28h；
The heat treatment are as follows: under an oxygen-containing atmosphere, in 400~1000 DEG C of 2~12h of calcining.
7. a kind of preparation method of big multiplying power manganate cathode material for lithium according to claim 5；It is characterized by: step 1
In, the solid electrolyte is selected from La-Li-Ti-O system solid electrolyte, Li-Al-Ti-P-O system solid electrolyte, Li-
La-Ta-O system solid electrolyte, Li-B-O system solid electrolyte, in Li-Ti-Zr-P-O system solid electrolyte at least
It is a kind of.
8. a kind of preparation method of big multiplying power manganate cathode material for lithium according to claim 5；It is characterized by:
In step 1, when ball milling coats, control rotational speed of ball-mill is 100~600rpm, and Ball-milling Time is 12~28h；
In step 1, after ball milling cladding, under an oxygen-containing atmosphere, in 400~1000 DEG C of 2~12h of calcining.
9. a kind of preparation method of big multiplying power manganate cathode material for lithium according to claim 5；It is characterized by: step 2
In, the high molecular polymer in the water soluble polymers such as polyvinylpyrrolidone, carboxymethyl cellulose extremely
Few one kind；
In the aqueous solution of high molecular polymer described in step 2, the mass fraction of high molecular polymer is 0.05%~3%.
In step 2, by solid-liquid mass ratio, 1:1.5-3 is by the spinel lithium manganate and high molecular polymerization after cladding obtained by step 1
Object aqueous solution mixed, slurrying.
10. a kind of preparation method of big multiplying power manganate cathode material for lithium according to claim 5；It is characterized by:
In step 2, the inlet temperature of spray drying is 200~350 DEG C, and outlet temperature is 85~130 DEG C；
In step 2, the heat treatment are as follows: under an oxygen-containing atmosphere, in 400~1000 DEG C of 2~12h of calcining.
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| CN114132966A (en) * | 2020-09-03 | 2022-03-04 | 星恒电源(滁州)有限公司 | Surface-modified lithium manganate material and preparation method thereof |
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| CN109004212B (en) | 2020-10-20 |
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Effective date of registration: 20221117 Address after: 417009 North of East West Second Street and west of North South Third Road, Second Industrial Park, Economic and Technological Development Zone, Loudi City, Hunan Province Patentee after: HUNAN DIANJIANGJUN NEW ENERGY CO.,LTD. Address before: Yuelu District City, Hunan province 410083 Changsha Lushan Road No. 932 Patentee before: CENTRAL SOUTH University |