CN107994226A - A kind of lithium-rich anode material of Mn adulterated lithium manganate and preparation method thereof - Google Patents
A kind of lithium-rich anode material of Mn adulterated lithium manganate and preparation method thereof Download PDFInfo
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- 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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Abstract
The present invention provides a kind of lithium-rich anode material of Mn adulterated lithium manganate and preparation method thereof, the lithium-rich anode material of the Mn adulterated lithium manganate is mixed by lithium source, manganese source, doped metal salt and metal chelating agent, spherical lithium manganate powder is made in ultrasonic aerosolization, calcining, is mixed, is coated and calcination process is prepared with spherical anode material powder.The positive electrode of the present invention is doped by the Mn positions in LiMn2O4, effectively suppress analysis oxygen, improve the voltage drop problem of cyclic process, the tap density of powder can be improved by mixing, and then the energy density of material is improved, realized by encapsulation steps and reduce the loss of Lacking oxygen and the migration of transition metal ions, improve efficiency first, the security performance of battery is lifted, improves the energy density of material.
Description
Technical field
The present invention relates to anode material for lithium-ion batteries technical field, and in particular to a kind of rich lithium of Mn adulterated lithium manganate
Positive electrode and preparation method thereof.
Background technology
Environmental pollution and energy crisis be the two big problems that present society faces, and fuel-engined vehicle widely uses exacerbation
The above problem.So in order to solve environment and energy problem, the new-energy automobile using electric automobile as representative is increasingly subject to people
Concern.Electric automobile currently on the market mostly using lithium ion battery as power resources, but current lithium-ion electric
The energy density in pond cannot still meet that country reaches the requirement of 350Wh/kg for single power battery energy density.Except in electricity
Outside the energy density that battery core is improved in core structure designs and manufacturing process, two main ways of the energy density of battery are improved
Footpath：First, improve the operating voltage of positive and negative pole material；Second, improve the specific capacity of material.
For negative material, positive electrode is in gram volume performance, power density, charge-discharge magnification, cycle life
There are problems that serious short slab with security performance etc., so, the lifting of power battery performance, particularly energy density carry
Height, is heavily dependent on the development progress of positive electrode.At present, commercial Li-ion battery positive electrode mainly has cobalt acid
Lithium, LiMn2O4, nickel-cobalt-manganese ternary composite material and LiFePO4 etc., but they there are some indexs not to reach power battery
Requirement.So the problem of based on the above, lithium-rich anode material is up to 300mAh/g, higher work because of its specific discharge capacity
Make voltage, high security and relatively low cost have been a great concern.
Although lithium-rich anode material is unrivaled with other positive electrodes on lithium ion battery energy density is improved
Advantage, but it is applied to lithium-ion-power cell, it is now recognized that following three must be solved the problems, such as：First, it is irreversible first
Capacitance loss is big, and head effects are relatively low；Second, high rate performance is poor, mainly thinks this and Li at present2MnO3Poor electric conductivity is related；
3rd, cyclic process is mainly considered that transition metal ions is moved from transition metal layer in charge and discharge process there is voltage drop
Lithium layer position is moved to, so as to cause the change of crystal structure；4th, it there are problems that in charging process analysing oxygen, this is because
Li2MnO3Material has oxygen atom to take part in charge compensation during de- lithium, causes structure that irreversible change occurs, capacity is not
Reversible decay.Meanwhile release oxygen can produce serious influence the security performance of battery, produce bulge even explosion etc. and ask
Topic.
The content of the invention
In view of the deficiencies of the prior art, the present invention provides lithium-rich anode material and its preparation of a kind of Mn adulterated lithium manganate
Method, it is intended to which overcoming head existing for current lithium-rich anode material to imitate, relatively low, high rate performance is poor, there are voltage drop, poor circulation
And the problems such as release oxygen, by adulterating variable valency metal at Mn, effectively suppress the analysis oxygen problem in charging process, make preparation
The high rate performance and power of lithium-rich anode material get a promotion, while there is stable structure and material circulation in charging process to stablize
The advantages that.
In order to solve the above technical problems, the present invention provides following technical solution：
On the one hand, the present invention provides a kind of preparation method of the lithium-rich anode material of Mn adulterated lithium manganate, including as follows
Step：
1) lithium source, manganese source, doped metal salt and metal chelating agent mixed by required proportioning, ultrasonic aerosolization, forged
Fire to obtain spherical lithium manganate powder；The lithium source, manganese source, the addition of doped metal salt and metal chelating agent are with molar ratio X：
Y1：Y2：Z is measured, wherein X=2.0~2.2, Y=Y1+Y2, Y2：Y=5%~10%, Z=1.2 (X+Y)；The doping
Metal salt is metal nitrate or metal sulfate；
2) by spherical lithium manganate powder obtained by step 1) with spherical anode material powder is fully dispersed uniformly obtains mixed powder
End；The spherical anode material powder includes spherical lithium cobalt (LiCoO2), spherical nickel-cobalt mangaic acid lithium ((Li (NiCoMn) O2, note
For NCM), spherical nickel-cobalt lithium aluminate (Li (NiCoAl) O2, it is denoted as NCA)；
3) mixed-powder progress surface cladding obtained by step 2) is handled to the mixed-powder coated；
4) mixed-powder for the cladding for obtaining step 3) is calcined to obtain Mn adulterated lithium manganate lithium-rich anode materials.
Further, in step 1), the blending process is as follows：By lithium source, manganese source, doped metal salt and metal chelating agent
55 DEG C~65 DEG C of high temperature pure water is dissolved in, when stirring 10~20 is small, is uniformly clarified to solution.
Further, the ultrasonic aerosolization is controlled in 1.0~2.0MPa with nitrogen as carrier gas, gas pressure.
Further, the temperature control of the calcining is at 400~600 DEG C, when calcination time is 4~6 small.
Further, the metal of the metal nitrate is selected from the one of the transition metals such as Fe, Ti, Mo, Cr, Ni, Ru
Kind or at most two kinds of combination；The metal of the metal sulfate is selected from the transition metals such as Fe, Ti, Mo, Cr, Ni, Ru
A kind of or at most two kinds of combination.
In an embodiment of the present invention doped metal salt doping requirement be：Metal nitrate, metal sulfate only adulterate
A kind of or at most two kinds of combination, or two kinds of doping at the same time but two kinds of one kind therein can only be selected from.
Further, the metal chelating agent is selected from citric acid, ammonium hydroxide, amion acetic acid, a kind in b diammonium edta or
At most two kinds of combination.
Further , Suo Shu Manganese sources are manganese acetate or manganese chloride.
Further, the lithium source is lithium acetate or lithium nitrate.
Further, it is fully dispersed in step 2) that batch mixing, batch mixing are uniformly carried out using high speed mixer or double-cone mixer
When time is 1~3 small.
Further, the NCM includes NCM111, NCM442, NCM523, NCM622, NCM811 etc..
Further, the granularity D of the spherical lithium manganate powder50For the granularity D of spherical anode material powder5014%
~16%, the doping of spherical lithium manganate powder is 1%~5%.
Further, the particle diameter of the spherical lithium manganate powder is 1~10 μm.
Further, it is Al surface coated covering material to be carried out in the step 3)2O3、TiO2、ZrO2、CeO2、SiO2、
ZnO、MgO、SnO2、AlPO4、CoPO4In it is one or two kinds of.
Further, surface is carried out in the step 3) to cover using individual layer cladding or inside and outside double-coating, is adopted
The method coated with dry mixed, integral coating amount are less than 5%.
Further, the method that dry mixed coats in the step 3) is coated, and detailed process is as follows：Will cladding
Material homogenate adds mixed-powder to be covered after being uniformly dispersed, stir, when drying 4~8 is small at a temperature of 120 DEG C,
When calcining 15~20 is small at 500~600 DEG C, the mixed-powder of cladding of the integral coating amount less than 5% is obtained.
Further, the parameter of calcining is as follows in the step 4)：Calcining heat is 600 DEG C~700 DEG C, and calcination time is
8~12 it is small when.
On the other hand, the present invention provides a kind of lithium-rich anode material of the Mn positions adulterated lithium manganate prepared with the above method
Material.
On the other hand, the present invention provides a kind of lithium battery anode, includes the Mn positions doping of the method preparation with the present invention
The lithium-rich anode material of LiMn2O4.
The present invention provides a kind of lithium-rich anode material of Mn adulterated lithium manganate and preparation method thereof, using doped metal salt
Modification is doped to lithium-rich anode material, doped metal salt therein adulterates variable valency metal at Mn, effectively suppresses to charge
The analysis oxygen problem of journey, the spherical lithium manganate powder of preparation and spherical positive electrode powder can improve shaking for powder after being mixed
Real density, and then the energy density of material is improved, loss and the transition metal ions for reducing Lacking oxygen are realized by encapsulation steps
Migration, improve discharge capacity first, improve the voltage drop problem of cyclic process, can also reduce the reaction of material and electrolyte,
Improve heat endurance, the security of material.
Beneficial effects of the present invention：
The present invention provides a kind of lithium-rich anode material of Mn adulterated lithium manganate and preparation method thereof, the Mn doping mangaic acid
Lithium lithium-rich anode material is by mixing, ultrasonic aerosolization, calcining, material mixes, cladding and calcination process are prepared, by
The Mn positions of LiMn2O4 are doped, and effectively suppress analysis oxygen, improve the voltage drop problem of cyclic process, improve efficiency first, lifting
The security performance of battery, improves the energy density of material, specifically with following advantage：
The lithium-rich anode material of the Mn adulterated lithium manganate, which is doped lithium-rich anode material using doped metal salt, to be changed
Property, doped metal salt therein adulterates variable valency metal at Mn, in charging process, Li+Abjection, variable valency metal is able to oxygen
Change, reduce the charge compensation of the oxygen atom in charge and discharge process, reduce the appearance of Lacking oxygen, effectively suppress in charging process
Analysis oxygen problem, and then improve security performance；In addition, the reduction of Lacking oxygen so that Li in discharge process+Can be embedding well
Enter, so as to improve discharge capacity, improve efficiency first；Meanwhile the stable structure of the positive electrode of preparation can also improve
Cycle performance of the battery under high power capacity performance, improves cycle life.
When preparing the lithium-rich anode material of Mn adulterated lithium manganates, the particle diameter of the spherical lithium manganate powder of mixing with it is spherical just
The proper ratio of the particle diameter of pole material powder and suitable mixing proportion can improve the tap density of powder well, further
The compacted density of anode pole piece is improved, and then lifts the energy density of the battery of material.
When preparing the lithium-rich anode material of Mn adulterated lithium manganates, using cladding mixing spherical lithium manganate powder with it is spherical
Positive electrode powder, it is possible to reduce the loss of Lacking oxygen and the migration of transition metal ions, improve discharge capacity, improvement first and follow
Voltage drop problem during ring；In addition cladding can reduce the reaction of material and electrolyte, improve the heat endurance of material, carry
High safety performance.
, can be with by being calcined to the mixed-powder of cladding when preparing the lithium-rich anode material of Mn adulterated lithium manganates
Particle surface is passivated, reduces the destruction of particle surface that process is brought early period；Can also be released particle internal stress,
Make system more stable.
The lithium-rich anode material of Mn positions adulterated lithium manganate prepared by the present invention discharges first reaches 275~282mAh/g, first
Effect reach 88.3~89%, 0.5C/0.5C circulation 800 circle, keep more than 95%~96%, in cyclic process voltage drop substantially subtract
It is small, while particle is mashed up so that mass energy density improves 14.5%~17% or so.
Embodiment
With specific embodiment, the present invention is further illustrated below, but the present invention is from the restriction of following embodiments.
Embodiment one
(1) by lithium acetate, manganese acetate, ferric nitrate and citric acid according to molar ratio 2.0：0.95:0.05：3.6 ratio into
Row dispensing, is dissolved in 60 DEG C of high temperature pure water, when stirring 10 is small, is uniformly clarified to solution, then pass through ultrasonic aerosolization (nitrogen pressure
1.2MPa), prefabricated spherical powder is formed, then 450 DEG C of sintering temperature is controlled in high-temperature calcination again, when sintering time 5 is small, removes
Moisture and organic matter is gone to decompose to obtain spherical Li2MnO3Powder；
(2) the spherical Li using high energy batch mixer to above-mentioned preparation2MnO3Powder (A powder) and uncoated NCM523 (B powder) into
When the uniform batch mixing 1 of row is small, D is controlled50(A powder) is D50The doping of 14.5%, the A powder of (B powder) is 1.6%；
(3) Al is used2O3Powder carries out surface cladding processing to above-mentioned mixed-powder, coats process：Al2O3Powder is first
It is homogenized in stirred tank, is dispersed to uniformly, adds mixed-powder to be covered, stir, subsequently dry (120 DEG C,
6 it is small when), then calcined when small (600 DEG C, 20), obtain the cladding powder that integral coating amount is less than 4%；
(4) cladding powder calcined under oxygen atmosphere, crushed, be classified, except magnetic, so that spherical cathode be prepared
Material, wherein 600 DEG C of calcining heat, when calcination time 8 is small.
Compared to the research level of current rich lithium material, Li is adulterated in the Mn positions prepared using the above method2MnO3Lithium-rich anode material
The electric discharge first of material reaches 275mAh/g, and head effects reach 89.0%, 0.5C/0.5C circulations, 800 circle, keep more than 96%, circulation
During voltage drop be obviously reduced, while particle is mashed up so that mass energy density improves 17% or so.
Embodiment two
(1) by lithium acetate, manganese chloride, Titanium Nitrate and amion acetic acid according to molar ratio 2.1：0.9：0.1：3.72 ratio into
Row dispensing, is dissolved in 65 DEG C of high temperature pure water, when stirring 15 is small, is uniformly clarified to solution, then pass through ultrasonic aerosolization (nitrogen pressure
1.5MPa), prefabricated spherical powder is formed, then 500 DEG C of sintering temperature is controlled in high-temperature calcination again, when sintering time 5 is small, removes
Moisture and organic matter is gone to decompose to obtain spherical Li2MnO3Powder；
(2) uniform batch mixing is carried out with uncoated NCM523 (B powder) to the powder (A powder) of above-mentioned preparation using high energy batch mixer
2 it is small when, control D50(A powder) is D50The doping of 15%, the A powder of (B powder) is 1.5%；
(3) TiO is used2Powder carries out surface cladding processing to above-mentioned mixed-powder, coats process：TiO2Powder exists first
It is homogenized in stirred tank, is dispersed to uniformly, adds mixed-powder to be covered, stir, subsequently dry (120 DEG C, 6
Hour), then when small (550 DEG C, 20) are calcined, obtain the cladding powder that integral coating amount is less than 4%；
(4) cladding powder calcined under oxygen atmosphere, crushed, be classified, except magnetic, so that spherical cathode be prepared
Material, wherein 650 DEG C of calcining heat, when calcination time 10 is small.
Compared to the research level of current rich lithium material, Li is adulterated in the Mn positions prepared using the above method2MnO3Lithium-rich anode material
The electric discharge first of material reaches 282mAh/g, and head effects reach 88.3%, 0.5C/0.5C circulations, 800 circle, keep more than 95.5%, follow
Voltage drop is obviously reduced during ring, while particle is mashed up so that mass energy density improves 14.5% or so.
Embodiment three
(1) by lithium nitrate, manganese chloride, ferric nitrate, Titanium Nitrate and ammonium hydroxide according to molar ratio 2.2：0.95：0.03：0.02：
3.84 ratio carries out dispensing, is dissolved in 55 DEG C of high temperature pure water, when stirring 20 is small, is uniformly clarified to solution, then pass through ultrasonic gas
It is atomized (nitrogen pressure 1.25MPa), forms prefabricated spherical powder, then controls 600 DEG C of sintering temperature in high-temperature calcination again, burn
When the knot time 6 is small, removes moisture and organic matter decomposes to obtain spherical Li2MnO3Powder；
(2) uniform batch mixing is carried out with uncoated NCM424 (B powder) to the powder (A powder) of above-mentioned preparation using high energy batch mixer
3 it is small when, control D50(A powder) is D50The doping of 14.6%, the A powder of (B powder) is 3.0%；
(3) ZrO is used2Powder carries out surface cladding processing to above-mentioned mixed-powder, coats process：ZrO2Powder exists first
It is homogenized in stirred tank, is dispersed to uniformly, adds mixed-powder to be covered, stir, subsequently dry (120 DEG C, 6
Hour), then when small (550 DEG C, 20) are calcined, obtain the cladding powder that integral coating amount is less than 4.5%；
(4) cladding powder calcined under oxygen atmosphere, crushed, be classified, except magnetic, so that spherical cathode be prepared
Material, wherein 650 DEG C of calcining heat, when calcination time 12 is small.
Compared to the research level of current rich lithium material, Li is adulterated in the Mn positions prepared using the above method2MnO3Lithium-rich anode material
The electric discharge first of material reaches 280mAh/g, and head effects reach 88.5%, 0.5C/0.5C circulations, 800 circle, keep more than 95%, circulation
During voltage drop be obviously reduced, while particle is mashed up so that mass energy density improves 15% or so.
The foregoing is only a preferred embodiment of the present invention, is not intended to limit the invention, for the skill of this area
For art personnel, the invention may be variously modified and varied.Within the spirit and principles of the invention, that is made any repaiies
Change, equivalent substitution, improvement etc., should all be included in the protection scope of the present invention.
Claims (10)
1. a kind of lithium-rich anode material of Mn adulterated lithium manganate and preparation method thereof, it is characterised in that include the following steps：
1) lithium source, manganese source, doped metal salt and metal chelating agent are mixed by required proportioning, ultrasonic aerosolization, calcining are made
Obtain spherical lithium manganate powder；The lithium source, manganese source, the addition of doped metal salt and metal chelating agent are with molar ratio X：Y1：Y2：
Z is measured, wherein X=2.0~2.2, Y=Y1+Y2, Y2：Y=5%~10%, Z=1.2 (X+Y)；The doped metal salt
For metal nitrate, metal sulfate or combination；
2) by spherical lithium manganate powder obtained by step 1) with spherical anode material powder is fully dispersed uniformly obtains mixed-powder；Institute
Stating spherical anode material powder includes spherical lithium cobalt, spherical nickel-cobalt mangaic acid lithium or spherical nickel-cobalt lithium aluminate；
3) mixed-powder progress surface cladding obtained by step 2) is handled to the mixed-powder coated；
4) mixed-powder for the cladding for obtaining step 3) is calcined to obtain Mn adulterated lithium manganate lithium-rich anode materials.
2. the preparation method of the lithium-rich anode material of Mn adulterated lithium manganate according to claim 1, it is characterised in that step
It is rapid 1) in, the blending process is as follows：Lithium source, manganese source, doped metal salt and metal chelating agent are dissolved in 55 DEG C~65 DEG C of height
Warm pure water, be sufficiently stirred 10~20 it is small when, uniformly clarified to solution；
The ultrasound aerosolization is controlled in 1.0~2.0MPa with nitrogen as carrier gas, gas pressure；
The temperature control of the calcining is at 400~600 DEG C, when calcination time is 4~6 small.
3. the preparation method of the lithium-rich anode material of Mn adulterated lithium manganate according to claim 1, it is characterised in that institute
State metal nitrate metal is a kind of in Fe, Ti, Mo, Cr, Ni, Ru or at most two kinds of combination；The metal sulfate
The metal of salt is a kind of in Fe, Ti, Mo, Cr, Ni, Ru or at most two kinds of combination.
4. the preparation method of the lithium-rich anode material of Mn adulterated lithium manganate according to claim 1, it is characterised in that institute
State metal chelating agent and be selected from citric acid, ammonium hydroxide, amion acetic acid, a kind or at most two kinds of combination in b diammonium edta；
Suo Shu Manganese sources are manganese acetate or manganese chloride；
The lithium source is lithium acetate or lithium nitrate.
5. the preparation method of the lithium-rich anode material of Mn adulterated lithium manganate according to claim 1, it is characterised in that step
It is rapid 2) in it is fully dispersed batch mixing is uniformly carried out using high speed mixer or double-cone mixer, mixing time for 1~3 it is small when.
6. the preparation method of the lithium-rich anode material of Mn adulterated lithium manganate according to claim 1, it is characterised in that institute
State the granularity D of spherical lithium manganate powder50For the granularity D of spherical anode material powder5014%~16%, spherical lithium manganate powder
The doping at end is 1%~5%, and the particle diameter of the spherical lithium manganate powder is 1~10 μm.
7. the preparation method of the lithium-rich anode material of Mn adulterated lithium manganate according to claim 1, it is characterised in that institute
It is Al to state and surface coated covering material is carried out in step 3)2O3、TiO2、ZrO2、CeO2、SiO2、ZnO、MgO、SnO2、AlPO4、
CoPO4In it is one or two kinds of；
Surface is carried out in the step 3) to cover using individual layer cladding or inside and outside double-coating, is coated using dry mixed
Method coated, detailed process is as follows：Mixed-powder to be covered is added after covering material homogenate is uniformly dispersed, is fully stirred
Mix uniformly, when drying 4~8 is small at a temperature of 120 DEG C, when calcining 15~20 is small at 500~600 DEG C, obtain integral coating amount
The mixed-powder of cladding less than 5%.
8. the preparation method of the lithium-rich anode material of Mn adulterated lithium manganate according to claim 1, it is characterised in that institute
The parameter for stating calcining in step 4) is as follows：Calcining heat is 600 DEG C~700 DEG C, when calcination time is 8~12 small.
A kind of 9. lithium-rich anode material of the Mn positions adulterated lithium manganate prepared with any method of claim 1~8.
10. a kind of lithium battery anode, it is characterised in that including the Mn positions prepared with any method of claim 1~8
The lithium-rich anode material of adulterated lithium manganate.
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| CN108847477A (en) * | 2018-05-25 | 2018-11-20 | 彩虹集团新能源股份有限公司 | A kind of nickle cobalt lithium manganate tertiary cathode material and preparation method thereof |
| CN109920993A (en) * | 2019-03-12 | 2019-06-21 | 四川纳创时代新能源科技有限公司 | A kind of surface modifying method of nickelic ternary material nickle cobalt lithium manganate |
| CN110438557A (en) * | 2019-07-16 | 2019-11-12 | 湖南长远锂科股份有限公司 | A kind of preparation method of sharpening monocrystalline high-voltage spinel nickel lithium manganate cathode material |
| CN110918043A (en) * | 2019-11-29 | 2020-03-27 | 成都泰利创富锂业科技有限公司 | Doped and coated lithium-rich layered lithium manganese oxide adsorption material and preparation method thereof |
| CN112897586A (en) * | 2021-02-01 | 2021-06-04 | 山东海科创新研究院有限公司 | Spinel lithium-rich lithium manganate and preparation method and application thereof |
| CN113735197A (en) * | 2021-11-05 | 2021-12-03 | 蜂巢能源科技有限公司 | Synthetic method for improving voltage drop of positive electrode material, positive electrode material and application |
| CN114180637A (en) * | 2021-11-25 | 2022-03-15 | 哈尔滨工业大学 | Cation disordered lithium-rich cathode material and preparation method thereof |
| CN114678522A (en) * | 2022-04-25 | 2022-06-28 | 西安理工大学 | Modification method of lithium-rich manganese-based positive electrode material by regulating manganese vacancy and application of material |
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| CN108847477B (en) * | 2018-05-25 | 2021-09-21 | 彩虹集团新能源股份有限公司 | Nickel cobalt lithium manganate ternary positive electrode material and preparation method thereof |
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| CN110918043A (en) * | 2019-11-29 | 2020-03-27 | 成都泰利创富锂业科技有限公司 | Doped and coated lithium-rich layered lithium manganese oxide adsorption material and preparation method thereof |
| CN112897586A (en) * | 2021-02-01 | 2021-06-04 | 山东海科创新研究院有限公司 | Spinel lithium-rich lithium manganate and preparation method and application thereof |
| CN113735197A (en) * | 2021-11-05 | 2021-12-03 | 蜂巢能源科技有限公司 | Synthetic method for improving voltage drop of positive electrode material, positive electrode material and application |
| CN114180637A (en) * | 2021-11-25 | 2022-03-15 | 哈尔滨工业大学 | Cation disordered lithium-rich cathode material and preparation method thereof |
| CN114678522A (en) * | 2022-04-25 | 2022-06-28 | 西安理工大学 | Modification method of lithium-rich manganese-based positive electrode material by regulating manganese vacancy and application of material |
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