CN102593445A - Aluminum clad manganese-base laminated composite lithium ion battery cathode material and preparation method thereof - Google Patents
Aluminum clad manganese-base laminated composite lithium ion battery cathode material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an aluminum clad manganese-base laminated composite lithium ion battery cathode material and a preparation method thereof. According to the anode material, aluminum salt is coated on an outer surface of a manganese-base cathode material with a laminated structure in a chemical formula of Li(LixMn1-y-zM1yM2z)O2. The preparation method comprises the following steps of: (1) preparing a mixture; (2) sintering and treating powder; (3) preparing a corresponding amount of soluble aluminum salt, adding the soluble aluminum salt into the manganese-base laminated cathode material, and uniformly stirring; (4) preparing a NH3.H2O solution, a NH4F solution or a NH4H2PO4 solution, adding the solution into slurry of aluminum nitrate and the manganese-base laminated cathode material, and uniformly stirring; and (5) drying the slurry obtained in the step (4), and sintering at the temperature of between 400 and 800 DEG C for 5 to 15 hours. The aluminum clad manganese-base laminated composite lithium ion battery cathode material has high capacity, low first charging voltage platform and excellent long cycle performance, takes an Mn element as a basis, and is low in raw material cost and particularly suitable for preparing large batteries such as batteries of electric vehicles.
Description
Technical field
The present invention relates to a kind of anode material for lithium-ion batteries and preparation method thereof, especially relate to a kind of aluminium wrapping manganese-base shape anode material for compound lithium ion battery and preparation method thereof.
Background technology
Present widely used anode material for lithium-ion batteries has cobalt acid lithium, lithium manganate having spinel structure, nickel cobalt binary material, nickel-cobalt-manganese ternary material and LiFePO4 etc.; Wherein cobalt acid lithium combination property is optimum, and mature preparation process be main flow positive electrode in the market, but cobalt resource is deficient, environment is produced pollute simultaneously.Lithium manganate having spinel structure is cheap, and security performance is excellent, but has the Jahn-Teller effect, also is prone to take place Mn
3+Disproportionation, make manganese generation solubilizing reaction, cause cycle performance relatively poor, so need to carry out modification from each side such as material and battery making.Nickel cobalt binary material has the high unique advantage of capacity, but the high inferior position of basicity also can't avoid, and is applied in the battery, to environment, to prepare range request very high, at present, all is difficult in most of at home batteries use.The nickel-cobalt-manganese ternary material has cooperative effect; Have the performance advantage of cobalt acid lithium, the price advantage of LiMn2O4 concurrently; And the high power capacity advantage of nickel cobalt binary material, but have the high and application problem that brings of basicity equally, and be limited by the use of cobalt acid lithium; When if the cobalt valency remains on lower level, the advantage on ternary material does not then have to use.The LiFePO4 cycle performance is excellent, but problems such as present ubiquity cost height, stable processing technique property difference and making difficulty.
The shape composite positive pole Li of manganese basic unit
2MnO
3-LiMO
2(M=Co, Ni, Fe, Ni
0.5Mn
0.5Deng) be main with manganese, have cheap, resourceful advantage, because Mn keeps tetravalence, so Stability Analysis of Structures, under high voltage, have the higher and constitutionally stable characteristic of capacity, be a kind of new material that has development prospect.Laboratory, Univ Chicago USA Argonne Co., Ltd Argonne is in U.S. Pat 6677082, US6680143 and the US7303840 of application in 2004; All mention about the synthetic and performance of this composite positive pole etc., wherein U.S. Pat 7303840 (also being No. 200480044357.4, Chinese patent) is to xLi
2MnO
3(1-x) LiMn
2-yM
yO
4(0<x<1,0≤y<1) coverage of combination electrode and use are set forth.While its laminate Li
2MnO
3Can be by xLi
2MnO
3(1-x) LiM ' O
2, or have α-MnO
2Or γ-MnO
2The Li of structure
2O zMnO
2Substitute LiMn
2-yM
yO
4Also can be by Li
2O zMnO
2Substitute.And spinel lithium manganate LiMn
2-yM
yO
4In substitute element M can be Li
+, Mg
2+, Ni
2+, Ni
3+, Co
2+, Co
3+, Al
3+, Ti
4+And Zr
4+In the ion one or more, stratiform LiM ' O
2In M ' be selected from Mn, Co and the Ni ion one or more.About the discharge capacity of this material, in the 2.0-5.0V voltage range, can reach 270mAh/g in the patent working example.Also mention in this patent document and use sulfuric acid, hydrochloric acid or nitric acid to carry out this combination electrode of acid activation processing, but concrete grammar is unexposed.
It is Li [Li that Chinese patent 200910186311.0 discloses a kind of general formula
(1-2x)/3Ni
X-aM
yMn
(2-x)/3-b] O
2Lithium-rich manganese-based anode material and preparation method thereof, one or more among M=Co, Al, Ti, Mg, the Cu wherein.The preparation method is: soluble metallic salt (sulfate, nitrate, chloride salt, acetate) is generated precursor in agitated reactor, mix the back high temperature sintering then with lithium compound, obtain final product.In this patent document, used double sintering technology, component is limited, do not handle but relate to coating.
There is the high and low shortcoming of efficiency for charge-discharge of initial charge voltage platform in existing manganese basic unit shape positive electrode.
Summary of the invention
The technical problem that the present invention will solve is, overcomes the deficiency of prior art, provides a kind of first charge-discharge efficiency and discharge capacity high, and the excellent aluminium wrapping manganese-base shape anode material for compound lithium ion battery of electrical property such as charge and discharge cycles and preparation method thereof.
The present invention solve the technical problem the technical scheme that is adopted:
The present invention's aluminium wrapping manganese-base shape anode material for compound lithium ion battery is to be Li (Li at chemical formula
xMn
1-y-zM1
yM2
z) O
2The outer surface of manganese-based anode material of layer structure be coated with aluminium salt; Covering amount is Al/ Li (Li
xMn
1-y-zM1
yM2
z) O
2Mass ratio be 0.01%-0.1%;
Chemical formula Li (Li
xMn
1-y-zM1
yM2
z) O
2In substitute element M1 be at least a among Ni, Fe, the Co;
Element M 2 is a doped chemical, is at least a among Al, Mg, the Ti;
0.1≤x in the formula≤0.5,0.1≤y＜0.4,0.01≤z≤0.1;
Said aluminium salt is Al (NO
3)
3, AlF
3, AlPO
4In a kind of.
The preparation method of the present invention's aluminium wrapping manganese-base shape anode material for compound lithium ion battery may further comprise the steps:
(1) preparation compound: by molecular formula is Li (Li
xMn
1-y-zM1
yM2
z) O
2Ratio, with theory measurement than for Mn
1-y-zM1
yHydroxide precursor and lithium carbonate (Li
2CO
3), and the micron order oxide of doped chemical M2, join in the mixing tank, mix, getting element set becomes Li (Li
xMn
1-y-zM1
yM2
z) O
2Mixture;
(2) sintering and powder handling: under 600-1000 ℃, step (1) gained element set is become Li (Li
xMn
1-y-zM1
yM2
z) O
2Mixture constant temperature sintering 10-30 hour, after reacting completely, be powder with the sintered products ball milling, after the 150-300 mesh sieve, molecular formula be Li (Li
xMn
1-y-zM1
yM2
z) O
2Manganese basic unit shape positive electrode;
(3) press Al/ Li (Li
xMn
1-y-zM1
yM2
z) O
2Mass ratio be 0.01%-0.2%, the preparation respective amount the soluble aluminum salting liquid, joining step (2) gained molecular formula is Li (Li
xMn
1-y-zM1
yM2
z) O
2Manganese basic unit shape positive electrode in, stir, the slurry of nitrate and manganese basic unit shape positive electrode;
(4) according to the reaction mol ratio, the NH of the amount of preparation respective substance
3H
2O solution, NH
4F solution or NH
4H
2PO
4Solution joins in the slurry of aluminum nitrate described in the step (3) and manganese basic unit shape positive electrode, stirs, and gets the slurry of aluminium wrapping manganese-base shape anode material for compound lithium ion battery, said NH
3H
2O, NH
4F or NH
4H
2PO
4With the mol ratio of Al be 1 ︰ 1-2;
(5) behind the slurry drying with step (4) gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery, place Muffle furnace,, get aluminium wrapping manganese-base shape anode material for compound lithium ion battery at 400-800 ℃ of following sintering 5-15h.
Further, in the step (1), the time of mixing, preferred 1-5 hour.
The present invention is employed in and crosses Li on the theory measurement mol ratio, can obtain the layered crystal structure positive electrode of pure phase; Doped chemical gets into lattice through high-temperature process and substitutes host element Mn or M1; At least a host element M1 substitutes; And the doping of at least a doped chemical M2, can eliminate the oxygen defect that brings in the high-temperature sintering process, stable crystal structure; The doping of M2 also can improve first charge-discharge efficiency to a certain extent, reduces the initial charge voltage platform; Aluminium coats the low and high problem of platform of efficient in the first charge-discharge process that can further solve, and can obviously improve cycle performance.
The present invention's aluminium wrapping manganese-base shape anode material for compound lithium ion battery, capacity is high, and the low and long cycle performance of initial charge voltage platform is excellent; It is the basis with the Mn element, and cost of material is lower, is specially adapted to the preparation of large-sized battery such as batteries of electric automobile.
Description of drawings
Fig. 1 is the synthetic manganese shape positive electrode Li (Li of basic unit of embodiment 1
xMn
1-y-zM1
yM2
z) O
2And the XRD figure that coats the back material is composed;
Fig. 2 is embodiment 1 aluminium wrapping manganese-base shape positive electrode Li (Li
xMn
1-y-zM1
yM2
z) O
2The SEM collection of illustrative plates;
Fig. 3 is embodiment 1 aluminium wrapping manganese-base shape positive electrode Li (Li
xMn
1-y-zM1
yM2
z) O
2Detain electric first charge-discharge curve;
Fig. 4 is embodiment 1 aluminium wrapping manganese-base shape positive electrode Li (Li
xMn
1-y-zM1
yM2
z) O
225 ℃ of loop attenuation collection of illustrative plates of button electricity.
Embodiment
Below in conjunction with embodiment the present invention is done further explain.
Embodiment 1
The aluminium wrapping manganese-base shape anode material for compound lithium ion battery of present embodiment is to be Li (Li at chemical formula
0.2Mn
0.65Ni
0.33Al
0.02) O
2The outside of manganese-based anode material of layer structure be coated with aluminium salt; Covering amount is Al/ Li (Li
0.2Mn
0.65Ni
0.33Al
0.02) O
2Mass ratio be 0.02%.
Its preparation method is:
(1) preparation compound: by molecular formula is Li (Li
0.2Mn
0.65Ni
0.33Al
0.02) O
2Ratio, be that hydroxide precursor nickel hydroxide manganese 10.000Kg and the 35.979kg purity of Mn ︰ Ni=0.65 ︰ 0.33 is 96% lithium carbonate (Li with mol ratio
2CO
3), 3.119kg purity is 99% micron order Al
2O
3, join in the mixing tank, mix, getting element set becomes Li (Li
0.2Mn
0.65Ni
0.33Al
0.02) O
2Mixture;
(2) sintering and grinding: under 900 ℃, step (1) gained element set is become Li (Li
0.2Mn
0.65Ni
0.33Al
0.02) O
2Mixture constant temperature sintering 20 hours, after reacting completely,, cross 200 mesh sieves with the sintered products ball mill grinding, Dmax is that molecular formula below 74 microns is Li (Li
0.2Mn
0.65Ni
0.33Al
0.02) O
2Manganese basic unit shape positive electrode;
(3) press Al/ Li (Li
0.2Mn
0.65Ni
0.33Al
0.02) O
2Mass ratio=0.02%, take by weighing the Al (NO of 2782.435g
3)
39H
2O is mixed with Al (NO in the adding 5L water
3)
3Solution, the positive electrode after the step (2) of getting 10kg is then sieved adds wherein, stir, the slurry of aluminum nitrate and manganese basic unit shape positive electrode;
(4) take by weighing the NH of 274.536g
4F adds in the 5L water, is mixed with NH
4F solution joins in the slurry of aluminum nitrate described in the step (3) and manganese basic unit shape positive electrode, stirs, and gets the slurry of aluminium wrapping manganese-base shape anode material for compound lithium ion battery;
(5) behind the slurry drying with step (4) gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery, place Muffle furnace,, promptly get aluminium wrapping manganese-base shape anode material for compound lithium ion battery at 700 ℃ of following sintering 10h.
Testing graininess
With Ma Erwen 2000 particle size analyzers present embodiment gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery is carried out testing graininess; The synthetic product granularity is controlled in the particle size distribution accumulative total volume distributed median, and to reach 50% D50 be 10.0 ± 1.0 microns, and specific area is 0.5 ± 0.1m
2/ g, tap density is 2.0 ± 0.5g/cm
3
The XRD figure analysis of spectrum
Present embodiment gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery and step (2) gained manganese basic unit shape positive electrode are carried out the XRD figure analysis of spectrum; Its result is as shown in Figure 1; Show that present embodiment gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery and step (2) gained manganese basic unit shape positive electrode all are pure phase stratiform, perfect crystalline.
ESEM (SEM) test
Present embodiment gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery is carried out ESEM (SEM) test; Its result is as shown in Figure 2; Present embodiment gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery crystallization type of being is spherical; Form by reunion attitude particle, have desirable pattern characteristic.
The electrical property assessment
Present embodiment gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery and step (2) gained manganese basic unit shape positive electrode are assembled into CR2432 model button cell; Carry out the electrical property assessment; Negative pole is a metal lithium sheet, the LD-124 that electrolyte uses Dongguan China fir China fir new material Co., Ltd to produce.At first in the ratio of manganese base layered cathode material material ︰ SP (conductive carbon black) ︰ PVDF (binding agent)=90 ︰ 5 ︰ 5 with mixing of materials; Then it is uniformly coated on the Al paper tinsel collector; After oven dry, section, process positive plate, in glove box, add electrolyte, barrier film, negative pole then and assemble.Battery testing charging and discharging currents density is 20mA/g, and voltage range is 2.0-4.8V, and selecting temperature is 25 ℃ of normal temperature tests.Its first charge-discharge curve is as shown in Figure 3, all has the higher problem of initial charge voltage platform, but than the stratiform manganese-based anode material that does not coat, after carrying out aluminium coating processing, the charging voltage platform has obvious reduction.The first charge-discharge efficiency that coats with the aluminium clad material is not respectively 71.4% and 78.8%, and while discharge capacity reduction is less, is respectively 256.2 and 251.2mAh/g.The result shows; Present embodiment gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery and step (2) gained manganese basic unit shape positive electrode capacity are all more than 250mAh/g; Efficient is all more than 70% first, coats after handling through aluminium that efficient and charging voltage platform have clear improvement first.
Button electricity normal temperature (25 ℃) the loop attenuation collection of illustrative plates of present embodiment gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery and step (2) gained manganese basic unit shape positive electrode is as shown in Figure 4.At the circulation initial stage; The phenomenon that the manganese basic unit shape anode material for compound lithium ion battery that does not coat exists obvious capacity to rise; After 5 circulations, can reach 270mAh/g from initial 256.2mAh/g; The capacity trend that significantly decreases in the cyclic process subsequently is 95.1% than the initial capacity conservation rate after the circulation of 30 weeks.Aluminium wrapping manganese-base shape anode material for compound lithium ion battery is not decay of capacity in 30 all cyclic processes, and keeps the slightly trend of rising.Aluminium wrapping manganese-base shape anode material for compound lithium ion battery is in limited reduction material capacity, and cycle performance is effectively improved.
Embodiment 2-4:
The difference of embodiment 2-4 and embodiment 1 is listed in the table 1, and other are operated with embodiment 1.
Not coating and aluminium wrapping manganese-base shape positive electrode that table 1 different condition is synthetic
| Embodiment | Component | Coat used material | Coat Al mass percent (%) | Discharge capacity (mAh/g) first | First charge-discharge efficiency (%) | |
| 2 | Li(Li 0.2Mn 0.65Fe 0.30Al 0.05)O 2 | Aluminum nitrate, ammoniacal liquor | 0.02 | 228.5 | 69.8 | 97.4 |
| 2 reference examples | Li(Li 0.2Mn 0.65Fe 0.30Al 0.05)O 2 | - | - | 235.1 | 64.0 | 93.7 |
| 3 | Li(Li 0.2Mn 0.60Co 0.38Mg 0.02)O 2 | Aluminum nitrate, ammonium fluoride | 0.05 | 246.7 | 81.6 | 98.6 |
| 3 reference examples | Li(Li 0.2Mn 0.60Co 0.38Mg 0.02)O 2 | - | - | 250.6 | 73.2 | 94.5 |
| 4 | Li(Li 0.2Mn 0.648Ni 0.228 Co 0.114Ti 0.01)O 2 | Aluminum nitrate, ammonium dihydrogen phosphate | 0.10 | 253.4 | 79.3 | 99.5 |
| 4 reference examples | Li(Li 0.2Mn 0.648Ni 0.228 Co 0.114Ti 0.01)O 2 | - | - | 258.5 | 72.1 | 96.2 |
Claims (5)
1. an aluminium wrapping manganese-base shape anode material for compound lithium ion battery is characterized in that, is to be Li (Li at chemical formula
xMn
1-y-zM1
yM2
z) O
2The outer surface of manganese-based anode material of layer structure be coated with aluminium salt; Covering amount is Al/ Li (Li
xMn
1-y-zM1
yM2
z) O
2Mass ratio be 0.01%-0.1%;
Chemical formula Li (Li
xMn
1-y-zM1
yM2
z) O
2In substitute element M1 be at least a among Ni, Fe, the Co;
Element M 2 is a doped chemical, is at least a among Al, Mg, the Ti;
0.1≤x in the formula≤0.5,0.1≤y＜0.4,0.01≤z≤0.1.
2. aluminium wrapping manganese-base shape anode material for compound lithium ion battery according to claim 1 is characterized in that said aluminium salt is Al (NO
3)
3, AlF
3, AlPO
4In a kind of.
3. the preparation method of an aluminium wrapping manganese-base shape anode material for compound lithium ion battery according to claim 1 or claim 2 is characterized in that, may further comprise the steps:
(1) preparation compound: by molecular formula is Li (Li
xMn
1-y-zM1
yM2
z) O
2Ratio, with theory measurement than for Mn
1-y-zM1
yHydroxide precursor and lithium carbonate, and the micron order oxide of doped chemical M2 joins in the mixing tank, mix, element set become Li (Li
xMn
1-y-zM1
yM2
z) O
2Mixture;
(2) sintering and powder handling: under 600-1000 ℃, step (1) gained element set is become Li (Li
xMn
1-y-zM1
yM2
z) O
2Mixture constant temperature sintering 10-30 hour, after reacting completely, be powder with the sintered products ball milling, after the 150-300 mesh sieve, molecular formula be Li (Li
xMn
1-y-zM1
yM2
z) O
2Manganese basic unit shape positive electrode;
(3) press Al/ Li (Li
xMn
1-y-zM1
yM2
z) O
2Mass ratio be 0.01%-0.1%, the preparation respective amount the soluble aluminum salting liquid, joining step (2) gained molecular formula is Li (Li
xMn
1-y-zM1
yM2
z) O
2Manganese basic unit shape positive electrode in, stir, the slurry of aluminum soluble salt and manganese basic unit shape positive electrode;
(4) according to the reaction mol ratio, the NH of the amount of preparation respective substance
3H
2O solution, NH
4F solution or NH
4H
2PO
4Solution joins in the slurry of aluminum nitrate described in the step (3) and manganese basic unit shape positive electrode, stirs, and gets the slurry of aluminium wrapping manganese-base shape anode material for compound lithium ion battery;
(5) behind the slurry drying with step (4) gained aluminium wrapping manganese-base shape anode material for compound lithium ion battery, place Muffle furnace,, get aluminium wrapping manganese-base shape anode material for compound lithium ion battery at 400-800 ℃ of following sintering 5-15h.
4. the preparation method of aluminium wrapping manganese-base shape anode material for compound lithium ion battery according to claim 3 is characterized in that, in the step (1), the time of mixing is 1-5 hour.
5. according to the preparation method of claim 3 or 4 described aluminium wrapping manganese-base shape anode material for compound lithium ion battery, it is characterized in that, in the step (4),, said NH
3H
2O, NH
4F or NH
4H
2PO
4With the mol ratio of Al be 1:1-2.
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| CN103094553A (en) * | 2013-01-12 | 2013-05-08 | 上海大学 | Method for modifying surface of anode material for lithium ion battery |
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| CN103311513B (en) * | 2013-06-03 | 2017-04-05 | 青岛乾运高科新材料股份有限公司 | A kind of high-performance layed solid-solution lithium electricity positive electrode and preparation method thereof |
| CN103647073A (en) * | 2013-12-17 | 2014-03-19 | 惠州亿纬锂能股份有限公司 | Lithium ion battery anode material and preparation method thereof |
| CN103647073B (en) * | 2013-12-17 | 2016-08-17 | 惠州亿纬锂能股份有限公司 | A kind of anode material for lithium-ion batteries and preparation method thereof |
| CN116169284A (en) * | 2016-01-04 | 2023-05-26 | 上海钜领科技有限公司 | Method for preparing cathode material of lithium ion battery |
| CN106558688A (en) * | 2016-11-18 | 2017-04-05 | 贵州振华新材料有限公司 | High-voltage lithium-battery cathode material, battery and preparation method and application |
| CN112447952A (en) * | 2019-09-02 | 2021-03-05 | 宁德时代新能源科技股份有限公司 | Positive active material, preparation method thereof, positive pole piece and lithium ion secondary battery |
| CN110600714A (en) * | 2019-10-12 | 2019-12-20 | 福建师范大学 | Preparation method of nickel-cobalt-manganese-doped ternary material coated with polymeric aluminum |
| CN114400330A (en) * | 2022-03-23 | 2022-04-26 | 湖南长远锂科新能源有限公司 | Al/B co-coated positive electrode material and preparation method thereof |
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