CN108545785A - A kind of large single crystal nickel cobalt manganese anode material and preparation method thereof - Google Patents

A kind of large single crystal nickel cobalt manganese anode material and preparation method thereof Download PDF

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CN108545785A
CN108545785A CN201810185159.3A CN201810185159A CN108545785A CN 108545785 A CN108545785 A CN 108545785A CN 201810185159 A CN201810185159 A CN 201810185159A CN 108545785 A CN108545785 A CN 108545785A
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nickel cobalt
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许开华
张文艳
徐世国
陈玉君
张明龙
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Greenmei (Hubei) new energy materials Co.,Ltd.
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Abstract

The present invention is suitable for technical field of lithium batteries, provides a kind of large single crystal nickel cobalt manganese anode material and preparation method thereof, and the present invention rationally prepares the presoma of magnesium Doped with Titanium cladding first, and is dried to obtain Li at low temperatureaNixCoyMnzMgpO·qTiO2Oxide, this mode will not destroy crystal structure, and a large amount of magnesium source of people then will be mixed in obtained oxide and mends lithium, then high temperature sintering is carried out, it only is passed through 0.5~0.1% spray water in the temperature rise period in sintering process, constant temperature and temperature-fall period are neither passed through, the Li being sinteredbMgM(NixCoyMnzMgNTiq)O2Positive electrode need not crush strongly, be sieved after need to only disperseing in high-speed mixer and can be obtained D50For the large single crystal positive electrode of 6~8um, preparation process is simple, and for obtained positive electrode grain through big, good evenness can also obtain high power capacity and long cycle characteristics under high voltages.

Description

A kind of large single crystal nickel cobalt manganese anode material and preparation method thereof
Technical field
The invention belongs to technical field of lithium batteries more particularly to a kind of large single crystal nickel cobalt manganese anode material and its preparation sides Method.
Background technology
Present ternary developing direction mainly has two lines, when it is nickelic, second is that high voltage.Nickel is crossed high security and is obtained not To guarantee, so many research staff select high voltage direction.Nickel control improves point voltage in a certain range and Gao Rong can be obtained Measure the ternary product product of high safety.Structure collapses are be easy to cause using secondary ball particle under high voltage, performance is unstable.So Ternary material is only made the performance that monocrystalline pattern could bring into play under high voltages.
Patent CN 106910882A and patent CN107311242A are disclosing a kind of lithium ion battery large single crystal stratiform just The preparation method of pole material, the new method based on presoma substep plus lithium prepare micron order large single crystal layered cathode material：(1) will Ni-Co-Mn or Co-Mn presomas are mixed with the lithium source of stoichiometric ratio, wherein the molar ratio of elemental lithium and transition metal element It between 0-1, calcines at high temperature, the Spinel formed due to lacking lithium at this time contributes to the fusion and life of a crystal grain It is long, obtain crystal grain of the larger compound phase of micron-scale or pure phase；(2) lithium secondly is supplemented into the crystal grain of above-mentioned preparation, Large single crystal layered cathode material is can be obtained after being calcined under high temperature.This method carries out high-temperature calcination in the case that lithium is insufficient, must The crystal structure that lattice lacks lithium has so been formed, in second of high-temperature calcination since first time lattice has been formed, second The lithium of supplement will not reenter in the lattice formed, since Li lacks in lattice, capacity can be caused to reduce, recycled Structure collapses in the process.The existing technology for making large single crystal uses high-temperature calcination mostly in the case of lithium abundance Method, i.e. firing temperature are significantly larger than the temperature of positive electrode synthesis, and temperature is excessively high to lead to lithium nickel cation mixing, capacity and follow Ring simultaneously declines.It is simple in order to which disposable crystal grain grows up to obtain the positive electrode of monocrystalline to improve temperature, sacrifices capacity.
Invention content
In view of the above problems, the purpose of the present invention is to provide a kind of 701515 positive electrode of large single crystal and its preparation sides Method, it is intended to solve existing nickelic positive electrode and cannot achieve acquisition high power capacity and macrocyclic technical problem under high voltage.
On the one hand, the preparation method of the large single crystal nickel cobalt manganese anode material includes the following steps：
Step S1, mixed aqueous solution and alkali continuous into reaction kettle or that be passed through nickel source, cobalt source, manganese source, magnesium salts indirectly Solution；
Step S2, N is blasted into reaction kettle2, and between pH value is transferred to 12-14, NiCoMnMg sediments are stirred to get, The NiCoMnMg sediments are directly washed to centrifugation and obtain NiCoMnMg precursor pulps；
Step S3, the NiCoMnMg precursor pulps are dispersed in water, LiOH and titanium salt are taken to be dissolved in aqueous solution respectively, It is first quantitatively adding titanium salt solution, adds LiOH aqueous solutions, water is directly evaporated do after mixing, obtained containing NiCoMnMg Presoma, Ti (OH)4, LiOH mix precursor；
Step S4, the mix precursor is dried into 4-6h at 400-600 DEG C, obtains LiaNixCoyMnzMgpO· qTiO2Oxide；
Step S5, by the LiaNixCoyMnzMgpO·qTiO2Oxide is mixed with magnesium source and lithium source, then in air or Under the atmosphere of oxygen, 0.5~0.1% spray water is passed through into roaster in temperature-rise period, constant temperature and temperature-fall period are neither Be passed through, at 700-800 DEG C be burnt into 8~for 24 hours, you can obtain LibMgM(NixCoyMnzMgNTiq)O2Positive electrode；
Step S6, by the LibMgM(NixCoyMnzMgNTiq)O2Positive electrode is sieved after disperseing in high-speed mixer D can be obtained50For the large single crystal nickel cobalt manganese anode material of 6-8um.
Further, in step S1, the nickel source, cobalt source, manganese source, magnesium salts be respectively nickel sulfate, cobaltous sulfate, manganese sulfate, Magnesium sulfate, the aqueous slkali are the mixed liquor of sodium hydroxide solution and ammonia spirit, wherein Mg/Me=0.2~2mol%, here Me is the moles total number of nickel cobalt manganese.
Further, in step S3, the titanium salt is Titanium Citrate, the Ti (OH)4For NiCoMnMg presomas surface Sediment, by being obtained after LiOH and Titanium Citrate precipitation, wherein Ti/Me=0.2~2mol%, Me is that nickel cobalt manganese being rubbed here That total amount.
Further, in step S2, the D of the NiCoMnMg precursor pulps50=2~4um, (D90-D10)/D50≤ 0.5。
Further, in step S5, by the LiaNixCoyMnzMgpO·qTiO2Oxide is mixed with magnesium source and lithium source, The magnesium source is Mg (OH)2Or MgO, the lithium source are Li2CO3Or LiOH, here the additive amount in magnesium source be Mg/Me=20~ 60mol%, Me are the moles total number of nickel cobalt manganese.
On the other hand, the large single crystal nickel cobalt manganese anode material is prepared by the above method, is prepared LiaNixCoyMnzMgpO·qTiO2In oxide, 0 ＜ a≤0.1, x=0.7 ± 0.02, y=0.15 ± 0.02, z=0.15 ± 0.02,0.002≤p, q≤0.02.The Li being preparedbMgM(NixCoyMnzMgNTiq)O2In positive electrode, 0.90≤b≤ 1.2, x=0.7 ± 0.02, y=0.15 ± 0.02, z=0.15 ± 0.02,0.002≤p≤0.02,0 ＜ q≤0.02,0.2≤M +N≤0.6。
The beneficial effects of the invention are as follows：The presoma that the present invention is coated by rationally preparing magnesium Doped with Titanium, and at low temperature It is dried to obtain LiaNixCoyMnzMgpO·qTiO2Oxide, this mode will not destroy crystal structure, then will obtain The a large amount of magnesium source of people is mixed in oxide and mends lithium, then carries out high temperature sintering, 0.5 only is passed through in the temperature rise period in sintering process~ 0.1% spray water, constant temperature and temperature-fall period are neither passed through, the Li being sinteredbMgM(NixCoyMnzMgNTiq)O2Positive electrode It need not crush strongly, be sieved after need to only disperseing in high-speed mixer and can be obtained D50For the large single crystal anode material of 6~8um Material, preparation process is simple, and for obtained positive electrode grain through big, good evenness can also obtain high power capacity and length under high voltages Cycle characteristics.
Description of the drawings
Fig. 1 is the preparation method flow chart of large single crystal nickel cobalt manganese anode material provided in an embodiment of the present invention；
Fig. 2 is the electron microscope that the embodiment of the present invention provides the large single crystal nickel cobalt manganese anode material prepared.
Specific implementation mode
In order to make the purpose , technical scheme and advantage of the present invention be clearer, with reference to the accompanying drawings and embodiments, right The present invention is further elaborated.It should be appreciated that the specific embodiments described herein are merely illustrative of the present invention, and It is not used in the restriction present invention.
The preparation method of large single crystal nickel cobalt manganese anode material provided by the invention includes the following steps：
Step S1, mixed aqueous solution and alkali continuous into reaction kettle or that be passed through nickel source, cobalt source, manganese source, magnesium salts indirectly Solution.
The nickel source, cobalt source, manganese source, magnesium salts are nickel sulfate, cobaltous sulfate, manganese sulfate, magnesium sulfate respectively, and the aqueous slkali is The mixed liquor of sodium hydroxide solution and ammonia spirit, wherein Mg/Me=0.2~2mol%, Me is the mole total of nickel cobalt manganese here Amount.
Step S2, N is blasted into reaction kettle2, and between pH value is transferred to 12-14, NiCoMnMg sediments are stirred to get, The NiCoMnMg sediments are directly washed to centrifugation and obtain NiCoMnMg precursor pulps.
The D of the NiCoMnMg precursor pulps50=2~4um, (D90-D10)/D50≤0.5。
Step S3, the NiCoMnMg precursor pulps are dispersed in water, LiOH and titanium salt are taken to be dissolved in aqueous solution respectively, It is first quantitatively adding titanium salt solution, adds LiOH aqueous solutions, water is directly evaporated do after mixing, obtained containing NiCoMnMg Presoma, Ti (OH)4, LiOH mix precursor.
The titanium salt is Titanium Citrate, the Ti (OH)4For the sediment on NiCoMnMg presomas surface, by LiOH and lemon It is obtained after lemon acid titanium precipitation, wherein Ti/Me=0.2~2mol%, Me is the moles total number of nickel cobalt manganese here.The NiCoMnMg Presoma uses (NiCoMnMg) (OH)2It indicates.
Step S4, the mix precursor is dried into 4-6h at 400-600 DEG C, obtains LiaNixCoyMnzMgpO· qTiO2Oxide, 0 ＜ a≤0.1, x=0.7 ± 0.02, y=0.15 ± 0.02, z=0.15 ± 0.02,0.002≤p≤0.2, 0 q≤0.02 ＜.
Step S5, by the LiaNixCoyMnzMgpO·qTiO2Oxide is mixed with magnesium source and lithium source, then in air or Under the atmosphere of oxygen, 0.5~0.1% spray water is passed through into roaster in temperature-rise period, constant temperature and temperature-fall period are neither Be passed through, at 700-800 DEG C be burnt into 8~for 24 hours, you can obtain LibMgM(NixCoyMnzMgNTiq)O2Positive electrode, 0.90≤b≤ 1.2, x=0.7 ± 0.02, y=0.15 ± 0.02, z=0.15 ± 0.02,0.002≤p≤0.02,0 ＜ q≤0.02,0.2≤M +N≤0.6。
In this step, the magnesium source is Mg (OH)2Or MgO, the lithium source are Li2CO3Or LiOH, the addition in magnesium source here Amount is Mg/Me=20~60mol%, and Me is the moles total number of nickel cobalt manganese.
Step S6, (3) positive electrode need not crush strongly, by the LibMgM(NixCoyMnzMgNTiq)O2Positive material Sieving can be obtained D after material disperses in high-speed mixer50For the large single crystal nickel cobalt manganese anode material of 6-8um.
The effect of the large single crystal nickel cobalt manganese anode material of the invention prepared is verified below by embodiment.
Embodiment：
(1) mixed aqueous solution that is continuous or being passed through nickel sulfate, cobaltous sulfate, manganese sulfate, magnesium sulfate indirectly into reaction kettle, with And the mixed liquor of sodium solution and ammonia spirit, wherein Mg/Me=0.2mol%.
(2), N is blasted into reaction kettle2, and between pH value is transferred to 12-14, NiCoMnMg sediments are stirred to get, it will The NiCoMnMg sediments directly wash centrifugation and obtain NiCoMnMg precursor pulps, the NiCoMnMg precursor pulps D50=2~4um, (D90-D10)/D50≤0.5。
(3), the NiCoMnMg precursor pulps are dispersed in water, LiOH and titanium salt is taken to be dissolved in aqueous solution, Ti/ respectively Me=0.2~2mol% is first quantitatively adding titanium salt solution, adds LiOH aqueous solutions, directly evaporates water do after mixing, It obtains containing NiCoMnMg presomas, Ti (OH)4, LiOH mix precursor.
(4), the mix precursor is dried into 6h at 400 DEG C, obtains LiaNixCoyMnzMgpO·qTiO2Oxidation Object.
(5), by the LiaNixCoyMnzMgpO·qTiO2Oxide and Mg (OH)2And Li2CO3Mixing, then in air Atmosphere under, 0.1% spray water is passed through into roaster in temperature-rise period, constant temperature and temperature-fall period are neither passed through, 800 12h is burnt at DEG C, you can obtain LibMgM(NixCoyMnzMgNTiq)O2Positive electrode.Here Mg (OH)2Additive amount be Mg/Me =20~60mol%.
(6) by the LibMgM(NixCoyMnzMgNTiq)O2Positive electrode is sieved after disperseing in high-speed mixer and can obtain To D50For the large single crystal nickel cobalt manganese anode material of 6-8um, electron microscope is as shown in Figure 2.
The large single crystal positive electrode is tested under half-cell, it is as follows to obtain result：2.75-4.4V 0.2C capacity is 195mAh/g, the 50 circle cycle conservation rate 99% at 1C/1C, lithium battery capacity and cycle performance, which have, under high voltages obviously carries It rises.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention All any modification, equivalent and improvement etc., should all be included in the protection scope of the present invention made by within refreshing and principle.

Claims (8)

1. a kind of preparation method of large single crystal nickel cobalt manganese anode material, which is characterized in that the method includes following step：
Step S1, continuous into reaction kettle or be passed through nickel source, cobalt source, manganese source, the mixed aqueous solution of magnesium salts and alkali soluble indirectly Liquid；
Step S2, N is blasted into reaction kettle2, and between pH value is transferred to 12-14, NiCoMnMg sediments are stirred to get, by institute State NiCoMnMg sediments directly wash centrifugation obtain NiCoMnMg precursor pulps；
Step S3, the NiCoMnMg precursor pulps are dispersed in water, LiOH and titanium salt is taken to be dissolved in aqueous solution respectively, it is first fixed Titanium salt solution is added in amount, adds LiOH aqueous solutions, directly evaporates water do after mixing, obtain containing NiCoMnMg forerunner Body, Ti (OH)4, LiOH mix precursor；
Step S4, the mix precursor is dried into 4-6h at 400-600 DEG C, obtains LiaNixCoyMnzMgpO·qTiO2 Oxide；
Step S5, by the LiaNixCoyMnzMgpO·qTiO2Oxide is mixed with magnesium source and lithium source, then in air or oxygen Atmosphere under, 0.5~0.1% spray water is passed through into roaster in temperature-rise period, constant temperature and temperature-fall period are neither passed through, At 700-800 DEG C firing 8~for 24 hours, you can obtain LibMgM(NixCoyMnzMgNTiq)O2Positive electrode；
Step S6, by the LibMgM(NixCoyMnzMgNTiq)O2Positive electrode is sieved after disperseing in high-speed mixer and can obtain To D50For the large single crystal nickel cobalt manganese anode material of 6-8um.
2. the preparation method of large single crystal nickel cobalt manganese anode material as described in claim 1, which is characterized in that described in step S1 Nickel source, cobalt source, manganese source, magnesium salts are nickel sulfate, cobaltous sulfate, manganese sulfate, magnesium sulfate respectively, and the aqueous slkali is sodium hydroxide solution With the mixed liquor of ammonia spirit, wherein Mg/Me=0.2~2mol%, Me is the moles total number of nickel cobalt manganese here.
3. the preparation method of large single crystal nickel cobalt manganese anode material as described in claim 1, which is characterized in that described in step S3 Titanium salt is Titanium Citrate, the Ti (OH)4For the sediment on NiCoMnMg presomas surface, after LiOH and Titanium Citrate precipitation It obtains, wherein Ti/Me=0.2~2mol%, Me is the moles total number of nickel cobalt manganese here.
4. the preparation method of large single crystal nickel cobalt manganese anode material as described in claim 1, which is characterized in that described in step S2 The D of NiCoMnMg precursor pulps50=2~4um, (D90-D10)/D50≤0.5。
5. the preparation method of large single crystal nickel cobalt manganese anode material as described in claim 1, which is characterized in that in step S5, by institute State LiaNixCoyMnzMgpO·qTiO2Oxide is mixed with magnesium source and lithium source, and the magnesium source is Mg (OH)2Or MgO, the lithium source For Li2CO3Or LiOH, the additive amount in magnesium source is Mg/Me=20~60mol% here, and Me is the moles total number of nickel cobalt manganese.
6. a kind of large single crystal nickel cobalt manganese anode material, which is characterized in that the large single crystal nickel cobalt manganese anode material is wanted by such as right Any one of 1-5 the methods are asked to be prepared.
7. large single crystal nickel cobalt manganese anode material as claimed in claim 6, which is characterized in that be prepared LiaNixCoyMnzMgpO·qTiO2In oxide, 0 ＜ a≤0.1, x=0.7 ± 0.02, y=0.15 ± 0.02, z=0.15 ± 0.02,0.002≤p≤0.02,0 q≤0.02 ＜.
8. large single crystal nickel cobalt manganese anode material as claimed in claim 7, which is characterized in that the Li being preparedbMgM (NixCoyMnzMgNTiq)O2In positive electrode, 0.90≤b≤1.2, x=0.7 ± 0.02, y=0.15 ± 0.02, z=0.15 ± 0.02,0.002≤p≤0.02, q≤0.02,0.2≤M+N≤0.6.
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CN109786734A (en) * 2018-09-29 2019-05-21 北京泰丰先行新能源科技有限公司 A kind of preparation method of the nickelic positive electrode of lithium secondary battery
CN110980817A (en) * 2019-10-10 2020-04-10 格林美（无锡）能源材料有限公司 High-power and long-cycle lithium battery positive electrode material and preparation method thereof
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CN116598475A (en) * 2023-06-15 2023-08-15 宁波容百新能源科技股份有限公司 Positive electrode material, preparation method thereof and lithium ion battery

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