CN108545785B - Large single crystal nickel-cobalt-manganese positive electrode material and preparation method thereof - Google Patents
Large single crystal nickel-cobalt-manganese positive electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention is suitable for the technical field of lithium batteries, and provides a large single crystal nickel-cobalt-manganese positive electrode material and a preparation method thereofPrecursor and drying at low temperature to obtain LiaNixCoyMnzMgpO·qTiO2The crystal structure of the oxide cannot be damaged in the mode, then a large amount of magnesium source is doped into the obtained oxide, lithium is supplemented, then high-temperature sintering is carried out, 0.5-0.1% of atomized water is only introduced in the temperature rising stage in the sintering process, the temperature keeping stage and the temperature reducing stage are not introduced, and Li obtained by sintering is not introduced in the constant-temperature stage and the temperature reducing stagebMgM(NixCoyMnzMgNTiq)O2The positive electrode material does not need to be strongly crushed, and can be obtained by dispersing in a high-speed mixer and then sieving50The preparation method is a 6-8um large single crystal anode material, the preparation process is simple, the obtained anode material particles are large in size and good in uniformity, and high capacity and long cycle characteristics can be obtained under high voltage.
Description
Technical Field
The invention belongs to the technical field of lithium batteries, and particularly relates to a large single crystal nickel-cobalt-manganese positive electrode material and a preparation method thereof.
Background
The current ternary development direction mainly has two routes, namely high nickel and high voltage. Too high safety of nickel cannot be guaranteed, so many researchers choose the high voltage direction. When the nickel is controlled in a certain range, the point voltage is increased, and a high-capacity and high-safety ternary product can be obtained. The use of secondary spherical particles at high voltage easily causes structural collapse and unstable performance. Therefore, good performance can be achieved at high voltage only by making the ternary material into a single crystal shape.
Patent CN 106910882a and patent CN107311242A disclose a preparation method of large single crystal layered cathode material for lithium ion battery, which is based on a new method of adding lithium step by step from precursor to prepare micron-sized large single crystal layered cathode material: (1) mixing a Ni-Co-Mn or Co-Mn precursor with a lithium source with a stoichiometric ratio, wherein the molar ratio of a lithium element to a transition metal element is 0-1, calcining at high temperature, and a spinel phase formed by lithium deficiency at the moment is helpful for the fusion and growth of primary grains to obtain a composite phase or pure phase primary grain with a large micron size; (2) and then supplementing lithium into the prepared crystal grains, and calcining at high temperature to obtain the large single crystal layered cathode material. The method is used for carrying out high-temperature calcination under the condition of lithium deficiency, a crystal structure with lattice lacking lithium is inevitably formed, the first lattice is formed during the second high-temperature calcination, the lithium supplemented for the second time cannot enter the formed lattice again, the capacity is reduced due to the lack of Li in the lattice, and the structure collapses in the circulation process. The existing technology for manufacturing large single crystals mostly adopts a high-temperature calcination method even under the condition of sufficient lithium, namely, the sintering temperature is far higher than the temperature for synthesizing the anode material, and the lithium-nickel cation is mixed and discharged due to overhigh temperature, so that the capacity and the cycle are simultaneously reduced. The temperature is increased only for one-time grain growth to obtain single-crystal anode materials, and the capacity is sacrificed.
Disclosure of Invention
In view of the above problems, the present invention aims to provide a large single crystal 701515 positive electrode material and a preparation method thereof, and aims to solve the technical problem that the existing high nickel positive electrode material cannot achieve high capacity and long cycle under high voltage.
On one hand, the preparation method of the large single crystal nickel-cobalt-manganese cathode material comprises the following steps:
step S1, continuously or indirectly introducing a mixed aqueous solution of a nickel source, a cobalt source, a manganese source and a magnesium salt and an alkali solution into the reaction kettle;
step S2, blowing N into the reaction kettle2Adjusting the pH value to 12-14, stirring to obtain a NiCoMnMg precipitate, and directly washing and centrifuging the NiCoMnMg precipitate to obtain NiCoMnMg precursor slurry;
step S3, dispersing the NiCoMnMg precursor slurry in water, respectively dissolving LiOH and titanium salt in aqueous solution, firstly adding titanium salt solution in a certain amount, then adding LiOH aqueous solution, mixing uniformly, and directly evaporating water to dryness to obtain the NiCoMnMg precursor, Ti (OH)4A mixture precursor of LiOH;
step S4, the mixture precursor is addedDrying for 4-6h at the temperature of 400-aNixCoyMnzMgpO·qTiO2An oxide;
step S5, mixing the LiaNixCoyMnzMgpO·qTiO2Mixing oxide with magnesium source and lithium source, then introducing 0.5-0.1% of mist water into the roasting furnace in the temperature rising process in the atmosphere of air or oxygen, not introducing the water in the constant temperature and temperature lowering stage, and sintering the mixture for 8-24 h at the temperature of 700 plus materials 800 ℃ to obtain LibMgM(NixCoyMnzMgNTiq)O2A positive electrode material;
step S6, mixing the LibMgM(NixCoyMnzMgNTiq)O2Dispersing the anode material in a high-speed mixer and sieving to obtain D50Is a large monocrystal nickel-cobalt-manganese anode material with the thickness of 6-8 um.
Further, in step S1, the nickel source, the cobalt source, the manganese source, and the magnesium salt are nickel sulfate, cobalt sulfate, manganese sulfate, and magnesium sulfate, respectively, and the alkali solution is a mixed solution of a sodium hydroxide solution and an ammonia solution, where Mg/Me is 0.2 to 2mol%, where Me is a total molar amount of nickel, cobalt, and manganese.
Further, in step S3, the titanium salt is titanium citrate, the Ti (OH)4The NiCoMnMg precursor is a precipitate on the surface of a NiCoMnMg precursor, and is obtained by precipitation of LiOH and titanium citrate, wherein the Ti/Me is 0.2-2 mol%, and Me is the molar total amount of nickel, cobalt and manganese.
Further, in step S2, D of the NiCoMnMg precursor slurry50＝2～4um，(D90-D10)/D50≤0.5。
Further, in step S5, the Li is addedaNixCoyMnzMgpO·qTiO2The oxides being mixed with a source of magnesium, Mg (OH)2Or MgO, the lithium source is Li2CO3Or LiOH, wherein the addition amount of the magnesium source is 20-60 mol% of Mg/Me, and Me is the total mole amount of nickel, cobalt and manganese.
On the other hand, the large single-crystal nickel-cobalt-manganese cathode material is prepared by the method, and the prepared LiaNixCoyMnzMgpO·qTiO2In the oxide, a is more than 0 and less than or equal to 0.1, x is 0.7 +/-0.02, y is 0.15 +/-0.02, z is 0.15 +/-0.02, 0.002 and less than or equal to p, and q is less than or equal to 0.02. Preparation of the obtained LibMgM(NixCoyMnzMgNTiq)O2In the anode material, b is more than or equal to 0.90 and less than or equal to 1.2, x is 0.7 +/-0.02, y is 0.15 +/-0.02, z is 0.15 +/-0.02, p is more than or equal to 0.002 and less than or equal to 0.02, q is more than 0 and less than or equal to 0.02, and M + N is more than or equal to 0.2 and less than or equal to 0.6.
The invention has the beneficial effects that: the invention reasonably prepares the precursor coated with magnesium-doped titanium and dries at low temperature to obtain LiaNixCoyMnzMgpO·qTiO2The crystal structure of the oxide cannot be damaged in the mode, then a large amount of magnesium source is doped into the obtained oxide, lithium is supplemented, then high-temperature sintering is carried out, 0.5-0.1% of atomized water is only introduced in the temperature rising stage in the sintering process, the temperature keeping stage and the temperature reducing stage are not introduced, and Li obtained by sintering is not introduced in the constant-temperature stage and the temperature reducing stagebMgM(NixCoyMnzMgNTiq)O2The positive electrode material does not need to be strongly crushed, and can be obtained by dispersing in a high-speed mixer and then sieving50The preparation method is a 6-8um large single crystal anode material, the preparation process is simple, the obtained anode material particles are large in size and good in uniformity, and high capacity and long cycle characteristics can be obtained under high voltage.
Drawings
FIG. 1 is a flow chart of a method for preparing a large single crystal nickel-cobalt-manganese cathode material according to an embodiment of the present invention;
FIG. 2 is an electron microscope image of a large single crystal Ni-Co-Mn positive electrode material prepared by the embodiment of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
The preparation method of the large single crystal nickel-cobalt-manganese anode material provided by the invention comprises the following steps:
and step S1, continuously or indirectly introducing a mixed aqueous solution of a nickel source, a cobalt source, a manganese source and a magnesium salt and an alkali solution into the reaction kettle.
The nickel source, the cobalt source, the manganese source and the magnesium salt are respectively nickel sulfate, cobalt sulfate, manganese sulfate and magnesium sulfate, the alkali solution is a mixed solution of a sodium hydroxide solution and an ammonia water solution, wherein Mg/Me is 0.2-2 mol%, and Me is the total mole amount of nickel, cobalt and manganese.
Step S2, blowing N into the reaction kettle2And adjusting the pH value to 12-14, stirring to obtain a NiCoMnMg precipitate, and directly washing and centrifuging the NiCoMnMg precipitate to obtain NiCoMnMg precursor slurry.
D of the NiCoMnMg precursor slurry50＝2～4um，(D90-D10)/D50≤0.5。
Step S3, dispersing the NiCoMnMg precursor slurry in water, respectively dissolving LiOH and titanium salt in aqueous solution, firstly adding titanium salt solution in a certain amount, then adding LiOH aqueous solution, mixing uniformly, and directly evaporating water to dryness to obtain the NiCoMnMg precursor, Ti (OH)4And a mixture precursor of LiOH.
The titanium salt is titanium citrate, the Ti (OH)4The NiCoMnMg precursor is a precipitate on the surface of a NiCoMnMg precursor, and is obtained by precipitation of LiOH and titanium citrate, wherein the Ti/Me is 0.2-2 mol%, and Me is the molar total amount of nickel, cobalt and manganese. (NiCoMnMg) (OH) for the NiCoMnMg precursor2And (4) showing.
Step S4, drying the mixture precursor at the temperature of 400-600 ℃ for 4-6h to obtain LiaNixCoyMnzMgpO·qTiO2Oxide, a is more than 0 and less than or equal to 0.1, x is 0.7 +/-0.02, y is 0.15 +/-0.02, z is 0.15 +/-0.02, p is more than or equal to 0.002 and less than or equal to 0.2, and q is more than 0 and less than or equal to 0.02.
Step S5, mixing the LiaNixCoyMnzMgpO·qTiO2Oxide and magnesium sourceMixing with a lithium source, introducing 0.5-0.1% of atomized water into the roasting furnace in the temperature rise process in the atmosphere of air or oxygen, not introducing the atomized water in the constant temperature and temperature reduction stages, and sintering at the temperature of 700-bMgM(NixCoyMnzMgNTiq)O2The positive electrode material has b not less than 0.90 and not more than 1.2, x is 0.7 +/-0.02, y is 0.15 +/-0.02, z is 0.15 +/-0.02, p is not less than 0.002 and not more than 0.02, q is more than 0 and not more than 0.02, and M + N is not less than 0.2 and not more than 0.6.
In this step, the magnesium source is Mg (OH)2Or MgO, the lithium source is Li2CO3Or LiOH, wherein the addition amount of the magnesium source is 20-60 mol% of Mg/Me, and Me is the total mole amount of nickel, cobalt and manganese.
Step S6, (3) the positive electrode material is not required to be strongly pulverized, and the Li is addedbMgM(NixCoyMnzMgNTiq)O2Dispersing the anode material in a high-speed mixer and sieving to obtain D50Is a large monocrystal nickel-cobalt-manganese anode material with the thickness of 6-8 um.
The effect of the large single crystal nickel cobalt manganese anode material prepared by the invention is verified by the following examples.
Example (b):
(1) and continuously or indirectly introducing a mixed aqueous solution of nickel sulfate, cobalt sulfate, manganese sulfate and magnesium sulfate and a mixed solution of a sodium solution and an ammonia water solution into the reaction kettle, wherein the Mg/Me is 0.2 mol%.
(2) Blowing N into the reaction kettle2Adjusting the pH value to 12-14, stirring to obtain NiCoMnMg precipitate, directly washing and centrifuging the NiCoMnMg precipitate to obtain NiCoMnMg precursor slurry, and D of the NiCoMnMg precursor slurry50＝2～4um，(D90-D10)/D50≤0.5。
(3) Dispersing the NiCoMnMg precursor slurry in water, respectively dissolving LiOH and a titanium salt in an aqueous solution, wherein Ti/Me is 0.2-2 mol%, adding a titanium salt solution in a certain amount, adding a LiOH aqueous solution, uniformly mixing, and directly evaporating water to dryness to obtain the NiCoMnMg precursor and Ti (OH) containing)4And a mixture precursor of LiOH.
(4) Drying the mixture precursor for 6h at 400 ℃ to obtain LiaNixCoyMnzMgpO·qTiO2An oxide.
(5) The Li is addedaNixCoyMnzMgpO·qTiO2Oxides and Mg (OH)2And Li2CO3Mixing, introducing 0.1% atomized water into the roasting furnace in the air atmosphere during the temperature rise process, keeping constant temperature and cooling, and sintering at 800 deg.C for 12 hr to obtain LibMgM(NixCoyMnzMgNTiq)O2And (3) a positive electrode material. Here Mg (OH)2The amount of Mg/Me added is 20 to 60 mol%.
(6) Subjecting the Li tobMgM(NixCoyMnzMgNTiq)O2Dispersing the anode material in a high-speed mixer and sieving to obtain D50The electron microscope image of the large single crystal nickel cobalt manganese anode material with the thickness of 6-8um is shown in figure 2.
The large single crystal positive electrode material was tested under a half cell with the following results: 2.75-4.4V, the 0.2C capacity of 195mAh/g, the circulation retention rate of 99% at 50 turns at 1C/1C, and the capacity and the circulation performance of the lithium battery are obviously improved at high voltage.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (3)
1. A preparation method of a large single crystal nickel-cobalt-manganese cathode material is characterized by comprising the following steps:
step S1, continuously or indirectly introducing a mixed aqueous solution of a nickel source, a cobalt source, a manganese source and a magnesium salt and an alkali solution into the reaction kettle;
step S2, blowing N into the reaction kettle2Adjusting the pH value to 12-14, stirring to obtain a NiCoMnMg precipitate, and directly washing and centrifuging the NiCoMnMg precipitate to obtain NiCoMnMg precursor slurry;
step S3, dispersing the NiCoMnMg precursor slurry in water, respectively dissolving LiOH and titanium salt in aqueous solution, firstly adding titanium salt solution in a certain amount, then adding LiOH aqueous solution, mixing uniformly, and directly evaporating water to dryness to obtain the NiCoMnMg precursor, Ti (OH)4A mixture precursor of LiOH;
step S4, drying the mixture precursor at the temperature of 400-600 ℃ for 4-6h to obtain LiaNixCoyMnzMgpO·qTiO2An oxide;
step S5, mixing the LiaNixCoyMnzMgpO·qTiO2Mixing oxide with magnesium source and lithium source, then introducing 0.5-0.1% of mist water into the roasting furnace in the temperature rising process in the atmosphere of air or oxygen, not introducing the water in the constant temperature and temperature lowering stage, and sintering the mixture for 8-24 h at the temperature of 700 plus materials 800 ℃ to obtain LibMgM（NixCoyMnzMgNTiq）O2A positive electrode material;
step S6, mixing the LibMgM（NixCoyMnzMgNTiq）O2Dispersing the anode material in a high-speed mixer and sieving to obtain D50Is a large single crystal nickel cobalt manganese anode material of 6-8 um;
in step S2, D of the NiCoMnMg precursor slurry50=2~4um，（D90-D10）/D50≤0.5；
In step S5, the LiaNixCoyMnzMgpO·qTiO2The oxides being mixed with a source of magnesium, Mg (OH)2Or MgO, the lithium source is Li2CO3Or LiOH, wherein the addition amount of the magnesium source is Mg/Me = 20-60 mol%, and Me is the total mole amount of nickel, cobalt and manganese.
2. The method for preparing a large single crystal nickel-cobalt-manganese cathode material according to claim 1, wherein in step S1, the nickel source, the cobalt source, the manganese source, and the magnesium salt are respectively nickel sulfate, cobalt sulfate, manganese sulfate, and magnesium sulfate, and the alkali solution is a mixture of a sodium hydroxide solution and an ammonia solution, where Mg/Me = 0.2-2 mol%, where Me is a total molar amount of nickel, cobalt, and manganese.
3. The method for preparing large single crystal Ni-Co-Mn positive electrode material according to claim 1, wherein in step S3, the Ti salt is titanium citrate, and the Ti (OH)4The NiCoMnMg precursor is a precipitate on the surface of a NiCoMnMg precursor, and is obtained by precipitating LiOH and titanium citrate, wherein the Ti/Me = 0.2-2 mol%, and Me is the molar total amount of nickel, cobalt and manganese.
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| CN107311242A (en) * | 2017-08-10 | 2017-11-03 | 济南大学 | A kind of lithium ion battery improved preparation method of large single crystal layered cathode material |
| CN107768619A (en) * | 2017-09-26 | 2018-03-06 | 格林美（无锡）能源材料有限公司 | A kind of nickelic anode material of lithium battery of high power capacity monocrystalline and preparation method thereof |
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| CN104134791A (en) * | 2014-07-10 | 2014-11-05 | 宁波金和新材料股份有限公司 | High-voltage mono-crystal lithium nickel cobalt manganese oxide anode material and preparation method thereof |
| CN107311242A (en) * | 2017-08-10 | 2017-11-03 | 济南大学 | A kind of lithium ion battery improved preparation method of large single crystal layered cathode material |
| CN107768619A (en) * | 2017-09-26 | 2018-03-06 | 格林美（无锡）能源材料有限公司 | A kind of nickelic anode material of lithium battery of high power capacity monocrystalline and preparation method thereof |
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