CN105655572A - Spherical lithium nickel manganese positive electrode material preparation method - Google Patents
Spherical lithium nickel manganese positive electrode material preparation method Download PDFInfo
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- CN105655572A CN105655572A CN201410636593.0A CN201410636593A CN105655572A CN 105655572 A CN105655572 A CN 105655572A CN 201410636593 A CN201410636593 A CN 201410636593A CN 105655572 A CN105655572 A CN 105655572A
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Abstract
The present invention relates to a spherical lithium nickel manganese positive electrode material preparation method, which comprises preparing a nickel-manganese oxide precursor, and further comprises: (1) uniformly mixing a melting salt lithium source comprising a lithium source and a flux and the nickel-manganese oxide precursor at a high speed to form a nickel-manganese oxide precursor and lithium matching mixture; (2) sintering the nickel-manganese oxide precursor and lithium matching mixture to obtain a sintered product; and (3) carrying out a heat treatment on the sintered product, and screening to complete the preparation process of the spherical lithium nickel manganese positive electrode material. According to the present invention, the nickel-manganese oxide precursor and the melting salt lithium source are subjected to high temperature sintering, the melting salt lithium source forms the liquid phase during the high temperature sintering, and the tap density of the lithium nickel manganese material can achieves 2.5 g/cm<3> and the specific surface area is as small as 0.3 m<2>/g, such that the dissolving of Ni ions and Mn ions in the electrolyte during the material cycle process is reduced, the electrical property and the cycle stability of the material are improved, the workability of the electrode is improved, and the method is suitable for large scale commercial production.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, the preparation method particularly relating to a kind of spherical nickel-lithium manganate anode material.
Background technology
Spherical nickel-lithium manganate anode material has theoretical specific energy high for 146.7mAh/g and the high theoretical discharge voltage platform of 4.7V, and has environmental friendliness and feature with low cost, and therefore it is with a wide range of applications as power battery anode material.
Currently known spherical nickel-lithium manganate anode material all adopts solid phase method or liquid-phase coprecipitation. Although solid phase method is less costly, but nickel manganese element is difficult to be uniformly distributed, and high temperature sintering is easily caused the generation of impurity phase, has a strong impact on capacity and the cycle performance of spherical nickel-lithium manganate anode material. Spherical nickel-lithium manganate anode material prepared by liquid-phase coprecipitation, although for spherical morphology, but loosely organized, in some instances it may even be possible to and generating hollow structure, loose structure exists that material tap density is low (is generally 1.5-1.8g/cm3Between) and specific surface area (be typically in 1.5m greatly2/ more than g) deficiency, thus causing electrode machining performance and material circulation poor-performing.
Summary of the invention
The present invention solves that the technical problem existed in known technology provides a kind of capacity and tap density high, specific surface area is little, effectively reduce spherical nickel-lithium manganate anode material Ni, Mn ion dissolving in the electrolytic solution in cyclic process, there is electrical property and stable circulation performance, electrode processability is good, the preparation method being suitable for the spherical nickel-lithium manganate anode material that large-scale commercial produces.
The present invention includes following technical scheme:
The preparation method of spherical nickel-lithium manganate anode material, including preparing nickel manganese oxide presoma, is characterized in: also include following preparation process:
(1) the fuse salt lithium source and the described nickel manganese oxide presoma mixed at high speed that are formed in lithium source and flux are uniform, form the mixture after nickel manganese oxide presoma joins lithium;
(2) the mixture after described nickel manganese oxide presoma being joined lithium is placed in sintering furnace, heats up with the speed of 0.5-10 DEG C/min, Isothermal sinter 6-20h at 800-1000 DEG C, naturally cools to room temperature with stove, forms sinter;
(3) being placed in sintering furnace by described sinter, heat up with the speed of 0.5-5 DEG C/min, at 600 DEG C-850 DEG C, heat treatment 3-20h, naturally cools to room temperature with stove, sieves, and completes the preparation process of spherical nickel-lithium manganate anode material of the present invention.
The present invention can also adopt following technical measures:
Described lithium source is LiOH, Li2CO3Or LiOH and Li2CO3Mixture.
Described flux is LiCl, LiF, Li3PO4��B2O3��Li2O��MoO3In one or more mixture.
Described (1) high speed hybrid mode is high-speed stirred mixing or the mixing of high speed ball milling.
The present invention has the advantage that and good effect:
Present invention employs and nickel manganese oxide presoma and fuse salt lithium source are carried out high temperature sintering, the liquid phase that fuse salt lithium source is formed when high temperature sintering, reduce the sintering temperature of nickel ion doped, and mass transfer rate when adding nickel ion doped high temperature sintering, improve the tap density of nickel ion doped material (up to 2.5g/cm3), grain growth effect and crystal formation integrity degree and specific discharge capacity (1C gram up to 130-133mAh/g), the specific surface area reducing nickel ion doped material (can to 0.3m2/ g), thus reducing spherical nickel-lithium manganate anode material Ni, Mn ion dissolving in the electrolytic solution in cyclic process, improve electrical property and the stable circulation performance of spherical nickel-lithium manganate anode material, improve the processability of electrode, be suitable for large-scale commercial and produce.
Accompanying drawing explanation
Fig. 1 is the spherical nickel-lithium manganate anode material SEM figure of the embodiment of the present invention 1 preparation;
Fig. 2 is the spherical nickel-lithium manganate anode material SEM figure of currently known comparative example 1 preparation;
Fig. 3 is the embodiment of the present invention 1 and the spherical nickel-lithium manganate anode material room temperature cycles correlation curve figure of comparative example 1 preparation;
Fig. 4 is the embodiment of the present invention 1 and 50 DEG C of high temperature circulation correlation curve figure of spherical nickel-lithium manganate anode material of comparative example 1 preparation.
Detailed description of the invention
For the summary of the invention of the present invention, feature and effect can be disclosed further, describe in detail as follows especially exemplified by following instance.
The preparation method of spherical nickel-lithium manganate anode material, including preparing nickel manganese oxide presoma, is characterized in: also include following preparation process:
(1) the fuse salt lithium source and the described nickel manganese oxide presoma mixed at high speed that are formed in lithium source and flux are uniform, form the mixture after nickel manganese oxide presoma joins lithium;
(2) the mixture after described nickel manganese oxide presoma being joined lithium is placed in sintering furnace, heats up with the speed of 0.5-10 DEG C/min, Isothermal sinter 6-20h at 800-1000 DEG C, naturally cools to room temperature with stove, forms sinter;
(3) being placed in sintering furnace by described sinter, heat up with the speed of 0.5-5 DEG C/min, at 600 DEG C-850 DEG C, heat treatment 3-20h, naturally cools to room temperature with stove, sieves, and completes the preparation process of spherical nickel-lithium manganate anode material of the present invention.
Described lithium source is LiOH, Li2CO3Or LiOH and Li2CO3Mixture.
Described flux is LiCl, LiF, Li3PO4��B2O3��Li2O��MoO3In one or more mixture.
Described (1) high speed hybrid mode is high-speed stirred mixing or the mixing of high speed ball milling.
Embodiment 1:
Step 1: according to nickel: manganese mol ratio is 1:3, is configured to the nickel manganese mixed solution that total ion concentration is 3.6mol/L by nickel sulfate and manganese sulfate; The proportioning being 0.2 with ammonia alkali mole, adds ammonia, as Task-size Controlling solution in the sodium carbonate liquor of 4mol/L; Being continuously fed in stirred autoclave by nickel manganese mixed solution and Task-size Controlling solution with also stream mode, the flow rate set of reactor is 300ml/min, and mixing speed is 200r/min, and reaction temperature is 55 DEG C, and pH value is 9, successive reaction 24-48h, forms material;
Step 2: the material formed in step 1 is carried out solid-liquid separation in filter pressing solid-liquid separator, the washing of isolated solid material is after 7.5 to pH value, carries out 120 DEG C in an oven, and 15h's is dry, obtains nickelous carbonate manganese presoma;
Step 3: the nickelous carbonate manganese presoma obtained in step 2 is placed in sintering furnace and decomposes 10h in 700 DEG C, obtain nickel manganese oxide presoma;
Step 4: according to LiMn1.5Ni0.5O4Component, according to the nickel manganese oxide presoma will made in step 3 and 50%Li2CO3+ 47%LiOH+3%B2O3The fuse salt lithium source of composition is placed in high speed mixer mix homogeneously, forms the mixture after nickel manganese oxide presoma joins lithium;
Step 5: the nickel manganese oxide presoma that step 4 is made join lithium after mixture be placed in sintering furnace, sinter 15h in 930 DEG C, naturally cool to room temperature with stove, form sinter;
Step 6: sinter step 5 made is placed in sintering furnace, in 700 DEG C of heat treatment 10h, naturally cools to room temperature with stove, sieves, complete the preparation process of spherical nickel-lithium manganate anode material of the present invention. Embodiment 2:
Step 1: according to nickel: manganese mol ratio is 1:3, is configured to the nickel manganese mixed solution that total ion concentration is 4mol/L by nickel sulfate and manganese sulfate; The proportioning being 0.3 with ammonia alkali mole, adds ammonia, as Task-size Controlling solution in the sodium carbonate liquor of 4mol/L; Being continuously fed in stirred autoclave by nickel manganese mixed solution and Task-size Controlling solution with also stream mode, the flow rate set of reactor is 300ml/min, and mixing speed is 200r/min, and reaction temperature is 60 DEG C, and pH value is 8.5, successive reaction 24-48h, forms material;
Step 2: the material formed in step 1 is carried out solid-liquid separation in filter pressing solid-liquid separator, the washing of isolated solid material is after 7.5 to pH value, carries out 100 DEG C in an oven, and 15h's is dry, obtains nickelous carbonate manganese presoma;
Step 3: the nickelous carbonate manganese presoma obtained in step 2 is placed in sintering furnace and decomposes 10h in 650 DEG C, obtain nickel manganese oxide presoma;
Step 4: according to LiMn1.5Ni0.5O4Component, by the nickel manganese oxide presoma made in step 3 and 30%Li2CO3The fuse salt lithium source of+65%LiOH+5%LiCl composition is placed in high speed mixer mix homogeneously, forms the mixture after nickel manganese oxide presoma joins lithium;
Step 5: the nickel manganese oxide presoma that step 4 is made join lithium after mixture be placed in sintering furnace, sinter 15h in 930 DEG C, naturally cool to room temperature with stove, form sinter
Step 6: sinter step 5 made is placed in sintering furnace, in 650 DEG C of heat treatment 10h, naturally cools to room temperature with stove, sieves, complete the preparation process of spherical nickel-lithium manganate anode material of the present invention. Embodiment 3:
Step 1: according to nickel: manganese mol ratio is 1:3, is configured to the nickel manganese mixed solution that total ion concentration is 2mol/L by nickel sulfate and manganese sulfate; The proportioning being 0.4 with ammonia alkali mole, adds ammonia, as Task-size Controlling solution in the sodium carbonate liquor of 2mol/L; Being continuously fed in stirred autoclave by nickel manganese mixed solution and Task-size Controlling solution with also stream mode, the flow rate set of reactor is 400ml/min, and mixing speed is 300r/min, and reaction temperature is 60 DEG C, and pH value is 8, successive reaction 24-48h, forms material;
Step 2: the material formed in step 1 is carried out solid-liquid separation in filter pressing solid-liquid separator, the washing of isolated solid material is after 7 to pH value, carries out 130 DEG C in an oven, and 15h's is dry, obtains nickelous carbonate manganese presoma;
Step 3: the nickelous carbonate manganese presoma obtained in step 2 is placed in sintering furnace and decomposes 10h in 750 DEG C, obtain nickel manganese oxide presoma;
Step 4: according to LiNi0.45Mn1.45Cr0.1O4Component, by the nickel manganese oxide presoma made in step 3 and 64%Li2CO3+ 30%LiOH+3%LiCl+3%Li2The fuse salt lithium source of O composition is placed in high speed mixer mix homogeneously, forms the mixture after nickel manganese oxide presoma joins lithium;
Step 5: the nickel manganese oxide presoma that step 4 is made join lithium after mixture be placed in sintering furnace, sinter 15h in 950 DEG C, naturally cool to room temperature with stove, form sinter
Step 6: sinter step 5 made is placed in sintering furnace, in 650 DEG C of heat treatment 10h, naturally cools to room temperature with stove, sieves, complete the preparation process of spherical nickel-lithium manganate anode material of the present invention. Comparative example 1:
Step 1: select nickel sulfate and manganese sulfate, according to nickel: manganese mol ratio is the 1:3 nickel manganese mixed solution being configured to 3.6mol/L; In the sodium carbonate liquor of 4mol/L, ammonia is added, as Task-size Controlling solution with the proportioning that ammonia alkali mole is 0.2; Being continuously fed in stirred autoclave by nickel manganese mixed solution and Task-size Controlling solution with also stream mode, the flow rate set of reactor is 300ml/min, and mixing speed is 200r/min, and reaction temperature is 55 DEG C, and pH value is 9, successive reaction 24-48h, forms material;
Step 2: the material formed in step 1 is carried out solid-liquid separation in filter pressing solid-liquid separator, the washing of isolated solid material is after 7.5 to pH value, carries out 120 DEG C in an oven, and 15h's is dry, obtains nickelous carbonate manganese presoma;
Step 3: the nickelous carbonate manganese presoma obtained in step 2 is placed in sintering furnace and decomposes 10h in 700 DEG C, obtain nickel manganese oxide presoma;
Step 4: according to LiMn1.5Ni0.5O4Component, by the nickel manganese oxide presoma made in step 3 and Li2CO3The fuse salt lithium source of composition is placed in high speed mixer mix homogeneously, forms the mixture after nickel manganese oxide presoma joins lithium;
Step 5: the nickel manganese oxide presoma that step 4 is made join lithium after mixture be placed in sintering furnace, sinter 15h in 950 DEG C, naturally cool to room temperature with stove, form sinter
Step 6: sinter step 5 made is placed in sintering furnace, in 650 DEG C of heat treatment 10h, naturally cools to room temperature with stove, sieves, complete the preparation process of currently known spherical nickel-lithium manganate anode material.
Fig. 1 is the spherical nickel-lithium manganate anode material LiNi of the embodiment of the present invention 1 preparation0.5Mn1.5O4SEM figure, Fig. 2 be currently known comparative example 1 preparation spherical nickel-lithium manganate anode material LiNi0.5Mn1.5 O4The SEM figure of positive electrode; Drawing from Fig. 1 and Fig. 2, spherical nickel-lithium manganate anode material tap density prepared by the present invention is up to 2.3g/cm3, specific surface area can be as small as 0.41m2/ g, one time crystal grain mean size is 1.2 ��m; And spherical nickel-lithium manganate anode material tap density prepared by currently known method is 1.6g/cm3, specific surface area is 2.6m2/ g, one time crystal grain mean size is 0.3 ��m. Comparative result shows, spherical nickel-lithium manganate anode material prepared by the present invention has tap density height, grain growth effect and crystal formation integrity degree, the feature that specific surface area is little.
The spherical nickel-lithium manganate anode material respectively prepared by the embodiment of the present invention 1 and currently known comparative example 1 carries out 3.5-4.95V, 1.2C discharge and recharge test at room temperature, circulating discharge curve in Fig. 3 to find out, the spherical nickel-lithium manganate anode material of embodiment 1 preparation keeps initial capacity 95% 300 times;The spherical nickel-lithium manganate anode material of comparative example 1 preparation keeps initial capacity 64% 300 times.
The spherical nickel-lithium manganate anode material respectively prepared by the embodiment of the present invention 1 and currently known comparative example 1 carries out 3.5-4.95V, 1.2C discharge and recharge test in 50 DEG C of high temperature, circulating discharge curve in Fig. 4 to find out, the spherical nickel-lithium manganate anode material of embodiment 1 preparation keeps initial capacity 88.4% 210 times; The spherical nickel-lithium manganate anode material of comparative example 1 preparation keeps initial capacity 49.1% 110 times.
Test shows, spherical nickel-lithium manganate anode material prepared by the present invention, no matter at room temperature environment or in high temperature circulation, is respectively provided with good cycle performance.
The operation principle of the present invention:
Spherical nickel-lithium manganate anode material is in high temperature circulation process, and in material, the dissolving in the electrolytic solution of Ni, Mn ion is the major reason causing cycle performance rapid decay.
Present invention employs co-precipitation and prepare nickel manganese oxide presoma, and the fuse salt lithium source that mixing is made up of lithium source and flux carries out high temperature sintering, due to the liquid phase that fuse salt lithium source is formed when high temperature sintering, reduce the sintering temperature of nickel ion doped, and mass transfer rate when adding nickel ion doped high temperature sintering, improve the tap density of nickel ion doped material, grain growth effect and crystal formation integrity degree, reduce the specific surface area of nickel ion doped material, thus reducing spherical nickel-lithium manganate anode material Ni in cyclic process, the dissolving in the electrolytic solution of Mn ion, improve electrical property and the stable circulation performance of spherical nickel-lithium manganate anode material, improve the processability of electrode, it is suitable for large-scale commercial to produce.
Although above the preferred embodiments of the present invention being described; but the invention is not limited in above-mentioned detailed description of the invention; above-mentioned detailed description of the invention is merely schematic; it is not restrictive; those of ordinary skill in the art is under the enlightenment of the present invention; without departing under present inventive concept and scope of the claimed protection situation, it is also possible to make a lot of form. These belong within protection scope of the present invention.
Claims (4)
1. the preparation method of spherical nickel-lithium manganate anode material, including preparing nickel manganese oxide presoma, it is characterised in that: also include following preparation process:
(1) the fuse salt lithium source and the described nickel manganese oxide presoma mixed at high speed that are formed in lithium source and flux are uniform, form the mixture after nickel manganese oxide presoma joins lithium;
(2) the mixture after described nickel manganese oxide presoma being joined lithium is placed in sintering furnace, heats up with the speed of 0.5-10 DEG C/min, Isothermal sinter 6-20h at 800-1000 DEG C, naturally cools to room temperature with stove, forms sinter;
(3) being placed in sintering furnace by described sinter, heat up with the speed of 0.5-5 DEG C/min, at 600 DEG C-850 DEG C, heat treatment 3-20h, naturally cools to room temperature with stove, sieves, and completes the preparation process of spherical nickel-lithium manganate anode material of the present invention.
2. the preparation method of spherical nickel-lithium manganate anode material according to claim 1, it is characterised in that: described lithium source is LiOH, Li2CO3Or LiOH and Li2CO3Mixture.
3. the preparation method of spherical nickel-lithium manganate anode material according to claim 1, it is characterised in that: described flux is LiCl, LiF, Li3PO4��B2O3��Li2O��MoO3In one or more mixture.
4. the preparation method of spherical nickel-lithium manganate anode material according to any one of claim 1-3, it is characterised in that: described (1) high speed hybrid mode is high-speed stirred mixing or the mixing of high speed ball milling.
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| CN109037672A (en) * | 2018-09-13 | 2018-12-18 | 广东邦普循环科技有限公司 | A kind of preparation method of power battery nickel-cobalt lithium manganate material |
| CN109873145A (en) * | 2019-02-25 | 2019-06-11 | 合肥国轩电池材料有限公司 | A kind of nickel-cobalt-manganese ternary anode sphere material and preparation method thereof |
| CN110304665A (en) * | 2019-07-11 | 2019-10-08 | 兰州理工大学 | A kind of preparation method of micron-order single-crystal nickel lithium manganate anode material |
| CN117038956A (en) * | 2023-10-09 | 2023-11-10 | 浙江帕瓦新能源股份有限公司 | Cobalt-free high-nickel positive electrode material, preparation method thereof and lithium ion battery |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109037672A (en) * | 2018-09-13 | 2018-12-18 | 广东邦普循环科技有限公司 | A kind of preparation method of power battery nickel-cobalt lithium manganate material |
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| CN109873145B (en) * | 2019-02-25 | 2022-04-19 | 合肥国轩电池材料有限公司 | Nickel-cobalt-manganese ternary positive electrode spherical material and preparation method thereof |
| CN110304665A (en) * | 2019-07-11 | 2019-10-08 | 兰州理工大学 | A kind of preparation method of micron-order single-crystal nickel lithium manganate anode material |
| CN117038956A (en) * | 2023-10-09 | 2023-11-10 | 浙江帕瓦新能源股份有限公司 | Cobalt-free high-nickel positive electrode material, preparation method thereof and lithium ion battery |
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Application publication date: 20160608 |