CN108493447B - preparation method of high-quality high-nickel multi-element positive electrode material - Google Patents
preparation method of high-quality high-nickel multi-element positive electrode material Download PDFInfo
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Abstract
The invention relates to a preparation method of a high-quality high-nickel multi-element anode material, which comprises the following steps: and (2) uniformly mixing the high-nickel multi-element precursor with a lithium source, then loading the mixture into a sagger with vent holes on the side wall and the bottom and a high-temperature-resistant organic film inside, then sending the sagger into a sintering furnace, sintering at high temperature under the condition of introducing oxygen, and crushing, sieving and demagnetizing after sintering to obtain the high-quality high-nickel multi-element cathode material. The preparation method can reduce the performance difference of the upper layer material and the lower layer material after sintering, improve the overall performance of the materials, prepare high-quality products while ensuring the production efficiency, and prolong the service life of the sagger.
Description
Technical Field
The invention relates to the technical field of preparation of lithium ion battery anode materials, in particular to a preparation method of a high-quality high-nickel multi-element anode material.
Background
At present, the main preparation method of the high-nickel multi-element anode material is solid-phase sintering, namely, a nickel-cobalt-manganese hydroxide precursor and a lithium source (lithium carbonate or lithium hydroxide) are uniformly mixed, then the mixture is put into a ceramic sagger, and then the ceramic sagger is put into a sintering furnace for high-temperature calcination, and after the calcination, the crushing, the grading and the screening are carried out, so that the multi-element material can be obtained. However, this method has the following drawbacks:
1. In the process of calcining and crystallizing a multi-element material, a stable layered crystal structure is formed, a large amount of oxygen is needed to participate in the reaction, and a certain oxygen partial pressure is needed to inhibit the deoxidation of the material in the crystallization conversion process, when the material in the sagger is thick, the oxygen is difficult to enter the bottom of the sagger through diffusion, so that the performance difference of upper and lower layer materials is large due to the oxygen deficiency of the lower layer material, and the overall performance of the material is influenced;
2. in the sintering process, the materials are in direct contact with the saggar, and the lithium source easily enters the saggar through high-temperature diffusion in the melting process to change the microstructure of the saggar materials, so that the saggar is peeled and broken, and the service life of the saggar is short.
Disclosure of Invention
based on the above, the present invention provides a method for preparing a high-quality high-nickel multi-element cathode material, which can reduce the performance difference between the upper and lower layer materials after sintering, improve the overall performance of the material, ensure the production efficiency, simultaneously prepare a high-quality product, and prolong the service life of a sagger.
The technical scheme adopted by the invention is as follows:
A preparation method of a high-quality high-nickel multi-element cathode material comprises the following steps:
And (2) uniformly mixing the high-nickel multi-element precursor with a lithium source, then loading the mixture into a sagger with vent holes on the side wall and the bottom and a high-temperature-resistant organic film inside, then sending the sagger into a sintering furnace, sintering at high temperature under the condition of introducing oxygen, and crushing, sieving and demagnetizing after sintering to obtain the high-quality high-nickel multi-element cathode material.
The sagger for sintering the high-nickel multi-element anode material is improved, so that the defects of the conventional sintering technology of the high-nickel multi-element anode material are overcome. A layer of high-temperature resistant organic film is arranged between the inside of the saggar and the materials, so that the materials can be prevented from leaking out of the vent holes of the saggar in the sintering process, in the early stage of sintering, oxygen diffused from the upper layer of the material to the inside can completely meet the oxidation requirement of metal elements, even if a high-temperature resistant organic film exists, the high-temperature resistant organic film does not have great adverse effect, and when a certain sintering temperature is reached, the organic film starts to decompose, and the material loses fluidity due to high temperature, so the material cannot flow out from the vent hole, after the organic film is decomposed, oxygen can enter from the vent holes on the side wall and the bottom of the saggar, so that the oxygen partial pressure of the lower layer material in the sintering process is increased, the crystal oxygen defect caused by the deoxidation and decomposition of the product due to the small oxygen partial pressure in the high-temperature calcination process of the material is prevented, thereby better crystallizing, reducing the performance difference of the upper layer and the lower layer, and improving the overall performance of the material.
moreover, because the side wall and the bottom of the sagger are provided with the vent holes, the gas diffusion effect is greatly improved, the loading capacity of the sagger sintering material can be increased to a greater extent, the maximum loading height available for the loading height does not influence the product quality, the production efficiency of the product is improved, and the productivity of the product is improved.
In addition, the high-temperature-resistant organic film isolates the direct contact of the lithium source and the saggar in the melting process, reduces the damage of single sintering of the saggar, and prolongs the service life of the saggar.
Further, the following steps: the molecular formula of the high-nickel multi-element precursor is NixCoyMnzM(1-x-y-z)(OH)2Wherein x is more than or equal to 0.6 and less than 1, y is more than 0 and less than or equal to 0.2, z is more than or equal to 0 and less than or equal to 0.2, and M is any one of Al, Mg, Zr and Ti; the lithium source is any one or more of lithium carbonate, lithium hydroxide, lithium acetate and lithium oxalate.
Further, the high nickel multi-element precursor and the lithium source are uniformly mixed according to the molar ratio of (Ni + Co + Mn + M) to Li ═ 1 (1-1.05).
Furthermore, the decomposition temperature of the high-temperature resistant organic film is higher than 400 ℃, no obvious melting point exists, and the high-temperature resistant organic film is not softened at the temperature below 400-600 ℃. According to empirical data, the sintered material loses fluidity due to high temperature at about 400-600 ℃, so that the organic film with the decomposition temperature higher than 400 ℃ is selected to avoid the material from flowing out of the vent hole before solidification. The high temperature resistant organic film may be polyimide or other high temperature resistant organic material.
Furthermore, the thickness of the high-temperature resistant organic film is 2-20 μm, and on the basis of preventing material leakage of the product, the dosage of the organic film material is reduced, so that the oxygen consumption and the increase of impurity elements caused by the decomposition of excessive organic film material are prevented.
Furthermore, the side wall and the bottom of the sagger are respectively provided with a plurality of vent holes, the aperture of each vent hole is 2-10mm, and the surface density of the vent holes is 2500-10000 per meter2。
Further, the preparation method specifically comprises the following steps:
(1) Adding the high-nickel multi-element precursor and a lithium source into a mixer for mixing;
(2) Putting the uniformly mixed materials into a sagger, and then carrying out block cutting or jack processing on the materials, so as to be beneficial to gas diffusion in the subsequent sintering process;
(3) feeding the loaded sagger into a sintering furnace, and sintering at high temperature under the condition of introducing oxygen, wherein the sintering temperature is 200-1000 ℃, the sagger is divided into 3-6 heat preservation sections, and the total time is 10-42 hours;
(4) And after the sintering is finished and the temperature is reduced, crushing, sieving and demagnetizing the materials obtained by sintering to obtain the high-quality high-nickel multi-element positive electrode material.
Further, the number of the cut pieces in the step (2) is 4-36.
Further, in the step (3), the high-temperature sintering is divided into the following 3 heat preservation sections: firstly heating to 500-550 ℃ and preserving heat for 4 hours, then heating to 650-700 ℃ and preserving heat for 3 hours, and then heating to 810-870 ℃ and preserving heat for 12 hours.
The early-stage heat preservation section is used for the loss of burning of carbon and water in the lithium source and the precursor and primary solid solution; the main heat preservation section in the middle stage is used for forming and growing the product crystals under the high-temperature condition; the later-stage heat preservation section is used for annealing, and the stress of the material calcined at high temperature is relieved through low-temperature heat preservation, so that the appearance of the product is improved, and the particle strength is further improved.
Further, the aperture of the sieve in the step (4) is 400 meshes.
for a better understanding and practice, the invention is described in detail below with reference to the accompanying drawings.
Drawings
FIG. 1 is a schematic view of a sagger used in the present invention.
Detailed Description
Example 1
the positive electrode material is prepared by the following steps:
(1) Adding 622 ternary precursor (molecular formula: Ni) according to the molar ratio of (Ni + Co + Mn) and Li ═ 1:1.030.6Co0.2Mn0.2(OH)2) Adding the lithium carbonate and the mixture into a high-speed mixer to be mixed for 40 minutes.
(2) And (3) putting the uniformly mixed materials into a sagger, and then cutting the materials into pieces, namely uniformly cutting the materials into 36 pieces.
As shown in figure 1, the bottom of the sagger is square, the side length of the sagger is 320mm, the height of the sagger is 130mm, the material filling height of the sagger is 100mm, the side wall and the bottom of the sagger are respectively provided with a plurality of vent holes, the aperture of each vent hole is 4mm, and each vent hole is provided with a holeHas an areal density of 5000 pieces/m2。
and a high-temperature-resistant organic film with the thickness of 10 mu m is padded in the saggar, covers the bottom and the side wall of the saggar and is positioned between the saggar and the material, and the material is specifically polyimide.
(3) And (3) feeding the loaded sagger into a sintering furnace, and sintering at high temperature under the condition that oxygen with the purity of more than 95% is introduced, wherein the sintering temperature curve is set as follows: firstly heating to 550 ℃ and preserving heat for 4 hours, then heating to 700 ℃ and preserving heat for 3 hours, and then heating to 870 ℃ and preserving heat for 12 hours.
(4) after sintering and natural cooling, mechanically crushing the sintered material, sieving with a 400-mesh sieve, and demagnetizing to obtain the finished product LiNi0.6Co0.2Mn0.2O2And (3) a positive electrode material.
Example 2
the positive electrode material is prepared by the following steps:
(1) according to the molar ratio of (Ni + Co + Mn) and Li being 1:1.05, 811 ternary precursor (molecular formula: Ni)0.8Co0.1Mn0.1(OH)2) Adding the lithium carbonate and the mixture into a high-speed mixer to be mixed for 40 minutes.
(2) and (3) putting the uniformly mixed materials into a sagger, and then cutting the materials into pieces, namely uniformly cutting the materials into 36 pieces.
As shown in figure 1, the bottom of the sagger is square, the side length of the sagger is 320mm, the height of the sagger is 130mm, the material filling height of the sagger is 100mm, the side wall and the bottom of the sagger are respectively provided with a plurality of vent holes, the aperture of each vent hole is 4mm, and the surface density of the vent holes is 5000/m2。
And a high-temperature-resistant organic film with the thickness of 10 mu m is padded in the saggar, covers the bottom and the side wall of the saggar and is positioned between the saggar and the material, and the material is specifically polyimide.
(3) And (3) feeding the loaded sagger into a sintering furnace, and sintering at high temperature under the condition that oxygen with the purity of more than 95% is introduced, wherein the sintering temperature curve is set as follows: the temperature is raised to 500 ℃ and kept for 4 hours, then raised to 650 ℃ and kept for 3.5 hours, and then raised to 820 ℃ and kept for 12 hours.
(4) After sintering and natural cooling, mechanically crushing the sintered material, sieving with a 400-mesh sieve, and demagnetizing to obtain the finished product LiNi0.8Co0.1Mn0.1O2and (3) a positive electrode material.
Example 3
The positive electrode material is prepared by the following steps:
(1) Preparing NCA precursor (molecular formula: Ni) according to the molar ratio of (Ni + Co + Al) and Li (1: 1.05)0.8Co0.15Al0.05(OH)2) Adding the lithium carbonate and the mixture into a high-speed mixer to be mixed for 40 minutes.
(2) And (3) putting the uniformly mixed materials into a sagger, and then cutting the materials into pieces, namely uniformly cutting the materials into 36 pieces.
As shown in figure 1, the bottom of the sagger is square, the side length of the sagger is 320mm, the height of the sagger is 130mm, the material filling height of the sagger is 100mm, the side wall and the bottom of the sagger are respectively provided with a plurality of vent holes, the aperture of each vent hole is 4mm, and the surface density of the vent holes is 5000/m2。
And a high-temperature-resistant organic film with the thickness of 10 mu m is padded in the saggar, covers the bottom and the side wall of the saggar and is positioned between the saggar and the material, and the material is specifically polyimide.
(3) And (3) feeding the loaded sagger into a sintering furnace, and sintering at high temperature under the condition that oxygen with the purity of more than 95% is introduced, wherein the sintering temperature curve is set as follows: the temperature is raised to 500 ℃ and kept for 4 hours, then raised to 650 ℃ and kept for 3 hours, and then raised to 810 ℃ and kept for 12 hours.
(4) After sintering and natural cooling, mechanically crushing the sintered material, sieving with a 400-mesh sieve, and demagnetizing to obtain the finished product LiNi0.8Co0.15Al0.05O2And (3) a positive electrode material.
Comparative example 1
The positive electrode material is prepared by the following steps:
(1) Adding 622 ternary precursor (molecular formula: Ni) according to the molar ratio of (Ni + Co + Mn) and Li ═ 1:1.030.6Co0.2Mn0.2(OH)2) Adding the lithium carbonate and the mixture into a high-speed mixer to be mixed for 40 minutes.
(2) And (3) putting the uniformly mixed materials into a common sagger, and then cutting the materials into pieces, namely uniformly cutting the materials into 36 pieces. The bottom of the common sagger is square, the side length is 320mm, the height is 130mm, and the material filling height is 100 mm.
(3) And (3) feeding the loaded sagger into a sintering furnace, and sintering at high temperature under the condition that oxygen with the purity of more than 95% is introduced, wherein the sintering temperature curve is set as follows: firstly heating to 550 ℃ and preserving heat for 4 hours, then heating to 700 ℃ and preserving heat for 3 hours, and then heating to 870 ℃ and preserving heat for 12 hours.
(4) After sintering and natural cooling, mechanically crushing the sintered material, sieving with a 400-mesh sieve, and demagnetizing to obtain the finished product LiNi0.6Co0.2Mn0.2O2and (3) a positive electrode material.
Comparative example 2
The positive electrode material is prepared by the following steps:
(1) According to the molar ratio of (Ni + Co + Mn) and Li being 1:1.05, 811 ternary precursor (molecular formula: Ni)0.8Co0.1Mn0.1(OH)2) Adding the lithium carbonate and the mixture into a high-speed mixer to be mixed for 40 minutes.
(2) and (3) putting the uniformly mixed materials into a common sagger, and then cutting the materials into pieces, namely uniformly cutting the materials into 36 pieces. The bottom of the common sagger is square, the side length is 320mm, the height is 130mm, and the material filling height is 100 mm.
(3) And (3) feeding the loaded sagger into a sintering furnace, and sintering at high temperature under the condition that oxygen with the purity of more than 95% is introduced, wherein the sintering temperature curve is set as follows: the temperature is raised to 500 ℃ and kept for 4 hours, then raised to 650 ℃ and kept for 3 hours, and then raised to 855 ℃ and kept for 12 hours.
(4) After sintering and natural cooling, mechanically crushing the sintered material, sieving with a 400-mesh sieve, and demagnetizing to obtain the finished product LiNi0.8Co0.1Mn0.1O2And (3) a positive electrode material.
comparative example 3
The positive electrode material is prepared by the following steps:
(1) Preparing NCA precursor (molecular formula: Ni) according to the molar ratio of (Ni + Co + Al) and Li (1: 1.05)0.8Co0.15Al0.05(OH)2) Adding the lithium carbonate and the mixture into a high-speed mixer to be mixed for 40 minutes.
(2) And (3) putting the uniformly mixed materials into a common sagger, and then cutting the materials into pieces, namely uniformly cutting the materials into 36 pieces. The bottom of the common sagger is square, the side length is 320mm, the height is 130mm, and the material filling height is 100 mm.
(3) And (3) feeding the loaded sagger into a sintering furnace, and sintering at high temperature under the condition that oxygen with the purity of more than 95% is introduced, wherein the sintering temperature curve is set as follows: the temperature is raised to 500 ℃ and kept for 4 hours, then raised to 650 ℃ and kept for 3 hours, and then raised to 810 ℃ and kept for 12 hours.
(4) After sintering and natural cooling, mechanically crushing the sintered material, sieving with a 400-mesh sieve, and demagnetizing to obtain the finished product LiNi0.8Co0.15Al0.05O2And (3) a positive electrode material.
Performance evaluation
Sampling the upper layer and the lower layer of the materials in the saggar after sintering in the step (3) in the examples 1-3 and the comparative examples 1-3 respectively, then respectively carrying out mechanical crushing, 400-mesh sieve sieving and demagnetization to obtain 12 parts of positive electrode material samples, and respectively carrying out electrical property evaluation.
The evaluation method is as follows: assembling a positive electrode material sample, a conductive agent carbon black and a binder PVDF into a 2016 type button cell in a glove box according to a mass ratio of 90:5:5, and then carrying out charge-discharge cycle test, wherein the voltage is 3.0-4.35V, the current density is 1C/1C and 0.2C/0.2C, and the evaluation results are shown in the following table.
As can be seen from the above table, the upper and lower layer materials prepared in examples 1 to 3 were substantially identical in performance by providing the sagger with the vent hole and cushioning the sagger with the high temperature resistant organic film, whereas the upper and lower layer materials prepared in comparative examples 1 to 3 using the general sagger were significantly different in performance.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention.
Claims (7)
1. A preparation method of a high-nickel multi-element cathode material is characterized by comprising the following steps: the method comprises the following steps:
(1) Adding the high-nickel multi-element precursor and a lithium source into a mixer for mixing;
(2) loading the uniformly mixed materials into a sagger with vent holes on the side wall and the bottom and a high-temperature-resistant organic film inside, and then cutting the materials into blocks or inserting holes;
(3) And (3) feeding the loaded sagger into a sintering furnace, and sintering at high temperature under the condition of introducing oxygen, wherein the sagger is divided into the following 3 heat preservation sections: firstly heating to 500-550 ℃, preserving heat for 4 hours, then heating to 650-700 ℃, preserving heat for 3 hours, and then heating to 810-870 ℃, preserving heat for 12 hours;
(4) After the sintering is finished and the temperature is reduced, crushing, sieving and demagnetizing the materials obtained by sintering to obtain the high-nickel multi-element cathode material;
Wherein the high-temperature resistant organic film is polyimide.
2. The method for preparing a high-nickel multi-element positive electrode material according to claim 1, wherein: the molecular formula of the high-nickel multi-element precursor is NixCoyMnzM(1-x-y-z)(OH)2Wherein x is more than or equal to 0.6<1，0<y is not more than 0.2, z is not less than 0 and not more than 0.2, and M is any one of Al, Mg, Zr and Ti; the lithium source is any one or more of lithium carbonate, lithium hydroxide, lithium acetate and lithium oxalate.
3. The method for preparing a high-nickel multi-element cathode material according to claim 2, wherein: and uniformly mixing the high-nickel multi-element precursor with a lithium source according to the molar ratio of (Ni + Co + Mn + M) to (Li-1-1.05).
4. The method for preparing a high-nickel multi-element positive electrode material according to claim 1, wherein: the thickness of the high-temperature resistant organic film is 2-20 mu m.
5. the method for preparing a high-nickel multi-element positive electrode material according to claim 1, wherein: the side wall and the bottom of the sagger are respectively provided with a plurality of vent holes, the aperture of each vent hole is 2-10mm, and the surface density of the vent holes is 2500-10000 per meter2。
6. The method for preparing a high-nickel multi-element positive electrode material according to claim 1, wherein: the number of the blocks in the step (2) is 4-36.
7. The method for preparing a high-nickel multi-element positive electrode material according to claim 1, wherein: the aperture of the sieve in the step (4) is 400 meshes.
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| CN109686973A (en) * | 2018-12-12 | 2019-04-26 | 无锡晶石新型能源股份有限公司 | A kind of preparation method of the nickelic positive electrode of low-cost high-quality |
| CN114560511B (en) * | 2022-01-26 | 2023-07-18 | 泾河新城陕煤技术研究院新能源材料有限公司 | High-nickel positive electrode material with high cycle stability and preparation method thereof |
| CN114249358B (en) * | 2022-03-01 | 2022-05-06 | 宜宾锂宝新材料有限公司 | Cathode material and preparation method thereof |
| CN115247958B (en) * | 2022-07-28 | 2023-07-18 | 广西立劲新材料有限公司 | Preparation method and device of long-life power lithium manganate |
| CN115504511A (en) * | 2022-09-28 | 2022-12-23 | 安徽博石高科新材料股份有限公司 | Collinear production method of anode material |
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| CN103094545A (en) * | 2013-01-24 | 2013-05-08 | 湖南桑顿新能源有限公司 | Preparation method for cathode material of high-nickel lithium ion battery |
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