CN114084917B - Nickel-cobalt-manganese ternary precursor with XRD diffraction bifurcation double peak and preparation method thereof - Google Patents
Nickel-cobalt-manganese ternary precursor with XRD diffraction bifurcation double peak and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a nickel-cobalt-manganese ternary precursor with an XRD diffraction bifurcation double peak and a preparation method thereof. In the powder X-ray diffraction measurement of the precursor by CuK alpha rays, the peak shape of 2 theta at 32.5 +/-1 degrees, 38.5 +/-1 degrees, 52.5 +/-1.5 degrees and 58.5 +/-2 degrees is double. In the process of preparing the precursor by coprecipitation, the additive is added, and the surface activity of the metal ions is improved by utilizing the excellent compatibility of the additive.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a nickel-cobalt-manganese ternary precursor with an XRD diffraction bifurcation double peak and a preparation method thereof.
Background
The nickel-cobalt-manganese hydroxide is generally prepared by a coprecipitation method, and the sphere-like nickel-cobalt-manganese hydroxide is formed by utilizing nickel salt, cobalt salt, manganese salt, hydroxide and ammonia water in a certain reaction system. With the increase of nickel content, after the nickel-cobalt-manganese hydroxide synthesized by the traditional method is baked into a positive electrode material, a series of defects such as poor crystallinity, overhigh internal stress, increased charge-discharge irreversible reaction, poor cycle performance, poor stability and the like are easy to occur when the nickel-cobalt-manganese hydroxide is applied to a battery.
Chinese patent No. CN111509214B discloses the following technical contents: in a powder X-ray diffraction measurement using CuK α rays, diffraction peaks at diffraction angles 2 θ =65 ± 1 ° are split, and the two diffraction peak positions are 2 θ =64.5 ± 0.5 ° (α) and 2 θ =64.9 ± 0.5 ° (β), respectively. The diffraction peak at a diffraction angle 2 θ of 65 ± 1 ° is cleaved, which indicates that the positive electrode material has good crystallinity, but the above patent studies the positive electrode material after high-temperature sintering and does not represent a precursor. The positive electrode material has very strong inheritance to the morphology and performance of a precursor of the positive electrode material, and the research on the precursor with diffraction peak cleft has very important significance for further improving the crystallinity of the positive electrode material.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a nickel-cobalt-manganese ternary precursor with an XRD diffraction bifurcation double peak. The other purpose of the invention is to provide a preparation method of the precursor.
In order to achieve the above object, the present invention provides the following technical solutions.
A Ni-Co-Mn ternary precursor with XRD diffraction bifurcation has a chemical general formula of Ni1-x-yCoxMny(OH)2X is more than or equal to 0.1, and Y is more than 0. Said front partIn powder X-ray diffraction measurement of the precursor by CuK alpha rays, the peak shape of 2 theta at 32.5 +/-1 degrees, 38.5 +/-1 degrees, 52.5 +/-1.5 degrees and 58.5 +/-2 degrees is double peak. The double peak is composed of two single peaks, the half-peak width of the double peak is 0.7-0.99, and the half-peak width of the single peak is 0.15-0.9. The diffraction peak height of the precursor is 70-4000.
Furthermore, the median particle diameter D50 of the precursor is 3-20 μm, and the diameter distance is 0.4-1.2.
The calculation method of the radial distance is (D90-D10)/D50.
Further, the BET of the precursor is 3-18m2(ii) g, tap density of 0.4-2.6g/cm3。
Further, the diffraction peak positions of the precursors are shifted by 0.094-1.217 ° at 2 θ angles (100), (101), (102), (110), (111), (112), (002), (003) compared with JCPDS standard cards 14-0117 or 73-1520.
Based on the same inventive concept, the invention provides a preparation method of the nickel-cobalt-manganese ternary precursor with XRD diffraction bifurcation double peaks. The preparation method adopts a coprecipitation method, and the precursor generates XRD diffraction bifurcate double peaks by adding the additive. The method specifically comprises the following steps:
preparing a nickel-cobalt-manganese mixed salt solution, an alkali solution and an ammonia water solution;
step (2), adding pure water as a base solution into a reaction kettle;
step (3), adding the mixed salt solution, the alkali solution and the ammonia water solution into a reaction kettle in a concurrent flow manner, and adjusting the pH value of the reaction system to be 10-12 and the alkalinity to be 3-18 g/L;
adding an additive in at least one stage of the reaction process of the step (3) in the process of preparing a mixed salt solution, the process of preparing an ammonia water solution, the base solution and the like;
and (4) stopping the reaction after the granularity D50 of the reaction slurry reaches 3-20 μm, filtering and separating to obtain a solid phase, and aging, washing and drying the solid phase to obtain the nickel-cobalt-manganese ternary precursor with the XRD diffraction bifurcation double peak.
Further, the additive is at least one of ammonium dodecyl sulfate, triethanolamine dodecyl sulfate and concentrated ammonia water.
Furthermore, the amount of the additive required by each ton of precursor finished product is 400-3600 g based on the precursor finished product.
Furthermore, the total concentration of metal ions in the mixed salt solution is 1.0-2.5mol/L, the concentration of the ammonia water solution is 0.1-6mol/L, and the concentration of the alkali solution is 2.4-10 mol/L.
Further, the temperature of the bottom liquid of the reaction kettle is adjusted to be 30-80 ℃.
Further, the temperature of the reaction system is kept between 30 and 80 ℃ during the reaction process of the step (3).
Further, the rotating speed of the reaction system in the reaction process of the step (3) is 3.7-9.3m/s (linear speed).
Further, in the step (3), the flow rate of the mixed metal salt solution is 100-500 ml/min.
In the process of preparing the precursor by coprecipitation, the additive is added, and the excellent compatibility of the additive is utilized to improve the surface activity of metal ions, so that the precursor product with two branches at the positions of 2 theta =32.5 +/-1 degrees, 38.5 +/-1 degrees, 52.5 +/-1.5 degrees and 58.5 +/-2 degrees is prepared.
The precursor prepared by the invention has crystal distortion, and can reduce side reactions in the charging and discharging process when being applied to a battery after being roasted into a positive electrode material, thereby effectively reducing irreversible reactions and inhibiting gas generation.
Drawings
FIG. 1 is an XRD powder diffraction pattern of the precursors prepared in examples 1-5.
Fig. 2 is an SEM image of 20000 magnifications of the precursor prepared in example 1.
Fig. 3 is a 10000-magnification SEM image of the precursor prepared in example 1.
Fig. 4 is a 10000-magnification SEM image of the precursor prepared in example 2.
Fig. 5 is a 5000-magnification SEM image of the precursor prepared in example 3.
Fig. 6 is a 5000-magnification SEM image of the precursor prepared in example 4.
Fig. 7 is a 5000-magnification SEM image of the precursor prepared in example 5.
Fig. 8 is a 5000-magnification SEM image of the precursor prepared in example 6.
Detailed Description
The present invention will now be described in detail with reference to the drawings, which are given by way of illustration and explanation only and should not be construed to limit the scope of the present invention in any way.
It is to be noted that, unless otherwise specified, technical or scientific terms used herein shall have the ordinary meaning as understood by those skilled in the art to which the invention pertains.
Example 1:
preparing a mixed sulfate solution of nickel, cobalt and manganese with the total metal ion concentration of 2.4mol/L in advance, wherein the molar ratio of Ni to Co to Mn is =5 to 2 to 3, adding 100g of ammonium dodecyl sulfate into 54L of 3mol/L concentrated ammonia water for sufficient ablation, and marking as solution A. Adding pure water into a reaction kettle, wherein the volume of the pure water is 1/3 of the reaction kettle, starting heating and stirring, the temperature is 55 ℃, the initial linear velocity of stirring is 6.5m/s, continuously pumping a mixed sulfate solution, 10mol/L concentrated alkali and A solution into a synthesis tank in a parallel flow manner for coprecipitation reaction, keeping the pH value of a reaction system at 12, the alkalinity at 6g/L, the temperature at 55 ℃, the stirring linear velocity at 6.5m/s, stopping the reaction when the median particle diameter of reaction slurry is 16.5 mu m, filtering the reaction slurry, aging the obtained solid phase for 30 minutes by using 10wt% diluted alkali, filtering and washing the solid phase until the pH value is less than 8.2, and drying at 110 ℃ to obtain a precursor.
Example 2:
a mixed sulfate solution of nickel, cobalt and manganese with a total metal ion concentration of 2.0mol/L was prepared in advance, wherein Ni: Co: Mn =6:2:2 (molar ratio). 150g of lauryl sulfate triethanolamine is added into 54L of 5mol/L concentrated ammonia water for sufficient ablation and is marked as solution A. Adding pure water into a reaction kettle, wherein the volume of the pure water is 1/3 of the reaction kettle, starting heating and stirring, adjusting the temperature to 50 ℃, stirring the initial linear velocity to be 6.5m/s, continuously pumping the mixed sulfate solution, 8mol/L concentrated alkali and A solution into a synthesis tank in a parallel flow manner for reaction, controlling the pH value of a reaction system to be 11, the alkalinity to be 10g/L, the reaction temperature to be 50 ℃, stirring the linear velocity to be 6.5m/s, stopping the reaction when the median particle diameter of the reaction slurry is 17.5 mu m, filtering the reaction slurry, aging the obtained solid phase for 30 minutes by using 10wt% diluted alkali, filtering and washing the solid phase until the pH value is less than 8.2, and drying at 110 ℃ to obtain a precursor.
Example 3:
a mixed sulfate solution of nickel, cobalt and manganese with a total metal ion concentration of 2.0mol/L was prepared in advance, wherein Ni: Co: Mn =9:0.2:0.8 (molar ratio). Adding pure water into the reaction kettle, wherein the volume of the pure water is 1/3 of the volume of the reaction kettle, starting heating and stirring, adjusting the temperature to 65 ℃, and the rotating speed of a stirring paddle to be 4.5 m/s. Adding 150g of ammonium dodecyl sulfate into a reaction kettle, continuously pumping a mixed sulfate solution, a 5mol/L concentrated alkali solution and a 2.5mol/L ammonia water solution into a synthesis tank in a parallel flow manner for reaction, controlling the pH value of a reaction system to be 10, the alkalinity to be 15g/L, the reaction temperature to be 65 ℃, the stirring linear velocity to be 6.5m/s, stopping the reaction when the median particle diameter of reaction slurry is 17.5 mu m, filtering the reaction slurry, aging the obtained solid phase for 30 minutes by using a 10wt% diluted alkali solution, washing the solid phase by using pure water until the pH value is less than 8.2, and drying the solid phase at 110 ℃ to obtain a precursor.
Example 4:
a mixed sulfate solution of nickel, cobalt and manganese with a total metal ion concentration of 2.0mol/L was prepared in advance, wherein Ni: Co: Mn =9:0.3:0.7 (molar ratio). Adding pure water into the reaction kettle, wherein the volume of the pure water is 1/3 of the volume of the reaction kettle, starting heating and stirring, the temperature is 65 ℃, and the stirring linear speed is 6.5 m/s. Adding 300g of lauryl triethanolamine sulfate into a reaction kettle, using concentrated ammonia water to adjust the initial alkalinity of a base solution to 12g/L, continuously pumping a mixed sulfate solution, 10mol/L concentrated alkali and 5.5mol/L ammonia water into a synthesis tank for reaction in a parallel flow manner, controlling the pH value of a reaction system to be 10, the alkalinity to be 12g/L, the reaction temperature to be 65 ℃, the stirring linear velocity to be 6.5m/s, stopping the reaction when the median particle diameter of reaction slurry is 17.5 mu m, filtering the reaction slurry, aging the obtained solid phase for 30 minutes by using 10wt% of dilute alkali solution, washing the solid phase by using pure water until the pH value is less than 8.2, and drying the solid phase at 110 ℃ to obtain a precursor.
Example 5:
a mixed sulfate solution of nickel, cobalt and manganese with a total metal ion concentration of 2.0mol/L was prepared in advance, wherein Ni: Co: Mn =8:1:1 (molar ratio). Adding pure water into the reaction kettle, wherein the volume of the pure water is 1/3 of the volume of the reaction kettle, starting heating and stirring, the temperature is 65 ℃, and the stirring linear speed is 9.3 m/s. 300g of triethanolamine dodecyl sulfate and 150g of ammonium dodecyl sulfate are added into a reaction kettle together, and concentrated ammonia water is used for adjusting the initial alkalinity of the base solution to 9 g/L. Continuously pumping a mixed sulfate solution, 10mol/L concentrated alkali and 1.8mol/L ammonia water into a synthesis tank in a parallel flow manner for reaction, controlling the pH value of a reaction system to be 12, the alkalinity to be 13g/L, the reaction temperature to be 65 ℃, the stirring linear velocity to be 9.3m/s, stopping the reaction when the median particle size of the reaction slurry is 20 mu m, filtering the reaction slurry, aging the obtained solid phase with 5wt% of dilute alkali for 30 minutes, washing with pure water until the pH value is less than 8.2, and drying at 110 ℃ to obtain a precursor.
Example 6:
a mixed sulfate solution of nickel, cobalt and manganese with a total metal ion concentration of 2.0mol/L was prepared in advance, wherein Ni: Co: Mn =8:1:1 (molar ratio). 300g of triethanolamine dodecyl sulfate and 150g of ammonium dodecyl sulfate are added into 54L of mixed salt solution together and marked as solution A, adding pure water into a reaction kettle, wherein the volume of the pure water is 1/3 of the reaction kettle, starting heating and stirring, the reaction temperature is 65 ℃, the initial linear velocity of stirring is 9.3m/s, using concentrated ammonia to adjust the alkalinity of the initial base solution to be 9g/L, pumping the solution A, 8mol/L concentrated alkali and 6mol/L ammonia into a synthesis tank in a certain proportion for reaction, controlling the pH value of a reaction system to be 12, the alkalinity to be 9g/L, the reaction temperature to be 65 ℃, the stirring linear velocity to be 9.3m/s, stopping the reaction when the median particle size is 20 mu m, using 5% dilute alkali to age for 30 minutes, using the pure water to wash the ternary precursor until the pH value is less than 8.2, and drying at 110 ℃ to obtain the precursor.
The precursors prepared in examples 1 to 6 were measured by powder X-ray diffraction using CuK α rays, and the diffraction pattern shown in fig. 1 was obtained. As can be seen from the figure, the diffraction peak 2 theta has a double peak shape at 32.5 +/-1 degrees, 38.5 +/-1 degrees, 52.5 +/-1.5 degrees and 58.5 +/-2 degrees.
FIGS. 2 to 8 are SEM images of the precursors prepared in examples 1 to 6, respectively, and it can be seen from the SEM images that the morphology of the primary particles of the precursors is greatly different and the circularities of the secondary particles are different. The prepared precursors all have special diffraction peaks, and the special diffraction peaks can be determined not to be caused by surface structure or roundness.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (6)
1. The nickel-cobalt-manganese ternary precursor with XRD diffraction bifurcation double peaks is characterized in that the chemical general formula of the precursor is Ni1-x-yCoxMny(OH)2X is more than or equal to 0.1, and y is more than 0; in the powder X-ray diffraction measurement of the precursor by adopting CuK alpha rays, the peak shape of 2 theta at 32.5 +/-1 degrees, 38.5 +/-1 degrees, 52.5 +/-1.5 degrees and 58.5 +/-2 degrees is a double peak; the double peak consists of two single peaks, the half-peak width of the double peak is 0.7-0.99, and the half-peak width of the single peak is 0.15-0.9; the diffraction peak height of the precursor is 70-4000; BET of the precursor is 3-18m2(ii) g, tap density of 0.4-2.6g/cm3(ii) a The median particle diameter D50 of the precursor is 3-20 μm, and the diameter distance is 0.4-1.2.
2. The method for preparing the nickel-cobalt-manganese ternary precursor with the XRD diffraction bifurcated double peak according to claim 1, comprising the following steps:
preparing a nickel-cobalt-manganese mixed salt solution, an alkali solution and an ammonia water solution;
step (2), adding pure water as a base solution into a reaction kettle;
step (3), adding the mixed salt solution, the alkali solution and the ammonia water solution into a reaction kettle in a concurrent flow manner, and adjusting the pH value of the reaction system to be 10-12 and the alkalinity to be 3-18 g/L;
adding an additive in at least one stage of the reaction process of the step (3) in the process of preparing a mixed salt solution, the process of preparing an ammonia water solution, the base solution and the like; the additive is at least one of ammonium dodecyl sulfate and triethanolamine dodecyl sulfate; the amount of the additive required by each ton of precursor finished product is 400-3600 g calculated by the precursor finished product;
and (4) stopping the reaction after the granularity D50 of the reaction slurry reaches 3-20 μm, filtering and separating to obtain a solid phase, and aging, washing and drying the solid phase to obtain the nickel-cobalt-manganese ternary precursor with the XRD diffraction bifurcation double peak.
3. The method according to claim 2, wherein the total concentration of the metal ions in the mixed salt solution is 1.0 to 2.5mol/L, the concentration of the aqueous ammonia solution is 0.1 to 6mol/L, and the concentration of the alkali solution is 2.4 to 10 mol/L.
4. The method of claim 2, wherein the temperature of the bottom solution of the reaction kettle is 30-80 ℃; and (3) keeping the temperature of the reaction system at 30-80 ℃ in the reaction process of the step (3).
5. The production method according to claim 2, wherein the rotation speed of the reaction system during the reaction in the step (3) is 3.7 to 9.3 m/s.
6. The method according to claim 2, wherein the mixed metal salt solution is added at a flow rate of 100 ml/min in step (3).
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| JP2005336004A (en) * | 2004-05-26 | 2005-12-08 | Mitsubishi Chemicals Corp | Nickel manganese cobalt based multiple oxide, lamellar lithium nickel manganese cobalt based multiple oxide, lithium secondary cell positive electrode material, positive electrode for lithium secondary cell and lithium secondary cell using the same |
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| CN111204821A (en) * | 2020-02-22 | 2020-05-29 | 华友新能源科技（衢州）有限公司 | Nickel-cobalt-manganese hydroxide with particle size in bimodal distribution and preparation method thereof |
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