AU2020101817A4 - Mg-Zr co-doped high nickel ternary cathode material and preparation method and application thereof - Google Patents
Mg-Zr co-doped high nickel ternary cathode material and preparation method and application thereof Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22C—ALLOYS
- C22C19/00—Alloys based on nickel or cobalt
- C22C19/03—Alloys based on nickel or cobalt based on nickel
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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- H01M4/40—Alloys based on alkali metals
- H01M4/405—Alloys based on lithium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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Abstract
The invention discloses a Mg-Zr co-doped high nickel ternary anode material for lithium-ion
batteries and a preparation method and application thereof. A high nickel ternary precursor
containing cations such as Mg and Zr is prepared by a co-precipitation method, and the obtained
precursor is mixed with a lithium source and sintered to obtain the Mg-Zr co-doped high nickel
ternary anode material. The doped Mg ions can stabilize the material structure and inhibit Li/Ni
mixing; the doping of Zr ions reduces the oxygen evolution of the materials, which solves the
problems of Li/Ni mixed discharge and oxygen evolution of the high nickel ternary materials
and improves the cycle stability of the battery.
Description
Mg-Zr co-doped high nickel ternary cathode material and preparation method and application thereof
[01] The invention belongs to the field of batteries, and particularly relates to a Mg-Zr co-doped high nickel ternary anode material and a preparation method and application thereof.
[02] Lithium-ion batteries have attracted much attention because of their advantages, such as high energy density, long cycle life, environmental friendliness, memoryless response and so on. Although lithium-ion batteries have made remarkable achievements in the field of portable digital electronic products, their energy density needs to be continuously improved to meet the application in new energy vehicles. The high nickel ternary material- LiNio.8Coo.1Mno.102 is regarded as an ideal cathode material for lithium-ion batteries with high energy density due to its high reversible capacity (~4.3V, 200mAh/g) and low cost. However, the nickel content as high as 80% will also bring a series of problems, such as the ionic radius of Ni 2+ is close to the radius of Li', and it is easy for Ni to occupy Li site in the actual cycle process, resulting in the mixed discharge of Ni/Li, so the battery capacity is attenuated. In addition, the high nickel ternary material LiNio.8Coo.1Mno.102 will undergo H2-H3 phase transition at about 4.1V. With the precipitation of lattice oxygen, the electrolyte will be oxidized, and the structure of the material will change from lamellar to spinel and rock salt, which will lead to the decrease of material cycle stability.
[03] In order to solve the problems of Ni / Li ion mixed discharge and lattice oxygen precipitation in the practical application of high nickel ternary material LiNio.8Coo.1Mno.102 , the invention provides a Mg-Zr co-doped high nickel ternary cathode material for solving these problems.
[04] To achieve the above purpose, the present invention provides a Mg-Zr co doped high nickel ternary cathode material and its preparation method and application. The specific technical scheme is as follows.
[05] According to one technical scheme of the invention, the chemical formula of the Mg-Zr co-doped high-nickel ternary cathode material is LiNio.8Coo.1Mn.1-x yMgxZryO2, wherein x+yO0.05.
[06] According to the second technical scheme of the invention, the Mg-Zr co doped high nickel ternary cathode material is applied to lithium-ion batteries.
[07] According to the third technical scheme of the invention, the preparation method of the Mg-Zr co-doped high nickel ternary cathode material comprises the following steps.
[08] Si. Preparation of Mg-Zr co-doped high nickel ternary cathode material precursor
[09] According to the chemical formula Nio.8Coo.1Mno.1-x-yMgxZry(OH)2, wherein x+y<0.05, weigh nickel salt, manganese salt, cobalt salt, magnesium salt and zirconium salt, add water and mix evenly after weighing, adjust the pH value to 11-12. Keep stirring, and after stirring, precipitate, filter, clean the filter residue and dry it to obtain the Mg-Zr co-doped high nickel ternary cathode material precursor.
[010] S2. Preparation of Mg-Zr co-doped high nickel ternary cathode material
[011] According to the molar ratio of Li to Ni+Co+Mn+Mg+Zr of 1.05:1, mix and stir the lithium source and the precursor obtained in Sl, then filter, dry and sinter it to obtain the Mg-Zr co-doped high nickel ternary cathode material.
[012] Furthermore, the nickel salt, manganese salt, cobalt salt, magnesium salt and zirconium salt in S are Ni(N3)2, Co(NO3)2, Mn(N3)2, Mg(N03)2, Zr(N03)4, and the lithium source in S2 is lithium hydroxide.
[013] Furthermore, in Si, the purity of nickel salt, manganese salt, cobalt salt, magnesium salt and zirconium salt are all greater than 98%; in S2, the purity of lithium source is more than 98%.
[014] Furthermore, in Sl, NaOH solution and ammonia water are used to adjust the pH value, wherein the concentration of NaOH solution is 2mol/L and the concentration of ammonia water is 0.5mol/L.
[015] Furthermore, the pH value in S Iis adjusted to 12.
[016] Further, in Si, adding water means adding deionized water; the stirring time is 1 to 3 hours; the drying temperature is 60°C and the drying time is 11 to 12 hours.
[017] Further, in S2, the stirring time is 4 to 6 hours; the drying temperature is °C and the drying time is 11 to12 hours.
[018] Further, in S2, the sintering is divided into two times, wherein the first sintering temperature is 440-460°C and time is 5 to 6 hours. The second sintering temperature is 730-770°C and time is 13 to 17 hours. The heating rate of the first and second sintering is 2C/min and oxygen is continuously introduced in the sintering process.
[019] The invention has the following beneficial technical effects.
[020] The invention synthesizes a precursor of Mg-Zr co-doped high-nickel ternary cathode material by a co-precipitation method, wherein the chemical formula of the precursor is Nio.8Coo.1Mn.1-x-yMgxZry(OH)2 and x+y<0.05. Then mixing a lithium source with the prepared precursor in proportion; and finally annealing at high temperature to obtain the Mg-Zr co-doped high-nickel ternary cathode material with the chemical formula of LiNio.8Co.1Mn.1-x-yMgxZryO2,wherein x+y<0.05. The doped Mg ions can enter Li site, which further stabilizes the material structure and reduces Li/Ni mixed discharge, while doped Zr ions enter Ni site, thereby reducing the problem of lattice oxygen evolution in the materials, Based on the synergistic effect of Mg and
Zr co-doped, high nickel material LiNio.Co.1Mn.1-x-yMgxZryO2 is used as the cathode material of lithium-ion battery, which solves the problems of Li/Ni mixed discharge and oxygen evolution and thus effectively improves the cycle stability of the battery.
[021] Various exemplary embodiments of the present invention will now be described in detail, which should not be regarded as a limitation of the present invention, but rather as a more detailed description of certain aspects, characteristics and embodiments of the present invention. It should be understood that the terms described here are only for describing specific embodiments, and are not intended to limit the present invention.
[022] In addition, as for the numerical range, it should be understood that every intermediate value between the upper limit and the lower limit of the range is also specifically disclosed. Intermediate values within any stated value or stated range and every smaller range between any other stated value or intermediate values within the stated range are also included. The upper and lower limits of these smaller ranges can be independently included or excluded from the range.
[023] Unless otherwise stated, all technical and scientific terms used herein have the same meanings as commonly understood by those skilled in the art to which the present invention relates. Although the present invention only describes preferred methods and materials, any methods and materials similar or equivalent to those described herein may be used in the practice or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe methods and/or materials related to the documents. In case of conflict with any incorporated documents, the contents of this specification shall prevail.
[024] Example 1
[025] The method for preparing Mg-Zr co-doped high nickel ternary cathode material comprises the following steps.
[026] Si. Preparation of Mg-Zr co-doped high nickel ternary precursor
[027] Weigh Ni(N03)2, Co(NO3)2, Mn(N03)2, Mg(N03)2, Zr(N03)4 according to the molar ratio of Ni: Co: Mn+Mg+Zr of 8:1:1, wherein Mn: Mg: Zr is 3: 1: 1. Add the above samples into deionized water and mix them evenly. Adjust the pH value of the mixed solution to 12 with 2mol/L NaOH solution and 0.5mol/L ammonia water. Stir for 2 hours, stand for precipitation, filter, clean the filter residue, and dry them at 60°C
for 12 hours in a blast drying oven to obtain precursor Nio.8Coo.1Mno.o6Mgo.o2Zro.o2(OH)2.
[028] S2. Preparation of Mg-Zr co-doped high nickel ternary cathode material
[029] LiOH and precursor Nio.8Coo.1Mno.o6Mgo.o2Zro.o2(OH)2 are mixed in ethanol according to the molar ratio of Li to Ni+Co+Mn+Mg+Zr of 1.05:1. Stir for 4h, then filter, and dry at 60°C for 12 hours in a blast drying oven. Then sinter it in a tubular
furnace, first at 450°C for 5 hours and second at 750°C for 15 hours. The heating rate
of the first and second sintering is 2C/min, oxygen is continuously introduced in the
sintering process, and the Mg-Zr co-doped high nickel ternary cathode material is obtained after cooling.
[030] Example 2
[031] The method for preparing Mg-Zr co-doped high nickel ternary cathode material comprises the following steps.
[032] S1. Preparation of Mg-Zr co-doped high nickel ternary precursor
[033] Weigh Ni(N03)2, Co(NO3)2, Mn(N03)2, Mg(N03)2, Zr(N03)4 according to
the molar ratio of Ni: Co: Mn+Mg+Zr of 8:1:1, wherein Mn: Mg: Zr is 6: 3: 1. Add the above samples into deionized water and mix them evenly. Adjust the pH value of the mixed solution to 12 with 2mol/L NaOH solution and 0.5mol/L ammonia water. Stir for 1 hour, stand for precipitation, filter, clean the filter residue, and dry them at 60°C for 12 hours in a blast drying oven to obtain precursor Nio.8Coo.1Mno.o6Mgo.o3Zro.oi(OH)2.
[034] S2. Preparation of Mg-Zr co-doped high nickel ternary cathode material
[035] LiOH and precursor Nio.8Coo.1Mno.o6Mgo.3Zro.oi(OH)2 are mixed in ethanol according to the molar ratio of Li to Ni+Co+Mn+Mg+Zr of 1.05:1. Stir for 5 hours, then filter, and dry it at 60°C for 12 hours in a blast drying oven. Then sinter it in a tubular furnace, first at 440°C for 6 hours and second at 770°C for 13 hours. The heating rate of the first and second sintering is 2°C/min, oxygen is continuously introduced in the sintering process, and the Mg-Zr co-doped high nickel ternary cathode material is obtained after cooling.
[036] Example 3
[037] The method for preparing Mg-Zr co-doped high nickel ternary cathode material comprises the following steps.
[038] Sl. Preparation of Mg-Zr co-doped high nickel ternary precursor
[039] Weigh Ni(N03)2, Co(NO3)2, Mn(N03)2, Mg(N03)2, Zr(N03)4according to the molar ratio of Ni: Co: Mn+Mg+Zr of 8:1:1, wherein Mn: Mg: Zr is 6: 1: 3. Add the above samples into deionized water and mix them evenly. Adjust the pH value of the mixed solution to 11 with 2mol/L NaOH solution and 0.5mol/L ammonia water. Stir for 3 hours, stand for precipitation, filter, clean the filter residue, and dry them at 60°C for 12 hours in a blast drying oven to obtain precursor Nio.8Coo.1Mno.o6Mgo.oiZro.o3(OH)2.
[040] S2. Preparation of Mg-Zr co-doped high nickel ternary cathode material
[041] LiOH and precursor Nio.8Coo.1Mno.o6Mgo.oiZro.o3(OH)2 are mixed in ethanol according to the molar ratio of Li to Ni+Co+Mn+Mg+Zr of 1.05:1. Stir for 6 hours, then filter, and dry it at 60°C for 12 hours in a blast drying oven. Then sinter it in a tubular furnace, first at 460°C for 5 hours and second at 730°C for 17 hours. The heating rate of the first and second sintering is 2°C/min, oxygen is continuously introduced in the sintering process, and the Mg-Zr co-doped high nickel ternary cathode material is obtained after cooling.
[042] In order to compare the advantages of the present invention, a comparative example is also set during the experiment.
[043] Comparative Example 1
[044] The method for preparing high nickel ternary cathode material comprises the following steps.
[045] Si. Preparation of high nickel ternary precursor
[046] Weigh Ni(N03)2, Co(NO 3) 2, Mn(N03)2, Mg(N03)2 according to the molar ratio of Ni: Co: M is 8: 1: 1. Add the above samples into deionized water and mix them evenly. Adjust the pH value of the mixed solution to 10 with 2mol/L NaOH solution and 0.5mol/L ammonia water. Stir for 2 hours, stand for precipitation, filter, clean the filter residue, and dry them at 60°C for 12 hours in a blast drying oven to obtain
precursor Nio.8Co.1Mn.1(OH)2.
[047] S2. Preparation of high nickel ternary cathode material
[048] LiOH and precursor Nio.8Coo.1Mn.1(OH)2 are mixed in ethanol according to the molar ratio of Li to Ni+Co+Mn of 1.05:1. Stir for 4 hours, then filter, and dry it at 60°C for 12 hours in a blast drying oven. Then sinter it in a tubular furnace, first at
450°C for 5 hours and second at 750°C for 15 hours. The heating rate of the first and
second sintering is 2°C/min, oxygen is continuously introduced in the sintering process,
and the high nickel ternary cathode material is obtained after cooling.
[049] Comparative Example 2
[050] The method for preparing Mg doped high nickel ternary cathode material comprises the following steps.
[051] Si. Preparation of Mg doped high nickel ternary precursor
[052] Weigh Ni(N03)2, Co(NO3)2, Mn(N03)2, Mg(N03)2 according to the molar ratio of Ni: Co: Mn+Mg of 8:1:1, wherein Mn: Mg is 3: 1. Add the above samples into deionized water and mix them evenly. Adjust the pH value of the mixed solution to 12 with 2mol/L NaOH solution and 0.5mol/L ammonia water. Stir for 2 hours, stand for precipitation, filter, clean the filter residue, and dry them at 60°C for 12 hours in a blast drying oven to obtain precursor Nio.Coo.1Mno.6Mgo.o4(OH)2.
[053] S2. Preparation of Mg doped high nickel ternary cathode material
[054] LiOH and precursor Nio.Coo.1Mno.o6Mgo.o4(OH)2 are mixed in ethanol according to the molar ratio of Li to Ni+Co+Mn+Mg of 1.05:1. Stir for 4 hours, then filter, and dry it at 60°C for 12 hours in a blast drying oven. Then sinter it in a tubular furnace, first at 450°C for 5 hours and second at 750°C for 15 hours. The heating rate of the first and second sintering is 2C/min, oxygen is continuously introduced in the sintering process, and the M doped high nickel ternary cathode material is obtained after cooling.
[055] The materials prepared in Examples 1, 2 and 3 and Comparative Examples 1 and 2 are applied to button batteries, and the 100-week cycle capacity retention rates of button batteries corresponding to each material are evaluated. The results are as follows.
[056] The 100-week cycle retention rates of 0.1C button batteries with Mg-Zr co doped high nickel ternary cathode materials prepared in Example 1, 2 and 3 are 96.2%, 95.3% and 95.8%, respectively, which are all above 95%. The 100-week cycle retention rate of 0.1C button battery with the high nickel ternary cathode material prepared in Comparative Example 1 is 87.1%. The 100-week cycle retention rate of 0.1C button battery with Mg-doped high nickel ternary cathode material prepared in Comparative Example 2 is 93.6%.
[057] According to the test results of 100-cycle capacity retention rate of button batteries, Mg-Zr co-doped can obviously improve the cycle stability of batteries with high nickel ternary cathode materials.
[058] The above embodiments only describe the preferred mode of the invention, but do not limit the scope of the invention. On the premise of not departing from the design spirit of the invention, various modifications and improvements made by ordinary technicians in the field to the technical scheme of the invention shall fall within the protection scope determined by the claims of the invention.
[059] Although the invention has been described with reference to specific examples, it will be appreciated by those skilled in the art that the invention may be embodied in many other forms, in keeping with the broad principles and the spirit of the invention described herein.
[060] The present invention and the described embodiments specifically include the best method known to the applicant of performing the invention. The present invention and the described preferred embodiments specifically include at least one feature that is industrially applicable
Claims (12)
1. A kind of Mg-Zr co-doped high nickel ternary cathode material is
characterized in that its chemical formula is LiNia.sCoo.1Mno.1-x-yMgxZryO2,wherein
x+yS0.05.
2. The application of the Mg-Zr co-doped high nickel ternary cathode material
according to claim 1 in Lithium-ion batteries.
3. The preparation method of Mg-Zr co-doped high nickel ternary cathode
material according to claim 1 is characterized in that the preparation method comprises
the following steps.
Si. Preparation of Mg-Zr co-doped high nickel ternary cathode material
precursor
According to the chemical formula Nio.Coo.1Mno.1-x-yMgxZry(OH)2, wherein
x+yS0.05, weigh nickel salt, manganese salt, cobalt salt, magnesium salt and zirconium
salt, add water and mix evenly after weighing, adjust the pH value to 11-12. Keep
stirring, and after stirring, precipitate, filter, clean the filter residue and dry it to obtain
the Mg-Zr co-doped high nickel ternary cathode material precursor.
S2. Preparation of Mg-Zr co-doped high nickel ternary cathode material
According to the molar ratio of Li to Ni+Co+Mn+Mg+Zr of 1.05:1, mix and
stir the lithium source and the precursor obtained in Si, then filter, dry and sinter it to
obtain the Mg-Zr co-doped high nickel ternary cathode material.
4. The preparation method according to claim 4 is characterized in that in Si, the
nickel salt, manganese salt, cobalt salt, magnesium salt and zirconium salt are Ni(N03)2,
Co(NO3)2, Mn(N03)2, Mg(N03)2, Zr(N03)4 . The lithium source in S2 is lithium
hydroxide.
5. The preparation method according to claim 3 is characterized in that in S1, the
purity of nickel salt, manganese salt, cobalt salt, magnesium salt and zirconium salt is
greater than 98%; in S2, the purity of lithium source is more than 98%.
6. The preparation method according to claim 3 is characterized in that in S1,
NaOH solution and ammonia water are used for adjusting pH value, wherein the
concentration of NaOH solution is 2mol/L and the concentration of ammonia water is
0.5 mol/L.
7. The preparation method according to claim 3 is characterized in that in Si,
adding water means adding deionized water; the stirring time is 1-3h; the drying
temperature is 60°C and the drying time is 11 to 12 hours.
8. The preparation method according to claim 3 is characterized in that in S2, the
stirring time is 4 to 6 hours; the drying temperature is 60°C and the drying time is 11 to
12 hours.
9. The preparation method according to claim 3 is characterized in that in S2, the
sintering is carried out twice, wherein the first sintering temperature is 440-460°C, the
time is 5 to 6 hours and the second sintering temperature is 730-770°C, the time is 13 to 17 hours.
The heating rate of the first and second sintering is 2°C/min, and oxygen is continuously introduced in the sintering process.
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| CN112490417A (en) * | 2020-11-05 | 2021-03-12 | 佛山科学技术学院 | Mg-Zr co-doped high-nickel ternary material and preparation method and application thereof |
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| CN116177617A (en) * | 2022-12-07 | 2023-05-30 | 青海师范大学 | Na-Ti co-doped modified high-nickel ternary positive electrode material and preparation method thereof |
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2020
- 2020-08-14 AU AU2020101817A patent/AU2020101817A4/en not_active Ceased
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| CN112490417A (en) * | 2020-11-05 | 2021-03-12 | 佛山科学技术学院 | Mg-Zr co-doped high-nickel ternary material and preparation method and application thereof |
| CN112811403B (en) * | 2020-12-31 | 2022-08-05 | 南通瑞翔新材料有限公司 | Mg/Ti co-doped Li 3 PO 4 Coated high-nickel ternary cathode material and preparation method thereof |
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