AU2020101813A4 - Al-doped high-nickel ternary material and preparation method and application thereof - Google Patents
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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- 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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Abstract
The invention discloses an Al-doped high-nickel ternary material and preparation method and
application thereof, relates to the technical field of electrode materials. The present invention
first mixes the nickel source, cobalt source, manganese source and aluminium source
according to a certain molar ratio, prepares a high-nickel ternary material precursor
containing Al ions based on the co-precipitation method, and then mixes the lithium source
with the precursor, After two sintering, Al-doped high-nickel ternary material is prepared.
The invention uses the incorporation of Al ions to reduce the Ni/Li mixing, which can
improve the stability of the Ni-O bond in the material, reduce the dissolution of Ni element,
and help reduce the precipitation of oxygen in the material crystal lattice during the cycle. In
turn, the electrochemical performance of the material is improved.
Description
PATENTS ACT 1990
Al-doped high-nickel ternary material and preparation method and application thereof
The invention is described in the following statement:-
Al-doped high-nickel ternary material and preparation method and
application thereof
The invention relates to the technical field of electrode materials, in particular to an Al
doped high-nickel ternary material, and a preparation method and application thereof.
Lithium-ion batteries have attracted attention because of their advantages such as high
capacity, high working potential, low pollution and no memory response. At present,
lithium-ion batteries have been widely used in portable digital electronic products.
However, further improving the battery energy density to meet people's increasing
demand is an important trend in the development of lithium-ion batteries.
The high-nickel ternary LiNio.8Coo.1Mno.102 material is considered to be an ideal high
energy density lithium ion battery cathode material because of its reversible capacity as
high as 200mAh/g. However, the practical application of the high-nickel ternary
LiNio.8Coo.1Mno.102 material still faces huge challenges. The radius of Ni2' and Li' in the
material are relatively close, so the material is prone to mixed Ni/Li in the process of
lithium insertion and removal. That is, the position of Li is occupied by Ni, which
causes the battery capacity to decline. The high-nickel ternary LiNi.Coo.Mno.102
material will undergo a H2-H3 phase transition at about 4.1V. This process is
accompanied by the precipitation of lattice oxygen, which further causes electrolyte
oxidation and transition metal dissolution (such as Ni), this has a greater impact on the
cycle stability of the material.
Therefore, improving the performance of the high-nickel ternary LiNi.Coo.1Mno.102
material to make it have high capacity and cycle stability is an urgent problem to be
solved.
The purpose of the present invention is to provide an Al-doped high-nickel ternary
material and a preparation method and application thereof to solve the above-mentioned
problems in the prior art.
In order to achieve the above objectives, the present invention provides the following
solutions:
One of the objectives of the present invention is to provide a method for preparing Al
doped high-nickel ternary material, which includes the following steps:
Si: Preparation of Nio.8Coo.1Mn.1-xAlx(OH)2 precursor: According to the molar ratio
Ni:Co:(Mn+Al) is 8:1:1, the nickel source, cobalt source, manganese source, aluminum
source are weighed, and mixed in deionized water to obtain a mixed solution, adjust the
pH value of the mixed solution to 11-12, continue to stir for 1-3h, let the precipitate stand
still, wash the precipitate after filtration and dry to obtain the Ni.8Co.1Mn.1-xAlx(OH)2
precursor;
S2: Preparation of LiNio.8Co.1Mn.1-xAlxO2: According to the molar ratio of Li to
Ni+Co+Mn+Al of 1.05:1, the lithium source and the Ni.Coo.1Mn.1-xAlx(OH)2 precursor
prepared in step SIwere dispersed and mixed in ethanol, stirring continuously for 4-6h, the precipitate is filtered and dried, and then sintered twice in the presence of oxygen to obtain Al-doped high-nickel ternary material LiNi.Co.1Mn.1-xAlxO2.
Further, the nickel source is Ni(N03)2, the cobalt source is Co(N3)2, the manganese
source is Mn(N03)2, the aluminium source is Al(NO3)3, the lithium The source is LiOH.
Further, the purity of the nickel source, cobalt source, manganese source, aluminium
source and lithium source are all greater than 98%.
Further, in the Nio.8Co.1Mn.1-xAlx(OH)2and LiNio.8Co.1Mn.1-xAlxO2,x<0.05.
Further, in the step Si, the drying temperature is 60° C, and the drying time is 12 hours.
Further, in the step Si, NaOH solution and ammonia water are used to adjust the pH
value of the mixed solution; the NaOH solution concentration is 2 mol/L, and the
ammonia water concentration is 0.5 mol/L.
Further, in the step S2, the first sintering temperature is 450°C, the sintering time is 3-7h,
the second sintering temperature is 740-760°C, and the sintering time is 13-17h.
Further, in the step S2, the heating rate between two sintering is 2° C/min.
The second objective of the present invention is to provide an Al-doped high-nickel
ternary material prepared by the above-mentioned Al-doped high-nickel ternary material
preparation method.
The third object of the present invention is to provide an application of the above
mentioned Al-doped high-nickel ternary material in a lithium ion battery.
The present invention discloses the following technical effects:
1. After the high-nickel ternary material of the present invention is modified by Al co
doping, the mixing degree of Ni2' and Li' is low, the layered structure is stable, the
migration rate of lithium ions and electrons is improved, and it has high capacity and
excellent cycle stability.
2. The method of the present invention has simple synthesis process, readily available
raw materials required by the reactants, non-toxic, low cost, easy control of reaction
conditions, and suitability for industrial production.
3. When the high-nickel ternary material is prepared by the present invention, two
sintering can improve the stability of the ternary material, and can also improve the
external stability of the ternary material, thereby increasing the capacity and cycle
performance of the ternary material.
Various exemplary embodiments of the present invention will now be described in detail.
The detailed description should not be considered as a limitation to the present invention,
but should be understood as a more detailed description of certain aspects, characteristics,
and embodiments of the present invention.
It should be understood that the terms described in the present invention are only used to
describe specific embodiments and are not used to limit the present invention. In addition,
for the numerical range in the present invention, it should be understood that each
intermediate value between the upper limit and the lower limit of the range is also
specifically disclosed. Each smaller range between any stated value or intermediate value
within the stated range and any other stated value or intermediate value within the stated range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded from the range.
Unless otherwise specified, all technical and scientific terms used herein have the same
meaning as commonly understood by those skilled in the art in the field of the present
invention. Although the present invention only describes preferred methods and
materials, any methods and materials similar or equivalent to those described herein can
also 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 the event of conflict with any incorporated
document, the content of this manual shall prevail.
Without departing from the scope or spirit of the present invention, various improvements
and changes can be made to the specific embodiments of the present specification, which
is obvious to those skilled in the art. Other embodiments derived from the description of
the present invention will be obvious to the skilled person. The specification and
examples of this application are only exemplary.
As used herein, "including", "having", "containing", etc,are all open terms, which means
including but not limited to.
Unless otherwise specified, the "parts" in the present invention are based on parts by
mass.
The purity of the nickel source, cobalt source, manganese source, aluminum source, and
lithium source used in the embodiment of the present invention are all greater than 98%.
Example 1:
The preparation method of Al-doped high-nickel ternary material includes the following
steps:
Si: Preparation of Nio.8Coo.1Mno.a5Alo.o(OH)2 precursor: According to the molar ratio
Ni:Co:(Mn+Al) is 8:1:1, where Mn:Al=1:1, weigh Ni(N03)2, Co(NO3)2, Mn(N03)2,
Al(NO3)3, add deionized water and mix, adjust the pH of the resulting mixed solution to
11 with NaOH solution and ammonia, the concentration of the NaOH solution used is 2
mol/L, and the concentration of the ammonia is 0.5 mol/L, stirring is continued for 1
hour, and the precipitate is allowed to stand after filtering, the precipitate is washed and
driedat60°C for 12 hours to obtain aNio.8Coo.1Mno.5Alo.o5(OH)2 precursor.
S2: Preparation of LiNio.8Coo.1Mno.aAlo.o502: According to the molar ratio of Li to
Ni+Co+Mn+Al of 1.05:1, combine the lithium source with the
Nio.8Coo.1Mno.a5Alo.5(OH)2 precursor prepared in step S Iwere dispersed and mixed in
ethanol, stirred for 4 hours, filtered and dried, then, in a tube furnace fed with oxygen,
sintered at 450°C for 3h, then controlled the heating rate to 2C/min, and continued
sintering at 740°C for 13h to obtain the final product LiNi.Co.1Mno.5Alo.o502.
Example 2
The preparation method of Al-doped high-nickel ternary material includes the following
steps:
Sl: Preparation of Nio.8Coo.1Mno.a6Alo.4(OH)2 precursor: According to the molar ratio
Ni:Co:(Mn+Al) is 8:1:1, where Mn:A=3:2, weigh Ni(N03)2, Co(NO3)2, Mn(N03)2,
Al(NO3)3, add deionized water and mix, adjust the pH of the resulting mixture with
NaOH solution and ammonia to 12, the concentration of NaOH solution used is 2mol/L,
and the concentration of ammonia is 0.5mol/L, stirring is continued for 3 hours, and the
precipitate is allowed to stand. After filtering, the precipitate is washed and dried at 60° C
for 12 hours to obtain a Ni.Coo.1Mno.6Alo.o4(OH)2 precursor.
S2: Preparation of LiNio.8Coo.1Mno.aAlo.402: According to the molar ratio of Li to
Ni+Co+Mn+Al of 1.05:1, the lithium source and the prepared
Nio.8Coo.1Mno.aAlo.o4(OH )2 disperse and mix the precursor in ethanol, keep stirring for 6
hours, filter the precipitate and dry, then, in a tube furnace fed with oxygen, sintered at
450°C for 7 hours, then controlled the heating rate to 2°C/min, and continued sintering at
760°C for 17 hours to obtain the final product LiNi.Coo.1Mno.6Alo.o402.
Example 3
The preparation method of Al-doped high-nickel ternary material includes the following
steps:
Si: Preparation of Nio.8Coo.1Mno.a7Alo.3(OH)2 precursor: According to the molar ratio
Ni:Co:(Mn+Al) is 8:1:1, where Mn:A=7:3, weigh Ni(N03)2, Co(NO3)2, Mn(N03)2,
Al(NO3)3, add deionized water and mix, adjust the pH of the resulting mixture with
NaOH solution and ammonia to 12, the concentration of NaOH solution used is 2mol/L,
and the concentration of ammonia is 0.5mol/L, continue to stir for 2h, stand still to
precipitate, filter and wash the precipitate and dry at 60°C for 12h to obtain
Nio.8Coo.1Mno.a7Alo.3(OH)2 precursor.
S2: Preparation of LiNio.8Coo.1Mno.a7Alo.302: According to the molar ratio of Li to
Ni+Co+Mn+Al of 1.05:1, combine the lithium source with the
Nio.8Coo.1Mno.a7Alo.o3(OH)2 precursor prepared in step S were dispersed and mixed in
ethanol, stirred for 5 hours, filtered and dried, then in a tube furnace fed with oxygen,
sintered at 450°C for 4h, then controlled the heating rate to 2C/min, and continued
sinteringat750°C for 15h to obtain the final product LiNio.8Coo.1Mno.a7Alo.o302.
Example 4
The preparation method of Al-doped high-nickel ternary material includes the following
steps:
Sl: Preparation of Nio.8Coo.1Mno.o8Al.o2(OH)2 precursor: According to the molar ratio
Ni:Co:(Mn+Al) is 8:1:1, where Mn:A=4:1, weigh Ni(N03)2, Co(NO3)2, Mn(N03)2,
Al(NO3)3, add deionized water and mix, adjust the pH of the resulting mixed solution to
11 with NaOH solution and ammonia, the concentration of the NaOH solution used is 2
mol/L, and the concentration of the ammonia is 0.5 mol/L, continue to stir for 2h, stand
still to precipitate, filter and wash the precipitate and dry at 60°C for 12h to obtain
Nio.8Coo.1Mno.o8Al.o2(OH)2 precursor.
S2: Preparation of LiNio.8Coo.1Mno.o8Al.o202: According to the molar ratio of Li to
Ni+Co+Mn+Al of 1.05:1, combine the lithium source with the
Nio.8Coo.1Mno.o8Alo.o2(OH)2 the precursor prepared instep Sl were dispersed and
mixed in ethanol, stirred for 5 hours, filtered and dried, then, in a tube furnace with
oxygen, sintered at 450°C for 6h, then controlled the heating rate to 2C/min, and continued sintering at 760°C for 14h to obtain the final product
LiNio.8Coo.1Mn.asAlo.o202
Example 5
The preparation method of Al-doped high-nickel ternary material includes the following
steps:
SI: Preparation of Nio.8Coo.1Mno.o9Alo.oi(OH)2 precursor: According to the molar ratio
Ni:Co:(Mn+Al) is 8:1:1, where Mn:A=9:1, weigh Ni(N03)2, Co(NO3)2, Mn(N03)2,
Al(NO3)3, add deionized water and mix, adjust the pH of the resulting mixture with
NaOH solution and ammonia to 12, the concentration of NaOH solution used is 2mol/L,
and the concentration of ammonia is 0.5mol/L, continue stirring for 3 hours, let the
precipitate stand still, filter the precipitate, wash it and dry it at 60°C for 12 hours to
obtain Nio.8Coo.1Mno.o9Alo.oi(OH)2 precursor.
S2: Preparation of LiNio.8Coo.1Mno.o9Alo.oiO2: According to the molar ratio of Li to
Ni+Co+Mn+Al of 1.05:1, combine the lithium source with the
Nio.8Coo.1Mno.o9Alo.oi(OH)2 the precursor prepared in step S Iwere dispersed and mixed
in ethanol, stirred for 4 hours, filtered and dried, then, in a tube furnace fed with oxygen,
sintered at 450°C for 6h, then controlled the heating rate to 2C/min, and continued
sinteringat745°C for 16h to obtain the final product LiNi.Co.1Mno.o9Alo.o102.
Comparative example 1
The same as Example 1, the difference is that Al(NO3)3 is not added.
Comparative example 2
Same as Example 1, the difference is that the aluminum source Al(NO3)3 is replaced with
Cr(N03)3.
Using HAADF-STEM, the high-nickel ternary materials prepared in Examples 1-5 and
Comparative Examples 1-2 were characterized on the atomic scale, and the mixing
degree of the corresponding materials was calculated. The results are shown in Table 1:
Table 1
Material mixing degree(%)
Example 1 1.8
Example 2 1.7
Example 3 1.7
Example 4 1.8
Example 5 1.7
Comparative example 1 5.9
Comparative example 2 5.8
Comparative example 3 5.8
Comparative example 4 5.9
Comparative example 5 5.8
Performance Testing:
The high-nickel ternary materials prepared in Examples 1-5 and Comparative Examples
1-2 were mixed with polyvinylidene fluoride in a mass ratio of 9:1, ground into a slurry,
coated on aluminum foil, dried in 60°C vacuum drying for 24h, take it out and cut, then a
lithium battery pole piece can be obtained; the pole piece prepared by the above method is used as the positive electrode, the metal lithium piece is used as the negative electrode, and the electrolyte is added to manufacture a lithium battery.
The battery capacity tester is used to measure the battery capacity, calculate the specific
capacity, and characterize the capacity performance of the positive electrode material; the
lithium battery prepared by the above method is cycled 200 times at IC, and the capacity
change value is measured. Calculate the capacity retention rate and characterize the
capacity loss characteristics during deep discharge,the results are shown in Table 2.
Table 2
Comparative Comparative Example 1 Example 2 Example 3 Example 4 Example 5 exmple exmple example 1 example 2 Capacity of 200 cycles at 178 168 170 169 172 126 131 iC (mAh/g) Capacity retention 94.1 94.2 94.1 93.9 93.8 69.1 72.3 rate (%)
The result shows that the Al-doped high-nickel ternary material prepared by the
preparation method of the present invention has excellent cycle stability.
The above-mentioned embodiments only describe the preferred modes of the present
invention, and do not limit the scope of the present invention. Without departing from the
design spirit of the present invention, various modifications and improvements made by those of ordinary skill in the art to the technical solution of the present invention shall fall within the protection scope determined by the claims of the present invention.
Claims (10)
1. A preparation method of Al-doped high-nickel ternary material is characterized in
that it comprises the following steps:
Sl: Preparation of Nio.8Coo.1Mno.1-xAlx(OH)2 precursor: According to the molar ratio
Ni:Co:(Mn+Al) is 8:1:1, the nickel source, cobalt source, manganese source, and
aluminum source are weighed, and mixed in deionized water to obtain a mixed solution,
adjust the pH value of the mixed solution to 11-12, continue to stir for 1-3h, let the
precipitate stand still, wash the precipitate after filtration and dry to obtain the
Nio.8Coo.1Mno.1-xAlx(OH)2 precursor;
S2: Preparation of LiNio.8Coo.1Mn.1-xAlx02: According to the molar ratio of Li to
Ni+Co+Mn+Al of 1.05:1, the lithium source and the Ni.sCoo.Mn.1-xAlx(OH)2
precursor prepared in step S Iare dispersed and mixed in ethanol, stirring continuously
for 4-6h, the precipitate is filtered and dried, and then sintered twice in the presence of
oxygen to obtain Al-doped high-nickel ternary material LiNio.8Coo.1Mn.1-xAlxO2.
2. A method for preparing Al-doped high-nickel ternary material according to claim
1, characterized in that: The nickel source is Ni(N03)2, the cobalt source is Co(N03)2, the
manganese source is Mn(N03)2, the aluminum source is Al(N03)3, and the lithium source
is LiOH.
3. The method for preparing an Al-doped high-nickel ternary material according to
claim 1, wherein the purity of the nickel source, cobalt source, manganese source,
aluminum source and lithium source is greater than 98%.
4. The method for preparing an Al-doped high-nickel ternary material according to
claim 1, wherein the Nio.8Coo.1Mno.1-xAlx(OH)2 and LiNio.8Coo.1Mno.1 -xAlx02 in x<0.05.
5.The method for preparing an Al-doped high-nickel ternary material according to
claim 1, characterized in that, in the step S, the drying temperature is 60°C, and the
drying time is 12 hours.
6. The method for preparing an Al-doped high-nickel ternary material according to
claim 1, wherein in the step S, NaOH solution and ammonia water are used to adjust the
pH value of the mixed solution; the concentration of the NaOH solution is 2mol/L, The
concentration of the ammonia water is 0.5 mol/L.
7.The preparation method of an Al-doped high-nickel ternary material according to
claim 1, characterized in that, in the step S2, the first sintering temperature is 450°C, and
the sintering time is 3-7h, The second sintering temperature is 740-760°C, and the
sintering time is 13-17h.
8.The method for preparing an Al-doped high-nickel ternary material according to
claim 1, characterized in that, in the step S2, the heating rate between two sintering is
2°C/min.
9. An Al-doped high-nickel ternary material prepared by the method for preparing
an Al-doped high-nickel ternary material according to any one of claims 1-8.
10. The application of the Al-doped high-nickel ternary material of claim 9 in a lithium
ion battery.
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| CN112490418A (en) * | 2020-11-05 | 2021-03-12 | 佛山科学技术学院 | Al-doped high-nickel ternary material and preparation method and application thereof |
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2020
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112490418A (en) * | 2020-11-05 | 2021-03-12 | 佛山科学技术学院 | Al-doped high-nickel ternary material and preparation method and application thereof |
| CN112608488A (en) * | 2020-12-15 | 2021-04-06 | 荆门市格林美新材料有限公司 | MOFs-based precursor for cobalt-free lithium battery, positive electrode material and preparation method of MOFs-based precursor |
| CN112608488B (en) * | 2020-12-15 | 2023-06-02 | 荆门市格林美新材料有限公司 | MOFs-based precursor for cobalt-free lithium battery, positive electrode material and preparation method of MOFs-based precursor |
| CN113258058A (en) * | 2021-04-27 | 2021-08-13 | 浙江帕瓦新能源股份有限公司 | Aluminum and titanium lanthanum lithium phosphate co-modified nickel-rich cathode material precursor and cathode material |
| CN113387400A (en) * | 2021-05-26 | 2021-09-14 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Continuous production method and device for in-situ doping of high-nickel ternary cathode material precursor of lithium ion battery |
| CN113387400B (en) * | 2021-05-26 | 2023-09-05 | 江苏集萃安泰创明先进能源材料研究院有限公司 | Continuous production method and device for in-situ doping of high-nickel ternary positive electrode material precursor of lithium ion battery |
| CN113896253A (en) * | 2021-09-24 | 2022-01-07 | 合肥国轩电池材料有限公司 | Ternary cathode material and preparation method and application thereof |
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