CN113716623B - High-nickel ternary material LiNi0.80Co0.15Al0.05O2Coating method of - Google Patents
High-nickel ternary material LiNi0.80Co0.15Al0.05O2Coating method of Download PDFInfo
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- 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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Abstract
The invention relates to the field of energy materials, in particular to a high-nickel ternary material LiNi0.80Co0.15Al0.05O2The coating method of (1). The high-nickel ternary material LiNi of the invention0.80Co0.15Al0.05O2The coating method of (1) is to make the coating material and the high-nickel ternary material LiNi through precipitation conversion reaction0.80Co0.15Al0.05O2Forming a uniform and uniform coating body. According to the invention, through precipitation conversion reaction, the coating material and the NCA material can form a uniform and unified coating body, the falling and crushing of the coating material are effectively prevented, and the cycle stability is improved by more than 30%.
Description
Technical Field
The invention relates to the field of energy materials, in particular to a high-nickel ternary material LiNi0.80Co0.15Al0.05O2The coating method of (1).
Background
High nickel ternary material LiNi0.80Co0.15Al0.05O2The high energy density and low cost of (NCA for short) attract great attention. However, highly reactive NCA materials suffer from severe interfacial reactions. The coating is a simple and effective way for serving as a protective material and has wide application in the field of battery materials, however, the coating process at present is generally to coat a coating on a material main body in a core-shell mode by a physical blending mode or by utilizing chemical hydrolysis, the phenomenon of core-shell separation easily occurs in the use process of the material due to the non-uniformity of the coating and the weaker combination action between a core layer and the main body material, and the coating effect is ineffective.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a high nickel material LiNi by using a precipitation conversion reaction0.80Co0.15Al0.05O2The coating method of (NCA) is to combine the coating material and the NCA material more tightly and firmly, prevent the falling and the crushing of the coating material and improve the cycle stability.
The invention provides a high-nickel ternary material LiNi0.80Co0.15Al0.05O2The coating method of (1) is to make the coating material and the high-nickel ternary material LiNi through precipitation conversion reaction0.80Co0.15Al0.05O2Forming a uniform and uniform coating, comprising the steps of:
s1, preparing an NCA material precursor: dissolving and dispersing nickel-cobalt-aluminum acetate in ultrapure water, and adding oxalic acid for precipitation reaction to obtain an NCA oxalic acid precursor solution;
s2, respectively weighing a coating raw material alpha and a coating raw material beta, and preparing a coating raw material alpha solution and a coating raw material beta solution;
wherein the weight of the coating raw material is w% n M,
in the formula: n, amount of substance of NCA oxalic acid precursor;
m, the molar mass of the coating raw material;
w%, the coating material accounts for the mol percentage of the amount of the NCA oxalic acid precursor substance, and w% is 0.5-6 mol%;
s3, adding the coating raw material alpha solution into the NCA oxalic acid precursor solution to perform precipitation conversion reaction, and performing constant temperature, stirring and aging;
s4, adding a coating raw material beta solution into the NCA oxalic acid precursor solution aged in the S3 for precipitation reaction, and carrying out constant temperature, stirring and aging to obtain an NCA oxalic acid precursor C;
and S5, carrying out suction filtration, drying and calcination on the NCA oxalic acid precursor C to obtain the coated high-nickel ternary material.
Further, in S2, the coating raw material α is diammonium hydrogen phosphate or lithium acetate, and the coating raw material β is zirconium oxychloride or sulfonated graphene.
Further, the constant temperature conditions in S3 and S4 are 25-80 ℃, the stirring speed is 200-500r/min, and the aging time is 2-12 h.
Further, the suction filtration time in S5 is 10-60min, the drying mode is vacuum drying, the drying temperature range is 100-150 ℃, and the drying time is 6-24 h.
Further, the calcination process in S5 includes two calcination processes of a first stage calcination and a second stage calcination:
the temperature condition of the first-stage calcination is 400-500 ℃, the time condition is 5-12h, and an NCA oxide precursor D is obtained after calcination;
the second stage calcination conditions were: firstly, with MLi/MNCA oxide precursor DWeighing LiOH & H in a molar ratio of 1.0-1.22O, reaction of LiOH. H2After the O and the NCA oxide precursor D are uniformly mixed, calcining for 6 hours at 500-600 ℃ in an oxygen atmosphere, and then adjusting the calcining temperature to 700-900 ℃ for calcining for 10-24 hours.
The technical scheme provided by the invention has the following beneficial effects: according to the invention, through precipitation conversion reaction, the coating material and the NCA material can form a uniform and unified coating body, the falling and crushing of the coating material are effectively prevented, and the cycle stability is improved by more than 30%.
Drawings
FIG. 1 is an electrochemical specific capacity curve of a high nickel-coated ternary material in example 1 of the present invention;
FIG. 2 is an electrochemical specific capacity curve of the high nickel-coated ternary material in example 2 of the present invention;
fig. 3 is an electrochemical specific capacity curve of the sulfonated graphene coated high nickel ternary material in example 3 of the present invention;
FIG. 4 is an electrochemical specific capacity curve of the clad high nickel ternary material of comparative example 1 of the present invention;
FIG. 5 is a transmission electron micrograph (10nm) of the high-nickel-coated ternary material in example 1 of the present invention;
FIG. 6 is a transmission electron micrograph (5nm) of the high nickel-coated ternary material in example 2 of the present invention.
Detailed Description
To make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be further described with reference to the accompanying drawings.
The invention selects proper insoluble salt to realize the precipitation of alkali metal: according to the invention, oxalate precursors are prepared by oxalic acid precipitation; and then the surface of the oxalate precursor and a coating raw material alpha are converted into insoluble salt with smaller solubility product, and the coating raw material alpha of the invention needs to be selected to be capable of chemically reacting with the precursor to generate insoluble salt precipitate or a product connected with the precursor by chemical action. Finally, the precursor surface after conversion with the coating raw material alpha is subjected to stronger precipitation reaction with the coating raw material beta, so as to realize uniform and firm combination of the coating material on the NCA material.
< example 1>
High-nickel ternary material LiNi0.80Co0.15Al0.05O2The coating method comprises the following specific steps:
a) weighing 2.0108g of nickel acetate, 0.3774 g of cobalt acetate and 0.0819g of basic aluminum acetate according to the molar ratio of Ni to Co to Al of 0.80 to 0.15 to 0.05, adding 950mL of ultrapure water for dissolving, and preparing a substrate solution A with the concentration of 0.01 mol/L;
b) placing in an oil bath pan, adjusting the temperature setting of the oil bath pan to maintain the temperature of the substrate solution A at 50 ℃ and maintain the stirring speed of 300r/min for dispersion for 2 h;
c) preparing 5mol/L oxalic acid solution B, feeding the substrate solution A at the speed of 10mL/h by using an injection pump, keeping the stirring speed of 300r/min in the injection process to be 50mL in total, and aging for 6h after the injection is finished to obtain NCA oxalic acid precursor solution;
d) weighing 0.011g of diammonium hydrogen phosphate according to the weight of coating raw materials w% n M, wherein n is 0.007mol, and w% is 1 mol%, preparing 50mL of diammonium hydrogen phosphate solution, feeding the NCA oxalic acid precursor solution by an injection pump at the speed of 10mL/h, wherein the total amount is 50mL, keeping vigorous stirring in the injection process, and aging for 2h after the injection is finished; it should be noted that, in order to improve the conversion efficiency of diammonium hydrogen phosphate, diammonium hydrogen phosphate is dissolved into a solution and then reacts with the NCA oxalic acid precursor, but in practical application, a target weight of solid diammonium hydrogen phosphate substance can be directly added into the NCA oxalic acid precursor solution for reaction;
e) weighing 0.0396g of zirconium oxychloride according to the weight of the coating material w% n M, wherein n is 0.007mol, and w% is 0.5 mol%, preparing 50mL of zirconium oxychloride solution, feeding the NCA oxalic acid precursor solution aged in d) by an injection pump at the speed of 10mL/h, keeping the stirring speed of 300r/min in the injection process, and aging for 2h after the injection is finished to obtain an NCA oxalic acid precursor C;
f) carrying out suction filtration and washing on the NCA oxalic acid precursor solution C, drying in a vacuum drying oven at 120 ℃ for 12h, then primarily grinding by using an agate mortar, putting into an alumina porcelain boat, then placing into a muffle furnace, heating at the speed of 5 ℃/min, and calcining at 450 ℃ for 6h to obtain an NCA oxide precursor D;
g) with MLi/MNCA oxide precursor DWeighing LiOH & H according to the molar ratio of 1.052And O, grinding and uniformly mixing the precursor with the NCA oxide precursor D, putting the mixture into an alumina porcelain boat, putting the alumina porcelain boat into a tubular furnace, calcining the mixture for 6 hours at the temperature of 550 ℃ at the speed of 5 ℃/h in the oxygen atmosphere, and calcining the mixture for 12 hours at the temperature of 750 ℃ at the speed of 5 ℃/h to obtain the coated NCA material.
< example 2>
High-nickel ternary material LiNi0.80Co0.15Al0.05O2The coating method comprises the following specific steps:
a) weighing 2.0108g of nickel acetate, 0.3774 g of cobalt acetate and 0.0819g of basic aluminum acetate according to the molar ratio of Ni to Co to Al of 0.80 to 0.15 to 0.05, adding 950mL of ultrapure water for dissolving, and preparing a substrate solution A with the concentration of 0.01 mol/L;
b) placing in an oil bath pan, adjusting the temperature setting of the oil bath pan to maintain the temperature of the substrate solution A at 50 ℃ and maintain the stirring speed of 300r/min for dispersion for 2 h;
c) preparing 5mol/L oxalic acid solution B, feeding the substrate solution A at the speed of 10mL/h by using an injection pump, keeping the stirring speed of 300r/min in the injection process to be 50mL in total, and aging for 6h after the injection is finished to obtain NCA oxalic acid precursor solution;
d) weighing 0.064g of diammonium phosphate according to the weight of the coating raw materials w% n M, wherein n is 0.007mol, and w% is 6 mol%, preparing 50mL of diammonium phosphate solution, feeding the NCA oxalic acid precursor solution by an injection pump at the speed of 10mL/h, adding 50mL in total, keeping vigorous stirring in the injection process, and aging for 2h after the injection is finished;
e) weighing 0.1188g of zirconium oxychloride according to the weight of the coating raw materials w% n M, wherein n is 0.007mol, and w% is 3 mol%, preparing 50mL of zirconium oxychloride solution, feeding the NCA oxalic acid precursor solution aged in d) at a speed of 10mL/h by using an injection pump, wherein the total amount is 50mL, maintaining the stirring speed of 300r/min during the injection process, and aging for 6h after the injection is finished to obtain an NCA oxalic acid precursor C;
f) carrying out suction filtration and washing on the NCA oxalic acid precursor solution C, drying in a vacuum drying oven at 120 ℃ for 12h, then primarily grinding by using an agate mortar, putting into an alumina porcelain boat, putting into a muffle furnace, heating at the speed of 5 ℃/min, and calcining at 450 ℃ for 6h to obtain an NCA oxide precursor D;
g) with MLi/MNCA oxide precursor DWeighing LiOH & H according to the molar ratio of 1.102O, and the NCA oxide precursor D are ground and mixed uniformly, then are put into an alumina porcelain boat and are placed into a tube furnace,the coated NCA material was obtained by calcining in an oxygen atmosphere at a rate of 5 ℃/h up to 550 ℃ for 6h followed by a rate of 5 ℃/h up to 750 ℃ for 12 h.
< example 3>
High-nickel ternary material LiNi0.80Co0.15Al0.05O2The coating method comprises the following specific steps:
a) weighing 2.0108g of nickel acetate, 0.3774 g of cobalt acetate and 0.0819g of basic aluminum acetate according to the molar ratio of Ni to Co to Al of 0.80 to 0.15 to 0.05, adding 950mL of ultrapure water for dissolving, and preparing a substrate solution A with the concentration of 0.01 mol/L;
b) placing in an oil bath pan, adjusting the temperature setting of the oil bath pan to maintain the temperature of the substrate solution A at 50 ℃ and maintain the stirring speed of 300r/min for dispersion for 2 h;
c) preparing 5mol/L oxalic acid solution B, feeding the substrate solution A at the speed of 10mL/h by using an injection pump, keeping the stirring speed of 300r/min in the injection process, and aging for 6h after the injection is finished, wherein the total amount of the oxalic acid solution B is 50 mL;
d) weighing 0.0440g of lithium acetate according to the weight of the coating raw materials w% n M, wherein n is 0.007mol, and w% is 5 mol%, preparing 50mL of lithium acetate solution, feeding NCA oxalic acid precursor solution by an injection pump at the speed of 10mL/h, keeping vigorous stirring in the injection process, and aging for 2h after the injection is finished;
e) weighing 0.077g of sulfonated graphene according to the weight of coating raw materials w% n M, wherein n is 0.007mol, and w% is 5 mol%, preparing 50mL of sulfonated graphene solution, feeding the aged NCA oxalic acid precursor solution in d) by an injection pump at a speed of 10mL/h for 50mL in total, keeping the stirring speed of 300r/min in the injection process, and aging for 6h after the injection is finished to obtain an NCA oxalic acid precursor C;
f) carrying out suction filtration and washing on the NCA oxalic acid precursor solution C, drying in a vacuum drying oven at 120 ℃ for 12 hours, then primarily grinding in an agate mortar, putting into an alumina porcelain boat, putting into a muffle furnace, heating at the rate of 5 ℃/min, and calcining at 450 ℃ for 6 hours to obtain an NCA oxide precursor D;
h) with MLi/MNCA oxide precursor DWeighing LiOH & H in a molar ratio of 1.202O, and NCAnd grinding and uniformly mixing the A oxide precursor D, putting the mixture into an alumina porcelain boat, putting the alumina porcelain boat into a tube furnace, calcining for 6h at the temperature of 550 ℃ at the speed of 5 ℃/h in an oxygen atmosphere, and calcining for 12h at the temperature of 750 ℃ at the speed of 5 ℃/h to obtain the coated NCA material.
< comparative example 1>
High-nickel ternary material LiNi0.80Co0.15Al0.05O2The coating method comprises the following specific steps:
a) weighing 2.0108g of nickel acetate, 0.3774 g of cobalt acetate and 0.0819g of basic aluminum acetate according to the molar ratio of Ni to Co to Al of 0.80 to 0.15 to 0.05, adding 950mL of ultrapure water for dissolving, and preparing a substrate solution A with the concentration of 0.01 mol/L;
b) placing in an oil bath pan, adjusting the temperature setting of the oil bath pan to maintain the temperature of the substrate solution A at 50 ℃ and maintain the stirring speed of 300r/min for dispersion for 2 h;
c) preparing 5mol/L oxalic acid solution B, feeding the substrate solution A at the speed of 10mL/h by using an injection pump, keeping the stirring speed of 300r/min in the injection process to be 50mL in total, and aging for 6h after the injection is finished to obtain NCA oxalic acid precursor solution;
d) weighing 0.1979g of zirconium oxychloride according to the weight of the coating raw materials w% n M, wherein n is 0.007 mol% and w% is 5 mol%, preparing 50mL of zirconium oxychloride solution, feeding the NCA oxalic acid precursor solution aged in d) by an injection pump at the speed of 10mL/h, keeping the stirring speed of 300r/min in the injection process, and aging for 6h after the injection is finished to obtain an NCA oxalic acid precursor C;
e) carrying out suction filtration and washing on the NCA oxalic acid precursor solution C, drying in a vacuum drying oven at 120 ℃ for 12h, then primarily grinding by using an agate mortar, putting into an alumina porcelain boat, heating in a muffle furnace at the speed of 5 ℃/min, and calcining at 450 ℃ for 6h to obtain an NCA oxide precursor D;
g) with MLi/MNCA oxide precursor DWeighing LiOH & H according to the molar ratio of 1.052Grinding and mixing O and the NCA oxide precursor D uniformly, putting the mixture into an alumina porcelain boat, putting the alumina porcelain boat into a tube furnace, calcining the mixture for 6 hours at the temperature of 550 ℃ at the speed of 5 ℃/h in the oxygen atmosphere, and then increasing the temperature at the speed of 5 ℃/hCalcining at 750 ℃ for 12h to obtain the coated NCA material.
The NCA materials coated in examples 1 to 3 and comparative document 1 were subjected to an electrochemical performance test (test method is a pull-out) and an electrochemical specific capacity curve was obtained, and the results are shown in fig. 1, table 1 and fig. 1 to 4.
TABLE 1
As can be seen from table 1, the capacity retention rates of the final products examples 1 to 3 prepared by the present invention after 200 cycles at a rate of 1C are superior to those of the comparative samples in cycle performance. Through testing, the method obviously improves the performance of the NCA material and is very suitable for industrial scale-up production.
As can be seen from fig. 1 to 4, the cycle performance of the materials coated by the coating method of the present invention is respectively example 1 (85.1%), example 2 (89.5%), example 3 (88.7%) and comparative sample (41.7%), and the cycle performance is significantly improved. The coating strategy can be used for uniformly and controllably coating a single coating material and can also be applied to other coating materials.
The transmission electron microscope images of the NCA materials coated in the examples 1 and 2 are obtained, the structures of the NCA materials are shown in fig. 5-6, and it can be seen from fig. 5-6 that the coating thickness on the surface of the material is increased from 1-2nm to 4-5nm along with the increase of the coating dosage (1 mol% → 6 mol%), which shows that the method can realize the uniform and controllable coating thickness on the surface of the material.
In this document, the terms front, back, upper and lower are used to define the components in the drawings and the positions of the components relative to each other, and are used for clarity and convenience of the technical solution. It is to be understood that the use of the directional terms should not be taken to limit the scope of the claims.
The features of the embodiments and embodiments described herein above may be combined with each other without conflict.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. High-nickel ternary material LiNi0.80Co0.15Al0.05O2Characterized in that the coating material and the high nickel ternary material LiNi are subjected to precipitation conversion reaction0.80Co0.15Al0.05O2Forming a uniform and uniform coating, comprising the steps of:
s1, preparing an NCA material precursor: dissolving and dispersing nickel-cobalt-aluminum acetate in ultrapure water, and adding oxalic acid for precipitation reaction to obtain an NCA oxalic acid precursor solution;
s2, respectively weighing a coating raw material alpha and a coating raw material beta, and preparing a coating raw material alpha solution and a coating raw material beta solution, wherein the coating raw material alpha is diammonium hydrogen phosphate, and the coating raw material beta is zirconium oxychloride;
wherein the weight of the coating raw material is w% n M,
in the formula: n, amount of substance of NCA oxalic acid precursor;
m, the molar mass of the coating raw material;
w%, the coating raw material accounts for the mol percentage of the amount of the NCA oxalic acid precursor substance, and w% is 0.5-6 mol%;
s3, adding the coating raw material alpha solution into the NCA oxalic acid precursor solution to perform precipitation conversion reaction, and performing constant temperature, stirring and aging;
s4, adding a coating raw material beta solution into the aged NCA oxalic acid precursor solution obtained in the S3 for precipitation reaction, and carrying out constant temperature, stirring and aging to obtain an NCA oxalic acid precursor C;
and S5, carrying out suction filtration, drying and calcination on the NCA oxalic acid precursor C to obtain the coated high-nickel ternary material.
2. The high nickel ternary material LiNi according to claim 10.80Co0.15Al0.05O2The coating method is characterized in that the constant temperature conditions in S3 and S4 are 25-80 ℃, the stirring speed is 200-500r/min, and the aging time is 2-12 h.
3. The high nickel ternary material LiNi according to claim 10.80Co0.15Al0.05O2The coating method is characterized in that the suction filtration time in S5 is 10-60min, the drying mode is vacuum drying, the drying temperature range is 100-150 ℃, and the drying time is 6-24 h.
4. The high nickel ternary material LiNi according to claim 30.80Co0.15Al0.05O2The coating method of (5), wherein the calcination process in S5 includes two calcination processes of a first stage calcination and a second stage calcination:
the temperature condition of the first stage calcination is 400-500 ℃, the time condition is 5-12h, and an NCA oxide precursor D is obtained after calcination;
the second stage calcination conditions were: firstly, with MLi/MNCA oxide precursor DWeighing LiOH & H in a molar ratio of 1.0-1.22O, reaction of LiOH. H2After the O and the NCA oxide precursor D are uniformly mixed, calcining for 6 hours at 500-600 ℃ in an oxygen atmosphere, and then adjusting the calcining temperature to 700-900 ℃ for calcining for 10-24 hours.
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