CN112875766B - Method for preparing ternary cathode material by microwave heating solution method with carbon source added - Google Patents
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- C01G53/42—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2
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- C01G53/50—Complex oxides containing nickel and at least one other metal element containing alkali metals, e.g. LiNiO2 containing manganese of the type (MnO2)n-, e.g. Li(NixMn1-x)O2 or Li(MyNixMn1-x-y)O2
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Abstract
The invention provides a method for preparing a ternary cathode material by a microwave heating solution method with added carbon source, wherein the ternary cathode material is of a single crystal structure and has a chemical formula of LiNi 1‑x‑y Co x Mn y O 2 ，1‑x‑y≥0.5，0<x<1，0<y<1, the method comprising the steps of: (1) Dissolving a lithium source, a nickel source, a cobalt source and a manganese source in deionized water to prepare a mixed salt solution; (2) Adding a carbon source into the mixed salt solution and uniformly stirring to obtain a mixed solution; (3) Placing the mixed solution in a microwave heater, and heating the mixed solution to decompose the mixed solution to obtain a powdery black fluffy ternary nano-oxide precursor; (4) And carrying out heat treatment on the ternary nano oxide precursor to obtain the ternary cathode material. The method for preparing the ternary cathode material by the solution method provided by the invention has the advantages of short required time and low energy consumption, and the prepared ternary cathode material has the advantages of good dispersibility, high compaction density and good cycle performance.
Description
Technical Field
The invention relates to the technical field of battery material preparation, in particular to a method for preparing a ternary cathode material by a microwave solution heating method with carbon source addition.
Background
Lithium ion batteries have the advantages of high voltage, high energy density, good cycle performance and the like, and have been widely applied to the fields of digital electronic products, electric bicycles, electric automobiles and the like. The performance and cost of lithium ion batteries depend to a large extent on the positive electrode material. Currently, lithium ion battery positive electrode materials in mass production include lithium cobaltate, lithium manganate, lithium iron phosphate, lithium nickel cobalt manganese, and the like, wherein lithium Nickel Cobalt Manganese (NCM) and derivatives lithium Nickel Cobalt Aluminate (NCA) thereof, and lithium Nickel Cobalt Manganese Aluminate (NCMA) are collectively called ternary positive electrode materials.
At present, the method for synthesizing the ternary cathode material on a large scale mainly adopts the high-temperature solid-phase reaction of a nickel-cobalt-manganese hydroxide precursor mixed with lithium salt, and a coprecipitation method is the most commonly used method for synthesizing the precursor.
The precursor synthesized by the solution method can realize the atomic-scale mixing, and theoretically, the synthesized material has accurate stoichiometric ratio and uniform distribution of metal elements. In general, in the solution synthesis method, soluble metal salts such as lithium, nickel, cobalt, manganese and the like are dissolved in a solvent, a complexing agent is added at the same time, the solution is evaporated to obtain sol gel, then the gel is heated to promote self-propagating combustion, and a ternary positive electrode precursor is obtained, for example, patents with publication numbers of CN108574100A, CN 107403903B, CN104009221B and CN 104934593B all disclose that a ternary positive electrode precursor is prepared by adopting a solution synthesis method, glucose, citric acid, ethylene glycol, ethylene diamine tetraacetic acid or urea and the like are used as fuels, self-propagating violent combustion is caused by adopting a traditional kiln or microwave heating, the temperature in the combustion process is difficult to control, and the optimal performance of a target material is difficult to obtain. In addition, the soluble salt of transition metal has a weak microwave absorbing ability, and particularly if a carbon-containing hydrogen-combustible compound is not added in the solution method, it is difficult to reach the decomposition temperature of the soluble salt of transition metal by microwave heating.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a method for preparing a ternary cathode material by a microwave heating solution method with carbon sources added, wherein the ternary cathode material has a single crystal structure and has a chemical formula of LiNi 1-x-y Co x Mn y O 2 ，1-x-y≥0.5，0<x<1，0<y<1, the method comprising the steps of:
(1) Dissolving a lithium source, a nickel source, a cobalt source and a manganese source in deionized water according to the molar ratio of the chemical formula to prepare a mixed salt solution;
(2) Adding a carbon source into the mixed salt solution and uniformly stirring to obtain a mixed solution, wherein the carbon source is used as a microwave absorption medium;
(3) Placing the mixed solution in a microwave heater for microwave heating treatment to obtain a powdery black fluffy ternary nano oxide precursor;
(4) And carrying out heat treatment on the ternary nano oxide precursor to obtain the ternary cathode material.
Further, in the step (1), the lithium source is lithium nitrate or lithium chloride, the nickel source is nickel nitrate or nickel chloride, the cobalt source is cobalt nitrate or cobalt chloride, and the manganese source is manganese nitrate or manganese chloride.
Further, in the step (1), the molar weight of the lithium source is 1 to 1.2 times of the sum of the molar weights of the nickel source, the cobalt source and the manganese source, and the concentration of the metal ions in the mixed salt solution is 0.5 to 5mol/L.
Further, in the step (2), the carbon source is one of activated carbon, acetylene black, graphene and carbon nanotubes.
Further, in the step (3), the frequency of the microwave heater is 2.45GHz, the heating power is 200 to 750W, and the microwave heating treatment mode is as follows: raising the temperature to 300-500 ℃ by using microwave, and keeping the temperature for 10-20 minutes.
Further, in the step (4), the heat treatment mode is as follows: firstly, ball-milling and crushing the ternary nano oxide precursor, and then sintering in air or oxygen atmosphere at 800-980 ℃ for 6-15 hours.
The method for preparing the ternary cathode material by the solution method does not contain hydrocarbon combustible compounds, combustion reaction does not occur in the heating decomposition process, the required time is short, the energy consumption is low, and the prepared ternary cathode material has the advantages of good dispersibility, high compaction density and good cycle performance. The carbon source with specific proportion is added as a microwave absorbing medium, and the heating condition of a microwave heater is controlled, so that the mixed solution can be quickly heated to evaporate water, the solid precipitate can quickly reach the decomposition temperature to obtain the target material, the preparation time is effectively shortened, the energy consumption is low, and the whole heating decomposition process does not generate combustion reaction.
Drawings
FIG. 1 is an SEM image of a ternary cathode material prepared in example 3 of the present invention;
fig. 2 is an SEM image of the ternary cathode material prepared in comparative example 1 of the present invention.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
A method for preparing a ternary cathode material by a microwave heating solution method with carbon source addition comprises the following steps:
(1) Dissolving lithium nitrate, nickel nitrate, cobalt nitrate and manganese nitrate in deionized water according to a molar ratio of 1.08;
(2) Adding activated carbon into the mixed salt solution and uniformly stirring to obtain a mixed solution, wherein the activated carbon is used as a microwave absorption medium, and the weight ratio of the activated carbon to the mixed solution is 1;
(3) Putting the mixed solution into a ceramic sagger, putting the ceramic sagger into a microwave heater, and heating the mixed solution by using microwaves to decompose the mixed solution to obtain a powdery black fluffy ternary nano oxide precursor, wherein the frequency of the microwave heater is 2.45GHz, the heating power is 250W, and the microwave heating treatment mode is as follows: raising the temperature to 400 ℃ by using microwaves, and keeping the temperature for 15 minutes;
(4) Ball-milling and crushing the ternary nano oxide precursor, then placing the crushed ternary nano oxide precursor in an air atmosphere, heating to 960 ℃ and sintering for 9 hours to obtain the LiNi with the single crystal morphology 0.5 Co 0.2 Mn 0.3 O 2 The SEM image of the ternary cathode material shows that the single crystal dispersion performance is good.
Example 2
A method for preparing a ternary cathode material by a microwave heating solution method with carbon source addition comprises the following steps:
(1) Dissolving lithium chloride, nickel chloride, cobalt chloride and manganese chloride in deionized water according to a molar ratio of 1.08;
(2) Adding graphene/acetylene black into the mixed salt solution and uniformly stirring to obtain a mixed solution, wherein activated carbon is used as a microwave absorption medium, and the weight ratio of the graphene/acetylene black to the mixed solution is 1;
(3) Putting the mixed solution into a ceramic sagger, putting the ceramic sagger into a microwave heater, and heating the mixed solution by using microwaves to decompose the mixed solution to obtain a powdery black fluffy ternary nano oxide precursor, wherein the frequency of the microwave heater is 2.45GHz, the heating power is 400W, and the microwave heating treatment mode is as follows: raising the temperature to 500 ℃ by utilizing microwave, and keeping the temperature for 20 minutes;
(4) Ball-milling and crushing the ternary nano oxide precursor, and then placing the crushed ternary nano oxide precursor in an air atmosphere to heat to 870 ℃ for sintering for 15 hours to obtain the LiNi with the single crystal morphology 0.5 Co 0.2 Mn 0.3 O 2 The SEM image shows that the single crystal dispersion performance of the ternary cathode material is good.
Example 3
A method for preparing a ternary cathode material by a microwave heating solution method with carbon source addition comprises the following steps:
(1) Dissolving lithium nitrate, nickel nitrate, cobalt nitrate and manganese nitrate in deionized water according to a molar ratio of 1.06;
(2) Adding carbon nanotubes into the mixed salt solution, and uniformly stirring to obtain a mixed solution, wherein activated carbon is used as a microwave absorption medium, and the weight ratio of the activated carbon to the mixed solution is 1;
(3) The mixed solution is filled in a ceramic sagger, the ceramic sagger is arranged in a microwave heater, the mixed solution is heated by microwaves to be decomposed, and a powdery black fluffy ternary nano oxide precursor is obtained, wherein the frequency of the microwave heater is 2.45GHz, the heating power is 300W, and the microwave heating treatment mode is as follows: raising the temperature to 500 ℃ by using microwave, and keeping the temperature for 20 minutes;
(4) Ball-milling and crushing the ternary nano oxide precursor, then placing the crushed ternary nano oxide precursor in an oxygen atmosphere, heating to 900 ℃ and sintering for 12 hours to obtain the LiNi with the single crystal morphology 0.7 Co 0.1 Mn 0.2 O 2 The SEM image shows that the single crystal dispersion performance of the ternary cathode material is good.
Comparative example 1
A method for preparing a ternary cathode material by a solution method comprises the following steps:
(1) Dissolving lithium nitrate, nickel nitrate, cobalt nitrate and manganese nitrate in deionized water according to a molar ratio of 1.06;
(2) And (2) putting the mixed salt solution into a ceramic sagger, putting the ceramic sagger into a microwave heater, and heating the mixed solution by using microwaves, wherein the temperature of the mixed solution is reduced from 280 ℃ at most to 200 ℃ to obtain black and green blocky solids, the frequency of the microwave heater is 2.45GHz, the heating power is 300W, and the heating time is 20 minutes.
(3) Ball-milling and crushing the black-green blocky solid, and then placing the crushed solid in an oxygen atmosphere to be heated to 900 ℃ for sintering for 12 hours to obtain the LiNi with the single crystal morphology 0.7 Co 0.1 Mn 0.2 O 2 The SEM image shows that the single crystal particles are irregular in shape and have large size difference.
Comparative example 1 compared to example 3, no auxiliary carbon source was added in comparative example 1; comparative example 1, after the water content of the mixed salt solution is evaporated, the temperature of the solid precipitate is difficult to continue rising after rising to 280 ℃, which shows that the precipitated nitrate has weak microwave absorption capacity and is difficult to reach the decomposition temperature, so that the prepared ternary cathode material has uneven particles and poor dispersion performance; example 3, the carbon source with a specific ratio is added as a microwave absorbing medium, the mixed solution can be rapidly heated to evaporate water, the solid precipitate can rapidly reach the decomposition temperature, the solid precipitate is decomposed, and the prepared ternary cathode material has good dispersibility, and the SEM picture shows that the single crystal dispersibility is good.
While embodiments of the present invention have been shown and described, it will be understood by those of ordinary skill in the art that: various changes, modifications, substitutions and alterations can be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the claims and their equivalents.
Claims (4)
1. A method for preparing a ternary cathode material by a carbon source-added microwave heating solution method is characterized in that the ternary cathode material is of a single crystal structure and has a chemical formula of LiNi 1-x-y Co x Mn y O 2 ，1-x-y≥0.5，0<x<1，0<y<1, the method comprising the steps of:
(1) Dissolving a lithium source, a nickel source, a cobalt source and a manganese source in deionized water according to the molar ratio of the chemical formula to prepare a mixed salt solution;
(2) Adding a carbon source into the mixed salt solution and uniformly stirring to obtain a mixed solution, wherein the carbon source is used as a microwave absorption medium;
(3) Placing the mixed solution in a microwave heater for microwave heating treatment to obtain a powdery black fluffy ternary nano oxide precursor;
(4) Carrying out heat treatment on the ternary nano oxide precursor to obtain the ternary cathode material;
in the step (2), the carbon source is one of activated carbon, acetylene black, graphene and carbon nano tubes;
in the step (3), the frequency of the microwave heater is 2.45GHz, the heating power is 200-750W, and the microwave heating treatment mode is as follows: raising the temperature to 300-500 ℃ by using microwave, and keeping the temperature for 10-20 minutes.
2. The method for preparing the ternary cathode material according to claim 1, wherein in the step (1), the lithium source is lithium nitrate or lithium chloride, the nickel source is nickel nitrate or nickel chloride, the cobalt source is cobalt nitrate or cobalt chloride, and the manganese source is manganese nitrate or manganese chloride.
3. The method for preparing a ternary cathode material according to claim 1, wherein in the step (1), the molar amount of the lithium source is 1 to 1.2 times of the sum of the molar amounts of the nickel source, the cobalt source and the manganese source, and the concentration of the metal ions in the mixed salt solution is 0.5 to 5mol/L.
4. The method for preparing the ternary cathode material by the carbon source-added microwave solution heating method according to claim 1, wherein in the step (4), the heat treatment manner is as follows: firstly, ball-milling and crushing the ternary nano oxide precursor, and then sintering in air or oxygen atmosphere, wherein the sintering temperature is 800-980 ℃, and the sintering time is 6-15 hours.
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