CN111584832A - Lithium-manganese-rich cathode material coated with lithium metaaluminate and preparation method thereof - Google Patents
Lithium-manganese-rich cathode material coated with lithium metaaluminate and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a lithium-rich manganese anode material coated with lithium metaaluminate, which is Li2MnO3And LiMO2(M is nickel, cobalt, manganese, aluminum, iron, chromium metal element), the surface of the material particle is coated with a layer of lithium metaaluminate, and the preparation method of the lithium-rich manganese anode material coated with the lithium metaaluminate is to coat the lithium-rich manganese material with primary lithium metaaluminate on the surface of the material by adopting a carbon dioxide blowing secondary codeposition method to resist the corrosion of HFThe material has improved performance, and the normal charging voltage of the battery made of the material can reach 4.8V.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery materials, and particularly relates to a lithium-manganese-rich cathode material coated with lithium metaaluminate and a preparation method thereof.
Background
The capacities of the anode and the cathode of the conventional lithium ion battery are matched during design, the anode is almost twice of the cathode in terms of material usage, and the usage amount of silicon-based materials with higher gram capacities used for the cathode is less. The reason is mainly that the gram capacity of the anode material is low, the gram capacity of the high-nickel ternary material which can be applied in batch at present is only about 190mAh/g, and the gram capacity of the common graphite can reach 350mAh/g, so that the improvement of the gram capacity of the anode of the lithium ion battery material is not easy.
At present, most of research in the industry is lithium-rich manganese-based anode materials, the specific discharge capacity of the lithium-rich manganese-based anode materials reaches more than 300mAh/g, the gram capacity of 523 type ternary materials which are widely applied at present is only about 150mAh/g, and the gram capacity of the lithium-rich manganese-based anode materials is almost twice of that of the lithium-rich manganese-based anode materials. In addition, transition metals in the lithium-manganese-rich material are mainly manganese, the content of noble metals is low, lithium ion batteries manufactured by taking the transition metals as anode materials are more easily accepted by the market, and the safety performance of the lithium-manganese-rich material batteries is much better than that of the lithium-nickel ternary material batteries. Therefore, the lithium-rich manganese cathode material is an ideal choice for the next generation of lithium ion batteries, and is the key point for the lithium battery to break through 300Wh/Kg, even 400 Wh/Kg.
The lithium-rich manganese cathode material has high mass specific energy, good safety performance and low price, but needs to face a plurality of problems for mass application. When the lithium-rich manganese-based battery is charged for the first time to 4.5-4.8V, Li2MnO3Partially activated, Li+From Li2MnO3Middle extrusions with partial oxygen evolution, Li during discharge2Vacancies left in the bulk phase after O evolution are occupied by surface metal ions, leading to Li+Cannot be fully embedded back into the lattice. Therefore, Li in the lithium-manganese-rich cathode material2MnO3The activation process of the components is the root cause for providing high specific energy, and it is this process that causes some problems restricting the further industrial development.
Under high voltage, transition metal ions are easily dissolved in the electrolyte, and meanwhile, the surface of an electrode is easily corroded by HF generated by the electrolyte to generate an unstable Solid Electrolyte Interface (SEI) film, so that interface impedance is increased and the capacity is attenuated along with the increase; during the first charging period, oxygen loss causes transition metal ions to migrate from the surface to the bulk phase to occupy lithium and oxygen vacancies, the surface structure recombination of the material is initiated, the irreversible transformation from a layered structure to a spinel structure occurs in the crystal structure, and Li+The migration resistance increases, causing voltage decay and capacity decay.
Disclosure of Invention
In order to solve the two problems of capacity attenuation and voltage decline, the invention provides a lithium-manganese-rich cathode material coated with lithium metaaluminate and a preparation method thereof, and the technical scheme is as follows:
a lithium-manganese-rich cathode material coated with lithium metaaluminate, which is Li2MnO3And LiMO2(M is nickel, cobalt, manganese, aluminum, iron and chromium metal elements), and the surface of the material particles is coated with a layer of lithium metaaluminate.
A preparation method of a lithium-rich manganese anode material coated with lithium metaaluminate comprises the following steps:
firstly, taking soluble salts of divalent nickel, manganese and cobalt, adding the soluble salts into a strong alkali solution in proportion under protective gas, then adding a complexing agent, adjusting the pH value of the solution to 11-12, stirring at the temperature of 50-70 ℃ for 600 revolutions per minute, and reacting for 10-14 hours; then cleaning the codeposit with distilled water for 3 times, and drying for 10-12 hours at the temperature of 80-120 ℃ in vacuum, wherein the codeposit is a primary codeposit product; then adding aluminum nitrate into the strong alkaline solution according to the proportion until a stable metaaluminate solution is formed; then adding the primary codeposition product into a meta-aluminate solution in proportion, stirring at a certain temperature, introducing carbon dioxide, carrying out secondary sedimentation until the pH value is kept at 9-10, washing the codeposition product with distilled water for three times, and drying at 120 ℃ in vacuum for 24 hours to form a secondary sedimentation product; weighing the lithium compound according to the proportion, adding the lithium compound and the secondary codeposition product into a ball mill together, performing ball milling for 3 hours at 200 r/min, taking the materials, putting the materials into a push plate furnace, introducing oxygen for calcining for 4 to 8 hours at 450 ℃, introducing oxygen for calcining for 10 to 20 hours at 750 ℃, and cooling to obtain the product.
The soluble salts of divalent nickel, manganese and cobalt are divalent sulfate, hydrochloride and the like of nickel, divalent sulfate, hydrochloride and the like of manganese, divalent sulfate, sulfate and hydrochloride of cobalt.
The strong alkaline solution is sodium hydroxide, potassium hydroxide and lithium hydroxide solution, and the complexing agent is one or more of sodium carbonate, ammonium bicarbonate, ammonia water and the like.
The protective gas is nitrogen, helium or argon.
The secondary deposition temperature is 50-70 ℃, the stirring speed is about 500-800 r/min, and the blowing-in amount of carbon dioxide is carried out according to 45-55ml/min of 100 g of primary precipitate.
The lithium compound is one or more of lithium hydroxide, lithium carbonate and lithium oxalate.
The oxygen introduction calcination temperature is divided into two sections, one section is 400-500 ℃, and the other section is 700-900 ℃.
The invention has the advantages that the lithium-rich manganese material is coated with primary lithium metaaluminate on the surface by adopting a carbon dioxide blowing secondary codeposition method so as to resist the corrosion of HF and improve the performance of the material, and in addition, the normal charging voltage of the battery made of the material can reach 4.8V.
Detailed Description
The following describes a process for manufacturing a lithium-manganese-rich cathode material coated with lithium metaaluminate according to the present invention. This is a supplementary explanation of the present disclosure and not a limitation.
A lithium-manganese-rich cathode material coated with lithium metaaluminate, which is Li2MnO3And LiMO2(M is nickel, cobalt, manganese, aluminum, iron and chromium metal elements), and the surface of the material particles is coated with a layer of lithium metaaluminate.
A preparation method of a lithium-rich manganese anode material coated with lithium metaaluminate comprises the following steps:
firstly, taking soluble salts of divalent nickel, manganese and cobalt, adding the soluble salts into a strong alkali solution in proportion under protective gas, then adding a complexing agent, adjusting the pH value of the solution to 11-12, stirring at the temperature of 50-70 ℃ for 600 revolutions per minute, and reacting for 10-14 hours; then cleaning the codeposit with distilled water for 3 times, and drying for 10-12 hours at the temperature of 80-120 ℃ in vacuum, wherein the codeposit is a primary codeposit product; then adding aluminum nitrate into the strong alkaline solution according to the proportion until a stable metaaluminate solution is formed; then adding the primary codeposition product into a meta-aluminate solution in proportion, stirring at a certain temperature, introducing carbon dioxide, carrying out secondary sedimentation until the pH value is kept at 9-10, washing the codeposition product with distilled water for three times, and drying at 120 ℃ in vacuum for 24 hours to form a secondary sedimentation product; weighing the lithium compound according to the proportion, adding the lithium compound and the secondary codeposition product into a ball mill together, performing ball milling for 3 hours at 200 r/min, taking the materials, putting the materials into a push plate furnace, introducing oxygen for calcining for 4 to 8 hours at 450 ℃, introducing oxygen for calcining for 10 to 20 hours at 750 ℃, and cooling to obtain the product.
The soluble salts of divalent nickel, manganese and cobalt are divalent sulfate, hydrochloride and the like of nickel, divalent sulfate, hydrochloride and the like of manganese, divalent sulfate, sulfate and hydrochloride of cobalt.
The strong alkaline solution is sodium hydroxide, potassium hydroxide and lithium hydroxide solution, and the complexing agent is one or more of sodium carbonate, ammonium bicarbonate, ammonia water and the like.
The protective gas is nitrogen, helium or argon.
The secondary deposition temperature is 50-70 ℃, the stirring speed is about 500-800 r/min, and the blowing-in amount of carbon dioxide is carried out according to 45-55ml/min of 100 g of primary precipitate.
The lithium compound is one or more of lithium hydroxide, lithium carbonate and lithium oxalate.
The oxygen introduction calcination temperature is divided into two sections, one section is 400-500 ℃, and the other section is 700-900 ℃.
Example 1:
preparation of target 10 kg Li1.2Ni0.16Mn0.51Al0.05Co0.08O2. Firstly, 6.127 kg of NiSO4•6H2O, 12.561 kg MnSO4•H2O, 3.276 kg CoSO4•7H2O, adding 79.5L of 2.5mol/L NaOH strong base solution under the nitrogen atmosphere, and then dropwise adding a small amount of NH serving as a complexing agent3H2O (in a reaction kettle), adjusting the pH value of the solution to 11-12, stirring at 900 rpm at 65 ℃, and reacting for 10 hours. The co-precipitate was then washed 3 times with distilled water and dried under vacuum at 90 ℃ for 10 hours, which was the primary co-precipitate product. Then, 2.717 kg of Al (NO) with high purity was added3)3•9H2The O ratio is added to 16L of 3.0mol/L NaOH strong alkali solution until a stable lithium metaaluminate solution is formed. Then adding the primary codeposition product into the lithium metaaluminate solution according to the proportion, stirring at 700 r/min, keeping the temperature at 60 ℃, introducing 4.9L/min of carbon dioxide into the solution, injecting CO into the solution2. Until the pH value is kept between 9 and 10,the co-precipitated product was washed three times with distilled water and dried under vacuum at 120 ℃ for 12 hours. Weighing 3.920 kg of lithium hydroxide according to the proportion, adding the lithium hydroxide and the secondary codeposition product into a ball mill together, ball-milling for 3 hours at 200 r/min, taking the materials, putting the materials into a push plate furnace for 450 ℃, introducing oxygen for calcining for 7 hours, then introducing oxygen for calcining for 12 hours at 750 ℃, and cooling to obtain about 10 kg of Li1.2Ni0.16Mn0.51Al0.05Co0.08O2And (3) obtaining the product.
Example 2:
preparation of target 10 kg Li1.2Ni0.16Mn0.51Al0.05Co0.08O2. Firstly 6.779 kg of Ni (NO)3)2•6H2O, 18.654 kg Mn (NO)3)2•4H2O, 3.392 kg Co (NO)3)2•6H2O, adding 66.25L of 3.0mol/LKOH strong base solution under the nitrogen atmosphere, and then dripping a small amount of NH serving as a complexing agent3H2O (in a reaction kettle), adjusting the pH value of the solution to 11-12, stirring at 900 rpm at 65 ℃, and reacting for 10 hours. The co-precipitate was then washed 3 times with distilled water and dried under vacuum at 90 ℃ for 10 hours, which was the primary co-precipitate product. Then, 2.717 kg of Al (NO) with high purity was added3)3•9H2The O ratio was added to 16L of 3.0mol/L NaOH in strong alkaline solution until a stable lithium metaaluminate solution was formed. Then adding the primary codeposition product into the lithium metaaluminate solution according to the proportion, stirring at 700 r/min, keeping the temperature at 60 ℃, introducing 4.9L/min of carbon dioxide into the solution, injecting CO into the solution2. Until the pH remained at 9-10, the codeposited product was washed three times with distilled water and dried under vacuum at 120 ℃ for 12 hours. 8.344 kg of lithium oxalate is weighed according to the proportion, the lithium oxalate and the secondary codeposition product are added into a ball mill together, ball milling is carried out for 3 hours at 200 r/min, the materials are taken and then put into a push plate furnace for 450 ℃, oxygen is introduced for calcination for 7 hours, then the materials are introduced for calcination for 12 hours at 750 ℃, and the materials are cooled to obtain the Li of about 10 kg1.2Ni0.16Mn0.51Al0.05Co0.08O2And (3) obtaining the product.
Example 3:
prepare target 10 thousandGram of Li1.2Ni0.16Mn0.51Al0.05Co0.08O2. First, 5.540 kg of NiCl was taken2•6H2O, 14.705 kg of MnCl2•4H2O, 2.773 kg CoCl2•6H2O, adding 56.78L of 3.5mol/L NaOH strong base solution under the nitrogen atmosphere, and then dripping a small amount of NH serving as a complexing agent3H2O (in a reaction kettle), adjusting the pH value of the solution to 11-12, stirring at 900 rpm at 65 ℃, and reacting for 10 hours. The co-precipitate was then washed 3 times with distilled water and dried under vacuum at 90 ℃ for 10 hours, which was the primary co-precipitate product. Then, 2.717 kg of Al (NO) with high purity was added3)3•9H2The O ratio was added to 16L of 3.0mol/L NaOH in strong alkaline solution until a stable lithium metaaluminate solution was formed. Then adding the primary codeposition product into the lithium metaaluminate solution according to the proportion, stirring at 700 r/min, keeping the temperature at 60 ℃, introducing 4.9L/min of carbon dioxide into the solution, injecting CO into the solution2. Until the pH remained at 9-10, the codeposited product was washed three times with distilled water and dried under vacuum at 120 ℃ for 12 hours. Weighing 6.059 kg of lithium carbonate according to the proportion, adding the lithium carbonate and the secondary codeposition product into a ball mill together, ball milling for 3 hours at 200 r/min, taking the materials, putting the materials into a push plate furnace for 450 ℃, introducing oxygen for calcining for 7 hours, then introducing the oxygen for calcining for 12 hours at 750 ℃, and cooling to obtain about 10 kg of Li1.2Ni0.16Mn0.51Al0.05Co0.08O2And (3) obtaining the product.
Claims (8)
1. The lithium-manganese-rich cathode material coated with lithium metaaluminate is characterized in that the cathode material is Li2MnO3And LiMO2(M is nickel, cobalt, manganese, aluminum, iron and chromium metal elements), and the surface of the material particles is coated with a layer of lithium metaaluminate.
2. The method for preparing the lithium-manganese-rich cathode material coated with lithium metaaluminate according to claim 1, wherein the method comprises the following steps:
firstly, taking soluble salts of divalent nickel, manganese and cobalt, adding the soluble salts into a strong alkali solution in proportion under protective gas, then adding a complexing agent, adjusting the pH value of the solution to 11-12, stirring at the temperature of 50-70 ℃ for 600 revolutions per minute, and reacting for 10-14 hours; then cleaning the codeposit with distilled water for 3 times, and drying for 10-12 hours at the temperature of 80-120 ℃ in vacuum, wherein the codeposit is a primary codeposit product; then adding aluminum nitrate into the strong alkaline solution according to the proportion until a stable metaaluminate solution is formed; then adding the primary codeposition product into a meta-aluminate solution in proportion, stirring at a certain temperature, introducing carbon dioxide, carrying out secondary sedimentation until the pH value is kept at 9-10, washing the codeposition product with distilled water for three times, and drying at 120 ℃ in vacuum for 24 hours to form a secondary sedimentation product; weighing the lithium compound according to the proportion, adding the lithium compound and the secondary codeposition product into a ball mill together, performing ball milling for 3 hours at 200 r/min, taking the materials, putting the materials into a push plate furnace, introducing oxygen for calcining for 4 to 8 hours at 450 ℃, introducing oxygen for calcining for 10 to 20 hours at 750 ℃, and cooling to obtain the product.
3. The method as claimed in claim 1, wherein the soluble salts of divalent nickel, manganese and cobalt are divalent sulfates, hydrochlorides of nickel, divalent sulfates, sulfates and hydrochlorides of manganese, divalent sulfates, sulfates and hydrochlorides of cobalt.
4. The method for preparing the lithium-manganese-rich cathode material coated with lithium metaaluminate according to claim 1, wherein the strong alkaline solution is sodium hydroxide, potassium hydroxide or lithium hydroxide solution, and the complexing agent is one or more of sodium carbonate, ammonium bicarbonate, ammonia water and the like.
5. The method as claimed in claim 1, wherein the protective gas is selected from the group consisting of nitrogen, helium, and argon.
6. The method as claimed in claim 1, wherein the secondary deposition temperature is 50-70 ℃, the stirring speed is 500-800 rpm, and the blowing amount of carbon dioxide is 45-55ml/min for 100 g of primary precipitate.
7. The method for preparing a lithium-rich manganese cathode material coated with lithium metaaluminate according to claim 1, wherein the lithium compound is one or more of lithium hydroxide, lithium carbonate and lithium oxalate.
8. The method as claimed in claim 1, wherein the temperature of the oxygen-introduced calcination is divided into two sections, one section is 400-500 ℃ and the other section is 700-900 ℃.
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| CN113991097A (en) * | 2021-09-29 | 2022-01-28 | 太原理工大学 | Preparation method and application of magnesium aluminate coated lithium-rich manganese-based positive electrode material |
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| CN113991097A (en) * | 2021-09-29 | 2022-01-28 | 太原理工大学 | Preparation method and application of magnesium aluminate coated lithium-rich manganese-based positive electrode material |
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