CN114420904A - Production method of modified lithium manganate material - Google Patents
Production method of modified lithium manganate material Download PDFInfo
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- CN114420904A CN114420904A CN202111633660.XA CN202111633660A CN114420904A CN 114420904 A CN114420904 A CN 114420904A CN 202111633660 A CN202111633660 A CN 202111633660A CN 114420904 A CN114420904 A CN 114420904A
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- Prior art keywords
- lithium manganate
- modified lithium
- producing
- baking
- coating
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- 239000000463 material Substances 0.000 title claims abstract description 42
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical class [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 title claims abstract description 29
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000000576 coating method Methods 0.000 claims abstract description 19
- 239000011248 coating agent Substances 0.000 claims abstract description 17
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 12
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 10
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 10
- 238000001704 evaporation Methods 0.000 claims abstract description 10
- 230000008020 evaporation Effects 0.000 claims abstract description 9
- 238000001354 calcination Methods 0.000 claims abstract description 8
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000010438 heat treatment Methods 0.000 claims description 19
- 230000000694 effects Effects 0.000 claims description 7
- 229910052596 spinel Inorganic materials 0.000 claims description 6
- 239000011029 spinel Substances 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 239000003125 aqueous solvent Substances 0.000 claims description 4
- 238000005485 electric heating Methods 0.000 claims description 3
- 238000000034 method Methods 0.000 claims description 2
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 239000011572 manganese Substances 0.000 abstract description 8
- 239000003792 electrolyte Substances 0.000 abstract description 6
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 abstract description 6
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 5
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 5
- 239000007772 electrode material Substances 0.000 abstract description 4
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract description 3
- 239000002131 composite material Substances 0.000 abstract description 3
- 238000009831 deintercalation Methods 0.000 abstract description 3
- 238000004090 dissolution Methods 0.000 abstract description 3
- 229910052748 manganese Inorganic materials 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 2
- 229910002097 Lithium manganese(III,IV) oxide Inorganic materials 0.000 description 1
- 230000004075 alteration Effects 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
Classifications
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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
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/362—Composites
- H01M4/366—Composites as layered products
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/12—Manganates manganites or permanganates
- C01G45/1207—Permanganates ([MnO]4-) or manganates ([MnO4]2-)
- C01G45/1214—Permanganates ([MnO]4-) or manganates ([MnO4]2-) containing alkali metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- 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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- 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
- H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
- H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
Abstract
The invention relates to a production method of a modified lithium manganate material, which comprises the following steps of 1, mixing LiOH, Mn (NO3)2 and citric acid together, stirring, using concentrated ammonia water in a matching manner, adjusting the pH value of liquid to 5-7, and performing evaporation operation; 2. baking and preheating the material obtained in the step (1); 3. grinding the material obtained in the step (2) and carrying out calcination operation, so as to obtain lithium manganate; 4. and (3) coating a layer of film on the surface of the lithium manganate obtained in the step (3) to finish the operation, wherein the invention has the following beneficial effects: the surface appearance of the material is improved by coating the surface of the lithium manganate with a SnO2: Sb composite oxide film, and meanwhile, during coating, the direct contact between the electrolyte and an active substance is prevented, so that the dissolution of manganese in the electrolyte is reduced, the circulation stability of the electrode material is improved, and the conductivity of the material is improved, thereby being more beneficial to the deintercalation of lithium ions.
Description
Technical Field
The invention discloses a production method of a modified lithium manganate material, and belongs to the technical field of lithium manganate preparation.
Background
The lithium ion battery has the characteristics of small volume, light weight, long service life and the like, and can be widely used in various electronic devices in recent years, such as electric vehicles, mobile phones and mobile motors, and the shadow of the lithium ion battery can be seen.
However, the existing lithium manganate does not have stable cycling stability of electrode materials when in use, thereby affecting the effect of the lithium manganate when in use.
Disclosure of Invention
The invention aims to provide a production method of a modified lithium manganate material.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention relates to a production method of a modified lithium manganate material, which comprises the following steps:
1. mixing LiOH, Mn (NO3)2 and citric acid together, stirring, using concentrated ammonia water in a matching manner, adjusting the pH value of the liquid to 5-7, and performing evaporation operation;
2. baking and preheating the material obtained in the step (1);
3. grinding the material obtained in the step (2) and carrying out calcination operation, so as to obtain lithium manganate;
4. and (4) coating a layer of film on the surface of the lithium manganate obtained in the step (3) to finish the operation.
In a preferred embodiment of the present invention, LiOH, Mn (NO3)2 and citric acid are prepared, and the mixture is added to water in a molar ratio of 2:6:12 and stirred for 1 hour by a stirrer.
As a preferred technical scheme, concentrated ammonia water is added into the stirred solution, the pH of the solution is adjusted to 5-7 by using the concentrated ammonia water, then the solution is stirred for 10-15 min by a stirrer, and meanwhile, the temperature is increased to 70-90 ℃ so as to achieve the purpose of evaporation and water removal.
As a preferred technical scheme of the invention, the obtained material is placed into a baking oven, the baking temperature is 100-120 ℃, the baking time is 40-60 min, and after the baking is finished, the material is placed into an electric heating furnace, the temperature is 350-400 ℃, and the heating time is 4-6 h, so that the preheating effect is achieved.
As a preferred technical scheme of the invention, after preheating is finished, grinding treatment is carried out, and finally the ground material is placed into a calcining furnace at the temperature of 800 ℃ for 9-12 h.
In a preferred embodiment of the present invention, a sol of Sn and Sb is synthesized by using a sol of nonaqueous solvent, and then the synthesized spinel is weighed in a coating mass ratio of 0.6%, 1.2%, 2.2%, 4.2%, 8.4%, 10%, and the weighed spinel is dispersed in a sol of Sn and Sb nonaqueous solvent in a coating amount to a constant volume of 50 ml.
As a preferred technical scheme of the invention, the material is put into stirring equipment to be stirred and heated, the stirring time is 30min, and the heating temperature is 80-100 ℃, so as to realize the evaporation effect.
As a preferred technical scheme of the invention, after the final heating is finished, the coating sample is put into a crucible for heat treatment, the heating temperature is 600-700 ℃, and the heat treatment time is 1h, thus obtaining the coating sample.
The invention has the following beneficial effects: the surface appearance of the material is improved by coating the surface of the lithium manganate with a SnO2: Sb composite oxide film, and meanwhile, during coating, the direct contact between the electrolyte and an active substance is prevented, so that the dissolution of manganese in the electrolyte is reduced, the circulation stability of the electrode material is improved, and the conductivity of the material is improved, thereby being more beneficial to the deintercalation of lithium ions.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The invention relates to a production method of a modified lithium manganate material, which comprises the following steps:
1. mixing LiOH, Mn (NO3)2 and citric acid together, stirring, using concentrated ammonia water in a matching manner, adjusting the pH value of the liquid to 5-7, and performing evaporation operation;
2. baking and preheating the material obtained in the step (1);
3. grinding the material obtained in the step (2) and carrying out calcination operation, so as to obtain lithium manganate;
4. and (4) coating a layer of film on the surface of the lithium manganate obtained in the step (3) to finish the operation.
LiOH, Mn (NO3)2 and citric acid were prepared, and the mixture was put into water at a molar ratio of 2:6:12, and stirred with a stirrer for 1 hour.
Adding concentrated ammonia water into the stirred solution, adjusting the pH value of the solution to 5-7 by using the concentrated ammonia water, stirring for 10-15 min by using a stirrer, and simultaneously increasing the temperature to 70-90 ℃ to fulfill the aim of evaporating and removing water.
And then, putting the obtained material into a baking oven, wherein the baking temperature is 100-120 ℃, the baking time is 40-60 min, and after baking is finished, putting the material into an electric heating furnace, wherein the temperature is 350-400 ℃, and the heating time is 4-6 h, so that the preheating effect is achieved.
After preheating is completed, grinding is carried out, and finally the ground material is placed into a calcining furnace, wherein the temperature is 800 ℃, and the calcining time is 9-12 hours.
The method comprises the steps of synthesizing Sn and Sb sol by using a non-aqueous solvent sol, then respectively weighing the synthesized spinel according to coating mass ratios of 0.6%, 1.2%, 2.2%, 4.2%, 8.4% and 10%, and dispersing the weighed spinel in the Sn and Sb non-aqueous solvent sol metered according to the coating, wherein the constant volume is 50 ml.
Wherein, the mixture is put into stirring equipment for stirring and heating operation, the stirring time is 30min, and the heating temperature is 80-100 ℃, so as to realize the evaporation effect.
And after the final heating is finished, putting the sample into a crucible for heat treatment, wherein the heating temperature is 600-700 ℃, and the heat treatment time is 1h, so that the coated sample can be obtained.
The working principle is as follows: the prepared LiMn2O4 is coated with a SnO2 Sb composite oxide film by a sol-gel method, the coating method has no influence on the structure of the material, the surface appearance of the material is improved by the coating method, and during coating, the direct contact between electrolyte and active substances is prevented, so that the dissolution of manganese in the electrolyte is reduced, the circulation stability of an electrode material is improved, and the conductivity of the material is improved, thereby being more beneficial to the deintercalation of lithium ions.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.
Claims (8)
1. The production method of the modified lithium manganate material is characterized by comprising the following steps:
(1) mixing LiOH, Mn (NO3)2 and citric acid together, stirring, using concentrated ammonia water in a matching manner, adjusting the pH value of the liquid to 5-7, and performing evaporation operation;
(2) baking and preheating the material obtained in the step (1);
(3) grinding the material obtained in the step (2) and carrying out calcination operation, so as to obtain lithium manganate;
(4) and (4) coating a layer of film on the surface of the lithium manganate obtained in the step (3) to finish the operation.
2. The method for producing a modified lithium manganate material as set forth in claim 1, wherein LiOH, Mn (NO3)2 and citric acid are prepared, put into water in a molar ratio of 2:6:12, and stirred for 1 hour by a stirrer.
3. The method for producing the modified lithium manganate material of claim 2, wherein the concentrated ammonia water is added to the stirred solution, the pH of the solution is adjusted to 5-7 by using the concentrated ammonia water, and then the solution is stirred for 10-15 min by a stirrer, and the temperature is increased to 70-90 ℃ at the same time, so as to achieve the purpose of evaporation and water removal.
4. The method for producing the modified lithium manganate material of claim 3, wherein the obtained material is placed into a baking oven, the baking temperature is 100-120 ℃, the baking time is 40-60 min, and after the baking is completed, the material is placed into an electric heating furnace, the temperature is 350-400 ℃, and the heating time is 4-6 h, so as to achieve the preheating effect.
5. The method for producing the modified lithium manganate material of claim 4, wherein after preheating, grinding is carried out, and finally the ground material is placed into a calcining furnace at 800 ℃ for 9-12 h.
6. The method for producing a modified lithium manganate material as set forth in claim 5, characterized in that, the method comprises the steps of synthesizing Sn and Sb sol by using non-aqueous solvent sol, then weighing the synthesized spinel according to the coating mass ratio of 0.6%, 1.2%, 2.2%, 4.2%, 8.4% and 10%, and dispersing the weighed spinel in Sn and Sb non-aqueous solvent sol according to the coating amount to a constant volume of 50 ml.
7. The method for producing the modified lithium manganate material of claim 6, characterized in that, the modified lithium manganate material is placed into a stirring device to be stirred and heated, the stirring time is 30min, and the heating temperature is 80-100 ℃, so as to realize the evaporation effect.
8. The method for producing the modified lithium manganate material of claim 7, wherein after the final heating, the material is placed in a crucible for heat treatment, the heating temperature is 600 ℃ to 700 ℃, and the heat treatment time is 1h, so as to obtain a coated sample.
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| CN202111633660.XA CN114420904A (en) | 2021-12-29 | 2021-12-29 | Production method of modified lithium manganate material |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202111633660.XA CN114420904A (en) | 2021-12-29 | 2021-12-29 | Production method of modified lithium manganate material |
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| CN202111633660.XA Pending CN114420904A (en) | 2021-12-29 | 2021-12-29 | Production method of modified lithium manganate material |
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