CN113461067A - Ultrahigh-capacity cathode material Li1.25Mn0.5Cr0.25O2Method of synthesis of - Google Patents
Ultrahigh-capacity cathode material Li1.25Mn0.5Cr0.25O2Method of synthesis of Download PDFInfo
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- 239000010406 cathode material Substances 0.000 title claims description 17
- 230000015572 biosynthetic process Effects 0.000 title description 3
- 238000003786 synthesis reaction Methods 0.000 title description 3
- 239000000243 solution Substances 0.000 claims abstract description 55
- 239000011572 manganese Substances 0.000 claims abstract description 36
- 239000011651 chromium Substances 0.000 claims abstract description 34
- 238000006243 chemical reaction Methods 0.000 claims abstract description 29
- 238000001308 synthesis method Methods 0.000 claims abstract description 27
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims abstract description 22
- 238000001035 drying Methods 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000007795 chemical reaction product Substances 0.000 claims abstract description 16
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- 239000011259 mixed solution Substances 0.000 claims abstract description 14
- 238000005342 ion exchange Methods 0.000 claims abstract description 13
- 239000002243 precursor Substances 0.000 claims abstract description 13
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 229940099596 manganese sulfate Drugs 0.000 claims abstract description 12
- 235000007079 manganese sulphate Nutrition 0.000 claims abstract description 12
- 239000011702 manganese sulphate Substances 0.000 claims abstract description 12
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims abstract description 12
- 239000000843 powder Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 235000017557 sodium bicarbonate Nutrition 0.000 claims abstract description 11
- 229910000030 sodium bicarbonate Inorganic materials 0.000 claims abstract description 11
- GRWVQDDAKZFPFI-UHFFFAOYSA-H chromium(III) sulfate Chemical compound [Cr+3].[Cr+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O GRWVQDDAKZFPFI-UHFFFAOYSA-H 0.000 claims abstract description 8
- 239000000047 product Substances 0.000 claims abstract description 7
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 6
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 6
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- IIPYXGDZVMZOAP-UHFFFAOYSA-N lithium nitrate Chemical compound [Li+].[O-][N+]([O-])=O IIPYXGDZVMZOAP-UHFFFAOYSA-N 0.000 claims description 16
- 230000002572 peristaltic effect Effects 0.000 claims description 6
- XFTALRAZSCGSKN-UHFFFAOYSA-M sodium;4-ethenylbenzenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C1=CC=C(C=C)C=C1 XFTALRAZSCGSKN-UHFFFAOYSA-M 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 230000009471 action Effects 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 241000764238 Isis Species 0.000 claims 1
- 239000010405 anode material Substances 0.000 abstract description 7
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 abstract description 6
- 229910052744 lithium Inorganic materials 0.000 abstract description 6
- 239000002245 particle Substances 0.000 abstract description 6
- 230000009286 beneficial effect Effects 0.000 abstract description 3
- 239000000203 mixture Substances 0.000 abstract 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 11
- 229910001416 lithium ion Inorganic materials 0.000 description 11
- 238000000034 method Methods 0.000 description 8
- 239000000463 material Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 5
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 4
- 229910052748 manganese Inorganic materials 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- 239000012153 distilled water Substances 0.000 description 3
- 239000007774 positive electrode material Substances 0.000 description 3
- 238000001878 scanning electron micrograph Methods 0.000 description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 229910052708 sodium Inorganic materials 0.000 description 2
- 239000011734 sodium Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 2
- 239000004094 surface-active agent Substances 0.000 description 2
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- 238000009830 intercalation Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
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- 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
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1271—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [Mn2O8]n-, e.g. (LaSr3)Mn2O8
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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
- 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
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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
- H01M4/48—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
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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
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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- C01P2004/60—Particles characterised by their size
- C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses an ultra-high capacity anode material Li1.25Mn0.5Cr0.25O2The synthesis method comprises the following steps: dissolving chromium sulfate and manganese sulfate in deionized water to obtain a mixed solution A; dissolving 4-sodium styrene sulfonate in ethanol to obtain a clear solution B; dropwise adding the clear solution B into the mixed solution A to form a solution C; adding a sodium bicarbonate solution into the solution C to obtain a solution E; adjusting the pH value of the solution E to 5-8 by ammonia water; transferring the mixture into a reaction kettle for reaction; after the reaction is finished, cooling, centrifugally washing, drying and grinding to obtain precursor powder; feeding precursor powder and molten lithium nitrateCarrying out ion exchange reaction; filtering, washing and drying the reaction product to obtain the target product Li1.25Mn0.5Cr0.25O2. The synthesized anode material Li1.25Mn0.5Cr0.25O2The particle size distribution is uniform, which is beneficial to improving the electrochemical capacity.
Description
Technical Field
The invention belongs to the technical field of lithium ion batteries, and particularly relates to an ultrahigh-capacity cathode material Li1.25Mn0.5Cr0.25O2The method of (1).
Background
With the rapid development of modern society and economy, the reserves of traditional energy resources are reduced rapidly, and some problems such as environmental pollution come with, which compels people to develop clean and green new energy resources. The lithium ion battery has attracted wide attention since the advent as an important storage and output buffer link for clean energy. Meanwhile, the lithium ion battery has higher specific capacity and voltage and better stability, and is widely applied to various portable electronic devices. In addition, the lithium ion battery is also widely applied to the fields of large and medium-sized energy storage equipment, new energy electric vehicles and the like, and higher requirements are put forward on the performance of the lithium ion battery. At present, the positive electrode material is a key factor that restricts the performance of the lithium ion battery, so a positive electrode material with higher specific capacity is required to be developed to improve the energy density of the lithium ion battery.
In recent years, lithium-rich manganese-based positive electrode materials have been widely used in lithium ion batteries due to their advantages. The lithium-rich manganese-based anode material has the advantages of discharge specific capacity of over 250mAh/g and working voltage of over 3.5V, good thermal stability, good cycle performance, environmental friendliness and relatively low price, and can meet the requirement of new energy industries on high-energy-density lithium ion batteries. However, the lithium-rich manganese-based cathode material has some disadvantages, such as capacity fading during the circulation process, which is mainly caused by the transformation of the material structure from a layered structure to a spinel structure during the circulation process.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
Aim atThe invention provides a super-high capacity anode material Li based on the defects of the previous lithium-rich manganese-based anode material1.25Mn0.5Cr0.25O2The synthesis method prepares the lithium ion battery anode material with high capacity and good performance, and can effectively improve the capacity of the battery. The invention adopts an ion exchange method to synthesize Li1.25Mn0.5Cr0.25O2In the circulation process, the structure of the material is not converted to the spinel structure, and voltage attenuation can be effectively inhibited. Meanwhile, the surfactant is added in the process of preparing the precursor, so that particles with finer particle sizes are obtained, and the electrochemical performance of the material is improved.
In order to solve the technical problems, the invention adopts the following technical scheme:
ultrahigh-capacity cathode material Li1.25Mn0.5Cr0.25O2The synthesis method comprises the following specific steps:
(1) mixing chromium sulfate (Cr)2(SO4)3·18H2O) and manganese sulfate (MnSO)4) Dissolving in deionized water to obtain a mixed solution A;
(2) dissolving a certain amount of 4-styrene sodium sulfonate in an ethanol solvent to obtain a clear solution B;
(3) slowly dripping the clear solution B into the mixed solution A in the step (1) by using a peristaltic pump to form a solution C;
(4) dissolving a certain amount of sodium bicarbonate in deionized water to form a clear solution D;
(5) adding the solution D into the solution C under the action of a magnetic stirrer to obtain a stable mixed system, and marking as a solution E;
(6) dropwise adding ammonia water into the solution E to enable the pH value of the solution to be 5-8;
(7) then transferring the mixed solution into a reaction kettle for reaction;
(8) after the reaction is finished, cooling to room temperature, centrifugally washing, drying and grinding to obtain precursor powder;
(9) carrying out ion exchange reaction on the precursor powder and molten lithium nitrate;
(10) filtering the reaction product, washing the reaction product for a plurality of times by deionized water, and drying the reaction product in an oven to finally obtain a target product Li1.25Mn0.5Cr0.25O2。
Further, in the step (1) of the above synthesis method, chromium sulfate (Cr)2(SO4)3·18H2O) and manganese sulfate in a molar ratio of 1: 4.
Further, in the step (3) of the synthesis method, the molar ratio of the sodium 4-styrene sulfonate to the manganese sulfate is 1: 1.
Further, in the step (3) of the synthesis method, the dropping rate of the peristaltic pump is (100-150) ml/h.
Further, in the above synthesis method, step (5), sodium bicarbonate (NaHCO)3) And manganese sulfate in a molar ratio of 2.5: 1.
Further, in the step (5) of the synthesis method, the stirring speed of the magnetic stirrer is (180-240) rpm.
Further, in the step (7) of the synthesis method, the reaction temperature is (180-250) DEG C, and the hydrothermal reaction time is (24-30) hours.
Further, in the step (8) of the synthesis method, the rotating speed of the centrifuge is 5000r/min, and the centrifugation time is 10 min.
Further, in the step (8) of the synthesis method, the drying temperature is (70-105) DEG C, and the time is (10-15) h.
Further, in the step (9) of the above synthesis method, the molar ratio of lithium nitrate to sodium bicarbonate is 1: 1.
Further, in the step (9) of the synthesis method, the temperature of ion exchange is (270-450 ℃) and the time of ion exchange reaction is (1-15) h.
Further, in the step (10) of the synthesis method, the drying temperature is (80-100) DEG C, and the time is (12-18) hours.
The invention has the beneficial effects that: the invention adopts the synthetic method of ion exchange reaction to prepare the anode material Li1.25Mn0.5Cr0.25O2. In the synthesis process, lithium nitrate is selected as a lithium source for ion exchange, the ion exchange rate of the reaction is high, and the obtained target product is uniform in appearance and is in a porous structure with the size less than 200nm as can be seen from an SEM image. Meanwhile, the 4-styrene sodium sulfonate is used as a surfactant, so that particles with smaller particle size can be obtained. The electrode material synthesized by the method effectively improves the structural stability and the cycle performance of the material.
Drawings
FIG. 1 shows Li prepared in example 1 of the present invention1.25Mn0.5Cr0.25O2SEM image of (d).
FIG. 2 shows Li prepared in example 1 of the present invention1.25Mn0.5Cr0.25O2Charge and discharge curves at a current density of 20 mA/g.
FIG. 3 shows Li prepared in example 1 of the present invention1.25Mn0.5Cr0.25O2Cycling performance plot at 100mA/g current density.
Detailed Description
The present invention will be further described with reference to the following examples. It is to be understood that the following examples are illustrative only and are not intended to limit the scope of the invention, which is to be given numerous insubstantial modifications and adaptations by those skilled in the art based on the teachings set forth above.
Example 1
Ultrahigh-capacity cathode material Li1.25Mn0.5Cr0.25O2The synthesis method comprises the following specific steps:
(1) 8.95g (0.0125 mol) of chromium sulfate and 7.55g (0.05 mol) of manganese sulfate were dissolved in 100ml of deionized water to obtain a mixed solution A.
(2) 10.3095g (0.05 mol) of sodium 4-styrenesulfonate was dissolved in 50ml of ethanol solvent to obtain a clear solution B.
(3) The dropping rate of the peristaltic pump is 130ml/h, and the clear solution B is slowly dropped into the mixed solution A to form a solution C.
(4) Another 10.5012g (0.125 mol) of sodium bicarbonate was dissolved in 100ml of deionized water to form a clear solution D.
(5) And adding the solution D into the solution C, and stirring by a magnetic stirrer at the rotating speed of 240rpm while dropwise adding to obtain a solution E.
(6) And (3) dropwise adding ammonia water into the solution E to ensure that the pH value of the solution is 6.
(7) And transferring the solution E into a reaction kettle for reaction at 230 ℃ for 25 hours.
(8) After the reaction is finished, cooling to room temperature, centrifuging for 10min at the rotating speed of 5000r/min, washing for a plurality of times by using distilled water, drying for 10h at the temperature of 100 ℃, and grinding to obtain precursor powder.
(9) 8.6188g (0.125 mol) of lithium nitrate was weighed out and subjected to an ion exchange reaction with the precursor powder at 300 ℃ for 12 hours.
(10) Filtering the reaction product, washing the reaction product for a plurality of times by deionized water, putting the reaction product into an oven for drying at the drying temperature of 80 ℃ for 16 hours to finally obtain the target product Li1.25Mn0.5Cr0.25O2。
FIG. 1 Li prepared by the invention1.25Mn0.5Cr0.25O2The SEM image shows that the particle size of the obtained material is small and the distribution is uniform. The fine particle size can provide a better de-intercalation environment for lithium ions, and is beneficial to improving the electrochemical performance of the material.
FIG. 2 shows Li prepared by the present invention1.25Mn0.5Cr0.25O2Charge and discharge curves at a current density of 20 mA/g. The maximum specific discharge capacity is 323 mAh/g.
FIG. 3 shows Li prepared by the present invention1.25Mn0.5Cr0.25O2Cycling performance plot at 100mA/g current density. As can be seen from the figure, the initial capacity can reach 323mAh/g, and after 50 cycles, the capacity is 225 mAh/g.
Example 2
Ultrahigh-capacity cathode materialLi1.25Mn0.5Cr0.25O2The synthesis method comprises the following specific steps:
(1) 4.475g (0.00625 mol) of chromium sulfate and 3.775g (0.025 mol) of manganese sulfate were dissolved in 100ml of deionized water to obtain a mixed solution A.
(2) 5.1547g (0.025 mol) of sodium 4-styrenesulfonate was dissolved in 50ml of ethanol solvent to obtain a clear solution B.
(3) The dropping rate of the peristaltic pump is 100ml/h, and the clear solution B is slowly dropped into the mixed solution A to form a solution C.
(4) Another 5.2506g (0.0625 mol) of sodium bicarbonate was dissolved in 100ml of deionized water to form a clear solution D.
(5) And adding the solution D into the solution C, and stirring by a magnetic stirrer at the rotating speed of 180rpm while dropwise adding to obtain a solution E.
(6) And (3) dropwise adding ammonia water into the solution E to ensure that the pH value of the solution is 6.
(7) And transferring the solution E into a reaction kettle for reaction at the temperature of 230 ℃ for 24 hours.
(8) After the reaction is finished, cooling to room temperature, centrifuging for 10min at the rotating speed of 5000r/min, washing with distilled water for several times, drying for 12h at the temperature of 80 ℃, and grinding to obtain precursor powder.
(9) 4.3094g (0.0625 mol) of lithium nitrate was weighed out and subjected to an ion exchange reaction with the above precursor powder at 270 ℃ for 15 hours.
(10) Filtering the reaction product, washing the reaction product for a plurality of times by deionized water, putting the reaction product into an oven for drying at the drying temperature of 80 ℃ for 16 hours to finally obtain the target product Li1.25Mn0.5Cr0.25O2。
Example 3
Ultrahigh-capacity cathode material Li1.25Mn0.5Cr0.25O2The synthesis method comprises the following specific steps:
(1) 20.619g (0.1 mol) of chromium sulfate and 15.1g (0.1 mol) of manganese sulfate were dissolved in 100ml of deionized water to obtain a mixed solution A.
(2) 20.619g (0.1 mol) of sodium 4-styrenesulfonate was dissolved in 50ml of ethanol solvent to obtain a clear solution B.
(3) The dropping rate of the peristaltic pump is 100mL/h, and the clear solution B is slowly dropped into the mixed solution A to form a solution C.
(4) Another 21.0025g (0.25 mol) of sodium bicarbonate was dissolved in 100ml of deionized water to form a clear solution D.
(5) And adding the solution D into the solution C, and stirring by a magnetic stirrer at the rotating speed of 200rpm while dropwise adding to obtain a solution E.
(6) And (3) dropwise adding ammonia water into the solution E to enable the pH value of the solution to be 8.
(7) And transferring the solution E into a reaction kettle for reaction at the temperature of 200 ℃ for 26 hours.
(8) After the reaction is finished, cooling to room temperature, centrifuging for 10min at the rotating speed of 5000r/min, washing for a plurality of times by using distilled water, drying for 15h at the temperature of 100 ℃, and grinding to obtain precursor powder.
(9) 17.2375g (0.25 mol) of lithium nitrate was weighed out and subjected to an ion exchange reaction with the precursor powder at 350 ℃ for 10 hours.
(10) Filtering the reaction product, washing the reaction product for a plurality of times by deionized water, putting the reaction product into an oven for drying at the drying temperature of 100 ℃ for 12 hours to finally obtain the target product Li1.25Mn0.5Cr0.25O2。
The above-described embodiments are merely illustrative of the present invention, and although the preferred embodiments of the present invention and the accompanying drawings are disclosed for illustrative purposes, the present invention is not limited thereto, and various alternatives, variations and modifications may be possible by those skilled in the art without departing from the spirit and scope of the present invention and the appended claims. Therefore, the present invention should not be limited to the disclosure of the preferred embodiments and the accompanying drawings.
Claims (10)
1. Ultrahigh-capacity cathode material Li1.25Mn0.5Cr0.25O2The synthesis method is characterized by comprising the following steps:
(1) dissolving chromium sulfate and manganese sulfate in deionized water to obtain a mixed solution A;
(2) dissolving 4-sodium styrene sulfonate in ethanol to obtain a clear solution B;
(3) slowly dripping the clear solution B prepared in the step (2) into the mixed solution A in the step (1) by using a peristaltic pump to form a solution C;
(4) dissolving sodium bicarbonate in deionized water to form a clear solution D;
(5) adding the solution D into the solution C obtained in the step (3) under the action of a magnetic stirrer to obtain a stable mixed system, and marking as a solution E;
(6) dropwise adding ammonia water into the solution E to enable the pH value of the solution to be 5-8;
(7) then transferring the mixed solution into a reaction kettle for reaction;
(8) after the reaction is finished, cooling to room temperature, centrifugally washing, drying and grinding to obtain precursor powder;
(9) carrying out ion exchange reaction on the precursor powder obtained in the step (8) and molten lithium nitrate;
(10) filtering the reaction product, washing the reaction product for a plurality of times by deionized water, and then putting the reaction product into an oven for drying to obtain a target product Li1.25Mn0.5Cr0.25O2。
2. The ultra-high capacity cathode material Li according to claim 11.25Mn0.5Cr0.25O2The synthesis method is characterized in that: in the step (1), the molar ratio of the chromium sulfate to the manganese sulfate is 1: 4.
3. The ultra-high capacity cathode material Li according to claim 11.25Mn0.5Cr0.25O2The synthesis method is characterized in that: in the step (3), the molar ratio of the sodium 4-styrene sulfonate to the manganese sulfate is 1: 1; creeping worstedThe dropping speed of the dynamic pump is (100-150) mL/h.
4. The ultra-high capacity cathode material Li according to claim 11.25Mn0.5Cr0.25O2The synthesis method is characterized in that: in the step (5), the molar ratio of the sodium bicarbonate to the manganese sulfate is 2.5: 1; the stirring speed of the magnetic stirrer ranges from 180rpm to 240 rpm.
5. The ultra-high capacity cathode material Li according to claim 11.25Mn0.5Cr0.25O2The synthesis method is characterized in that: in the step (7), the reaction temperature is 180-250 ℃, and the reaction time is 24-30 h.
6. The ultra-high capacity cathode material Li according to claim 11.25Mn0.5Cr0.25O2The synthesis method is characterized in that: in the step (8), the rotating speed of the centrifugal machine is 5000r/min, and the centrifugal time is 10 min.
7. The ultra-high capacity cathode material Li according to claim 11.25Mn0.5Cr0.25O2The synthesis method is characterized in that: in the step (8), the drying temperature is 70-105 ℃, and the time is 10-15 h.
8. The ultra-high capacity cathode material Li according to claim 11.25Mn0.5Cr0.25O2The synthesis method is characterized in that: and (3) taking the amount of the sodium bicarbonate in the step (5) as a reference, wherein the molar ratio of the molten lithium nitrate to the molten sodium bicarbonate in the step (9) is 1: 1.
9. The ultra-high capacity cathode material Li according to claim 11.25Mn0.5Cr0.25O2The synthesis method is characterized in that: in the step (9), the temperature of ion exchange is 270-450 ℃ and the time isIs 1-15 h.
10. The ultra-high capacity cathode material Li according to claim 11.25Mn0.5Cr0.25O2The synthesis method is characterized in that: in the step (10), the drying temperature is 80-100 ℃, and the time is 12-18 h.
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| CN102569781A (en) * | 2012-03-27 | 2012-07-11 | 天津理工大学 | High-voltage lithium ion battery cathode material and preparation method thereof |
| KR20130143427A (en) * | 2012-06-21 | 2013-12-31 | 삼성에스디아이 주식회사 | Positive electrode active material for lithium secondary battery, preparing method thereof, positive electrode for lithium secondary battery including the same, and lithium secondary battery employing the same |
| CN111204813A (en) * | 2020-01-16 | 2020-05-29 | 昆明理工大学 | Preparation method of vanadium-doped lithium-rich manganese-based positive electrode material |
| CN112786877A (en) * | 2021-03-08 | 2021-05-11 | 昆明理工大学 | Preparation method of lithium-rich manganese-based positive electrode material |
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| CN102569781A (en) * | 2012-03-27 | 2012-07-11 | 天津理工大学 | High-voltage lithium ion battery cathode material and preparation method thereof |
| KR20130143427A (en) * | 2012-06-21 | 2013-12-31 | 삼성에스디아이 주식회사 | Positive electrode active material for lithium secondary battery, preparing method thereof, positive electrode for lithium secondary battery including the same, and lithium secondary battery employing the same |
| CN111204813A (en) * | 2020-01-16 | 2020-05-29 | 昆明理工大学 | Preparation method of vanadium-doped lithium-rich manganese-based positive electrode material |
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