CN112830521B - F-doped P2-Na0.7MnO2Electrode material and preparation method thereof - Google Patents
F-doped P2-Na0.7MnO2Electrode material and preparation method thereof Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000000463 material Substances 0.000 title abstract description 16
- 239000011734 sodium Substances 0.000 claims abstract description 18
- 229910014834 Na0.7MnO2 Inorganic materials 0.000 claims abstract description 10
- 238000010438 heat treatment Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000007772 electrode material Substances 0.000 claims abstract description 9
- 238000005245 sintering Methods 0.000 claims abstract description 9
- 229910001415 sodium ion Inorganic materials 0.000 claims abstract description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 238000001816 cooling Methods 0.000 claims abstract description 7
- 238000000227 grinding Methods 0.000 claims abstract description 7
- 150000002696 manganese Chemical class 0.000 claims abstract description 7
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 claims abstract description 5
- 159000000000 sodium salts Chemical class 0.000 claims abstract description 5
- 238000003756 stirring Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 239000000843 powder Substances 0.000 claims description 10
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Inorganic materials O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 claims description 8
- FKNQFGJONOIPTF-UHFFFAOYSA-N Sodium cation Chemical compound [Na+] FKNQFGJONOIPTF-UHFFFAOYSA-N 0.000 claims description 7
- 239000011572 manganese Substances 0.000 claims description 5
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- 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 claims description 3
- 238000011534 incubation Methods 0.000 claims 1
- 238000002156 mixing Methods 0.000 abstract description 3
- 238000009792 diffusion process Methods 0.000 abstract description 2
- 239000011229 interlayer Substances 0.000 abstract 1
- 230000000052 comparative effect Effects 0.000 description 10
- 239000012071 phase Substances 0.000 description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 3
- 230000002238 attenuated effect Effects 0.000 description 3
- 229910001416 lithium ion Inorganic materials 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 239000010406 cathode material Substances 0.000 description 2
- 230000001351 cycling effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004146 energy storage Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000002803 fossil fuel Substances 0.000 description 2
- 238000013507 mapping Methods 0.000 description 2
- 238000000643 oven drying Methods 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 229910000314 transition metal oxide Inorganic materials 0.000 description 2
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- JDZCKJOXGCMJGS-UHFFFAOYSA-N [Li].[S] Chemical compound [Li].[S] JDZCKJOXGCMJGS-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000012983 electrochemical energy storage Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000010354 integration Effects 0.000 description 1
- 229910052744 lithium Inorganic materials 0.000 description 1
- 229910001425 magnesium ion Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 230000002441 reversible effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- IKULXUCKGDPJMZ-UHFFFAOYSA-N sodium manganese(2+) oxygen(2-) Chemical compound [O-2].[Mn+2].[Na+] IKULXUCKGDPJMZ-UHFFFAOYSA-N 0.000 description 1
- 229910001488 sodium perchlorate Inorganic materials 0.000 description 1
- 239000007790 solid phase Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- 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
- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/1228—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type [MnO2]n-, e.g. LiMnO2, Li[MxMn1-x]O2
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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
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
-
- 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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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses F-doped P2-Na0.7MnO2An electrode material and a preparation method thereof. The method comprises the following steps of (1) mixing sodium salt and manganese salt according to a feeding ratio of 0.77: dissolving in alcohol solution, stirring uniformly, adding fluoride to dissolve continuously, wherein the proportion is 25-50% of the total Na content; heating in water bath, drying and grinding; sintering at 450 ℃ for 3h, slowly heating to 950-1050 ℃, preserving heat and then cooling to room temperature to obtain the electrode material. The invention widens the interlayer spacing by doping F, further improves the diffusion capability of sodium ions, and improves the electrochemical properties such as the multiplying power, the cycle performance and the like of the material.
Description
Technical Field
The invention belongs to the technical field of electrode material preparation, and relates to fluorine-doped P2-Na0.7MnO2An electrode material, a preparation method thereof and application thereof in a sodium ion battery.
Background
With the continuous development of social economy, the excessive consumption of fossil fuels and the problems of energy crisis caused by the excessive consumption of fossil fuels gradually attract people's attention, the demand for clean and renewable energy sources such as wind energy and solar energy is continuously increased, whether the high-efficiency integration of electric power generated by renewable energy sources can be integrated into a power grid system or not is critical, and the key point is that the development of a sustainable and low-cost energy storage technology becomes a very hot research subject at present. Electrochemical energy storage systems, especially commercial secondary battery systems, are compelling competitors to meet the strong demand, and lithium ion batteries have been widely used in portable electronic devices such as notebook computers and mobile phones, and electric vehicles, and have achieved great success and increased rapidly.
At present, besides lithium ion batteries, other battery technologies such as lithium sulfur batteries, sodium ion batteries, and magnesium ion batteries have attracted extensive attention of researchers due to advantages such as sustainability, low cost, and high capacity. Na and Li are elements of the same main group, the reserves are abundant, Na resources are uniformly distributed in the whole world, and the cost is low. Sodium ion batteries are likely to replace lithium ion batteries in large energy storage devices, and research on sodium ion batteries has attracted more and more researchers in recent years.
Among the cathode materials of sodium ion batteries, the layered transition metal oxide, particularly the sodium manganese oxide, has the characteristics of high specific capacity and working voltage, easiness in preparation, environmental friendliness, nontoxicity, low cost and the like, and in addition, compared with an O3 phase structure, the P2 type manganese-based layered oxide is a cathode material of a sodium ion battery with great potential, but pure P2 phase Na0.7MnO2The material has great volume change in the charge and discharge process due to many phase changes, so that the cycle performance and rate performance of the material are not ideal.
Disclosure of Invention
The invention aims to provide F-doped P2-Na0.7MnO2An electrode material and a preparation method thereof. The method carries out F doping through solid-phase sintering, and the electrochemical performance of the material is obviously improved.
The technical scheme for realizing the purpose of the invention is as follows:
f-doped P2-Na0.7MnO2The electrode material and the preparation method thereof comprise the following steps:
step 2, sintering at 450 ℃ for 3h, slowly heating to 950-1050 ℃, preserving heat for a period of time, and cooling to room temperature to obtain F-doped P2-Na0.7MnO2And (3) powder.
Preferably, in step 1, the sodium and manganese salts are dissolved in 70Vol% alcohol solution.
Preferably, in step 1, the sodium salt is NaAc and the manganese salt is Mn (Ac)2And the fluoride is NaF.
Preferably, in step 2, the holding time is 10 h.
Preferably, in step 2, the temperature rise rate is 1 ℃/min.
Preferably, in step 2, the cooling rate is 1 ℃/min.
Compared with the prior art, the invention has the following advantages:
according to the invention, the F is doped to replace the position of O in the crystal lattice, so that the distance between transition metal oxide laminates is widened, the diffusion rate of sodium ions is accelerated, and the electrochemical properties such as the multiplying power performance, the cycle performance and the like of the material are improved.
Drawings
FIG. 1 is P2-Na prepared in example 10.7MnO2XRD pattern of the powder.
FIG. 2 is P2-Na prepared in example 10.7MnO2SEM image of the powder.
FIG. 3 is P2-Na prepared in example 10.7MnO2Mapping elemental distribution of powder.
FIG. 4 is P2-Na prepared in example 10.7MnO2Powder rate curves between 2 and 4V.
FIG. 5 is P2-Na prepared in example 20.7MnO2CV curve of powder between 2-4V.
FIG. 6 is P2-Na prepared in comparative examples 1, 2, 3 and 40.7MnO2The cycling curves of the powders between 2 and 4V correspond to (a), (b), (c) and (d), respectively.
Detailed Description
The present invention will be described in further detail with reference to the following examples and the accompanying drawings.
The electrochemical tests described in the following examples all used the material as the positive electrode and the sodium sheet as the negative electrode, 1.0M NaClO4The test is carried out in an electrolyte working system with 1:1 Vol% and 5.0% FEC, and the test instrument is a Xinwei electrochemical workstation.
Example 1
Mixing NaAc, Mn (Ac)2According to the feed ratio of 0.77: 1, dissolving in 70 percent alcohol solution, stirring uniformly, adding NaF to continue dissolving, wherein the proportion is 25 percent of the total Na content. Heating in water bath at 80 deg.C, oven drying, and grinding. Sintering at 450 deg.C for 3h in a muffle furnace, heating to 950 deg.C at a rate of 1 deg.C/min, maintaining for 10h, cooling to room temperature at a rate of 1 deg.C/min, and grinding to obtain F-doped P2-Na0.7MnO2And (3) powder. FIGS. 1 to 3 are respectively an XRD spectrum, an SEM spectrum and a TEM-mapping spectrum of the material in a voltage interval of 2 to 4VThe cycle performance of the prepared material is shown as follows: the capacity of the material is attenuated by 5.0% after 100 cycles under the current density of 500mA/g, the multiplying power performance of the material in a voltage interval of 2-4V is shown in figure 4, and the multiplying power performance is improved by doping.
Example 2
Mixing NaAc, Mn (Ac)2According to the feed ratio of 0.77: 1, dissolving in 70 percent alcohol solution, stirring uniformly, adding NaF for continuous dissolution, wherein the proportion is 40 percent of the total Na content. Heating in water bath at 80 deg.C, oven drying, and grinding. Sintering at 450 deg.C for 3h in a muffle furnace, heating to 1000 deg.C at a rate of 1 deg.C/min, maintaining for 10h, cooling to room temperature at a rate of 1 deg.C/min, and grinding to obtain F-doped P2-Na0.7MnO2And (3) powder. In fig. 5, the CV curves of the prepared materials all show reversible phase transitions.
Comparative example 1
The comparative example is basically the same as the example 1, and the only difference is that the sintering temperature is 1050 ℃, the temperature is too high, the sintering doping effect ratio is low temperature difference, and the specific capacity is still obviously attenuated.
Comparative example 2
The comparative example is basically the same as the example 2, and the only difference is that F is not doped, the obtained product has poor cycle performance in a potential interval of 2-4V, and the specific capacity is obviously attenuated.
Comparative example 3
The comparative example is essentially the same as example 2, with the only difference that the F content is 25%, and the cycle performance of the obtained product is improved in the potential range of 2-4V compared with that of the product without doping.
Comparative example 4
This comparative example is essentially the same as example 2, except that the F content is 50% and the product obtained has a high F content leading to a reduction in the cycle performance in the potential interval of 2-4V.
FIG. 6 is a graph of the cycle time (a, b, c, d, respectively) of the materials of comparative examples 1-4 in the voltage interval of 2-4V, wherein the capacity still significantly decays due to the excessive sintering temperature in graph a; b, because the materials are not doped, the cycle performance of the materials is extremely poor; c, the doping amount of the graph is moderate, and the cycle performance is optimal; d plot F was doped too much, resulting in a slight degradation of cycling performance.
Claims (8)
1. F-doped P2-Na0.7MnO2The preparation method of the electrode material is characterized by comprising the following steps of:
step 1, according to the feeding ratio of sodium salt to manganese salt of 0.77: dissolving in alcohol solution, stirring, adding fluoride with 25-40 mol% of total Na content, dissolving continuously, heating in water bath at 80 ℃, drying and grinding;
step 2, sintering at 450 ℃ for 3h, slowly heating to 950-1000 ℃, keeping the temperature for a period of time, and cooling to room temperature to obtain F-doped P2-Na0.7MnO2And (3) powder.
2. The method of claim 1, wherein in step 1, the sodium and manganese salts are dissolved in 70Vol% alcohol.
3. The method of claim 1, wherein in step 1, the sodium salt is NaAc and the manganese salt is Mn (Ac)2And the fluoride is NaF.
4. The method of claim 1, wherein in step 2, the incubation time is 10 hours.
5. The method according to claim 1, wherein in step 2, the temperature rise rate is 1 ℃/min.
6. The method of claim 1, wherein in step 2, the cooling rate is 1 ℃/min.
7. F-doped P2-Na prepared by the method of any one of claims 1 to 60.7MnO2An electrode material.
8. F-doped P2-Na prepared by the method of any one of claims 1 to 60.7MnO2The application of the electrode material in a sodium ion battery.
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| CN114188529A (en) * | 2021-11-30 | 2022-03-15 | 湖南钠方新能源科技有限责任公司 | Composite positive electrode material, preparation method thereof, positive plate and sodium ion battery |
| CN115172695B (en) * | 2022-07-13 | 2024-02-13 | 南京理工大学 | Surface-coated layered transition metal oxide positive electrode material and preparation method thereof |
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| CN107093713A (en) * | 2017-04-07 | 2017-08-25 | 武汉大学 | A kind of anion doped sodium-ion battery oxide anode material |
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