CN110112375B - Double-transition metal manganese-based layered positive electrode material of sodium ion battery - Google Patents
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- 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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Abstract
The invention relates to a double-transition metal manganese-based layered positive electrode material of a sodium ion battery, which is characterized in that: having the general formula NaxMn1‑ yMyO2Wherein M is Ru, Ir, Nb, Bi, Sn, Ta or Sb, and x is more than or equal to 0.3 and less than or equal to 1 and is 0<y is less than or equal to 0.5. The material disclosed by the invention is simple in preparation method and high in practicability, and the synthesized material improves the electronic conductivity and the sodium ion mobility of the material, and inhibits the phase change in the sodium ion de-intercalation process under high voltage, so that the specific capacity, the rate capability and the cycle performance of the positive electrode material assembled into a sodium ion battery are effectively improved. The method has important significance for further optimizing the performance of the sodium-ion battery and the future commercialization of the sodium-ion battery.
Description
Technical Field
The invention relates to the field of electrochemistry, in particular to a double-transition metal manganese-based layered positive electrode material of a sodium-ion battery.
Background
Sodium is the sixth most abundant element in the earth's crust, and has similar physical and chemical properties and low price characteristics as lithium, so sodium-ion batteries are considered to be one of the most promising new energy storage devices to replace lithium-ion batteries. However, sodium ion batteries have problems such as difficulty in migration of sodium ions, poor stability, and low energy density.
In recent years, the layered transition metal oxide has a series of advantages of high specific capacity, simple preparation method, environmental friendliness and the like, and is widely concerned by researchers. Particularly, manganese-based layered materials are considered to be one of the most promising positive electrode materials for commercialization due to their low price and high capacity. However, the manganese-based layered material has inherent disadvantages that the material has a complex phase change process in an electrochemical process, and particularly, the phase change problem under high voltage causes huge volume change and structural distortion of the material, thereby causing the reduction of the cycle life of the battery.
At present, no sodium ion battery layered positive electrode material which meets the commercial requirements of sodium ion batteries and has environmental stability exists, so that the wide popularization of the sodium ion batteries is restricted.
The Chinese patent with the application number of 2017105709588 discloses a manganese-based positive electrode material of a sodium ion battery, wherein a layer of nano titanium-based oxide is constructed on the surface of a manganese-based layered positive electrode material, the particle size of the prepared positive electrode material is 2-10 mu m, and the specific discharge capacity of the positive electrode material needs to be further improved.
Disclosure of Invention
In order to solve the technical problems, the invention aims to provide a double-transition metal manganese-based layered positive electrode material of a sodium ion battery.
The invention provides a double-transition metal manganese-based layered positive electrode material of a sodium ion battery, and the general formula of the positive electrode material is NaxMn1- yMyO2Wherein M is Ru, Ir, Nb, Bi, Sn, Ta or Sb, and x is more than or equal to 0.3 and less than or equal to 1 and is 0<y≤0.5。
Preferably, M is Ru.
Preferably, 0.5. ltoreq. x.ltoreq.0.9, 0.02. ltoreq. y.ltoreq.0.3.
More preferably, the general formula of the double-transition metal manganese-based layered cathode material of the sodium-ion battery is Na0.6Mn0.93Ru0.07O2。
The double-transition metal manganese-based positive electrode material of the sodium ion battery has a layered crystal structure, and the content of Mn element in the positive electrode material is high, so that the main purposes of controlling the battery cost and improving the battery capacity are achieved. According to the double-transition metal manganese-based layered cathode material of the sodium ion battery, more sodium ion active sites in the cathode material structure are excited by uniformly doping a small amount of other metal M, the conductivity of the material is improved, and the phase change of the material under high voltage is inhibited, so that the specific capacity, the rate capability and the cycle performance of the electrode material are respectively improved, and the overall performance of the sodium ion battery is finally improved.
Preferably, the crystal structure of the cathode material belongs to P63A/mmc or
And (4) space group.
Further, the positive electrode material is uniform particles with a layered stacking structure, and the particle size of the positive electrode material is 0.2-1 μm.
Further, the preparation method of the double-transition metal manganese-based layered positive electrode material of the sodium-ion battery comprises the following steps:
uniformly mixing sodium salt, manganese salt and other metal oxides, tabletting, calcining at the temperature of 700-1100 ℃, and cooling to obtain the double-transition metal manganese-based layered positive electrode material of the sodium-ion battery; wherein the other metal oxide is selected from RuO2、IrO2、SnO2、Ta2O5、Bi2O3、Nb2O5And Sb2O5One or more of them.
Further, the sodium salt is Na2CO3、NaNO3And NaCl.
Further, the manganese salt is MnCO3And/or Mn (NO)3)2. Preferably, the manganese salt is MnCO3. The manganese salt is generated with gas during the calcination process, so that particles of the finally formed cathode material are small.
Furthermore, the molar ratio of sodium element, manganese element and other metal elements in the sodium salt, the manganese salt and other metal oxides is 0.3-1:0.5-1: 0.01-0.5.
Preferably, the molar ratio of the sodium element, the manganese element and other metal elements in the sodium salt, the manganese salt and other metal oxides is 0.5-0.9:0.6-0.9: 0.02-0.3.
Further, the mixture is uniformly mixed by adopting a ball milling method, the ball milling speed is 100-. The ball milling method can fully and uniformly mix the sodium salt, the manganese salt and other metal oxide precursors, thereby facilitating the subsequent reaction and fully and uniformly carrying out.
Further, tabletting is carried out under 1-50 MPa. The tabletting is carried out under the pressure, the precursor mixture can be pressed more tightly, the distance between particles is reduced, and the reaction between all the precursors is more sufficient and uniform during the subsequent heat treatment.
Further, the temperature is raised from room temperature to 700-1100 ℃ at a rate of 1-20 ℃/min during the calcination.
Further, the calcination is carried out in an oxygen atmosphere or an air atmosphere.
The invention adopts a solid-phase sintering method, and the reaction conditions are controlled to ensure that the manganese-based layered material is uniformly doped with other metal elements, thereby obtaining the stable sodium-containing manganese-based layered anode material, and having the structural characteristic of no phase change in a wide voltage range.
By the scheme, the invention at least has the following advantages:
(1) the raw materials adopted by the invention are cheap and easy to obtain, and the preparation method of solid-phase sintering is simple and easy to realize, and has practical operability and commercial popularization.
(2) The anode material prepared by the invention is uniform particles with a layered stacking structure, and the particle size is 0.2-1 mu m.
(3) The anode material prepared by the invention improves the electronic conductivity and the mobility of sodium ions of the material, and inhibits the phase change in the process of sodium ion deintercalation under high voltage, so that the anode material is highly reversible in the charging and discharging process and has high specific capacity when being assembled into a sodium ion battery, and the sodium ions and the electronic conductivity of the material are improved due to the doping of other metal elements, so that the rate capability of the electrode material is improved, and in addition, the doped metal elements effectively inhibit the phase change of the electrode material under high voltage, so that the cycle stability of the electrode material in the charging and discharging process is improved.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is an X-ray powder diffraction spectrum of a double-transition metal manganese-based layered cathode material of a sodium-ion battery prepared in example 1 of the invention;
fig. 2 is a scanning electron microscope image of the double transition metal manganese-based layered positive electrode material of the sodium ion battery prepared in example 1 of the present invention;
FIG. 3 is a transmission electron microscope image of a double transition metal manganese-based layered cathode material of a sodium-ion battery prepared in example 1 of the present invention;
FIG. 4 is a transmission electron microscope element scanning spectrum of the double transition metal manganese-based layered cathode material of the sodium-ion battery prepared in example 1 of the present invention;
FIG. 5 is a charge-discharge curve and an in-situ X-ray powder diffraction spectrum of a double-transition metal manganese-based layered positive electrode material of a sodium-ion battery prepared in example 1 of the present invention;
fig. 6 is a typical charge-discharge curve of the double transition metal manganese-based layered cathode material of the sodium-ion battery prepared in example 1 of the present invention;
fig. 7 is a multiplying power diagram of the double-transition metal manganese-based layered cathode material of the sodium-ion battery prepared in example 1 of the invention under different current densities;
FIG. 8 is a long cycle performance curve at a current density of 50mA/g for a dual transition metal manganese-based layered positive electrode material for a sodium-ion battery prepared in example 1 of the present invention;
fig. 9 is a charge-discharge curve diagram of the sodium-ion battery double-transition metal manganese-based layered cathode material prepared in example 1 of the present invention when the full-cell is assembled.
Detailed Description
The following examples further illustrate the present invention but are not to be construed as limiting the invention. Modifications and substitutions to methods, procedures, or conditions of the invention may be made without departing from the spirit and substance of the invention.
Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art.
(1) Accurately weighing NaNO with corresponding mass according to the molar ratio of 0.6:0.93:0.073、MnCO3And RuO2Adding into a ball milling tank, adding ball milling small balls into the ball milling tankBall milling is carried out for 5h under the condition of 300r/min, the precursors are uniformly mixed, and the uniformly mixed precursors are dried in an oven at 100 ℃ for 12 h.
(2) The ball-milled mixture was pressed into a disk with a diameter of 16mm under a pressure of 10 MPa.
(3) Placing the sheet sample obtained in the step (2) in a tubular furnace, heating to 900 ℃ at the speed of 5 ℃/min under the oxygen atmosphere, and calcining for 4 hours; cooling to room temperature, grinding into powder with molecular formula of Na0.6Mn0.93Ru0.07O2The particle size of the material particles is 0.2-1 μm.
The sodium-ion battery double-transition metal manganese-based positive electrode material prepared in the above way is characterized, and the results are shown in fig. 1-4, and fig. 1 shows the characteristic curve of the layered oxide, which indicates that the sample has a P63/mmc space group structure. FIG. 2 shows that the material is a homogeneous particle with a layered packing structure, the size of the particle being 0.2-1 μm. Figure 3 shows that the material is in a lamellar morphology. Fig. 4 shows that the four elements are uniformly distributed within the material. Fig. 5 shows that no new peak is generated in the X-ray powder diffraction spectrum of the material as charging and discharging progresses, which indicates that the material is a structure evolution mechanism without phase change in a wide voltage range.
The electrochemical performance of the prepared double-transition metal manganese-based layered cathode material of the sodium-ion battery is tested, and the results are shown in fig. 6-9. As can be seen from FIG. 6, the material was at 50mA g-1The first discharge specific capacity under the voltage condition of 1.5-4.5V is 209.3mAh g-1And 3 times of charge-discharge tests are carried out on the material, and the charge-discharge curves of the material are basically overlapped, so that the charge-discharge process of the material is highly reversible. FIG. 7 shows the multiplying power of the material at 5000mA g under different current densities-1Under the condition, the specific capacity still has 97.3mAh g-1. In fig. 8, the upper curve represents the charging and discharging coulombic efficiency, and the lower curve represents the specific capacity of the material, which shows that the specific capacity of the battery still has 75.3% of the original specific capacity after 200 cycles of long charging and discharging, and the coulombic efficiency of the battery is kept above 98% in the long charging and discharging cycles. FIG. 9 shows the total cell capacity at 50mA g after assembly of the material with a hard carbon negative electrode-1First discharge under voltage condition of 1.5-4.5VThe specific capacity of the electrolyte is 101.0mAh g-1And 3 times of charge and discharge tests are carried out on the material, and the charge and discharge curves of the material are basically overlapped, which shows that the charge and discharge process is highly reversible after the material is assembled into a full battery.
Example 2
Changing the molar ratio of each substance, and accurately weighing NaNO with corresponding mass according to the molar ratio of 0.6:0.99:0.013、MnCO3And RuO2The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.6Mn0.99Ru0.01O2。
Example 3
Changing the molar ratio of each substance, and accurately weighing NaNO with corresponding mass according to the molar ratio of 0.6:0.9:0.13、MnCO3And RuO2The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.6Mn0.9Ru0.1O2。
Example 4
Changing the molar ratio of each substance, and accurately weighing NaNO with corresponding mass according to the molar ratio of 0.6:0.8:0.23、MnCO3And RuO2The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.6Mn0.8Ru0.2O2。
Example 5
Changing the molar ratio of each substance, and accurately weighing NaNO with corresponding mass according to the molar ratio of 0.6:0.5:0.53、MnCO3And RuO2The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.6Mn0.5Ru0.5O2。
Example 6
Changing the molar ratio of each substance to accurately weigh NaNO with corresponding mass according to the molar ratio of 0.3:0.93:0.073、MnCO3And RuO2The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.3Mn0.0.93Ru0.07O2。
Example 7
Changing the molar ratio of each substance, and accurately weighing NaNO with corresponding mass according to the molar ratio of 1:0.93:0.073、MnCO3And RuO2The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na1Mn0.0.93Ru0.07O2。
Example 8
RuO in example 12By conversion to equimolar amounts of IrO2The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.6Mn0.93Ir0.07O2。
Example 9
RuO in example 12By substitution with 0.5 molar amount of Sb2O5The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based positive electrode material for sodium ion batteries, the molecular formula of which was Na0.6Mn0.93Sb0.07O2。
Example 10
RuO in example 12By substitution with 0.5 molar amount of Nb2O5The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based positive electrode material for sodium ion batteries, the molecular formula of which was Na0.6Mn0.93Nb0.07O2。
Example 11
RuO in example 12Conversion to equimolar amounts of SnO2The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.6Mn0.93Sn0.07O2。
Example 12
RuO in example 12By exchange with 0.5 molar amount of Ta2O5The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.6Mn0.93Ta0.07O2。
Example 13
RuO in example 12By conversion to Bi in an amount of 0.5 mol2O3The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.6Mn0.93Bi0.07O2。
Example 14
MnCO of example 13By conversion to equimolar amounts of Mn (NO)3)2The method of steps (1) to (3) in example 1 was followed to prepare a double transition metal manganese-based layered positive electrode material for a sodium-ion battery, the molecular formula of which was Na0.6Mn0.93Ru0.07O2。
Example 15
NaNO in example 13The sodium-ion battery double-transition metal manganese-based layered positive electrode material with the molecular formula of Na is prepared by replacing NaCl with equimolar amount and adopting the method of the steps (1) to (3) in the example 10.6Mn0.93Ru0.07O2。
Example 16
The calcination temperature of 900 ℃ in the example 1 is changed to 700 ℃, and the method of the steps (1) to (3) in the example 1 is adopted to prepare the double-transition metal manganese-based layered cathode material of the sodium-ion battery, the molecular formula of which is Na0.6Mn0.93Ru0.07O2。
Example 17
The calcination temperature of 900 ℃ in the example 1 is changed to 1100 ℃, and the method of the steps (1) to (3) in the example 1 is adopted to prepare the double-transition metal manganese-based layered positive electrode material of the sodium-ion battery, the molecular formula of which is Na0.6Mn0.93Ru0.07O2。
Example 18
The calcination atmosphere of oxygen in example 1 is changed into air, and the method of the steps (1) to (3) in example 1 is adopted to prepare the double-transition metal manganese-based layered positive electrode material of the sodium-ion battery, wherein the molecular formula of the double-transition metal manganese-based layered positive electrode material is Na0.6Mn0.93Ru0.07O2。
In conclusion, the material disclosed by the invention is simple in preparation method, rich in raw materials, low in price and high in practicability, and the synthesized anode material is uniform in particle size, is uniform particles with a layered accumulation structure, and has no phase change in a wide voltage range. When the material is assembled into a sodium ion battery, the structural stability of the material in the charging and discharging process can be greatly improved, so that the overall cycle performance of the battery is improved, and the rate capability and specific capacity of the material are also improved to a certain extent. In addition, the material of the invention is assembled into a full cell, and the full cell has excellent electrochemical performance in the charging and discharging processes. Therefore, the material and the preparation method have good application prospects in the aspect of optimizing the performance of the energy storage device of the sodium-ion battery.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, it should be noted that, for those skilled in the art, many modifications and variations can be made without departing from the technical principle of the present invention, and these modifications and variations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A double-transition metal manganese-based layered positive electrode material of a sodium ion battery is characterized in that: having the general formula Na0.6Mn0.93Ru0.07O2；
The positive electrode material is granular, and the grain diameter of the positive electrode material is 0.2-1 mu m;
the preparation method of the double-transition metal manganese-based layered positive electrode material of the sodium ion battery comprises the following steps of:
uniformly mixing sodium salt, manganese salt and other metal oxides, tabletting, calcining at the temperature of 700-1100 ℃, and cooling to obtain the double-transition metal manganese-based layered positive electrode material of the sodium-ion battery; wherein the content of the first and second substances,the manganese salt is MnCO3(ii) a The other metal oxide is selected from RuO2。
2. The sodium-ion battery double-transition metal manganese-based layered cathode material according to claim 1, characterized in that: the crystal structure of the anode material belongs to P63A/mmc or
And (4) space group.
3. The sodium-ion battery double-transition metal manganese-based layered cathode material according to claim 1, characterized in that: the sodium salt is Na2CO3、NaNO3And NaCl.
4. The sodium-ion battery double-transition metal manganese-based layered cathode material according to claim 1, characterized in that: the molar ratio of sodium element, manganese element and other metal elements in the sodium salt, manganese salt and other metal oxides is 0.6:0.93: 0.07.
5. The sodium-ion battery double-transition metal manganese-based layered cathode material according to claim 1, characterized in that: uniformly mixing by adopting a ball milling method, wherein the ball milling speed is 100-.
6. The sodium-ion battery double-transition metal manganese-based layered cathode material according to claim 1, characterized in that: tabletting under 1-50 MPa.
7. The sodium-ion battery double-transition metal manganese-based layered cathode material according to claim 1, characterized in that: the calcination time is 1-50h, and the heating rate is 1-20 ℃/min.
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| CN111180721B (en) * | 2020-01-06 | 2021-05-07 | 山东大学 | Preparation method of layered manganese-based sodium-ion battery positive electrode material |
| CN111268746B (en) * | 2020-02-05 | 2021-04-27 | 中国科学院化学研究所 | Layered positive electrode material of sodium-ion battery, preparation method and application thereof |
| CN114229900B (en) * | 2021-10-26 | 2023-12-12 | 广东邦普循环科技有限公司 | Preparation method of manganese-doped sodium ion battery anode material |
| CN115863559A (en) * | 2022-11-07 | 2023-03-28 | 常熟理工学院 | High-valence metal element modified P2 type sodium ion battery positive electrode material, and preparation method and application thereof |
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| CN104795555A (en) * | 2014-07-28 | 2015-07-22 | 中国科学院物理研究所 | Aqueous-solution sodium-ion battery and cathode material, preparation method and application thereof |
| CN104795552A (en) * | 2014-10-16 | 2015-07-22 | 中国科学院物理研究所 | Layered oxide material, preparation method, pole piece, secondary cell and application |
| CN108140826A (en) * | 2015-05-26 | 2018-06-08 | 尤米科尔公司 | To cathode material of the sodium manganese oxide doping divalent metal as sodium-ion battery |
| CN107644987A (en) * | 2017-09-19 | 2018-01-30 | 北京化工大学 | A kind of high Fe content manganese base sodium-ion battery positive material and preparation method thereof |
| CN107706375A (en) * | 2017-09-25 | 2018-02-16 | 济宁市无界科技有限公司 | The method for preparing manganese base sodium ion composite oxide positive pole material |
| CN109119610A (en) * | 2018-08-20 | 2019-01-01 | 武汉大学 | A kind of alkaline aqueous solution sodium-ion battery |
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