CN110921713A - Sodium manganate smoothing material and preparation method and application thereof - Google Patents
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- 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 the technical field of battery materials, in particular to a sodium manganate smoothing material as well as a preparation method and application thereof. The invention discloses a preparation method of a smooth sodium manganate material, which comprises the steps of forming a coating layer on the surface of sodium manganate, wherein oxide attachments on the surface of the sodium manganate can be taken away by falling off of the coating layer, so as to obtain sodium manganate particles with smooth surfaces, increase the contact area between the surface of the sodium manganate and the outside, improve the conductivity of the surface of the sodium manganate, reduce the resistance of ion deintercalation and intercalation, reduce the positions of SEI films formed after sodium manganate is assembled into a sodium battery, and improve the cycle performance of the battery. The method for removing the oxide attachments on the surface of the sodium manganate is simple and efficient, the cost is low, and the obtained sodium manganate has high added value and wide application prospect and feasibility.
Description
Technical Field
The invention relates to the technical field of battery materials, in particular to a sodium manganate smoothing material as well as a preparation method and application thereof.
Background
The development of science and technology is different day by day, one in daily lifeThe development of energy storage and reasonable energy utilization is the main melody of scientific and technological development. In 1991, sony announced the first commercial Lithium Ion Battery (LIB). Since then, the application of lithium ion batteries in daily life has become more widespread. Compared with other secondary batteries, the battery has the advantages of high LIB voltage, large specific capacity, long cycle life, good safety performance and excellent energy density. However, the materials for lithium ion batteries are relatively expensive (electrolyte is expensive, lithium is expensive, and copper foil is required). As battery applications are gradually moving towards large storage, such as electric buses, high energy density becomes less and less important. Meanwhile, the gradual depletion of lithium source and the abundant reserve of sodium make people pay attention to the development of sodium ion batteries close to lithium ion batteries. Thereby accelerating the development of the positive electrode system of the Na-based ion battery. At present, Na insertion chemistry is much less explored than Li insertion. Early studies showed that structures that do not fully exert the effect of lithium intercalation compounds are likely to be functional. Therefore, finding new electrode materials for NIB is an important link in the development of sodium ion batteries. Layered lithium transition metal oxide LiCoO2And related materials have become the primary positive electrodes of lithium ion batteries. Similarly, the layered Na transition metal compound NaMO2Also exhibit intercalation chemistry. NaFeO in contrast to the lithium analog2And NaCrO2Are electrochemically active. And layered LiMnO2In contrast, NaMnO2The compound can maintain the deintercalation of sodium without converting to a spinel structure.
NaxMnOyThe compound is one of representatives of sodium electric materials, and shows low specific capacity and poor cycle performance. Microscopically, derived from Na+Intrinsic defect-ion radius vs. Li+It is large, which also makes it more resistive into and out of the cell material. Macroscopically, this is due to NaxMnO2The surface of the material is provided with a plurality of oxide impurity particles, so that the contact area of the material and the outside is reduced, and the conductivity is reduced. Therefore, at present, from a microscopic viewpoint, there is a method using Mn site doping, such as Co, Mg doping, Co being able to lower the spinel structure because of a small expansion coefficientSwelling, improving the cyclicity, Mg can improve the valence state of Mn, and inhibit the oxidation of electrolyte, etc. However, from a macroscopic perspective, a method for improving the cycle performance of sodium manganate by surface modification is rarely reported.
Disclosure of Invention
In view of the above, the invention provides a sodium manganate smoothing material, a preparation method and an application thereof, and the preparation method of the sodium manganate smoothing material can efficiently and rapidly remove oxide attachments on the surface of sodium manganate, improve the conductivity of the sodium manganate material, reduce an SEI film of a sodium ion battery, and improve the cycle performance of the sodium ion battery.
The specific technical scheme is as follows:
the invention provides a preparation method of a sodium manganate smoothing material, which comprises the following steps:
step 1: dissolving sodium manganate in a liquid phase to obtain a mixed solution;
step 2: evaporating the liquid in the mixed solution to obtain a mixture;
and step 3: grinding the mixture into powder, sintering in a protective atmosphere, and cooling to obtain a smooth sodium manganate material;
the molecular formula of the sodium manganate is NaxMnOy(ii) a Wherein, 0<x<1，1<y<3, in the embodiment of the invention, the sodium manganate is Na0.7MnO2.05。
The liquid phase is one or more of a copper nitrate aqueous solution, a silver nitrate aqueous solution and a zinc nitrate aqueous solution.
In the invention, the solute in the liquid phase is sintered at high temperature on the surface of the sodium manganate to form an oxide film coating layer. Because the coating layer is thick and is 15-20nm, the coating layer falls off and takes away oxide particles originally attached to the surface of the sodium manganate through rapid cooling, so that the surface of the sodium manganate becomes smooth.
In step 1 of the invention, the preparation method of the sodium manganate specifically comprises the following steps: respectively grinding sodium carbonate and manganous oxide, mixing, preferably ball-milling to obtain a mixture, and preferably sintering in an oxygen atmosphere to obtain sodium manganate; what is needed isThe molar ratio of the sodium carbonate to the manganese sesquioxide is (1:1) to (4:5), preferably 1:1 or 4: 5; the ball-material ratio in the ball milling process is (20:1) - (30:1), preferably 20:1, and the ball milling time is 30-60 min; the sintering is specifically carried out at the temperature rise rate of 10-20 ℃/min to 650-750 ℃; the sodium manganate is preferably Na0.7MnO2.05。
In step 1 of the invention, the liquid phase is preferably an aqueous solution of copper nitrate, and copper oxide cladding is formed on the surface of sodium manganate after copper nitrate is sintered; the preparation method of the liquid phase comprises the following specific steps: putting the solute into deionized water, preferably stirring by adopting magnetons; the stirring time of the magnetons is 10-15 min;
the sodium manganate dissolved in the liquid phase is specifically as follows: putting sodium manganate into liquid phase to carry out water bath heating and magneton stirring; the temperature of the water bath heating is 30-50 ℃, and the stirring time is 30-60 min;
the mass ratio of the solute in the liquid phase to the sodium manganate is (3:100) - (8:100), preferably 5: 100.
In step 2 of the present invention, the liquid evaporation specifically comprises: and (3) heating the water bath to 50-60 ℃ until the liquid is evaporated, wherein the time required by the liquid evaporation is 3-5 h.
In order to further remove the liquid in the mixture completely, after the liquid is evaporated to dryness, the method further comprises the following steps: drying; the drying temperature is 50-60 ℃ and the drying time is 3-5 h.
In step 3 of the invention, the mixture is ground into powder with the particle size of 1.5-2 μm, preferably 2 μm; the protective atmosphere is inert gas; the powder sintering specifically comprises the following steps: heating to 650 plus 750 ℃ at the heating rate of 10-20 ℃/min, and preserving heat for 8-10 h;
the surface of the sodium manganate obtained after the powder is sintered is covered with a coating layer, and oxide particles on the surface of the sodium manganate can be taken away by the coating layer after the sodium manganate is cooled; the cooling time is 4-6h, preferably 4 h.
The invention also provides the sodium manganate smoothing material prepared by the preparation method. After oxide impurities are removed from the sodium manganate material, the surface of the sodium manganate material is smooth, so that the influence of the oxide impurities on the conductivity of the sodium manganate material is avoided, and the electrochemical performance of the sodium manganate material is improved.
The invention also provides a sodium ion battery, which comprises a positive electrode and a negative electrode;
the positive electrode is the sodium manganate material.
According to the technical scheme, the invention has the following advantages:
the invention provides a preparation method of a smooth sodium manganate material, which is characterized in that a coating layer is formed on the surface of sodium manganate, and oxide attachments on the surface of the sodium manganate can be taken away by falling off of the coating layer, so as to obtain sodium manganate particles with smooth surfaces, increase the contact area between the surface of the sodium manganate and the outside, improve the conductivity of the surface of the sodium manganate, reduce the resistance of ion deintercalation and intercalation, reduce the positions of SEI films formed after sodium manganate is assembled into a sodium battery, and improve the cycle performance of the battery. The method for removing the oxide attachments on the surface of the sodium manganate is simple and efficient, the cost is low, and the obtained sodium manganate has high added value and wide application prospect and feasibility.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without inventive exercise.
FIG. 1 is a scanning electron micrograph (1 μm on the scale) of sodium manganate provided in example 1 of the present invention;
FIG. 2 is a scanning electron micrograph (200 nm on scale) of the sodium manganate material provided in example 4 of the present invention;
FIG. 3 is a scanning electron micrograph (1 micron on the scale) of the sodium manganate material provided in example 5 of the present invention;
FIG. 4 is a Mapping line scan under a high resolution transmission electron microscope of the sodium manganate material provided in example 5 of the present invention;
FIG. 5 is a graph comparing the specific capacity and cycling performance of the sodium manganate materials provided in example 1 and example 4 of the present invention;
figure 6 is a graph comparing the impedance of the sodium manganate materials provided in example 1 of the present invention and the sodium permanganate materials provided in example 4 before and after treatment.
Detailed Description
In order to make the objects, features and advantages of the present invention more obvious and understandable, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it should be apparent that the embodiments described below are only a part of the embodiments of the present invention, and not all 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.
Example 1
The sodium manganate Na is adopted in the embodiment0.7MnO2.05Preparation of granules comprising the steps of:
(1) mixing a mixture of 1:1 of Na2CO3And Mn2O3Grinding and mixing the materials together to obtain an initial mixture; then putting the mixture into a 50ml ball milling tank, and carrying out ball milling for 30min according to the ball-material ratio of 20:1 to obtain a final mixture;
(2) placing the mixture obtained in the step (1) in a container, placing the container in a tube furnace, vacuumizing the tube for 3 times, introducing oxygen, filling the tube with oxygen, heating to 650 ℃ at a heating rate of 10 ℃/min, starting sintering, wherein the sintering time is 8 hours, and cooling to obtain a raw material sodium manganate Na0.7MnO2.05(NMO)。
Example 2
The sodium manganate Na is adopted in the embodiment0.7MnO2.05Preparation of granules comprising the steps of:
(1) mixing the components in a molar ratio of 4:5 of Na2CO3And Mn2O3Grinding and mixing the materials together to obtain an initial mixture; the mixture was then placed in a 50ml ball mill jarBall milling for 1h at a ball-to-material ratio of 20:1 to obtain a final mixture;
(2) placing the mixture obtained in the step (1) in a container, placing the container in a tube furnace, vacuumizing the tube for 3 times, introducing oxygen, filling the tube with oxygen, heating to 700 ℃ at a heating rate of 15 ℃/min, starting sintering, wherein the sintering time is 8 hours, and cooling to obtain a raw material, namely sodium manganate Na0.7MnO2.05(NMO)。
Example 3
The sodium manganate Na is adopted in the embodiment0.7MnO2.05Preparation of granules comprising the steps of:
(1) mixing the components in a molar ratio of 4:5 of Na2CO3And Mn2O3Grinding and mixing the materials together to obtain an initial mixture; then putting the mixture into a 50ml ball milling tank, and carrying out ball milling for 1h according to the ball-material ratio of 30:1 to obtain a final mixture;
(2) placing the mixture obtained in the step (1) in a container, placing the container in a tube furnace, vacuumizing the tube for 3 times, introducing oxygen, filling the tube with oxygen, heating to 750 ℃ at the heating rate of 20 ℃/min, starting sintering, wherein the sintering time is 8 hours, and cooling to obtain the raw material sodium manganate Na0.7MnO2.05(NMO)。
Example 4
This example is a preparation of a sodium permanganate material comprising the following steps:
(1) taking a beaker, and taking 3 wt% of copper nitrate (sodium manganate Na)0.7MnO2.05Quality as reference) is put into deionized water, and then a glass rod is used for continuously stirring for 10min to obtain a copper nitrate aqueous solution, and copper nitrate can be thoroughly dissolved into the deionized water;
(2) sodium manganate Na obtained in example 10.7MnO2.05Putting 100mg of the mixture into the aqueous solution of the nitric acid ketone obtained in the step (1), putting magnetons into a glass cup, putting the glass cup into a water bath, and continuously stirring for 30min to obtain a mixed solution, wherein the temperature of the water bath is kept at 30 ℃, and the water level of the water bath is kept at 1/5 of the beaker;
(3) putting the beaker obtained in the step (2) into a water bath kettle, heating, keeping the temperature at 50 ℃, evaporating dry liquid for 3 hours, and continuously adding water until the water level reaches 1/5 of the beaker in the process of evaporating the liquid in the dry beaker, wherein the water level of the water bath kettle is kept unchanged, so that a relatively dry cup bottom mixture is obtained;
(4) putting the beaker in the step (3) into a vacuum oven for drying, exhausting air from the vacuum oven to be in a vacuum state, adjusting the temperature to 50 ℃, keeping for 3 hours, taking out the beaker after drying, and taking out the mixture by using a spoon to obtain a mixture;
(5) and (3) putting the mixture obtained in the step (4) into a mortar, grinding for 30min until powder is obtained, putting the powder into a vessel, putting the vessel into a tube furnace, vacuumizing the tube of the tube furnace for 3 times, introducing argon gas, filling the argon gas into the tube furnace, heating and sintering, wherein the heating rate is 10 ℃/min, heating to 600 ℃ at the heating rate, keeping the temperature for sintering for 8h, opening a furnace cover without setting a cooling program after the sintering program is finished, naturally and rapidly cooling, and cooling for 4h to obtain the smooth sodium manganate material.
Fig. 1 is a scanning electron microscope image of sodium manganate provided in this embodiment. As shown in fig. 1, there are many attachments on the surface of the sodium manganate particles. Fig. 2 is a scanning electron microscope image of the sodium manganate material provided in this embodiment. As shown in fig. 2, the surface of the sodium manganate material was smooth and the adhesion was significantly reduced.
Figure 5 is a graph comparing the specific capacity and cycling performance of the sodium manganate provided in example 1 before and after treatment with the sodium permanganate material provided in this example. As shown in fig. 5, it can be seen that the specific capacity of the treated sodium manganate is significantly improved, and the treated sodium manganate still has a higher specific capacity after being cycled for a plurality of cycles.
Figure 6 is a graph comparing the impedance of the sodium manganate provided in example 1 with the sodium permanganate material provided in this example before and after treatment. As shown in fig. 6, there is a significant decrease in the resistance of the sodium permanganate material, whether to form an SEI film or the resistance of the entire battery material.
Example 5
This example is a preparation of a sodium permanganate material comprising the following steps:
(1) taking a beaker, and taking 5 wt% of copper nitrate(with sodium manganate Na0.7MnO2.05Quality as reference) is put into deionized water, and then a glass rod is used for continuously stirring for 12min to obtain a copper nitrate water solution, and the copper nitrate can be thoroughly dissolved into the deionized water;
(2) sodium manganate Na obtained in example 20.7MnO2.05Putting 100mg of the mixed solution into the copper nitrate aqueous solution obtained in the step (1), putting magnetons into a glass cup, putting the glass cup into a water bath kettle, and continuously stirring for 30min to obtain a mixed solution, wherein the temperature of the water bath kettle is kept at 40 ℃, and the water level of the water bath kettle is kept at 1/5 of the beaker;
(3) putting the beaker obtained in the step (2) into a water bath kettle, heating, keeping the temperature at 55 ℃, evaporating dry liquid for 4 hours, and continuously adding water until the water level reaches 1/5 of the beaker in the process of evaporating the liquid in the dry beaker, wherein the water level of the water bath kettle is kept unchanged, so that a relatively dry cup bottom mixture is obtained;
(4) putting the beaker in the step (3) into a vacuum oven for drying, exhausting air from the vacuum oven to be in a vacuum state, adjusting the temperature to 55 ℃, keeping for 3 hours, taking out the beaker after drying, and taking out the mixture by using a spoon to obtain a mixture;
(5) and (3) putting the mixture obtained in the step (4) into a mortar, grinding for 30min until powder is obtained, then putting the vessel into a tube furnace, vacuumizing the tube of the tube furnace for 3 times, introducing argon gas to fill inert gas in the tube furnace, heating up and sintering at a heating rate of 15 ℃/min, heating up to 650 ℃ at the heating rate, keeping the temperature for sintering for 9h, opening a furnace cover without setting a cooling program after the sintering program is finished, naturally and rapidly cooling for 5h to obtain the smooth sodium manganate material.
Fig. 3 is a scanning electron microscope image of the sodium manganate material provided in this embodiment. As shown in fig. 2, the surface of the sodium manganate material was smooth and the adhesion was significantly reduced.
Fig. 4 is a Mapping line scan of the sodium manganate material provided in this example observed under a high resolution transmission electron microscope. As the direction of line scanning was seen to be more Na oxide at the edge portion of the grain, and the two edge portions had different Na oxide contents, it was seen that a part of Na oxide had been removed.
Example 6
This example is a preparation of a sodium permanganate material comprising the following steps:
(1) taking a beaker, and taking 8% copper nitrate (sodium manganate Na)0.7MnO2.05Quality as reference) is put into deionized water, and then a glass rod is used for continuously stirring for 15min to obtain a copper nitrate water solution, and the copper nitrate can be thoroughly dissolved into the deionized water;
(2) sodium manganate Na obtained in example 30.7MnO2.05Putting 100mg of the powder into the copper nitrate aqueous solution obtained in the step (1), putting magnetons into a glass cup, putting the glass cup into a water bath kettle, and continuously stirring for 30min to obtain a solution, wherein the temperature of the water bath kettle is kept at 50 ℃, and the water level of the water bath kettle is kept at 1/4 parts of a beaker;
(3) putting the beaker obtained in the step (2) into a water bath kettle, heating, keeping the temperature at 60 ℃, evaporating dry liquid for 5 hours, and continuously adding water until the water level reaches 1/4 of the beaker in the process of evaporating the liquid in the dry beaker, wherein the water level of the water bath kettle is kept unchanged, so that a relatively dry cup bottom mixture is obtained;
(4) putting the beaker in the step (3) into a vacuum oven for drying, exhausting air from the vacuum oven to be in a vacuum state, adjusting the temperature to 60 ℃, keeping for 5 hours, taking out the beaker after drying, and taking out the mixture by using a spoon to obtain a mixture;
(5) and (3) putting the mixture obtained in the step (4) into a mortar, grinding for 30min until powder is obtained, putting the vessel into a tube furnace, vacuumizing the tube of the tube furnace for 3 times, introducing argon gas to fill inert gas in the tube furnace, heating up and sintering at a heating rate of 20 ℃/min, heating up to 700 ℃ at the heating rate, keeping the temperature for sintering for 10h, opening a furnace cover without setting a cooling program after the sintering program is finished, naturally and rapidly cooling for 6h to obtain the smooth sodium manganate.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some technical features may be equivalently replaced; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the sodium manganate smoothing material is characterized by comprising the following steps of:
step 1: dissolving sodium manganate in a liquid phase to obtain a mixed solution;
step 2: evaporating the liquid in the mixed solution to obtain a mixture;
and step 3: grinding the mixture into powder, sintering in a protective atmosphere, and cooling to obtain a smooth sodium manganate material;
the molecular formula of the sodium manganate is NaxMnOyWherein, 0<x<1，1<y<3；
The liquid phase is one or more of a copper nitrate aqueous solution, a silver nitrate aqueous solution and a zinc nitrate aqueous solution.
2. The method of claim 1, wherein the cooling time is 4-6 hours.
3. The method according to claim 1, wherein the sintering is in particular: heating to 650 plus 750 ℃ at the heating rate of 10-20 ℃/min, and preserving the heat for 8-10 h.
4. The production method according to claim 1, wherein the mass ratio of the solute in the liquid phase to the sodium manganate is (3:100) to (8: 100).
5. The method according to claim 1, wherein the liquid is evaporated at a temperature of 50-60 ℃ for 3-5 hours.
6. The method according to claim 1, wherein the powder has a particle size of 1.5 to 2 μm.
7. The method of claim 1, wherein the protective atmosphere is an inert gas.
8. The method according to claim 1, wherein the method further comprises, after evaporating the liquid to dryness: drying;
the drying temperature is 50-60 ℃ and the drying time is 3-5 h.
9. The sodium manganate smoothing material prepared by the preparation method of any one of claims 1 to 8.
10. A sodium ion battery is characterized by comprising a positive electrode and a negative electrode;
the positive electrode is the sodium permanganate material of claim 9.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114655991A (en) * | 2022-03-24 | 2022-06-24 | 西北工业大学深圳研究院 | Modified sodium manganate material and preparation method and application thereof |
| CN117902631A (en) * | 2024-03-14 | 2024-04-19 | 新乡学院 | Layered metal oxide Na0.7MnO2.05And a method for preparing the same |
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2019
- 2019-12-10 CN CN201911261614.4A patent/CN110921713A/en active Pending
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114655991A (en) * | 2022-03-24 | 2022-06-24 | 西北工业大学深圳研究院 | Modified sodium manganate material and preparation method and application thereof |
| CN114655991B (en) * | 2022-03-24 | 2024-01-09 | 西北工业大学深圳研究院 | Modified sodium manganate material and preparation method and application thereof |
| CN117902631A (en) * | 2024-03-14 | 2024-04-19 | 新乡学院 | Layered metal oxide Na0.7MnO2.05And a method for preparing the same |
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