CN114180633B - Preparation method and application of sodium manganate - Google Patents
Preparation method and application of sodium manganate Download PDFInfo
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- CN114180633B CN114180633B CN202010965228.XA CN202010965228A CN114180633B CN 114180633 B CN114180633 B CN 114180633B CN 202010965228 A CN202010965228 A CN 202010965228A CN 114180633 B CN114180633 B CN 114180633B
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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
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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
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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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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- 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
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Abstract
The application discloses a preparation method of sodium manganate, which at least comprises the following steps: a) heating and complexing an aqueous solution containing a manganese source and sodium citrate to obtain gel; b) drying the gel to obtain a precursor; c) and grinding the precursor, and calcining to obtain the sodium manganate. The sodium manganate has simple preparation process and simple material composition, and is suitable for mass production. Meanwhile, the sodium manganate material is applied to the positive electrode of a sodium ion battery and can show excellent long-cycle performance and rate capability.
Description
Technical Field
The invention relates to a preparation method and application of sodium manganate, and belongs to the field of sodium ion batteries.
Background
In recent years, energy storage devices, represented by lithium ion batteries, have been widely studied and applied to various electronic devices, and the demand for lithium resources has been increasing dramatically, resulting in a significant increase in the cost of lithium batteries. Sodium is abundant and widely distributed, and the natural abundance of sodium is more than 1000 times that of lithium, so that a Sodium Ion Battery (SIB) is considered as an economical and efficient substitute of a lithium ion battery.
However, the energy density of sodium ion batteries has so far been relatively low. The electrochemical energy density of a sodium-ion battery depends to a large extent on the inherent chemical properties of the positive electrode material. In order to improve the energy density of the battery, obtaining a proper cathode material is the key point for improving the specific capacity.
The need for the cathode material is a compromise between the cost of the raw materials, considering cost considerations. Manganese is a transition metal with abundant content, low cost and low toxicity on the earth. Among various cathode materials that have been studied, layered sodium transition metal oxide (Na) x TMO 2 ) Particularly manganese-based materials, are believed to have the potential to meet the above requirements and therefore have application in sodium ion batteriesHas great prospect. However, Na has been reported so far x MnO 2 Further optimization is needed because it exhibits poor rate capability and fast capacity fade without Na + diffusion pathways and complex phase transition processes.
Disclosure of Invention
According to one aspect of the application, the preparation method of the sodium manganate is provided, the sodium manganate with good crystallinity and excellent electrochemical performance can be obtained, and the preparation method is simple and is easy for large-scale production.
A preparation method of sodium manganate comprises the following steps:
a) heating and complexing an aqueous solution containing a manganese source and sodium citrate to obtain gel;
b) drying the gel to obtain a precursor;
c) and grinding the precursor, and calcining to obtain the sodium manganate.
Optionally, the sodium manganate is a single crystal.
Optionally, the crystal grain size of the sodium manganate is 5-30 μm.
Optionally, the sodium manganate has Na 0.7 MnO 2.05 And (5) crystal structure.
Optionally, the sodium manganate has a layered structure.
Optionally, in step a), the manganese source is selected from at least one of manganese acetate, manganese sulfate, manganese hydroxide and manganese phosphate.
Optionally, in the step a), the molar ratio of the sodium citrate to the manganese source in the aqueous solution containing the manganese source and the sodium citrate is 0.5-1.5: 1;
wherein the molar quantity of the manganese source is calculated by the mole number of manganese element contained in the manganese source;
the molar amount of sodium citrate is calculated as its own number of moles.
Optionally, the upper limit of the molar ratio of the sodium citrate to the manganese source is selected from 0.6: 1. 0.8: 1. 1: 1. 1.1: 1. 1.2: 1. 1.3: 1 or 1.5: 1; the lower limit is selected from 0.5: 1. 0.6: 1. 0.8: 1. 1: 1. 1.1: 1. 1.2: 1 or 1.3: 1.
optionally, in the aqueous solution containing the manganese source and the sodium citrate in the step a), the content of water can be selected according to actual conditions, and the manganese source and the sodium citrate can be dissolved.
Optionally, in step a), the heat complexing conditions are: stirring at 60-100 ℃; the stirring speed is 300-1000 rpm. As an embodiment, the step a) includes: and (3) dissolving sodium citrate matched with a manganese source into an aqueous solution, and heating and stirring by using an oil bath to obtain the gel.
Optionally, in the step b), the drying temperature is 100-180 ℃.
Optionally, the upper limit of the temperature of the drying is selected from 110 ℃, 120 ℃, 130 ℃, 140 ℃, 150 ℃, 160 ℃, 170 ℃ or 180 ℃; the lower limit is selected from 100 deg.C, 110 deg.C, 120 deg.C, 130 deg.C, 140 deg.C, 150 deg.C, 160 deg.C or 170 deg.C.
Alternatively, in step c), the calcination is a two-stage calcination; the first stage of calcination is presintering, the temperature is 350-450 ℃, and the presintering time is 4-12 hours; and the second stage of calcination is carried out at the temperature of 750-950 ℃ for 6-24 hours.
Optionally, in step c), the upper limit of the temperature of the first stage pre-sintering is selected from 360 ℃, 370 ℃, 380 ℃, 390 ℃, 400 ℃, 410 ℃, 420 ℃, 430 ℃, 440 ℃ or 450 ℃; the lower limit is selected from 350 deg.C, 360 deg.C, 370 deg.C, 380 deg.C, 390 deg.C, 400 deg.C, 410 deg.C, 420 deg.C, 430 deg.C, or 440 deg.C.
Optionally, in step c), the upper limit of the first prefiring time is selected from 6h, 8h, 10h or 12 h; the lower limit is selected from 4h, 6h, 8h or 10 h.
Optionally, in step c), the upper limit of the temperature of the second stage calcination is selected from 775 ℃, 800 ℃, 825 ℃, 850 ℃, 875 ℃, 900 ℃, 925 ℃ or 950 ℃; the lower limit is selected from 750 deg.C, 775 deg.C, 800 deg.C, 825 deg.C, 850 deg.C, 875 deg.C, 900 deg.C or 925 deg.C.
Alternatively, in step c), the upper limit of the time for the second stage calcination is selected from 8h, 12h, 16h, 20h or 24 h; the lower limit is selected from 6h, 8h, 12h, 16h or 20 h.
As an embodiment, in the step c), the calcination mode is divided into two stages, the calcination is performed firstly at a temperature of 350 to 450 ℃ for 4 to 12 hours, and then the calcination is performed at a temperature of 750 to 950 ℃ for 6 to 24 hours.
According to another aspect of the application, the application of the sodium manganate prepared according to any one of the preparation methods in batteries is provided.
Optionally, the battery is a sodium ion battery.
The beneficial effects that this application can produce include:
the preparation method provided by the application is simple, the raw material composition is simple, no complexing agent is required to be added, and the prepared sodium manganate has good crystallinity, excellent cycle performance and rate capability. The preparation method of the sodium manganate has the advantages of low cost, good economic benefit, contribution to industrial application and good application prospect in sodium ion batteries.
Drawings
FIG. 1 is a scanning electron micrograph of sodium manganate produced in example 1 of the present invention.
FIG. 2 is an enlarged scanning electron micrograph of sodium manganate produced in example 1 of the present invention.
Figure 3 is an XRD pattern of sodium manganate prepared in example 1 of the present invention.
FIG. 4 shows the sodium manganate half-cell prepared in example 1 of the present invention at 100 mA g -1 The current density of the current-voltage converter is in a cycle performance diagram, wherein the voltage range is 2-4V.
Fig. 5 is a rate cycle curve of the sodium manganate half-cell prepared in example 1 of the present invention, wherein the voltage range is 2-4V.
Detailed Description
The present application will be described in detail with reference to examples, but the present application is not limited to these examples.
The raw materials in the examples of the present application were all purchased commercially, unless otherwise specified.
The analytical methods in the examples of the present application are as follows:
the analysis and test of the sample morphology were carried out using scanning electron microscopy (SEM, JSM-7800F).
Analytical testing of the composition of the crystalline phases of the samples was carried out using an X-ray diffractometer (XRD, X' pert Pro).
Constant current charge/discharge tests were performed using a battery system (blue electronic, inc., wuhan) using the LAND CT 2001A.
Example 1
0.01mol of manganese acetate is added into 40mL of deionized water, and the mixture is heated and stirred for 1h at 80 ℃. Then 0.01mol of sodium citrate dihydrate is added and stirred for 2h at 80 ℃ and the stirring speed is 300 rpm. Then, the temperature was raised to 100 ℃ and the stirring speed was 500rpm, and the mixture was stirred until the solution became gel-like. Then the mixture is moved into an oven and dried at 120 ℃. And uniformly grinding the dried precursor. Then, a muffle furnace is used for heat treatment, and the sample is treated by using a sectional heating mode. Firstly heating to 350 ℃, preserving heat for 4 hours, then heating to 950 ℃, and preserving heat for 24 hours. To obtain the sodium manganate product.
As can be seen from a scanning electron micrograph (SEM, 10 mu m) shown in the attached figure 1, the prepared sodium manganate is a single crystal, and the grain size is 5-30 mu m; as can be seen from the scanning electron micrograph (SEM, 1 μm) of FIG. 2, the prepared sodium manganate has a layered structure. As can be seen by the X-ray diffraction pattern (XRD) of FIG. 3, the sodium manganate produced has Na 0.7 MnO 2.05 Crystal structure and good crystallinity.
The sodium manganate prepared in this example was used as the positive electrode of a sodium ion battery, and combined with a sodium metal negative electrode to form a half-cell, and the electrolyte was a Propylene Carbonate (PC) solution of 1m naclo4, which contained 5% fluoroethylene carbonate (FEC), and the separator was a glass fiber separator. And testing the electrochemical performance of the prepared sodium manganate. As can be seen from FIG. 4, at 100 mA g -1 The first discharge specific capacity of the prepared sodium manganate is 170.8 mAh g -1 After 200 cycles, the capacity still remains 111.5 mAh g -1 The capacity retention rate is 65.28%, and the cycle stability is excellent. The rate tests were performed on the prepared sodium manganate half cells, which can also be seen in fig. 5 at 100, 200, 400, 1000, 2000 and 4000 mA g -1 The average specific capacity of the battery is 163.89, 136.33, 118.97, 102.15, 86.01, 77.5 and 69.18mAh respectivelyg -1 . The prepared sodium manganate has excellent rate performance.
Example 2
0.1mol of manganese acetate is added into 100mL of deionized water, and the mixture is heated and stirred for 1h at 80 ℃. Then 0.12mol of sodium citrate dihydrate is added and stirred for 2h at 80 ℃ and the stirring speed is 500 rpm. Then, the temperature was raised to 100 ℃ and the stirring speed was 500rpm, and the mixture was stirred until the solution became gel-like. Then the mixture is moved into an oven and dried at 150 ℃. And uniformly grinding the dried precursor. Then, the sample is treated by a muffle furnace heat treatment and a sectional heating mode. Heating to 350 deg.C, holding for 4 hr, heating to 800 deg.C, and holding for 24 hr. To obtain the sodium manganate product. SEM, XRD and electrical property measurements of the product prepared in example 2 were similar to those of the sample prepared in example 1.
Example 3
0.1mol of manganese sulfate is added into 100mL of deionized water, and the mixture is heated and stirred for 1h at 90 ℃. Then 0.12mol of sodium citrate dihydrate is added and stirred for 2h at 90 ℃ and the stirring speed is 500 rpm. Then, the temperature was raised to 100 ℃ and the stirring speed was 500rpm, and the mixture was stirred until the solution became gel-like. Then the mixture is moved into an oven and dried at 120 ℃. And uniformly grinding the dried precursor. Then, the sample is subjected to heat treatment by using an argon atmosphere, and the sample is treated by using a sectional heating mode. Heating to 400 deg.C, holding for 4 hr, heating to 850 deg.C, and holding for 12 hr. To obtain the sodium manganate product. SEM, XRD and electrical property measurements of the product prepared in example 3 were all similar to those of the sample prepared in example 1.
Example 4
0.1mol of manganese acetate is added into 100mL of deionized water, and the mixture is heated and stirred for 1h at 80 ℃. Then 0.06mol of sodium citrate dihydrate is added and stirred for 2h at 80 ℃ and the stirring speed is 500 rpm. Then, the temperature was raised to 100 ℃ and the stirring speed was 500rpm, and the mixture was stirred until the solution became gel-like. Then the mixture is moved into an oven and dried at 120 ℃. And uniformly grinding the dried precursor. Then, the sample is treated by using a stage heating mode through heat treatment in an argon atmosphere. Heating to 350 deg.C, holding for 4 hr, heating to 950 deg.C, and holding for 12 hr. To obtain the sodium manganate product. SEM, XRD and electrical property measurements of the product prepared in example 4 were all similar to the sample prepared in example 1.
Example 5
0.1mol of manganese acetate is added into 100mL of deionized water, and the mixture is heated and stirred for 1h at 80 ℃. Then 0.15 mol of sodium citrate dihydrate is added and stirred for 2h at 80 ℃ and the stirring speed is 1000 rpm. Then, the temperature was raised to 100 ℃ and the stirring speed was 500rpm, and the mixture was stirred until the solution became gel-like. Then the mixture is moved into an oven and dried at 180 ℃. And uniformly grinding the dried precursor. Then, the sample is subjected to heat treatment by using an argon atmosphere, and the sample is treated by using a sectional heating mode. Firstly heating to 450 ℃, preserving heat for 4 hours, then heating to 750 ℃, and preserving heat for 12 hours. To obtain the sodium manganate product. SEM, XRD and electrical property measurements of the product prepared in example 5 were all similar to the sample prepared in example 1.
Although the present invention has been described with reference to a few preferred embodiments, it should be understood that various changes and modifications can be made without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (5)
1. The preparation method of sodium manganate is characterized by comprising the following steps:
a) heating and complexing a manganese source and an aqueous solution of sodium citrate to obtain gel;
b) drying the gel to obtain a precursor;
c) grinding the precursor, and calcining to obtain the sodium manganate;
the calcination is two-stage calcination; the first stage of calcination is presintering, the temperature is 350-450 ℃, and the presintering time is 4-12 hours; the second stage of calcination, the temperature is 750-950 ℃, and the calcination time is 6-24 hours;
in the step a), the manganese source is selected from at least one of manganese acetate, manganese sulfate, manganese hydroxide and manganese phosphate;
in the step a), the molar ratio of the sodium citrate to the manganese source in the aqueous solution of the manganese source and the sodium citrate is 0.5-1.5: 1;
wherein the molar quantity of the manganese source is calculated by the mole number of manganese element contained in the manganese source;
the molar amount of the sodium citrate is calculated by the number of moles of the sodium citrate;
in the step a), the heating and complexing conditions are as follows: stirring at 60-100 ℃; the stirring speed is 300-1000 rpm;
the sodium manganate has Na 0.7 MnO 2.05 A crystal form structure;
the sodium manganate has a layered structure.
2. The method of claim 1, wherein the sodium manganate is a single crystal.
3. The method for preparing sodium manganate according to claim 1, wherein the crystal grain size of said sodium manganate is 5 to 30 μm.
4. The method for preparing sodium manganate according to claim 1, wherein the drying temperature in step b) is 100-180 ℃.
5. Use of sodium manganate produced by the production method according to any of claims 1 to 4 in sodium ion batteries.
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