CN112978702A - Preparation method and application of carbon-coated sodium vanadium phosphate - Google Patents
Preparation method and application of carbon-coated sodium vanadium phosphate Download PDFInfo
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- CN112978702A CN112978702A CN201911276157.6A CN201911276157A CN112978702A CN 112978702 A CN112978702 A CN 112978702A CN 201911276157 A CN201911276157 A CN 201911276157A CN 112978702 A CN112978702 A CN 112978702A
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- C01B25/00—Phosphorus; Compounds thereof
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- C01B25/26—Phosphates
- C01B25/45—Phosphates containing plural metal, or metal and ammonium
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- H—ELECTRICITY
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Abstract
The application discloses a preparation method of carbon-coated sodium vanadium phosphate, which comprises the following steps: a) heating and complexing an aqueous solution containing a phosphorus source, a vanadium source and sodium citrate to obtain gel; b) drying the gel to obtain a precursor; c) and grinding the precursor, and calcining in an inactive atmosphere to obtain the carbon-coated sodium vanadium phosphate. The carbon-coated sodium vanadium phosphate has the advantages of simple preparation process, simple raw material composition and suitability for mass production. Meanwhile, the carbon-coated vanadium sodium phosphate material is applied to the positive electrode of the sodium-ion battery, and can show excellent long-cycle performance and rate performance.
Description
Technical Field
The invention relates to the field of sodium ion batteries, and in particular relates to a preparation method of a carbon-coated vanadium sodium phosphate positive electrode material of a sodium ion battery.
Background
Due to the low cost and wide availability of sodium resources, and the similarities between sodium ion batteries and lithium ion batteries in terms of chemical properties, intercalation characteristics and the like, battery technologies based on sodium ion batteries are rapidly developed and become one of the most promising alternatives for lithium ion batteries.
However, sodium ion batteries also have certain disadvantages, the most important of which is the relatively low energy density. Sodium has a greater relative atomic mass (Mw 23.0g mol) than lithium-1) And higher redox potential (psi Na)+/Na＝-2.71V vs.SHE；ψLi+-3.04V vs. she). In order to improve the energy density of the battery, obtaining a proper cathode material is the key point for improving the specific capacity.
Among all positive electrode materials for sodium ion batteries, polyanionic phosphates having NASICON (Na super ion conductor) structure are due to their rapid Na during electrochemical charge and discharge+Diffusion and stable structures are of great interest. Among them, sodium vanadium phosphate has a high specific capacity (117.6mAh/g) and a high voltage plateau (-3.4V), and is considered to be one of the most promising positive electrode materials for sodium ion batteries.
However, pure sodium vanadium phosphate has significant drawbacks, such as poor electronic conductivity, which severely hampers its practical application.
Disclosure of Invention
According to one aspect of the application, the preparation method of the carbon-coated sodium vanadium phosphate is provided, the carbon-coated sodium vanadium phosphate with good crystallinity and excellent electrochemical performance is obtained, and the preparation method is simple and is easy for large-scale production.
The preparation method of the carbon-coated sodium alum phosphate is characterized by comprising the following steps:
a) heating and complexing an aqueous solution containing a phosphorus source, a vanadium source and sodium citrate to obtain gel;
b) drying the gel to obtain a precursor;
c) and grinding the precursor, and calcining in an inactive atmosphere to obtain the carbon-coated sodium vanadium phosphate.
Optionally, the inert atmosphere is selected from at least one of nitrogen, helium, neon, argon. The non-reactive atmosphere acts as a protective atmosphere.
Optionally, the sodium citrate simultaneously functions as a sodium source, a carbon source, a complexing agent, and a reducing agent, without using other additional carbon sources, complexing agents, and reducing agents or reducing atmospheres.
Optionally, the carbon-coated sodium phosphate has a NASICON structure;
the sodium vanadium phosphate in the carbon-coated sodium vanadium phosphate is a crystal.
Optionally, the carbon-coated sodium vanadium phosphate has a 3D porous structure.
Optionally, the pore diameter of the pore structure in the carbon-coated sodium vanadium phosphate is 10-800 nm.
Optionally, in step a), the phosphorus source comprises at least one of diammonium hydrogen phosphate, ammonium dihydrogen phosphate, and phosphoric acid.
Optionally, in step a), the vanadium source includes at least one of ammonium metavanadate, vanadium pentoxide, vanadium oxalate hydrate, and vanadium chloride.
Optionally, in the step a), the molar ratio of the sodium citrate to the vanadium source to the phosphorus source in the aqueous solution containing the phosphorus source, the vanadium source and the sodium citrate is 3.0-3.6: 2: 3.
optionally, in the step a), the molar ratio of the sodium citrate to the vanadium source to the phosphorus source in the aqueous solution containing the phosphorus source, the vanadium source and the sodium citrate is 3.0-3.2: 2: 3.
optionally, in the aqueous solution containing the phosphorus source, the vanadium source and the sodium citrate in the step a), the content of water may be selected according to actual conditions, and the phosphorus source, the vanadium source and the sodium citrate may 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) using sodium citrate to match a phosphorus source and a vanadium source, and heating and stirring in an oil bath in an aqueous solution to obtain the gel.
Optionally, the oil bath temperature is 60-180 ℃, and the stirring speed is 300-1000 rpm.
Optionally, in the step b), the drying temperature is 100-180 ℃.
Alternatively, in step c), the calcination is a two-stage calcination; pre-burning for the first period at 350-450 ℃ for 4-8 hours; and the second stage of calcination is carried out at the temperature of 750-950 ℃ for 6-12 hours.
Optionally, in step c), the upper limit of the temperature of the first stage pre-firing is selected from 400 ℃ or 450 ℃; the lower limit is selected from 350 ℃ or 450 ℃.
Optionally, in step c), the upper limit of the first burn-in period is selected from 6h or 8 h; the lower limit is selected from 4h or 6 h.
Optionally, in step c), the upper limit of the temperature of the second stage calcination is selected from 750 ℃, 800 ℃, 850 ℃, 900 ℃ or 950 ℃; the lower limit is selected from 750 deg.C, 800 deg.C, 850 deg.C or 900 deg.C.
Alternatively, in step c), the upper limit of the time for the second stage calcination is selected from 6h, 8h, 10h or 12 h; the lower limit is selected from 6h, 8h or 10 h.
In one embodiment, in step c), the atmosphere for protecting the calcination is argon, and a reducing atmosphere such as hydrogen is not required. The calcination mode is divided into two sections, pre-sintering is firstly carried out at the temperature of 350-450 ℃ for 4-8 hours, and then calcination is carried out at the temperature of 750-950 ℃ for 6-12 hours.
According to another aspect of the present application, there is provided a use of the carbon-coated sodium vanadium phosphate prepared according to any one of the above-described preparation methods in a battery.
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, an additional carbon source, a complexing agent and a reducing agent or reducing atmosphere are not needed, and the prepared carbon-coated sodium vanadium phosphate has good crystallinity, excellent cycle performance and rate capability.
Drawings
Fig. 1 is a scanning electron microscope image of carbon-coated sodium vanadium phosphate prepared in example 1 of the present invention.
Fig. 2 is an XRD pattern of carbon-coated sodium vanadium phosphate prepared in example 1 of the present invention.
Fig. 3 is a graph of the cycle performance of the carbon-coated sodium vanadium phosphate half-cell prepared in example 1 of the present invention at a current density of 1C, wherein the voltage window is 2.5-3.8V, and 1C is 117.6 mAh/g.
Fig. 4 is a rate cycle curve of the carbon-coated sodium vanadium phosphate half-cell prepared in example 1 of the present invention, wherein the voltage window is 2.5-3.8V, and 1C is 117.6 mAh/g.
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 analysis method in the examples of the present application is 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
0.02mol of ammonium metavanadate is added into 40mL of deionized water, and the mixture is heated and stirred for 1h at 80 ℃. Then, 0.03mol of ammonium dihydrogen phosphate and 0.01mol of sodium citrate dihydrate were added thereto, and stirred at 80 ℃ for 2 hours at a stirring speed of 300 rpm. Then, the temperature was raised to 120 ℃ 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 350 deg.C, holding for 4 hr, heating to 800 deg.C, and holding for 8 hr. Obtaining the carbon-coated sodium vanadium phosphate product.
As can be seen from a Scanning Electron Microscope (SEM) image shown in the attached figure 1, the prepared carbon-coated sodium vanadium phosphate has a 3D porous structure, and the pore diameter of the porous structure is 10-800 nm. As can be seen from the X-ray diffraction pattern (XRD) of FIG. 2, the prepared carbon-coated sodium vanadium phosphate has a NASICON structure and has good crystallinity.
The carbon-coated sodium vanadium phosphate prepared in the embodiment is used as the positive electrode of the sodium ion battery, and forms a half battery with the sodium metal negative electrode, and the electrochemical performance of the prepared carbon-coated sodium vanadium phosphate is tested. As can be seen from the attached figure 3, under the current density of 1C, the first discharge specific capacity of the prepared carbon-coated sodium vanadium phosphate is 92.8mAh/g, after 500 cycles, the capacity is still 85.8mAh/g, the capacity retention rate is 92.46%, and the carbon-coated sodium vanadium phosphate has excellent cycle stability. The rate test is carried out on the prepared carbon-coated sodium vanadium phosphate half-cell, and the specific discharge capacity of the cell under the current densities of 1C, 2C, 5C, 10C, 20C, 30C and 50C is 91.01, 90.38, 86.34, 82.19, 76.83, 72.31 and 68.07mAh/g respectively as can also be seen in the attached figure 4. The prepared carbon-coated vanadium sodium phosphate has excellent rate performance.
Example 2
0.2mol of ammonium metavanadate is added into 100mL of deionized water, and the mixture is heated and stirred for 1h at 80 ℃. Then, 0.3mol of ammonium dihydrogen phosphate and 0.12mol of sodium citrate dihydrate were added and stirred at 80 ℃ for 2 hours at a stirring speed of 500 rpm. Then, the temperature was raised to 120 ℃ 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 350 deg.C, holding for 4 hr, heating to 800 deg.C, and holding for 8 hr. Obtaining the carbon-coated sodium vanadium phosphate 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 vanadium pentoxide is added into 100mL of deionized water, and the mixture is heated and stirred for 1h at 90 ℃. Then, 0.3mol of diammonium hydrogen phosphate and 0.12mol of sodium citrate dihydrate were added and stirred at 90 ℃ for 2 hours at a stirring speed of 500 rpm. Then, the temperature was raised to 120 ℃ 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 8 hr. Obtaining the carbon-coated sodium vanadium phosphate 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.
Although the present application has been described with reference to a few embodiments, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the application as defined by the appended claims.
Claims (10)
1. A preparation method of carbon-coated sodium vanadium phosphate is characterized by comprising the following steps:
a) heating and complexing an aqueous solution containing a phosphorus source, a vanadium source and sodium citrate to obtain gel;
b) drying the gel to obtain a precursor;
c) and grinding the precursor, and calcining in an inactive atmosphere to obtain the carbon-coated sodium vanadium phosphate.
2. The method of preparing carbon-coated sodium vanadium phosphate according to claim 1, wherein the carbon-coated sodium vanadium phosphate has a NASICON structure;
the sodium vanadium phosphate in the carbon-coated sodium vanadium phosphate is a crystal.
3. The method of claim 1, wherein the carbon-coated sodium phosphate has a 3D porous structure.
4. The method of claim 1, wherein in step a), the phosphorus source comprises at least one of diammonium phosphate, ammonium dihydrogen phosphate, and phosphoric acid.
5. The method according to claim 1, wherein in step a), the vanadium source comprises at least one of ammonium metavanadate, vanadium pentoxide, vanadium oxalate hydrate, and vanadium chloride.
6. The method for preparing carbon-coated sodium vanadium phosphate according to claim 1, wherein in the step a), the molar ratio of the sodium citrate to the vanadium source to the phosphorus source in the aqueous solution containing the phosphorus source, the vanadium source and the sodium citrate is 3.0-3.6: 2: 3.
7. the method for preparing carbon-coated sodium vanadium phosphate according to claim 1, wherein in step a), the heating and complexing conditions are as follows: stirring at 60-100 ℃; the stirring speed is 300-1000 rpm.
8. The method for preparing carbon-coated sodium vanadium phosphate according to claim 1, wherein the drying temperature in step b) is 100 to 180 ℃.
9. The method of claim 1, wherein the calcination is a two-stage calcination; pre-burning for the first period at 350-450 ℃ for 4-8 hours; and the second stage of calcination is carried out at the temperature of 750-950 ℃ for 6-12 hours.
10. Use of carbon-coated sodium vanadium phosphate prepared by the preparation method according to any one of claims 1 to 9 in a battery.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113526485A (en) * | 2021-09-15 | 2021-10-22 | 中南大学 | Porous sodium vanadium fluorophosphate composite material regulated and controlled by carbon quantum dots and preparation method and application thereof |
| CN114300660A (en) * | 2021-12-23 | 2022-04-08 | 大连博融新材料有限公司 | Polypyrrole coated carbon-doped sodium vanadium phosphate positive electrode material, and preparation method and application thereof |
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| CN113526485A (en) * | 2021-09-15 | 2021-10-22 | 中南大学 | Porous sodium vanadium fluorophosphate composite material regulated and controlled by carbon quantum dots and preparation method and application thereof |
| CN113526485B (en) * | 2021-09-15 | 2021-12-28 | 中南大学 | Porous sodium vanadium fluorophosphate composite material regulated and controlled by carbon quantum dots and preparation method and application thereof |
| CN114300660A (en) * | 2021-12-23 | 2022-04-08 | 大连博融新材料有限公司 | Polypyrrole coated carbon-doped sodium vanadium phosphate positive electrode material, and preparation method and application thereof |
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