CN113562715B - Ba 0.5 Ti 2 (PO 4 ) 3 Preparation method of/C nanosphere negative electrode material - Google Patents
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Abstract
The invention relates to a Ba 0.5 Ti 2 (PO 4 ) 3 A preparation method of a/C nanosphere negative electrode material. Firstly, adding tetrabutyl titanate into a mixed solvent of ethanol, acetone and deionized water to obtain a white suspension, then dissolving barium hydroxide octahydrate and ammonium dihydrogen phosphate into the suspension, finally adding sucrose and urea, stirring and dissolving, sealing into a polytetrafluoroethylene-lined steel kettle, placing into a forced air drying oven for hydrothermal reaction, calcining the obtained precursor material in a tubular furnace under the argon atmosphere, and finally obtaining Ba 0.5 Ti 2 (PO 4 ) 3 the/C nanosphere negative electrode material. Ba obtained by the invention 0.5 Ti 2 (PO 4 ) 3 the/C nanosphere has uniform diameter which is about 200-280 nm, and the in-situ coated carbon and the nano structure ensure that the nanosphere has excellent electrochemical performance in a potassium ion battery. The invention has the advantages of simple process, mild condition, short preparation period and the like.
Description
Technical Field
The invention relates to a potassium ion battery cathode material, in particular to a Ba 0.5 Ti 2 (PO 4 ) 3 A method for preparing a nanosphere negative electrode material.
Background
Under the push of people to pay more attention to environmental pollution and fossil energy crisis, the development of novel electrochemical energy storage devices is receiving wide attention. Lithium ion batteries have been widely used in the fields of portable electronic devices, electric vehicles, etc., but because of the uneven distribution and limited storage of lithium resources, people are forced to search for new energy storage methods. The potassium element has abundant reserves on the earth and low cost, the potassium ion battery has a similar working principle with the lithium ion battery, and the Stokes radii and the standard reduction potential of potassium and lithium are relatively close, so that the potassium ion battery is paid more and more attention.
NASICON-type materials are widely studied in the field of secondary batteries due to their open three-dimensional framework, ultra-high structural stability, and fast ion transport. Potassium titanium phosphate is a typical representative of NASICON-type anode materials in which large potassium ions can be rapidly transported, and has been widely used in potassium ion batteries. However, the fatal defects of poor conductivity and low theoretical specific capacity of the material often cause the problems of poor rate capability, low discharge/charge capacity and the like. And carbon coating is the simplest and most effective strategy for improving the conductivity. In addition, the nano material is beneficial to improving the specific surface area, shortening the ion transmission path and improving the ion/electron transmission rate, thereby improving the potassium storage performance. When divalent metal ions replace monovalent metal ions, more vacancies are left in the structure to store potassium ions, thereby increasing the battery capacity.
Based on the method, the in-situ carbon-coated barium titanium phosphate nanospheres are prepared by a simple hydrothermal method, and the in-situ coated carbon layer and the nanoscale size ensure Ba 0.5 Ti 2 (PO 4 ) 3 the/C nanosphere negative electrode material has better potassium storage performance.
Disclosure of Invention
The invention aims to provide a simple hydrothermal method for preparing Ba 0.5 Ti 2 (PO 4 ) 3 Method of nanospheres.
The technical scheme of the invention is as follows:
ba 0.5 Ti 2 (PO 4 ) 3 The preparation method of the/C nanosphere negative electrode material comprises the following steps of:
(1) Uniformly mixing ethanol, acetone and deionized water to obtain a mixed solvent, adding tetra-n-butyl titanate, and then magnetically stirring until complete hydrolysis to obtain a white suspension;
(2) Adding barium hydroxide octahydrate, ammonium dihydrogen phosphate, sucrose and urea into the suspension obtained in the step (1), stirring and dissolving, sealing into a steel kettle with a polytetrafluoroethylene lining, and placing into a forced air drying oven for hydrothermal reaction;
(3) Alternately washing the material obtained in the step (2) by using deionized water and ethanol, and drying to obtain a precursor material;
(4) Transferring the precursor material obtained in the step (3) into a porcelain ark, and then putting the porcelain ark into a tube furnace to calcine in the argon atmosphere to obtain Ba 0.5 Ti 2 (PO 4 ) 3 /C nanosphere negative electrode material.
Further, in the mixed solvent in the step (1), the volume ratio of ethanol to acetone to deionized water is 1-3: 1 to 2:4 to 6.
Further, in the step (2), the mass ratio of urea to tetra-n-butyl titanate is 1-1.5.
Further, in the step (2), the stirring time is 2.5-4h, and the stirring temperature is 35-70 ℃.
Furthermore, in the step (2), the temperature of the hydrothermal reaction is 160-200 ℃ and the time is 8-14h.
Further, in the step (3), the drying temperature is 50-80 ℃, and the drying time is 8-14h.
Further, in the step (4), the calcining temperature is 650-800 ℃, the calcining time is 4-8h, and the heating rate is 3-5 ℃/min.
It is worth to explain that all factors in the process of the invention act synergistically to finally obtain a product of the nanosphere with excellent performance and specific appearance, and all the factors are indispensable. If sucrose is not added, the obtained nanospheres are seriously agglomerated and do not have clear nanosphere shapes; if no urea is added, the obtained product is not in the shape of nanospheres, but in the shape of micrometer flowers.
The invention has the following technical effects:
(1) The invention adopts a hydrothermal method to synthesize Ba 0.5 Ti 2 (PO 4 ) 3 the/C nanosphere negative electrode material has a clear nanosphere shape and a uniform diameter of about 200-280 nm.
(2) The invention has simple preparation process and convenient operation, and the obtained Ba 0.5 Ti 2 (PO 4 ) 3 the/C nanosphere is a novel and simple battery cathode material, and the in-situ coated carbon and the nano structure enable the battery cathode material to have excellent electrochemical performance in a potassium ion battery.
Drawings
FIG. 1 is an X-ray diffraction pattern of materials prepared according to the present invention in example 2 (no sucrose added) and example 3 (no urea added).
FIG. 2 is a scanning electron micrograph of sucrose-free material prepared in example 2 of the present invention.
FIG. 3 is a scanning electron micrograph of a material prepared in example 3 of the present invention without urea addition.
FIG. 4 shows Ba prepared in example 4 0.5 Ti 2 (PO 4 ) 3 X-ray diffraction pattern of/C nanosphere material.
FIG. 5 shows Ba prepared in example 4 of the present invention 0.5 Ti 2 (PO 4 ) 3 Scanning electron microscope images of the/C nanosphere material.
FIG. 6 shows Ba prepared in example 4 of the present invention 0.5 Ti 2 (PO 4 ) 3 the/C nanospheres are used as a negative electrode material, and the potassium sheet is used as a counter electrode to assemble the button cell. 0.05A g under the temperature of 20-25 ℃ and the voltage range of 0.01-3.0V -1 A cycle life chart of a charge and discharge test at the current density of (1).
FIG. 7 shows Ba prepared in example 3 of the present invention 0.5 Ti 2 (PO 4 ) 3 the/C nanospheres are used as a negative electrode material, and the potassium sheet is used as a counter electrode to assemble the button cell. Under the temperature of 20-25 ℃, in the voltage range of 0.01-3.0V, the current density is 0.02A g -1 、0.05Ag -1 、0.1A g -1 、0.2A g -1 、0.5Ag -1 、1.0Ag -1 And 0.02Ag -1 The rate performance graph of the charge and discharge test was obtained.
Detailed Description
The present invention will be described in further detail below by way of examples to enable those skilled in the art to better understand the present invention, but the present invention is not limited to the following examples.
The test methods in the following examples are all conventional methods unless otherwise specified.
Example 1
(1) Uniformly mixing ethanol, acetone and deionized water in a volume ratio of 1;
(2) Adding 0.395g of barium hydroxide octahydrate, 0.863g of ammonium dihydrogen phosphate, 1.15g of sucrose and 1.34g of urea into the suspension obtained in the step (1), stirring for 3 hours at 50 ℃, sealing into a polytetrafluoroethylene-lined steel kettle after dissolving, and placing into a forced air drying oven for hydrothermal reaction for 12 hours at 180 ℃;
(3) Washing the material obtained in the step (2) with deionized water and ethanol alternately, and drying at 80 ℃ for 8h to obtain a nanosphere precursor;
(4) Transferring the precursor nanospheres obtained in the step (3) into a porcelain ark, and calcining the porcelain ark for 6 hours in a tube furnace at 750 ℃ in an argon atmosphere to obtain Ba 0.5 Ti 2 (PO 4 ) 3 a/C nanosphere.
Example 2
(1) Uniformly mixing ethanol, acetone and deionized water in a volume ratio of 1;
(2) Adding 0.395g of barium hydroxide octahydrate, 0.863g of ammonium dihydrogen phosphate and 1.34g of urea into the suspension obtained in the step (1), stirring at 50 ℃ for 3h to dissolve, sealing into a polytetrafluoroethylene-lined steel kettle, and placing in a forced air drying oven for hydrothermal reaction at 180 ℃ for 12h;
(3) Washing the material obtained in the step (2) with deionized water and ethanol alternately, and drying at 80 ℃ for 8h to obtain a nanosphere precursor;
(4) Transferring the precursor nanospheres obtained in the step (3) into a porcelain ark, and then putting the porcelain ark into a tube furnace to calcine for 6 hours at 750 ℃ in the argon atmosphere to obtain seriously-agglomerated Ba 0.5 Ti 2 (PO 4 ) 3 Nanospheres and containing TiP 2 O 7 Impurities.
Example 3
(1) Uniformly mixing ethanol, acetone and deionized water in a volume ratio of 1;
(2) Adding 0.395g of barium hydroxide octahydrate, 0.863g of ammonium dihydrogen phosphate and 1.15g of sucrose into the suspension obtained in the step (1), stirring at 50 ℃ for 3h to dissolve, sealing into a polytetrafluoroethylene-lined steel kettle, and placing in a forced air drying oven for hydrothermal reaction at 180 ℃ for 12h;
(3) Washing the material obtained in the step (2) by using deionized water and ethanol alternately, and drying at 80 ℃ for 8 hours to obtain a fish scale-shaped microsphere precursor;
(4) Transferring the precursor nanospheres obtained in the step (3) into a porcelain ark, and then putting the porcelain ark into a tube furnace to calcine for 6 hours at 750 ℃ in the argon atmosphere to obtain micrometer flower-like carbon-coated BaTiP 2 O 8 And TiP 2 O 7 。
Example 4
(1) Uniformly mixing ethanol, acetone and deionized water in a volume ratio of 1;
(2) Adding 0.395g of barium hydroxide octahydrate, 0.863g of ammonium dihydrogen phosphate, 1.15g of sucrose and 1.34g of urea into the suspension obtained in the step (1), stirring for 3 hours at 50 ℃, sealing into a polytetrafluoroethylene-lined steel kettle after dissolving, and placing into a forced air drying oven for hydrothermal reaction for 12 hours at 180 ℃;
(3) Washing the material obtained in the step (2) with deionized water and ethanol alternately, and drying at 80 ℃ for 8 hours to obtain Ba 0.5 Ti 2 (PO 4 ) 3 A nanosphere precursor;
(4) Transferring the precursor nanospheres obtained in the step (3) into a porcelain ark, and calcining the porcelain ark for 6 hours in a tube furnace at 750 ℃ in an argon atmosphere to obtain Ba 0.5 Ti 2 (PO 4 ) 3 a/C nanosphere.
The product obtained in example 4 was used for characterization, and the results are shown below.
As shown in fig. 4, by reacting with Ba 0.5 Ti 2 (PO 4 ) 3 As can be seen by comparing the standard card PDF #34-0094, the prepared Ba 0.5 Ti 2 (PO 4 ) 3 Composite material of/C nanosphere and Ba 0.5 Ti 2 (PO 4 ) 3 Characteristic diffraction peak ofThe fit is good, wherein the carbon is amorphous.
As shown in FIG. 5, ba was produced 0.5 Ti 2 (PO 4 ) 3 The diameter of the/C nanosphere is very uniform and is about 200-280 nm, so that the potassium ions can be more favorably embedded/separated, and the electrochemical performance is good.
As shown in FIG. 6, ba produced by the present invention 0.5 Ti 2 (PO 4 ) 3 the/C nanospheres are used as a negative electrode material, and the potassium sheet is used as a counter electrode to assemble the button cell. 0.05A g under the temperature of 20-25 ℃ and the voltage range of 0.01-3.0V -1 The first discharge specific capacity is 309.0mA h g -1 The charging specific capacity is 63.0mA h g -1 (ii) a The specific discharge capacity after 100 cycles is 146.2mA h g -1 The charging specific capacity is 144.3mA h g -1 (ii) a The specific discharge capacity after the circulation for 250 times is 149.0mA h g -1 The charging specific capacity is 146.5mA h g -1 . Thus, ba 0.5 Ti 2 (PO 4 ) 3 the/C nanosphere has excellent cycling stability as a negative electrode material.
As shown in FIG. 7, ba prepared by the present invention 0.5 Ti 2 (PO 4 ) 3 the/C nanospheres are used as a negative electrode material, and the potassium sheet is used as a counter electrode to assemble the button cell. Under the temperature of 20-25 ℃, in the voltage range of 0.01-3.0V, the different current densities are 0.02A g -1 、0.05A g -1 、0.1A g -1 、0.2A g -1 、0.5A g -1 、1.0A g -1 And 0.02A g -1 The rate performance graph of the charge and discharge test was obtained. At 0.02A g -1 The specific discharge capacity after 5 cycles of the current density of (1) is 111.9mAh g -1 When the current density is increased to 0.05A g -1 、0.1A g -1 、0.2A g -1 、0.5A g -1 、1.0A g -1 When the discharge specific capacity is higher than the discharge specific capacity, the discharge specific capacity is respectively 96.1mA h g -1 、84.0mA h g -1 、75.2mA h g -1 、62.9mA h g -1 、56.4mA h g -1 The current density returns to 0.02A g after charging and discharging by large current -1 Still respectively have 119.2mAh g -1 Specific discharge capacity of (2). Thus, ba 0.5 Ti 2 (PO 4 ) 3 the/C nanospheres have good rate performance as the negative electrode material of the potassium ion battery.
Claims (6)
1. Ba-Ba alloy 0.5 Ti 2 (PO 4 ) 3 The preparation method of the/C nanosphere negative electrode material is characterized by comprising the following steps of:
(1) Uniformly mixing ethanol, acetone and deionized water to obtain a mixed solvent, adding tetra-n-butyl titanate, and then magnetically stirring until complete hydrolysis to obtain a white suspension;
(2) Adding barium hydroxide octahydrate, ammonium dihydrogen phosphate, sucrose and urea into the suspension obtained in the step (1), wherein the mass ratio of the urea to the tetra-n-butyl titanate is 1-1.5 to 1.2-2.0, stirring to dissolve, sealing into a steel kettle with a polytetrafluoroethylene lining, and placing into an air-blowing drying oven for hydrothermal reaction;
(3) Alternately washing the material obtained in the step (2) by using deionized water and ethanol, and drying to obtain a precursor material;
(4) Transferring the precursor material obtained in the step (3) into a porcelain ark, and then putting the porcelain ark into a tube furnace to calcine in the argon atmosphere, wherein the calcining temperature is 650-800 ℃, and the calcining time is 4-8h, so that Ba is obtained 0.5 Ti 2 (PO 4 ) 3 the/C nanosphere negative electrode material.
2. Ba of claim 1 0.5 Ti 2 (PO 4 ) 3 The preparation method of the/C nanosphere negative electrode material is characterized in that in the mixed solvent in the step (1), the volume ratio of ethanol to acetone to deionized water is 1~3:1~2:4~6.
3. Ba of claim 1 0.5 Ti 2 (PO 4 ) 3 The preparation method of the/C nanosphere negative electrode material is characterized in that in the step (2), the stirring time is 2.5-4h, and the stirring temperature is 35-70 ℃.
4. Ba of claim 1 0.5 Ti 2 (PO 4 ) 3 The preparation method of the/C nanosphere negative electrode material is characterized in that in the step (2), the temperature of the hydrothermal reaction is 160-200 ℃, and the time is 8-14h.
5. Ba of claim 1 0.5 Ti 2 (PO 4 ) 3 The preparation method of the/C nanosphere negative electrode material is characterized in that in the step (3), the drying temperature is 50-80 ℃, and the drying time is 8-14h.
6. Ba of claim 1 0.5 Ti 2 (PO 4 ) 3 The preparation method of the/C nanosphere negative electrode material is characterized in that in the step (4), the temperature rise rate of calcination is 3-5 ℃/min.
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