CN107934923B - Nanosheet self-assembled flower spherical Sb2Se3Preparation method of negative electrode material of sodium-ion battery - Google Patents
Nanosheet self-assembled flower spherical Sb2Se3Preparation method of negative electrode material of sodium-ion battery Download PDFInfo
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Abstract
Nanosheet self-assembled flower spherical Sb2Se3The invention relates to a preparation method of a sodium ion battery cathode material, which takes common cheap substances such as antimony trichloride, selenium powder, sodium borohydride, ethanol and the like as raw materials, thereby reducing the production cost; the characteristics that the thermal environment of a solvent is easy to control the structure of a product are utilized, and the nano-sheet self-assembly monodisperse flower-spherical pure phase Sb is successfully prepared under the action of polyvinylpyrrolidone2Se3Nanocrystalline, low reaction temperature and good repeatability, and meets the requirement of large-scale production. Finally, the prepared Sb2Se3A series of processes of grinding, pulping, coating, drying and the like are carried out on the nanocrystalline to assemble the button type sodium ion battery, preliminary study is carried out on the electrochemical behavior of the nanocrystalline as the cathode material of the sodium ion battery, and the nano-sheet self-assembled flower-ball-shaped Sb prepared by the invention is found out2Se3The first discharge capacity of the negative electrode material of the sodium-ion battery is 780mA h g‑1Above theoretical capacity, the capacity is kept at 300mA h g for 50 cycles‑1The composite material has good circulation stability and good rate capability.
Description
Technical Field
The invention belongs to the field of electrochemical energy storage, and particularly relates to nanosheet self-assembled flower-shaped spherical Sb2Se3A preparation method of a negative electrode material of a sodium-ion battery.
Background
Electrochemical energy storage is one of the main energy storage modes in the current society, and mainly comprises a solar battery, a lead storage battery, a lithium ion battery, a sodium ion battery and the like. Wherein the sodium ion battery has storage capacityRich, little pollution, large specific energy, long cycle life and the like, and is one of the research hotspots in the field of electrochemical energy storage at present. Antimony-based selenide Sb2Se3As a sodium ion battery cathode material, the typical layered structure is beneficial to Na+And 1moL Sb2Se3Na capable of reacting with 12moL+The reaction, which results in a high theoretical capacity of 670mA h g-1, has attracted a great deal of attention from many researchers.
The literature reports that Sb2Se3 which is currently used as a negative electrode material of a sodium-ion battery is mainly in a one-dimensional structure. For example, Xing Qu et al synthesized a nanorod-like Sb2Se3/rGO composite material using a solvothermal method, with a capacity of 471mA h g-1(Ou X, Yang C, Xiong X, et al. A New rGO-coated Sb2Se3 nanoros Anode for Na + Battery: In Situ X-Ray diffraction study on a Live Sound/resolution Process [ J ]. Advanced functional materials,2017.) after 500 cycles at a current density of 1.0A g-1. Wenxi Zhao et al prepared a nano-rod Sb2Se3/N-GO composite material by a one-pot method, the first discharge capacity was 1000mA h g-1 at a current density of 0.1A g-1, and the capacity remained at 560mA h g-1 after 50 cycles (ZHao W, Li C M. Mesh-structured N-doped graphene @ Sb2Se3hybrid space anode for large capacity sources-batteries. [ J ] Journal of Colloid & Interface Science,2016,488: 356-phase 364). Luo W and the like prepare one-dimensional Sb2Se3nano materials into a film, and the film is used as a negative electrode material of a sodium ion battery, and the capacity is stabilized at 300mAh g < -1 > after circulation for 50 circles under the current density of 0.1A g < -1 >. (Luo W, Calas A, Tang C, et al. Ultralong Sb2Se3Nanowire-Based Free-Standing Membrane for Lithium/Sodium Ion Batteries [ J ]. 2016). Reports of other Sb2Se3nano materials as the cathode of the sodium-ion battery are less, and researches on electrochemical behaviors of Sb2Se3 materials with different morphologies as the cathode of the sodium-ion battery by a plurality of researchers are hindered.
Disclosure of Invention
The invention aims to provide a nanosheet self-assembled flower-shaped spherical Sb2Se3Preparation method of sodium ion battery negative electrode material and prepared Sb2Se3The nano material not only has a flower-ball-shaped special structure formed by self-assembly of thin sheets, but also has high charge and discharge capacity, good cycle stability and excellent rate performance when being used as a negative electrode material of a sodium ion battery.
In order to achieve the purpose, the invention adopts the technical scheme that:
1) adding 0.005-0.05 g of polyvinylpyrrolidone and 0.5-2 mmol of antimony trichloride into 35-75 ml of ethanol, stirring to obtain a transparent solution A, adding 0.75-3 mmol of selenium powder into 2-15ml of sodium borohydride aqueous solution with the concentration of 0.075-0.9 moL/L, stirring to obtain a transparent solution B, dropwise adding the solution B into the solution A under stirring, and uniformly stirring and dispersing to obtain a black mixed solution C;
2) transferring the mixed solution C to a polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a homogeneous reactor, reacting for 18-30 h at 150-200 ℃, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol, separating and precipitating, and obtaining black gray powder which is nanosheet self-assembled flower-shaped spherical Sb2Se3The negative electrode material of the sodium ion battery.
The average molecular weight of polyvinylpyrrolidone in the step 1) is 30000.
And (2) stirring in the step 1) by using a magnetic stirrer, wherein the stirring speed is 500-800 r/min, and the stirring time is 10-60 min.
The filling ratio of the mixed solution C transferred to the polytetrafluoroethylene lining in the step 2) is 50-80%.
The freeze drying temperature in the step 2) is-40 ℃, and the pressure is 60 Pa.
Compared with the prior art, the invention firstly takes common cheap substances such as antimony trichloride, selenium powder, sodium borohydride, ethanol and the like as raw materials, thereby reducing the production cost; further, by utilizing the characteristic that the thermal environment of a solvent is easy to control the structure of a product, the nano-flake self-assembly monodisperse flower-ball pure phase Sb is successfully prepared under the action of polyvinylpyrrolidone2Se3The nano-crystal has the thickness of about 10nm, the diameter of a flower ball of about 1 mu m, lower reaction temperature and good repeatability, and meets the requirement of large-scale production. Finally, the prepared Sb2Se3A series of processes of grinding, pulping, coating, drying and the like are carried out on the nanocrystalline to assemble the button type sodium ion battery, preliminary study is carried out on the electrochemical behavior of the nanocrystalline as the cathode material of the sodium ion battery, and the nano-sheet self-assembled flower-ball-shaped Sb prepared by the invention is found out2Se3The first discharge capacity of the negative electrode material of the sodium-ion battery is 780mA h g-1Above theoretical capacity, the capacity is kept at 300mA h g for 50 cycles-1The composite material has good circulation stability and good rate capability.
Drawings
FIG. 1 shows Sb prepared in example 1 of the present invention2Se3An X-ray diffraction (XRD) pattern of the electrode material;
FIG. 2 shows Sb prepared in example 1 of the present invention2Se3Scanning Electron Microscope (SEM) photographs of the electrode material;
FIG. 3 shows Sb prepared in example 1 of the present invention2Se3A cycle performance profile of the electrode material; wherein, Cycle number: the number of cycles; capacity: capacity;
FIG. 4 shows Sb prepared in example 6 of the present invention2Se3An X-ray diffraction (XRD) pattern of the electrode material;
FIG. 5 shows Sb prepared in example 6 of the present invention2Se3Scanning Electron Microscope (SEM) photographs of the electrode material;
FIG. 6 shows Sb prepared in example 6 of the present invention2Se3A rate performance graph of the electrode material; wherein, Cycle number: the number of cycles; capacity: capacity of
Detailed Description
The present invention will be described in further detail with reference to the accompanying drawings.
Example 1:
1) adding 0.005g of polyvinylpyrrolidone and 0.5mmol of antimony trichloride into 35ml of ethanol, stirring to obtain a transparent solution A, adding 0.75mmol of selenium powder into 15ml of sodium borohydride aqueous solution with the concentration of 0.075moL/L, stirring to obtain a transparent solution B, dropwise adding the solution B into the solution A under stirring, and uniformly stirring and dispersing to obtain a black mixed solution C;
the stirring adopts a magnetic stirrer, the stirring speed is 500r/min, and the stirring time is 60 min;
2) transferring the mixed solution C to a polytetrafluoroethylene lining according to the filling ratio of 50%, putting the polytetrafluoroethylene lining into a homogeneous reactor, reacting for 30 hours at 150 ℃, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying at-40 ℃ and 60Pa to obtain black gray powder, namely the nanosheet self-assembled flower spherical Sb2Se3The negative electrode material of the sodium ion battery.
Analysis of the samples (Sb) with a Japanese science D/max2000 PCX-ray diffractometer2Se3Powder), and Sb of an orthorhombic system having JCPDS numbers of 15 to 0861 was found in the sample2Se3The structure is consistent and no other miscellaneous peak appears (figure 1); when the sample was observed with a Field Emission Scanning Electron Microscope (FESEM) of S-4800 type, FEI corporation, USA, it was found that the prepared pure phase Sb was2Se3The nano-crystal is in a nano-sheet self-assembly single-dispersion flower ball shape, the thickness of the nano-sheet is about 10nm, and the diameter of the flower ball is about 1 μm (figure 2).
The black and gray powder is used as an active material, and is ground, slurry coated, dried and sliced with a conductive agent Super-p, a binding agent hydroxymethyl cellulose I CMC and polyacrylic acid PAA according to a mass ratio of 7:2:0.5:0.5 in deionized water, and then the black and gray powder is used as a negative electrode to be assembled into a button type sodium ion battery in a glove box filled with argon, and after the button type sodium ion battery is set aside for 48 hours, a blue tester is used for carrying out electrochemical performance test. At 0.1A g-1At a current density of (2), the first discharge capacity was 780mA h g-1Above theoretical capacity, the capacity is kept at 300mA h g for 50 cycles-1And has good cycle stability (figure 3).
Example 2:
1) adding 0.01g of polyvinylpyrrolidone and 0.75mmol of antimony trichloride into 42ml of ethanol, stirring to obtain a transparent solution A, adding 1.125mmol of selenium powder into 13ml of sodium borohydride aqueous solution with the concentration of 0.129moL/L, stirring to obtain a transparent solution B, dropwise adding the solution B into the solution A under stirring, and uniformly stirring and dispersing to obtain a black mixed solution C;
the stirring adopts a magnetic stirrer, the stirring speed is 800r/min, and the stirring time is 10 min;
2) transferring the mixed solution C to a polytetrafluoroethylene lining according to a filling ratio of 55%, putting the polytetrafluoroethylene lining into a homogeneous reactor, reacting for 28 hours at 160 ℃, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying at-40 ℃ and 60Pa to obtain black gray powder, namely the nanosheet self-assembled flower spherical Sb2Se3The negative electrode material of the sodium ion battery.
Example 3:
1) adding 0.02g of polyvinylpyrrolidone and 1mmol of antimony trichloride into 49ml of ethanol, stirring to obtain a transparent solution A, adding 1.5mmol of selenium powder into 11ml of sodium borohydride aqueous solution with the concentration of 0.204moL/L, stirring to obtain a transparent solution B, dropwise adding the solution B into the solution A under stirring, and uniformly stirring and dispersing to obtain a black mixed solution C;
the stirring adopts a magnetic stirrer, the stirring speed is 600r/min, and the stirring time is 40 min;
2) transferring the mixed solution C to a polytetrafluoroethylene lining according to the filling ratio of 60 percent, putting the polytetrafluoroethylene lining into a homogeneous reactor, reacting for 24 hours at 170 ℃, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying at-40 ℃ and 60Pa to obtain black gray powder, namely the nanosheet self-assembled flower spherical Sb2Se3The negative electrode material of the sodium ion battery.
Example 4:
1) adding 0.03g of polyvinylpyrrolidone and 1.25mmol of antimony trichloride into 56ml of ethanol, stirring to obtain a transparent solution A, adding 1.875mmol of selenium powder into 9ml of sodium borohydride aqueous solution with the concentration of 0.312moL/L, stirring to obtain a transparent solution B, dropwise adding the solution B into the solution A under stirring, and uniformly stirring and dispersing to obtain a black mixed solution C;
the stirring adopts a magnetic stirrer, the stirring speed is 700r/min, and the stirring time is 30 min;
2) transferring the mixed solution C to a polytetrafluoroethylene lining according to a filling ratio of 65%, putting the polytetrafluoroethylene lining into a homogeneous reactor, reacting at 180 ℃ for 22 hours, cooling to room temperature along with a furnace, and using deionized water and absolute ethyl alcoholRepeatedly washing, separating and precipitating, and freeze-drying at-40 deg.C and 60Pa to obtain black gray powder, i.e. nanosheet self-assembled flower-ball-shaped Sb2Se3The negative electrode material of the sodium ion battery.
Example 5:
1) adding 0.04g of polyvinylpyrrolidone and 1.5mmol of antimony trichloride into 63ml of ethanol, stirring to obtain a transparent solution A, adding 2.25mmol of selenium powder into 7ml of sodium borohydride aqueous solution with the concentration of 0.48moL/L, stirring to obtain a transparent solution B, dropwise adding the solution B into the solution A under stirring, and uniformly stirring and dispersing to obtain a black mixed solution C;
the stirring adopts a magnetic stirrer, the stirring speed is 650r/min, and the stirring time is 50 min;
2) transferring the mixed solution C to a polytetrafluoroethylene lining according to the filling ratio of 70 percent, putting the polytetrafluoroethylene lining into a homogeneous reactor, reacting for 320 hours at 190 ℃, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying at-40 ℃ and 60Pa to obtain black gray powder, namely the nanosheet self-assembled flower-shaped spherical Sb2Se3The negative electrode material of the sodium ion battery.
Example 6:
1) adding 0.05g of polyvinylpyrrolidone and 2mmol of antimony trichloride into 75ml of ethanol, stirring to obtain a transparent solution A, adding 3mmol of selenium powder into 5ml of sodium borohydride aqueous solution with the concentration of 0.9moL/L, stirring to obtain a transparent solution B, dropwise adding the solution B into the solution A under stirring, and uniformly stirring and dispersing to obtain a black mixed solution C;
the stirring adopts a magnetic stirrer, the stirring speed is 750r/min, and the stirring time is 20 min;
2) transferring the mixed solution C to a polytetrafluoroethylene lining according to the filling ratio of 80%, putting the polytetrafluoroethylene lining into a homogeneous reactor, reacting for 18 hours at 200 ℃, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying at-40 ℃ and 60Pa to obtain black gray powder, namely the nanosheet self-assembled flower spherical Sb2Se3The negative electrode material of the sodium ion battery.
Analysis of the sample with a Japanese science D/max2000 PCX-ray diffractometer (S)b2Se3Powder), and Sb of an orthorhombic system having JCPDS numbers of 15 to 0861 was found in the sample2Se3The structure was consistent and no other miscellaneous peaks appeared (fig. 4); when the sample was observed with a Field Emission Scanning Electron Microscope (FESEM) of S-4800 type, FEI corporation, USA, it was found that the prepared pure phase Sb was2Se3The nanocrystals are self-assembled nano-sheets and have single dispersed flower-ball shape, the diameter of the nano-sheets is about 10nm, and the diameter of the flower-ball is about 1 μm (figure 5).
The black and gray powder is used as an active material, and is ground, slurry coated, dried and sliced with a conductive agent Super-p, a binding agent hydroxymethyl cellulose I CMC and polyacrylic acid PAA according to a mass ratio of 7:2:0.5:0.5 in deionized water, and then the black and gray powder is used as a negative electrode to be assembled into a button type sodium ion battery in a glove box filled with argon, and after the button type sodium ion battery is set aside for 48 hours, a blue tester is used for carrying out electrochemical performance test. At 0.1A g-1The first discharge capacity is 767mA h g-1Higher than the theoretical capacity, and better rate performance (fig. 6).
Claims (3)
1. Nanosheet self-assembled flower spherical Sb2Se3The preparation method of the negative electrode material of the sodium-ion battery is characterized by comprising the following steps:
1) adding 0.005-0.05 g of polyvinylpyrrolidone and 0.5-2 mmol of antimony trichloride into 35-75 ml of ethanol, stirring to obtain a transparent solution A, adding 0.75-3 mmol of selenium powder into 2-15ml of sodium borohydride aqueous solution with the concentration of 0.075-0.9 moL/L, stirring to obtain a transparent solution B, dropwise adding the solution B into the solution A under stirring, and uniformly stirring and dispersing to obtain a black mixed solution C;
2) transferring the mixed solution C to a polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a homogeneous reactor, reacting for 18-30 h at 150-200 ℃, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol, separating and precipitating, and obtaining black gray powder which is nanosheet self-assembled flower-shaped spherical Sb2Se3A sodium ion battery negative electrode material;
the average molecular weight of polyvinylpyrrolidone in the step 1) is 30000;
the freeze drying temperature in the step 2) is-40 ℃, and the pressure is 60 Pa.
2. Nanosheet self-assembled flower spherical Sb as claimed in claim 12Se3The preparation method of the negative electrode material of the sodium-ion battery is characterized by comprising the following steps: and (2) stirring in the step 1) by using a magnetic stirrer, wherein the stirring speed is 500-800 r/min, and the stirring time is 10-60 min.
3. Nanosheet self-assembled flower spherical Sb as claimed in claim 12Se3The preparation method of the negative electrode material of the sodium-ion battery is characterized by comprising the following steps: the filling ratio of the mixed solution C transferred to the polytetrafluoroethylene lining in the step 2) is 50-80%.
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