CN107959024B - Flaky Sb for sodium ion battery cathode2Se3Method for preparing nanocrystalline - Google Patents

Flaky Sb for sodium ion battery cathode2Se3Method for preparing nanocrystalline Download PDF

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CN107959024B
CN107959024B CN201711085707.7A CN201711085707A CN107959024B CN 107959024 B CN107959024 B CN 107959024B CN 201711085707 A CN201711085707 A CN 201711085707A CN 107959024 B CN107959024 B CN 107959024B
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sodium
ion battery
polyvinylpyrrolidone
stirring
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CN107959024A (en
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曹丽云
郭玲
李嘉胤
黄剑锋
程娅伊
齐慧
李倩颖
仵婉晨
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Shaanxi University of Science and Technology
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00Electrodes
    • H01M4/02Electrodes composed of, or comprising, active material
    • H01M4/36Selection of substances as active materials, active masses, active liquids
    • H01M4/58Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
    • H01M4/581Chalcogenides or intercalation compounds thereof
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00Manufacture or treatment of nanostructures
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01MPROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00Secondary cells; Manufacture thereof
    • H01M10/05Accumulators with non-aqueous electrolyte
    • H01M10/054Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10Energy storage using batteries

Abstract

Sodium ion batteryFlake Sb for cell negative electrode2Se3The preparation method of the nanocrystalline comprises the steps of adding polyvinylpyrrolidone and tartaric acid into deionized water to obtain a solution A1, and then adding antimony potassium tartrate into the solution A1 to obtain a solution A2; adding sodium selenite into hydrazine hydrate to obtain solution B; dropwise adding the solution B into the solution A2 to obtain a mixed solution C; transferring the mixed solution C to a polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a homogeneous phase reactor, reacting at 100-150 ℃, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying to obtain the flaky Sb for the cathode of the sodium ion battery2Se3And (4) nanocrystals. The method adopts a one-step hydrothermal method, has simple equipment, is green and safe, has lower reaction temperature and good repeatability, and is suitable for large-scale production; the characteristic that the liquid phase environment is easy to control the appearance structure of the product is utilized, crystal development is induced under the action of polyvinylpyrrolidone and tartaric acid, and the flaky pure phase Sb is successfully prepared2Se3And (4) nanocrystals.

Description

Flaky Sb for sodium ion battery cathode2Se3Method for preparing nanocrystalline
Technical Field
The invention belongs to the field of electrochemical energy storage, and particularly relates to flaky Sb for a sodium ion battery cathode2Se3A method for preparing a nanocrystal.
Background
The development of lithium ion batteries starts in about 1980, and with the continuous progress of society and the continuous development of scientific technology, scientists gradually recognize the restriction of lithium resource shortage on the development of lithium ion batteries. Therefore, sodium ion batteries of the same main family and abundant reserves with similar electrochemical behavior are gradually attracting the attention of many researchers. Sb2Se3 as negative electrode material of Sb-base sodium selenide battery, a V-VI compound with laminated structureFor sodium ion battery negative electrode materials, 1mol of Sb2Se3 can be intercalated into 12mol of Na +, and the conversion reaction is a reversible process, which promotes Sb2Se3Has good electrochemical performance, such as high theoretical capacity: 678 mAh. g-1. However, the electrochemical performance of the electrochemical cell has yet to be improved from practical application.
According to the reports of the literature, the preparation of the nano material with the two-dimensional sheet structure is one of the most effective methods for improving the electrochemical performance, not only can the transmission path of ions and electrons be shortened in the thickness direction, but also the contact area between the nano material and the electrolyte is increased, and meanwhile, for some negative electrode materials with larger volume effect, such as Sb2Se3The nano-material can effectively relieve the structural damage and pulverization of the material in the process of sodium ion deintercalation, and remarkably improves the electrochemical performance. At present, for Sb having two-dimensional sheet shape2Se3Reports of the nanocrystalline as the negative electrode material of the sodium-ion battery are still less. Song H et al prepared two-dimensional flaky Sb by water molecule intercalation method2Se3(Song H,et al.,Highly Anisotropic Sb2Se3Nano sheets assembled vermiform Sb by solvent heat method of Nanosheets, title unfolding from the bulk condensers stress 1D crystalline Structure, adv Mater,2017.) Jin, R2Se3Has good hydrogen storage performance. (Jin, R.; Chen, G.; Wang, Q.; Sun, J.; Wang, Y., A facilesollvestril synthesis of theoretical Sb)2Se3Thus, disclosed is a simply prepared sheet-like Sb having a structure with a high chemical storage capacity, journal of Materials Chemistry 2011,21(18),6628.)2Se3The method of (a) and its partial test results as a sodium ion battery negative electrode material are very significant.
Disclosure of Invention
The invention aims to provide flaky Sb for a sodium ion battery negative electrode2Se3Method for preparing nanocrystalline and prepared Sb2Se3The nanocrystals have a two-dimensional sheet structure and are in the order of nanometers in the thickness direction, and are charged as sodium ionsThe cell anode material exhibits excellent cycling stability and rate capability.
In order to achieve the purpose, the invention adopts the technical scheme that:
1) the weight ratio of (0.001 g-0.005 g): (0.2 g-2 g): (0.169 g-1.0139 g) taking polyvinylpyrrolidone, tartaric acid and antimony potassium tartrate according to the mass ratio, adding the polyvinylpyrrolidone and the tartaric acid into 25-70 ml of deionized water, stirring until the polyvinylpyrrolidone and the tartaric acid are completely dissolved to obtain a transparent solution A1, then adding the antimony potassium tartrate into the solution A1, and continuously stirring to obtain a transparent solution A2;
2) according to the proportion that the ratio of potassium antimony tartrate to sodium selenite is 1: (1-3) adding sodium selenite into 3-10 mL of hydrazine hydrate according to the molar ratio, and stirring to obtain a wine red solution B; rapidly dropwise adding the solution B into the solution A2 under stirring, and uniformly stirring and dispersing to obtain a mixed solution C;
3) transferring the mixed solution C to a polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a homogeneous phase reactor, carrying out heat preservation reaction at 100-150 ℃ for 1-12 h, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying to obtain the flaky Sb for the sodium ion battery cathode2Se3And (4) nanocrystals.
The molecular weight of the polyvinylpyrrolidone in the step 1) is 30000.
And 2) stirring in the step 1) and the step 2) by using a magnetic stirrer, wherein the stirring speed is 500-800 r/min.
The mass percentage of hydrazine hydrate in the step 2) is 50%.
The filling ratio of the mixed solution C transferred to the polytetrafluoroethylene lining in the step 3) is 30-80%.
The freeze drying temperature in the step 3) is-40 ℃, and the pressure is 60 Pa.
Compared with the prior art, the invention has the following beneficial effects:
firstly, the method adopts a one-step hydrothermal method, has simple equipment, is green and safe, has lower reaction temperature and good repeatability, and is suitable for large-scale production; further, the characteristic that the liquid phase environment is easy to control the appearance structure of the product is utilized, and under the action of polyvinylpyrrolidone and tartaric acid, the crystal is induced to develop intoSuccessfully prepare flaky pure phase Sb2Se3The nanocrystals, the platelets of about 10nm thickness, were stacked together with voids. Prepared Sb2Se3The nanocrystalline is used as an active material, and the active material, a binder (polyvinylidene fluoride PVDF) and a conductive agent (conductive carbon black and conductive graphite) are ground, coated with slurry, dried and sliced in a solvent (nitrogen methyl pyrrolidone) according to a mass ratio of 8:1 (0.5:0.5) and then are used as a negative electrode to be assembled into the button sodium-ion battery in a glove box filled with argon. The electrochemical behavior of the Sb serving as the cathode material of the sodium-ion battery is preliminarily researched, and the flaky Sb prepared by the invention is discovered2Se3Negative electrode material of sodium ion battery, 0.1A g-1、0.2A g-1、0.5A g-1、1.0A g-1、2.0A g-1The discharge capacity was 550mAh g at the current density of (1)-1、400mAh g-1、350mAh g-1、300mAh g-1、200mAh g-1When the current density returns to 0.1A g again-1The capacity can be kept at 350mAh g-1The excellent rate capability is presented; and exhibits good cycling stability at high currents.
Drawings
FIG. 1 shows a sheet Sb for a negative electrode of a sodium-ion battery prepared in example 3 of the present invention2Se3An X-ray diffraction (XRD) pattern of the nanocrystal;
FIG. 2 shows the sheet Sb for the negative electrode of the sodium-ion battery prepared in example 32Se3Scanning Electron Microscope (SEM) photographs of the nanocrystals;
FIG. 3 shows the sheet Sb for negative electrode of sodium-ion battery prepared in example 32Se3A magnification map of the nanocrystals; wherein, Cycle number: the number of cycles; capacity: capacity.
The specific implementation mode is as follows:
example 1:
1) adding 0.001g of polyvinylpyrrolidone and 0.2g of tartaric acid into 25ml of deionized water, magnetically stirring at 500r/min until the polyvinylpyrrolidone and the tartaric acid are completely dissolved to obtain a transparent solution A1, then adding 0.169g of antimony potassium tartrate into the solution A1, and continuously stirring to obtain a transparent solution A2, wherein the molecular weight of the polyvinylpyrrolidone is 30000;
2) according to the proportion that the ratio of potassium antimony tartrate to sodium selenite is 1: 1, adding sodium selenite into 3mL of hydrazine hydrate with the mass percentage of 50%, and magnetically stirring at 500r/min to obtain a wine red solution B; rapidly dropwise adding the solution B into the solution A2 under stirring, and uniformly stirring and dispersing to obtain a mixed solution C;
3) transferring the mixed solution C into a polytetrafluoroethylene lining according to the filling ratio of 30%, putting the polytetrafluoroethylene lining into a homogeneous phase reactor, keeping the temperature at 100 ℃ for reaction for 12 hours, cooling the mixture to room temperature along with a furnace, repeatedly washing the mixture by deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying the precipitates at-40 ℃ and 60Pa to obtain the flaky Sb for the cathode of the sodium ion battery2Se3And (4) nanocrystals.
Example 2:
1) adding 0.002g of polyvinylpyrrolidone and 0.5g of tartaric acid into 45ml of deionized water, magnetically stirring at 600r/min until the polyvinylpyrrolidone and the tartaric acid are completely dissolved to obtain a transparent solution A1, then adding 0.338g of antimony potassium tartrate into the solution A1, and continuously stirring to obtain a transparent solution A2, wherein the molecular weight of the polyvinylpyrrolidone is 30000;
2) according to the proportion that the ratio of potassium antimony tartrate to sodium selenite is 1: 1.5, adding sodium selenite into 5mL of hydrazine hydrate with the mass percentage of 50%, and magnetically stirring at 600r/min to obtain a wine red solution B; rapidly dropwise adding the solution B into the solution A2 under stirring, and uniformly stirring and dispersing to obtain a mixed solution C;
3) transferring the mixed solution C into a polytetrafluoroethylene lining according to the filling ratio of 50%, putting the polytetrafluoroethylene lining into a homogeneous phase reactor, keeping the temperature at 120 ℃ for reaction for 8 hours, cooling the polytetrafluoroethylene lining to room temperature along with a furnace, repeatedly washing the cooled homogeneous phase reactor with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying the precipitates at-40 ℃ and 60Pa to obtain the flaky Sb for the cathode of the sodium ion battery2Se3And (4) nanocrystals.
Example 3:
1) adding 0.003g of polyvinylpyrrolidone and 1.0g of tartaric acid into 53ml of deionized water, magnetically stirring at 500r/min until the polyvinylpyrrolidone and the tartaric acid are completely dissolved to obtain a transparent solution A1, then adding 0.6759g of antimony potassium tartrate into the solution A1, and continuously stirring to obtain a transparent solution A2, wherein the molecular weight of the polyvinylpyrrolidone is 30000;
2) according to the proportion that the ratio of potassium antimony tartrate to sodium selenite is 1: 2, adding sodium selenite into 7mL of hydrazine hydrate with the mass percentage of 50%, and magnetically stirring at 500r/min to obtain a wine red solution B; rapidly dropwise adding the solution B into the solution A2 under stirring, and uniformly stirring and dispersing to obtain a mixed solution C;
3) transferring the mixed solution C into a polytetrafluoroethylene lining according to the filling ratio of 60%, putting the polytetrafluoroethylene lining into a homogeneous reactor, keeping the temperature at 130 ℃ for reaction for 6 hours, cooling the mixture to room temperature along with a furnace, repeatedly washing the mixture with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying the precipitates at-40 ℃ and 60Pa to obtain the flaky Sb for the cathode of the sodium ion battery2Se3And (4) nanocrystals.
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 nanocrystals are two-dimensional sheet structures with a thickness of about 10nm, and the sheets are stacked together with voids. (FIG. 2).
The prepared two-dimensional flaky pure phase Sb2Se3The preparation method comprises the following steps of grinding, slurry coating, drying, slicing, using the ground material as a negative electrode, assembling the ground material as the negative electrode into a button type sodium ion battery in a glove box filled with argon gas under the condition that azomethylpyrrolidone is used as a solvent, standing for 48 hours, and then carrying out electrochemical performance test by using a blue light tester. At 0.1A g-1、0.2A g-1、 0.5A g-1、1.0A g-1、2.0Ag-1The discharge capacity was 550mAh g at the current density of (1)-1、400mAh g-1、 350mAh g-1、300mAh g-1、200mAh g-1When the current density returns to 0.1A g again-1The capacity can be kept at 350mAh g-1Exhibit excellent rate performance(ii) a And exhibits good cycling stability at high current (figure 3).
Example 4:
1) adding 0.004g of polyvinylpyrrolidone and 1.5g of tartaric acid into 61ml of deionized water, magnetically stirring at 800r/min until the polyvinylpyrrolidone and the tartaric acid are completely dissolved to obtain a transparent solution A1, then adding 0.8848g of antimony potassium tartrate into the solution A1, and continuously stirring to obtain a transparent solution A2, wherein the molecular weight of the polyvinylpyrrolidone is 30000;
2) according to the proportion that the ratio of potassium antimony tartrate to sodium selenite is 1: 2.5, adding sodium selenite into 9mL of hydrazine hydrate with the mass percentage of 50%, and magnetically stirring at 800r/min to obtain a wine red solution B; rapidly dropwise adding the solution B into the solution A2 under stirring, and uniformly stirring and dispersing to obtain a mixed solution C;
3) transferring the mixed solution C into a polytetrafluoroethylene lining according to the filling ratio of 70 percent, putting the polytetrafluoroethylene lining into a homogeneous phase reactor, keeping the temperature at 140 ℃ for reaction for 4 hours, cooling the mixture to room temperature along with a furnace, repeatedly washing the mixture by deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying the precipitates at-40 ℃ and 60Pa to obtain the flaky Sb for the cathode of the sodium ion battery2Se3And (4) nanocrystals.
Example 5:
1) adding 0.005g of polyvinylpyrrolidone and 2g of tartaric acid into 70ml of deionized water, magnetically stirring at 700r/min until the polyvinylpyrrolidone and the tartaric acid are completely dissolved to obtain a transparent solution A1, then adding 1.0139g of antimony potassium tartrate into the solution A1, and continuously stirring to obtain a transparent solution A2, wherein the molecular weight of the polyvinylpyrrolidone is 30000;
2) according to the proportion that the ratio of potassium antimony tartrate to sodium selenite is 1: 3, adding sodium selenite into 10mL of hydrazine hydrate with the mass percentage of 50%, and magnetically stirring at 700r/min to obtain a wine red solution B; rapidly dropwise adding the solution B into the solution A2 under stirring, and uniformly stirring and dispersing to obtain a mixed solution C;
3) transferring the mixed solution C into a polytetrafluoroethylene lining according to the filling ratio of 80%, putting the polytetrafluoroethylene lining into a homogeneous phase reactor, keeping the temperature at 150 ℃ for reaction for 1h, cooling the polytetrafluoroethylene lining to room temperature along with a furnace, repeatedly washing the cooled polytetrafluoroethylene lining with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying the precipitates at-40 ℃ and 60Pa to obtain the cathode of the sodium ion batteryWith sheet Sb2Se3And (4) nanocrystals.

Claims (6)

1. Flaky Sb for sodium ion battery cathode2Se3The preparation method of the nanocrystalline is characterized by comprising the following steps:
1) the weight ratio of (0.001 g-0.005 g): (0.2 g-2 g): (0.169 g-1.0139 g) taking polyvinylpyrrolidone, tartaric acid and antimony potassium tartrate according to the mass ratio, adding the polyvinylpyrrolidone and the tartaric acid into 25-70 ml of deionized water, stirring until the polyvinylpyrrolidone and the tartaric acid are completely dissolved to obtain a transparent solution A1, then adding the antimony potassium tartrate into the solution A1, and continuously stirring to obtain a transparent solution A2;
2) according to the proportion that the ratio of potassium antimony tartrate to sodium selenite is 1: (1-3) adding sodium selenite into 3-10 mL of hydrazine hydrate according to the molar ratio, and stirring to obtain a wine red solution B; rapidly dropwise adding the solution B into the solution A2 under stirring, and uniformly stirring and dispersing to obtain a mixed solution C;
3) transferring the mixed solution C to a polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a homogeneous phase reactor, carrying out heat preservation reaction at 100-150 ℃ for 1-12 h, cooling to room temperature along with a furnace, repeatedly washing with deionized water and absolute ethyl alcohol to separate precipitates, and freeze-drying to obtain flaky Sb for the cathode of the sodium ion battery2Se3And (4) nanocrystals.
2. Flake Sb for sodium-ion battery negative electrode according to claim 12Se3The preparation method of the nanocrystalline is characterized by comprising the following steps: the molecular weight of the polyvinylpyrrolidone in the step 1) is 30000.
3. Flake Sb for sodium-ion battery negative electrode according to claim 12Se3The preparation method of the nanocrystalline is characterized by comprising the following steps: and 2) stirring in the step 1) and the step 2) by using a magnetic stirrer, wherein the stirring speed is 500-800 r/min.
4. Flake Sb for sodium-ion battery negative electrode according to claim 12Se3The preparation method of the nanocrystalline is characterized by comprising the following steps: the mass percent of hydrazine hydrate in the step 2)The number was 50%.
5. Flake Sb for sodium-ion battery negative electrode according to claim 12Se3The preparation method of the nanocrystalline is characterized by comprising the following steps: the filling ratio of the mixed solution C transferred to the polytetrafluoroethylene lining in the step 3) is 30-80%.
6. Flake Sb for sodium-ion battery negative electrode according to claim 12Se3The preparation method of the nanocrystalline is characterized by comprising the following steps: the freeze drying temperature in the step 3) is-40 ℃, and the pressure is 60 Pa.
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