CN113764687A - A bifunctional electrocatalyst for an air electrode of a high-efficiency zinc-air battery is disclosed: ultra-thin ternary nanosheet FePSe treated by plasma3Preparation and use of - Google Patents
A bifunctional electrocatalyst for an air electrode of a high-efficiency zinc-air battery is disclosed: ultra-thin ternary nanosheet FePSe treated by plasma3Preparation and use of Download PDFInfo
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- CN113764687A CN113764687A CN202010492147.2A CN202010492147A CN113764687A CN 113764687 A CN113764687 A CN 113764687A CN 202010492147 A CN202010492147 A CN 202010492147A CN 113764687 A CN113764687 A CN 113764687A
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Abstract
The invention relates to a bifunctional electrocatalyst FePSe of an air electrode of a high-efficiency zinc-air battery3Belonging to the technical field of metal-air batteries. The preparation method of the catalyst for the air electrode comprises the following steps: (1) preparation of ternary transition metal phosphorus selenium compound FePSe by chemical vapor deposition method3(ii) a (2) Carrying out ultrasonic stripping to obtain an ultrathin two-dimensional nanosheet; (3) using Ar/O2And inducing surface recombination by the two-dimensional nanosheet obtained through plasma treatment. Warp beamThrough ultrasonic stripping and plasma treatment, oxygen atom doping brings excellent oxygen electrocatalytic activity. The zinc-air battery prepared by the air electrode catalyst has smaller charging voltage gap and good cycling stability. This work provides new insight for the rational design of plasma treatment of two-dimensional nanoplates to optimize bifunctional oxygen electrocatalysts for metal-air battery air electrodes.
Description
Technical Field
The invention relates to an oxygen atom doped ultrathin ternary transition metal phosphorus sulfur compound nanosheet as an air electrode material of a metal-air battery, and belongs to the technical field of metal-air batteries.
Background
To address the growing global energy demand and the increasing environmental pollution, clean, high-capacity and renewable energy storage devices are key components of fossil fuel consumption reduction, such as regenerative fuel cells and metal air batteries. Among them, Zinc Air Batteries (ZABs) have been widely studied due to their high theoretical energy density, high safety and low cost. The efficiency of the Oxygen Evolution Reaction (OER) and the Oxygen Reduction Reaction (ORR) is greatly limited by slow kinetics involving four successive proton coupled electron transfer steps. Therefore, it is important to find an efficient oxygen electrocatalyst. In general, the noble metal catalyst Pt shows excellent ORR performance, and Ir and Ru show excellent OER performance, but the noble metal catalyst Pt and the Ir and Ru cannot simultaneously keep low overpotential to catalyze the two half reactions, and the battery performance of the metal-air battery depends on the ORR and OER performance of the catalyst. In addition, their limited reserves, high cost and scarcity greatly hinder their widespread use. Therefore, it is necessary to design and prepare a novel, cheap, stable and efficient oxygen electrocatalyst as a catalyst material for an air electrode of a zinc-air battery instead of a noble metal catalyst.
Transition metal phosphorus chalcogen compound with layered structure (general formula: MPX)3Wherein M represents metallic elements such as iron, nickel, manganese, cobalt and the like, and X represents a chalcogen main group element such as sulfur, selenium and the like) belongs to a monoclinic system, and each unit cell contains two [ P2Se6 ]]The 4-structure and two Fe ions, aligned along the c-axis, are stacked in layers by weak "van der waals forces" in the manner of "abcabcabc" and thus become thin nanostructures by exfoliation. Due to MPX3The bulk crystal has the advantages of easily available raw materials, low price, simple preparation process and certain catalytic activity, thereby being widely concerned by researchers. FePSe3Has strong anisotropy, strong magnetism, wide band gap and excellent electronic characteristics. Oxygen doped FePSe3The nano-sheet is an oxygen electro-catalyst with various excellent performances from a three-dimensional bulk material to a two-dimensional nano-sheetMaterial, FePSe3Unsaturated active sites on the surface of the nano-sheet are increased, and the introduction of oxygen atoms improves the electron transfer rate, so that the oxygen-doped FePSe3The nano-sheet becomes a bifunctional electrocatalyst with excellent ORR and OER performances, and has good chemical stability. So that oxygen-doped FePSe can be used3The nanosheet is used as an air electrode catalyst of the zinc-air battery to prepare the flexible solid zinc-air battery.
Disclosure of Invention
The invention aims to provide a bifunctional electrocatalyst FePSe of an air electrode of a high-efficiency zinc-air battery3The preparation method of (1). The technical scheme of the invention is realized by the following steps:
(1)FePSe3and (4) preparing crystals. Uniformly mixing Fe powder, P powder and Se powder according to a certain proportion, and preparing block FePSe by using a traditional Chemical Vapor Transport (CVT) method3And (4) crystals.
(2)FePSe3And (3) preparing the nano sheet. The FePSe in a block shape is put into3Dispersing the crystal in absolute ethyl alcohol solution for ultrasonic treatment to obtain uniformly dispersed black FePSe3Ethanol mixed solution, stripping by tip ultrasonic treatment, and reducing FePSe by centrifugation at different rotation speeds3Size distribution of nanosheets to obtain ultra-thin FePSe of smaller size3Nanosheets.
(3)FePSe3-preparation of O nanoplates. Mixing a certain mass of FePSe3The nano-sheets are evenly spread on a quartz boat and are in Ar/O2Plasma (plasma) processing is carried out at a certain power under the atmosphere, and after one hour, the FePSe is obtained after taking out3-O nanoplates.
(4) And preparing an air electrode. The prepared FePSe3Dispersing an-O nano sheet and a certain amount of conductive carbon powder in a mixed solution of Nafion, absolute ethyl alcohol and deionized water, performing ultrasonic treatment to obtain an evenly dispersed ink-like solution, slowly dripping the ink-like solution on carbon cloth with a certain size, and airing at room temperature to serve as an air anode of the flexible solid zinc-air battery.
(5) And (3) preparing a gel electrolyte. Mixing acrylic acid and N, N' -methylene-bisacrylamideBlending into 8.4M KOH, then mixing the solution with 0.3M K2S2O8Stirring to synthesize the gel electrolyte.
(6) And (4) preparing a metal negative electrode. And shearing the polished zinc foil into a certain size to be used as a metal cathode of the zinc-air battery.
(7) And (5) preparing a zinc-air battery. And (3) respectively placing the air anode (4) and the metal cathode (6) on two sides of the gel electrolyte (5) to prepare a sandwich-structured flexible solid-state battery, and finally coating the sandwich-structured flexible solid-state battery with an aluminum plastic film to obtain the flexible solid-state zinc-air battery.
(1) The molar mass ratio of the Fe powder, the P powder and the Se powder is 1: 3, the CVT is heated at 750 ℃ and is kept for 7 days.
(2) The medium centrifugation speeds were 1000, 4000 and 6000rpm, respectively.
(3) In which O is introduced2Ar/O at a concentration of 5%2And carrying out plasma treatment.
(4) Middle FePSe3The mass ratio of the-O nano sheet to the conductive carbon powder is 7: 3, and the dosage of Nafion, absolute ethyl alcohol and deionized water is 50 muL, 760 muL and 190 muL respectively. The size of the carbon cloth is 1x1.5cm2Dropping the ink solution at 1x1cm2The rest 0.5cm is convenient for fixing the electrode clamp, and the load is 0.6mg/cm2。
(5) The mass of the medium acrylic acid and the mass of the N, N' -methylene-bisacrylamide are 0.22g and 0.01g respectively, 8.4mol/L KOH and 0.3mol/L K2S2O8The volumes of (A) and (B) are 10mL and 80. mu.L, respectively.
Drawings
FIG. 1 shows FePSe prepared by the present invention3TEM image of O nanoplatelets.
FIG. 2 shows FePSe prepared by the present invention3-XRD pattern of O nanoplatelets.
FIG. 3 is a constant current discharge curve of a flexible solid zinc-air cell made in accordance with the present technology at a current density of 1mA/cm2. It can be seen from the graph that the battery has a stable discharge performance for a long period of time.
Fig. 4 is a discharge curve and power density curve for a flexible solid state zinc-air cell made in accordance with the present technology. It can be seen from the figure that the cell has a very high power density.
FIG. 5 shows the charge and discharge stability of a flexible solid zinc-air cell made in accordance with the present technology at a current density of 1mA/cm2. It can be seen from the graph that the battery has stable charge and discharge cycle characteristics.
Detailed Description
The experimental invention technique is further described in detail below. Unless otherwise specified, the experimental methods mentioned in the examples of the present invention are general experimental methods, and the drugs, reagents, and materials used in the examples of the present invention may be commercially available.
Example 1
(1)FePSe3And (4) preparing crystals. Fe powder (50nm), P powder and Se powder were weighed in a molar mass ratio of 1: 3 to total 500mg, sealed in a quartz tube under vacuum, having an inner diameter of about 16mm and a length of about 15cm, heated to 750 ℃ in a box furnace using CVT method, and kept for 7 days at a temperature rise rate of 2 ℃/min. Taking out the block FePSe after cooling to room temperature3The crystals were ground to a homogeneous powder and stored in a dry cabinet.
(2)FePSe3And (3) preparing the nano sheet. 200mg of FePSe in lump form are weighed3Dispersing the crystal in absolute ethyl alcohol solution for ultrasonic treatment to obtain uniformly dispersed black FePSe3The ethanol mixed solution was stripped by tip sonication, the mixed solution was centrifuged 3 times at 1000rpm for half an hour each, the supernatant was separated and collected, first 3 times at 4000rpm for half an hour each with deionized water, and then 3 times at 6000rpm with absolute ethanol for half an hour each. Finally collecting the precipitate, and placing the precipitate in a vacuum drying oven at 60 ℃ for 12 hours to obtain dried FePSe3Nanosheets.
(3)FePSe3-preparation of O nanoplates. 200mg of dried FePSe was taken3Grinding the nano-sheets uniformly, spreading the nano-sheets in a quartz boat, putting the quartz boat into a plasma reactor, and putting the quartz boat in an O state2Ar/O at a concentration of 5%2The atmosphere was evacuated until the pressure dropped to 0.65Pa, and plasma treatment was carried out at 100W power and maintained for 1 hour. To be treatedWhen the air release is recovered to the standard atmospheric pressure, taking out the prepared FePSe3-O nanoplates and stored in a drying cabinet.
(4) And preparing an air electrode. Taking 7mg of prepared FePSe3Grinding an-O nanosheet and 3mg of conductive carbon powder uniformly in a mortar, adding the ground material into a mixed solution of 50 mu L of Nafion, 760 mu L of absolute ethyl alcohol and 190 mu L of deionized water, carrying out ultrasonic treatment for 1 hour to obtain a uniformly dispersed ink-like solution, soaking the whole carbon cloth in concentrated nitric acid, carrying out ultrasonic pretreatment on the carbon cloth by using the deionized water, and cutting the dried carbon cloth into pieces with the length of 1x1.5cm2Size, 200. mu.L of ink solution was slowly dropped at 1X1cm2On the front and back sides, the amount of the drop on each side is ensured to reach 100 mu L so as to ensure that the loading amount is 0.6mg/cm2And the residual 0.5cm of the residual part is convenient for fixing an electrode clamp, and the electrode clamp is dried at room temperature to be used as an air anode of the flexible solid zinc-air battery.
(5) And (3) preparing a gel electrolyte. Weighing 2.204g of acrylic acid and 0.01g of N, N' -methylenebisacrylamide, stirring in an ice-water bath to prepare a mixed solution 1, weighing 10mL of deionized water and 5.534g of KOH (85 wt%) in the ice-water bath, stirring to prepare a KOH solution of 8.4mol/L, adding the prepared KOH solution into the mixed solution 1, continuing stirring in the ice-water bath to obtain a mixed solution 2, weighing 5mL of deionized water, adding 0.2g of K into the 5mL of deionized water2S2O8Stirring to obtain 0.3mol/L K2S2O8Solution, 80. mu.L of prepared K is weighed by a pipette2S2O8The solution was dropped into the mixed solution 2 with stirring for 30 seconds to synthesize a gel electrolyte.
(6) And (4) preparing a metal negative electrode. Respectively cleaning the polished zinc foil with deionized water and absolute ethyl alcohol, drying, cutting into 1x1.5cm2The size of the electrode is 0.5cm, and the residual amount is convenient for fixing the electrode clamp and is used as a metal cathode of the zinc-air battery.
(7) And (5) preparing a zinc-air battery. Cutting the aluminum plastic film into 1x1.5cm2Size, sticking double-sided adhesive tape, cutting a hole in the middle to facilitate air electrode contact, sticking the flexible carbon cloth air anode dried at room temperature in the step (4) on the double-sided adhesive tape for firm sticking, and cutting the gel electrolyte in the step (5) into 1x1cm2The size of the metal negative electrode is attached to the air electrode, the metal negative electrode polished in step (6) is attached to the gel electrolyte, the metal negative electrode is separated by the gel electrolyte and does not contact with the air negative electrode to form a short circuit, and the metal negative electrode is attached with 1x1.5cm of double-sided adhesive tape2And (3) lightly pressing the aluminum plastic film with the size to prepare the flexible solid zinc-air battery with the sandwich structure.
Example 2
A comparative sample was prepared substantially in the same manner as in example 1, except that the plasma treatment was not performed after the tip ultrasonic exfoliation treatment, to obtain a comparative sample catalyst, FePSe3Nanosheets.
(1)FePSe3And (4) preparing crystals. Fe powder (50nm), P powder and Se powder were weighed in a molar mass ratio of 1: 3 to total 500mg, sealed in a quartz tube under vacuum, having an inner diameter of about 16mm and a length of about 15cm, heated to 750 ℃ in a box furnace using CVT method, and kept for 7 days at a temperature rise rate of 2 ℃/min. Taking out the block FePSe after cooling to room temperature3The crystals were ground to a homogeneous powder and stored in a dry cabinet.
(2)FePSe3And (3) preparing the nano sheet. 200mg of FePSe in lump form are weighed3Dispersing the crystal in absolute ethyl alcohol solution for ultrasonic treatment to obtain uniformly dispersed black FePSe3The ethanol mixed solution was stripped by tip sonication, the mixed solution was centrifuged 3 times at 1000rpm for half an hour each, the supernatant was separated and collected, first 3 times at 4000rpm for half an hour each with deionized water, and then 3 times at 6000rpm with absolute ethanol for half an hour each. Finally collecting the precipitate, and placing the precipitate in a vacuum drying oven at 60 ℃ for 12 hours to obtain dried FePSe3Nanosheets.
(3) And preparing an air electrode. Taking 7mg of prepared FePSe3Uniformly grinding the nano-sheets and 3mg of conductive carbon powder in a mortar, adding the nano-sheets and the 3mg of conductive carbon powder into a mixed solution of 50 mu L of Nafion, 760 mu L of absolute ethyl alcohol and 190 mu L of deionized water, carrying out ultrasonic treatment for 1 hour to obtain a uniformly dispersed ink-like solution, soaking the whole carbon cloth in concentrated nitric acid and carrying out ultrasonic pretreatment on the carbon cloth by using the deionized water, and drying the carbon clothCutting carbon cloth into 1x1.5cm2Size, 200. mu.L of ink solution was slowly dropped at 1X1cm2On the front and back sides, the amount of the drop on each side is ensured to reach 100 mu L so as to ensure that the loading amount is 0.6mg/cm2And the residual 0.5cm of the residual part is convenient for fixing an electrode clamp, and the electrode clamp is dried at room temperature to be used as an air anode of the flexible solid zinc-air battery.
(4) And (3) preparing a gel electrolyte. Weighing 2.204g of acrylic acid and 0.01g of N, N' -methylenebisacrylamide, stirring in an ice-water bath to prepare a mixed solution 1, weighing 10mL of deionized water and 5.534g of KOH (85 wt%) in the ice-water bath, stirring to prepare a KOH solution of 8.4mol/L, adding the prepared KOH solution into the mixed solution 1, continuing stirring in the ice-water bath to obtain a mixed solution 2, weighing 5mL of deionized water, adding 0.2g of K into the 5mL of deionized water2S2O8Stirring to obtain 0.3mol/L K2S2O8Solution, 80. mu.L of prepared K is weighed by a pipette2S2O8The solution was dropped into the mixed solution 2 with stirring for 30 seconds to synthesize a gel electrolyte.
(5) And (4) preparing a metal negative electrode. Respectively cleaning the polished zinc foil with deionized water and absolute ethyl alcohol, drying, cutting into 1x1.5cm2The size of the electrode is 0.5cm, and the residual amount is convenient for fixing the electrode clamp and is used as a metal cathode of the zinc-air battery.
(6) And (5) preparing a zinc-air battery. Cutting the aluminum plastic film into 1x1.5cm2Size, sticking double-sided adhesive tape, cutting a hole in the middle to facilitate air electrode contact, sticking the flexible carbon cloth air anode dried at room temperature in the step (3) on the double-sided adhesive tape for firm sticking, and cutting the gel electrolyte in the step (4) into pieces of 1x1cm2The size of the metal negative electrode is attached to the air electrode, the metal negative electrode polished in step (5) is attached to the gel electrolyte, the metal negative electrode is separated by the gel electrolyte and does not contact with the air negative electrode to form a short circuit, and the metal negative electrode is attached with 1x1.5cm of double-sided adhesive tape2And (3) lightly pressing the aluminum plastic film with the size to prepare the flexible solid zinc-air battery with the sandwich structure.
Claims (4)
1. High-efficiency zinc air batteryDual-function electrocatalyst FePSe for air electrode of cell3The preparation method is characterized by comprising the following steps:
(1)FePSe3preparation of crystals: sealing Fe powder, P powder and Se powder in a quartz tube by using a chemical vapor deposition method, heating, taking out and obtaining FePSe3Grinding the crystal and storing in a drying cabinet;
(2)FePSe3preparing a nano sheet: FePSe obtained in the step (1)3Dispersing the crystal in absolute ethyl alcohol, carrying out ultrasonic stripping by using tip ultrasonic treatment, and centrifuging to obtain FePSe3Nanosheets;
(3)FePSe3-preparation of O nanoplates: taking the FePSe obtained in the step (2)3Nanosheets in Ar/O2And (4) treating the mixture by using plasma under an atmosphere, and finally taking out the mixture to be stored in a drying cabinet.
2. The bifunctional catalyst FePSe of air electrode of high-efficiency zinc-air battery as claimed in claim 13The method is characterized in that: FePSe in the step (1)3The crystals are layered, monoclinic, and can be exfoliated into thin layers.
3. The bifunctional catalyst FePSe of air electrode of high-efficiency zinc-air battery as claimed in claim 13The method is characterized in that: respectively centrifuging at different rotating speeds in the step (2) to obtain ultrathin FePSe with the size of about 200nm3Nanosheets. By peeling the crystals into two-dimensional nanosheets, the specific surface area becomes large and more catalytically active sites are exposed.
4. The bifunctional catalyst FePSe of air electrode of high-efficiency zinc-air battery as claimed in claim 13The method is characterized in that: in the step (3), the chemical structure is changed and an electronic effect is generated by doping heteroatom, and O atom is introduced into the ultrathin nano-chip to induce the electrocatalytic activity.
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Citations (2)
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|---|---|---|---|---|
| US20100130017A1 (en) * | 2008-11-21 | 2010-05-27 | Axcelis Technologies, Inc. | Front end of line plasma mediated ashing processes and apparatus |
| CN109847732A (en) * | 2018-11-21 | 2019-06-07 | 电子科技大学 | A kind of method and application preparing titanium dioxide nanoplate based on corona treatment |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100130017A1 (en) * | 2008-11-21 | 2010-05-27 | Axcelis Technologies, Inc. | Front end of line plasma mediated ashing processes and apparatus |
| CN109847732A (en) * | 2018-11-21 | 2019-06-07 | 电子科技大学 | A kind of method and application preparing titanium dioxide nanoplate based on corona treatment |
Non-Patent Citations (2)
| Title |
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| DEBDYUTI MUKHERJEE ET AL.: ""Few-Layer Iron Selenophosphate, FePSe3: Efficient Electrocatalyst toward Water Splitting and Oxygen Reduction Reactions"", 《ACS APPL. ENERGY MATER.》 * |
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Application publication date: 20211207 |