CN108987125B - Perovskite stannate supercapacitor electrode material, preparation method and application - Google Patents
Perovskite stannate supercapacitor electrode material, preparation method and application Download PDFInfo
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- Y02E60/13—Energy storage using capacitors
Abstract
The invention provides a perovskite stannate supercapacitor electrode material with high specific capacitance and a preparation method thereof. The electrode material has a perovskite structure and has a chemical formula of La x M1‑ x SnO3(M is a divalent metal atom such as Ba, Sr, Zn, etc., and is not more than 0xStannate nano powder less than or equal to 0.1), and the material is applied to a super capacitor as an electrode material. The stannate nano material is prepared by combining a citric acid sol-gel method and an in-situ coprecipitation method with a low-temperature roasting reaction, the size of nano powder crystal grains is 1-100nm, and the super capacitor electrode prepared by the stannate nano material has high specific capacitance, good chemical stability and simple material preparation method, and is suitable for large-scale production.
Description
Technical Field
The invention relates to an application of a barium stannate nano material with a perovskite structure and high specific capacitance in a super capacitor, belonging to the field of super capacitors.
Background
With the development of the 21 st century, people have higher and higher requirements on energy utilization, and power supplies used in aerospace, national defense science and technology, new energy power generation and wearable and movable electronic equipment in life are required to have high power density and high energy density. The development and development of new energy storage technologies are also ongoing, and at the same time, super capacitors are widely used and studied as an energy storage element. Compare in traditional parallel plate capacitor, ultracapacitor system's specific capacitance is higher, compares with traditional secondary battery simultaneously, and ultracapacitor system has higher power density, great output current, better performances such as quick charge-discharge, and cycle life is greater than the life-span of battery simultaneously far away, consequently becomes a big important part in the new forms of energy application field.
The super capacitor is a novel component for storing energy through an electrochemical process generated on an interface formed between an electrode and electrolyte, is an energy storage device between a traditional capacitor and a rechargeable battery, has the characteristics of quick charge and discharge of the capacitor, has the energy storage performance of the battery, has extremely high power density, but has relatively low energy density, and how to improve the energy density of the super capacitor becomes a hot problem for the research of the energy field in recent years.
The specific capacity and the voltage window of the electrode material in the super capacitor are main factors determining the energy density of the super capacitor, so the selection of the electrode material becomes a key point for improving the energy density of the super capacitor. The carbon material has the characteristics of good specific surface area, good conductivity, wide material source, environmental friendliness and the like, and is widely applied to supercapacitors for charging and discharging double electric layers formed by an electrode electrolyte interface. In contrast, metal oxides store energy through the faraday process with higher specific capacitance, for example: RuO2The theoretical specific capacity of the catalyst can reach 200F/g, but because the resource of ruthenium is scarce and the ruthenium is expensive, transition metal oxides such as: MnO2、NiO、Co2O3、NiCo2O4The electrochemical energy storage can be realized due to the valence change of the transition metal, the specific capacitance is larger, but the improvement of the electrochemical performance is limited due to the poorer conductivity.
In recent research reports, perovskite type oxides gradually attract attention as a class of supercapacitor electrode materials, and perovskite type oxide materials are gradually applied to supercapacitors due to good conductivity and very stable chemical properties and can generate pseudo-capacitance storage charges through oxygen-inserted reversible redox reactions in ionic solutions. For perovskite type oxides, the research on the electrochemical properties of the perovskite type oxides is still in the beginning, and the application of perovskite materials to supercapacitors is less reported, and the research relates toThe material is LaMnO3、La x Sr x1-Co0.1Mn0.9O3-δEtc.; the A site doping of the perovskite type material improves the conductivity of the material, and the electrochemical performance of the perovskite type oxide can be further improved. We note that these reported ABOs3The electrode material of the oxide super capacitor with the perovskite structure either shows high specific capacitance and small window voltage or has large window voltage but not high specific capacitance, so that the recent performance improvement of the super capacitor depends on preparing the electrode material with both high window voltage and large specific capacitance.
Disclosure of Invention
The invention aims to overcome the defects in the prior art, the perovskite stannate material is used as the electrode material of the super capacitor, and the stannate and stannate-doped nano powder are obtained by adopting two different preparation methods, so that the specific capacitance of the material is improved. The material is different from common perovskite type transition metal oxide (electrochemical energy storage is realized by transition metal valence change), the perovskite type stannate material is composed of main group elements, and the supercapacitor electrode made of the material can realize a larger voltage window with higher specific capacitance and higher energy density.
The technical scheme of the invention is as follows: the perovskite stannate is: barium stannate (BaSnO)3) Strontium stannate (SrSnO)3) Zinc stannate (ZnSnO)3) And lanthanum doped stannate La x M x1-SnO3(M is a divalent group of Ba, Sr, Zn,xin the range of 0-0.1); the perovskite stannate nano material is prepared by adopting a sol-gel method and an in-situ coprecipitation method and is used as an electrode material of a super capacitor, so that the energy density of the super capacitor is improved.
The perovskite stannate nano material prepared by the sol-gel method and the in-situ coprecipitation method has the grain size of 1-100 nm.
The process for preparing the perovskite stannate nano material by adopting the sol-gel method mainly comprises the following steps: tin (Sn)Preparation of an ion neutral solution of divalent metal ions (e.g. Ba)2+) The neutral solution is prepared, the metal salt solution is mixed to prepare sol, the colloid is dried to prepare dry gel, and the dry gel is ground into powder which is baked into a phase. (1) And (4) preparing a tin solution. Weighing a certain amount of stannous oxalate in a beaker, adding a small amount of ultrapure water, stirring on a magnetic stirrer, dispersing to form uniform suspension, then placing on a hot plate at 80 ℃, adding excessive hydrogen peroxide solution (the mass ratio of the stannous oxalate to the hydrogen peroxide is 1: 80), and stirring until dissolving to prepare transparent solution containing tin ions. And adding a certain amount of citric acid, wherein the mass ratio of tin ions to the citric acid is 1: 4-1: 8, stirring until the tin ions are dissolved, placing the mixture in a 80 ℃ water bath kettle, stirring while heating and refluxing for 1h, then placing the solution in an ice water bath for 3-5 min, then dropwise adding a La ion solution according to the stoichiometric amount, and finally adjusting the pH value to 7 by adopting concentrated ammonia water. (2) Divalent metal ion M2+And (4) preparing a solution. According to the stoichiometric proportion, nitrate or hydroxide (such as barium hydroxide octahydrate, strontium nitrate and zinc nitrate) of divalent metal ions is weighed, dissolved in 3mol/L citric acid solution while stirring, the mass ratio of the divalent metal ions to the citric acid is 1: 4-1: 8, the solution is transparent, and then concentrated ammonia water is added dropwise to adjust the pH value to 7. (3) And (3) preparing sol. Mixing the neutral solution of tin ions and the neutral solution of divalent metal ions, adding a small amount of glycol, and stirring the mixed solution in a water bath kettle at 85-95 ℃ for 1h to form sol with obvious Tyndall effect. (4) And drying the sol in an oven at 180 ℃ for 24 hours to form xerogel. (5) And grinding the dry gel into powder, and roasting at high temperature to obtain the perovskite stannate nano powder. The roasting procedure is as follows: keeping the temperature at 350 ℃ for 2.5h, keeping the temperature at 550 ℃ for 5h, keeping the temperature at 630 ℃ for 2.5h, keeping the temperature at 650-850 ℃ for 3-8 h, and cooling to room temperature.
The process for preparing perovskite stannate nano powder by the in-situ coprecipitation method comprises the following steps: firstly, weighing a certain amount of stannous oxalate in a beaker, adding a very small amount of ultrapure water to submerge the stannous oxalate, stirring on a magnetic stirrer to disperse the stannous oxalate into turbid liquid, then placing the turbid liquid on a hot plate at 80 ℃ for heating, adding excessive hydrogen peroxide to stir until the hydrogen peroxide is dissolved to obtain a clear and transparent solution, and then dropwise adding 30% concentrated ammonia water at room temperature to adjust the pH value to about 10. Then, a corresponding amount of carbonate of a divalent metal (for example, barium carbonate) is stoichiometrically weighed and added to the above-mentioned alkaline tin ion solution to form a suspension. And (4) heating the suspension in a water bath at 95 ℃, and standing and aging for 5 hours. Finally, filtering and washing by absolute ethyl alcohol, drying the precipitate for 8h at 120 ℃, grinding and then placing in a muffle furnace for roasting, wherein the roasting procedure is to preserve heat at 250 ℃ for 30 min, preserve heat at 450-650 ℃ for 2-7 h, and then furnace cooling is carried out to obtain stannate (such as barium stannate) nano powder.
When the perovskite stannate and lanthanum-doped stannate nano material is used as an electrode active substance in a super capacitor, the electrode manufacturing process of the nano powder comprises the following steps: dispersing perovskite type nanometer powder, conductive carbon black, and adhesive (such as polyvinylidene fluoride PVDF) in a proper amount of anhydrous ethanol according to a ratio of 1.5:7:1.5 to form a uniform dispersion system, coating on a conductive substrate (foamed nickel), drying at 60-100 deg.C, and pressing into 1 cm2The mass of the active material on the electrode slice is 1-3 mg/cm2. And (4) soaking the dried electrode slice in electrolyte for 24h for activation to obtain the super capacitor electrode with electrochemical activity.
The electrochemical performance test method of the perovskite stannate supercapacitor electrode material comprises the steps of fixing an electrode slice coated with perovskite stannate nano materials as a working electrode, a reference electrode and a platinum slice electrode in an electrolytic cell filled with KOH or LiOH electrolyte to form a three-electrode system for cyclic voltammetry scanning test.
The invention has the beneficial effects that:
the perovskite stannate nano powder is a super capacitor electrode material, has stable chemical property and higher specific capacitance, and the material preparation method has simple process and is suitable for large-scale production.
Description of the drawings:
FIG. 1 uses sol-gelBaSnO prepared by glue method through reaction at different temperatures3X-ray diffraction patterns of (a);
FIG. 2 shows BaSnO prepared by calcination at 500 ℃ by coprecipitation3X-ray diffraction patterns of (a);
FIG. 3 La0.05Ba0.95SnO3Cyclic voltammetry curves of the electrode measured in KOH electrolyte solutions of different concentrations at a voltage scan rate of 120 mV/s;
FIG. 4 La0.05Ba0.95SnO3Cyclic voltammograms of the electrodes measured in 4 mol/L LiOH electrolyte at different voltage scan rates.
The specific implementation mode is as follows:
example 1: preparation of perovskite stannate BaSnO by sol-gel method3A material.
The process comprises the following steps: 10mmol of stannous oxalate is weighed into a beaker, about 2ml of ultrapure water is added, the mixture is stirred on a magnetic stirrer to be dispersed into suspension, then the suspension is placed on a hot plate at 80 ℃, 80ml of hydrogen peroxide (30%) is added, and the mixture is stirred until the solution is dissolved, so that a transparent and clear solution is obtained. Then adding 60mmol of citric acid, stirring until the citric acid is dissolved, heating and refluxing in a water bath for 1h while stirring in a water bath kettle at the temperature of 80 ℃, and then placing the solution in an ice water bath, dropwise adding concentrated ammonia water, and adjusting the pH value to 7. Weighing 10mmol barium hydroxide octahydrate, stirring and dissolving in 3mol/L citric acid solution, Ba2+And the amount ratio of the citric acid to the citric acid is 1:6, so as to obtain a clear and transparent solution, and dropwise adding concentrated ammonia water to adjust the pH value to 7. Mixing the neutral solution of tin ions and the neutral solution of barium ions, adding 5ml of ethylene glycol, and placing the mixed solution in a water bath kettle to stir in a water bath at the temperature of 92 ℃ for 1 h. And then, drying the prepared colloid in an oven at 180 ℃ for 24 hours to obtain brown black xerogel. Grinding the dry gel into powder, and roasting at high temperature, wherein the roasting procedure is as follows: keeping the temperature at 350 ℃ for 2.5h, keeping the temperature at 550 ℃ for 5h, keeping the temperature at 630 ℃ for 2.5h, and keeping the temperature at 650 ℃, 750 ℃, 800 ℃ and 850 ℃ for 8h respectively to obtain BaSnO prepared by reaction at different roasting temperatures3The nano powder of (1).
FIG. 1 shows BaSnO prepared at different temperatures3X-ray diffraction pattern of material。
Example 2: preparation of perovskite stannate BaSnO by coprecipitation method3A material.
Weighing 2mmol of stannous oxalate in a beaker, adding about 2ml of ultrapure water, stirring on a magnetic stirrer to disperse the stannous oxalate into suspension, then placing the suspension on a hot plate at 80 ℃ for heating, adding 40ml of hydrogen peroxide, stirring until the hydrogen peroxide is dissolved to obtain clear and transparent tin ion solution, then dropwise adding 30% concentrated ammonia water at room temperature to adjust the pH value to about 10, then weighing 2mmol of barium carbonate, and adding the barium carbonate into the alkaline tin solution to form the suspension. And (3) placing the suspension in a water bath at 95 ℃, standing and aging for 5h to form white precipitate, then carrying out suction filtration to separate the precipitate, adding absolute ethyl alcohol to wash the precipitate, filtering the precipitate, drying the precipitate in an oven at 120 ℃ for 8h, taking out the dried precipitate, reacting at 500 ℃ for 4h, and cooling the dried precipitate along with the oven.
FIG. 2 shows BaSnO prepared at 500 deg.C3X-ray diffraction pattern of the material, showing BaSnO3Has standard perovskite structure and can be prepared at 500 ℃.
Example 3: la0.05Ba0.95SnO3And as an active material for use in an electrode for a supercapacitor.
9.5mmol of stannous oxalate is weighed into a beaker, about 2ml of ultrapure water is added, the mixture is stirred on a magnetic stirrer to be dispersed into suspension, then the suspension is placed on a hot plate at the temperature of 80 ℃, 80ml of hydrogen peroxide (30%) is added, and the mixture is stirred until the solution is dissolved, so that a transparent and clear solution is obtained. Adding 60mmol citric acid, stirring to dissolve, heating and refluxing in 80 deg.C water bath for 1 hr while stirring, placing the solution in ice water bath for 3min, and adding 0.5mmol La (NO)3)3The solution was then adjusted to pH 7 by dropwise addition of concentrated aqueous ammonia in an ice-water bath. Weighing 10mmol barium hydroxide octahydrate, stirring and dissolving in 3mol/L citric acid solution, Ba2+And the amount ratio of the citric acid to the citric acid is 1:6, so as to obtain a clear and transparent solution, and dropwise adding concentrated ammonia water to adjust the pH value to 7. Mixing the neutral solution of tin ions and the neutral solution of barium ions, adding 5ml of ethylene glycol, and placing the mixed solution in a water bath kettle to stir in a water bath at the temperature of 92 ℃ for 1 h. Thereafter, will makeThe prepared colloid is placed in an oven at 180 ℃ for drying for 24h to obtain brown-black xerogel. Grinding the dry gel into powder, and roasting at high temperature, wherein the roasting procedure is as follows: keeping the temperature at 350 ℃ for 2.5h, at 550 ℃ for 5h, at 630 ℃ for 2.5h, and at last at 750 ℃ for 8h to obtain La0.05Ba0.95SnO3The nano powder of (1).
La0.05Ba0.95SnO3Dispersing nanometer powder, conductive carbon black, and binder (such as polyvinylidene fluoride PVDF) in a ratio of 1.5:7:1.5 in appropriate amount of anhydrous ethanol to form uniform dispersion system, coating on foamed nickel conductive substrate, oven drying at 70 deg.C, and pressing into 1 cm2The mass of the active material on the electrode sheet is 3 mg/cm2. And (3) placing the dried electrode slice into electrolyte, soaking for 24h for activation to serve as a working electrode, fixing the working electrode together with the Hg/HgO reference electrode and the platinum slice counter electrode in electrolytic cells containing electrolytes (LiOH, KOH) with different types and concentrations to form a three-electrode system, and carrying out cyclic voltammetry scanning test.
FIG. 3 is La0.05Ba0.95SnO3Cyclic voltammetry curves of the electrode measured in KOH electrolyte solutions of different concentrations at a voltage scan rate of 120 mV/s;
FIG. 4 is La0.05Ba0.95SnO3Cyclic voltammograms of the electrodes measured in 4 mol/L LiOH electrolyte at different voltage scan rates.
Claims (2)
1. A preparation method of a perovskite stannate supercapacitor electrode material is characterized by comprising the following steps: the perovskite type stannate is lanthanum-doped stannate La x M x1-SnO3Wherein M is divalent Ba, Sr, Zn,xin the range of 0.05-0.1, the grain size of the nano powder is 1-100 nm;
the preparation method comprises the following steps:
(1) preparing a neutral solution of tin ions: weighing a certain amount of stannous oxalate in a beaker, adding a small amount of ultrapure water, stirring on a magnetic stirrer, dispersing to form uniform suspension, then placing on a hot plate at 80 ℃, adding excessive hydrogen peroxide solution, stirring until dissolving, and preparing transparent solution containing stannic ions, wherein the mass ratio of the stannous oxalate to the hydrogen peroxide is 1: 80; adding a certain amount of citric acid, wherein the mass ratio of tin ions to citric acid is 1: 4-1: 8, stirring until the tin ions and the citric acid are dissolved, placing the mixture in a 80 ℃ water bath kettle, stirring while heating and refluxing for 1h, then placing the solution in an ice water bath for 3-5 min, then dropwise adding a La ion solution according to the stoichiometric amount, and finally adjusting the pH value to 7 by adopting concentrated ammonia water;
(2) divalent metal ion M2+Preparing a neutral solution: weighing nitrate or hydroxide of divalent metal ions according to a corresponding proportion according to a stoichiometric amount, dissolving the nitrate or hydroxide into 3mol/L citric acid solution while stirring to ensure that the mass ratio of the divalent metal ions to the citric acid is 1: 4-1: 8 to obtain transparent solution, and then dropwise adding concentrated ammonia water to adjust the pH value to 7;
(3) mixing metal salt solutions to prepare sol; mixing the neutral solution of tin ions and the neutral solution of divalent metal ions, adding a small amount of glycol, stirring the mixed solution in a water bath kettle at 85-95 ℃ for 1h to form sol with obvious Tyndall effect;
(4) drying the colloid to obtain dry gel: drying the sol in an oven at 180 ℃ for 24h to form xerogel;
(5) grinding the dry gel into powder, baking and forming phases: grinding the dry gel into powder, and roasting at high temperature to prepare perovskite stannate nano powder; the roasting procedure is as follows: keeping the temperature at 350 ℃ for 2.5h, keeping the temperature at 550 ℃ for 5h, keeping the temperature at 630 ℃ for 2.5h, keeping the temperature at 650-850 ℃ for 3-8 h, and cooling to room temperature.
2. The method according to claim 1, wherein the hydroxide is barium hydroxide octahydrate, and the nitrate is strontium nitrate or zinc nitrate.
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| CN113769779B (en) * | 2021-08-16 | 2023-12-29 | 中化学朗正环保科技有限公司 | Photocatalyst for treating sewage containing amine organic matters, and preparation method and application thereof |
| CN114408963B (en) * | 2022-01-14 | 2022-12-09 | 中国科学院地球环境研究所 | Method for preparing perovskite oxide nano material by microwave method |
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