CN101950682A - Preparation method of super-capacitor manganese oxide material - Google Patents

Preparation method of super-capacitor manganese oxide material Download PDF

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Publication number
CN101950682A
CN101950682A CN2010102772287A CN201010277228A CN101950682A CN 101950682 A CN101950682 A CN 101950682A CN 2010102772287 A CN2010102772287 A CN 2010102772287A CN 201010277228 A CN201010277228 A CN 201010277228A CN 101950682 A CN101950682 A CN 101950682A
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manganese oxide
solution
preparation
autoclave
electrode
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CN101950682B (en
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邓梅根
陈英放
冯义红
方勤
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Jiangxi University of Finance and Economics
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Jiangxi University of Finance and Economics
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    • Y—GENERAL 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
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13—Energy storage using capacitors

Abstract

The invention relates to a preparation method of super-capacitor manganese oxide material, which comprises the steps of: respectively preparing 0.25 to 0.5 mol/L of NaHSO3 or Na2SO3 solution and 0.15 to 0.25 mol/L of KMnO4 solution; pouring the NaHSO3 or Na2SO3 solution and the KMnO4 solution, with the same volume, into an autoclave; stirring for 30 minutes; putting the autoclave into a blast drying box; keeping constant temperature of 80 to 130 DEG C for 7 to 11 hours; then reducing the temperature naturally; cooling; washing; filtering; drying and grinding to obtain a manganese oxide electrode material. The invention has the advantages of simple preparation method and easy operation, and prepared manganese oxide has the characteristics of high specific surface area, high specific volume and the like.

Description

Ultracapacitor manganese oxide preparation methods
Technical field
The present invention relates to a kind of ultracapacitor manganese oxide preparation methods.
Background technology
Ultracapacitor has very application fields and enormous and latent market as novel clean energy resource element, also is subjected to the extensive concern of national governments and enterprise.According to the difference of energy storage principle, ultracapacitor can be divided into double electric layer capacitor and fake capacitance device, and the electrode material of fake capacitance device has metal oxide and conducting polymer two classes.Typical case's representative as metal oxide, the preparation manganese oxide mostly is methods such as liquid-phase reduction, sol-gel at present, the manganese oxide that the present invention uses the anion reducing agent to prepare under thermal and hydric environment has the nano bar-shape structure, very high specific area and uniform space distributes, and has the performance of excellence as the electrode material of ultracapacitor.
Summary of the invention
The object of the present invention is to provide a kind of ultracapacitor manganese oxide preparation methods, by control anion HSO 3 -Or SO 3 2-With MnO 4 -Concentration, control temperature, the time of hydro-thermal reaction simultaneously, preparation is fit to the manganese oxide that ultracapacitor uses.
The present invention is achieved like this, and it is characterized in that method step is: dispose 0.25-0.5mol/LNaHSO respectively 3Or Na 2SO 3Solution, 0.15-0.25mol/L KMnO 4Solution is got the NaHSO of equal volume 3Or Na 2SO 3Solution and liquor potassic permanganate are poured in the autoclave, stir 30min, and autoclave is put into air dry oven, and 80-130 ℃ of constant temperature 7-11h lowers the temperature afterwards naturally, obtain the manganese oxide electrode material after washing after cooling off, filtration, drying, the grinding.
Advantage of the present invention is: the preparation method is simple, and is easy to operate, and the manganese oxide of preparation has high-specific surface area, characteristics such as high specific volume.
Description of drawings
Fig. 1 is embodiment 1 a gained manganese oxide SEM photo.
Fig. 2 is the electrode of super capacitor cyclic voltammetric test curve that embodiment 1 gained manganese oxide is made.
Fig. 3 is the electrode of super capacitor constant current charge-discharge curve that embodiment 1 gained manganese oxide is made.
Fig. 4 is embodiment 2 gained manganese oxide SEM photos.
Fig. 5 is embodiment 2 gained manganese oxide XRD curves.
Fig. 6 is the electrode of super capacitor constant current charge-discharge curve that embodiment 2 gained manganese oxide are made.
Embodiment
Embodiment 1
Dispose 0.3mol/L NaHSO respectively 3Solution, 0.2mol/L KMnO 4Solution.Get the anion solutions and the liquor potassic permanganate of equal volume and pour in the autoclave, stir 30min, autoclave is put into air dry oven, 130 ℃ of constant temperature 10h lower the temperature afterwards naturally, obtain the manganese oxide electrode material after washing after cooling off, filtration, drying, the grinding.As shown in Figure 1, prepare the nanometer rods that manganese oxide is diameter 20-30nm length 1 μ m.
The preparation of manganese oxide electrode: it is even that manganese oxide, carbon black and ptfe emulsion are pressed 65: 30: 5 mixed of mass ratio, the furnishing pulpous state, and evenly be coated on the nickel foam, with 15MPa pressure tablet forming, again electrode slice is put into 120 ℃ of vacuum drying chamber vacuumizes 24 hours with powder compressing machine.With the saturated calomel electrode is reference electrode, is to electrode with 2 * 2cm platinized platinum electrode, and electrolyte is 1M (NH 4) 2SO 4Solution carries out the cyclic voltammetric and the constant current charge-discharge characteristic test of manganese oxide electrode at German IM6ex electrochemical workstation.This sample is in the scope interscan of voltage-0.5～0.5V, sweep speed be 50 and during 100mv/s cyclic voltammetry curve present rectangle, as shown in Figure 2.Fig. 3 is that electrode is with 20mA/cm 2The test curve of gained during the constant current charge-discharge test, the specific volume of sample reaches 279.13F/g.
Embodiment 2
Dispose 0.3mol/L NaHSO respectively 3Or Na 2SO 3Solution, 0.2mol/L KMnO 4Solution.Getting the anion solutions and the liquor potassic permanganate of equal volume pours in the autoclave, stir 30min, autoclave is put into air dry oven, naturally cooling after 90 ℃ of constant temperature 11h, obtain the manganese oxide electrode material after cooling off back washing, filtration, drying, grinding, its pattern also is the nano bar-shape structure that presents diameter 20-30nm length 1 μ m as shown in Figure 4.Fig. 5 is the XRD figure spectrum of this manganese oxide, this figure diffraction maximum and α-MnO 2Diffraction maximum fit like a glove.
The preparation of manganese oxide electrode: it is even that manganese oxide, carbon black and ptfe emulsion are pressed 65: 30: 5 mixed of mass ratio, the furnishing pulpous state, and evenly be coated on the nickel foam, with 15MPa pressure tablet forming, again electrode slice is put into 120 ℃ of vacuum drying chamber vacuumizes 24 hours with powder compressing machine.With the saturated calomel electrode is reference electrode, is to electrode with 2 * 2cm platinized platinum electrode, and electrolyte is 1M (NH 4) 2SO 4Solution carries out the cyclic voltammetric and the constant current charge-discharge characteristic test of manganese oxide electrode at German IM6ex electrochemical workstation.This electrode is in the increase along with electric current, and the attenuation rate of capacity is very low, as shown in Figure 6.With 10mA/cm 2During the constant current charge-discharge test, the specific volume of sample reaches 288.26F/g.

Claims (1)

1. a ultracapacitor manganese oxide preparation methods is characterized in that method step is: dispose 0.25-0.5mol/L NaHSO respectively 3Or Na 2SO 3Solution, 0.15-0.25mol/L KMnO 4Solution is got the NaHSO of equal volume 3Or Na 2SO 3Solution and liquor potassic permanganate are poured in the autoclave, stir 30min, autoclave is put into air dry oven, the air dry oven temperature is set to 80-130 ℃, constant temperature 7-11h lowers the temperature afterwards naturally, obtains the manganese oxide electrode material after washing after cooling off, filtration, drying, the grinding.
CN2010102772287A 2010-09-09 2010-09-09 Preparation method of super-capacitor manganese oxide material Expired - Fee Related CN101950682B (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104803420A (en) * 2015-04-17 2015-07-29 同济大学 Method for preparing manganese dioxide nano-material with high ammonia gas specific response
CN112588302A (en) * 2020-12-22 2021-04-02 河池学院 alpha-MnO-containing2Photocatalytic system, preparation method and application thereof

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101281821A (en) * 2008-05-20 2008-10-08 中山大学 Nano thread-shaped manganese dioxide load carbon silica aerogel as well as preparation method and application thereof
CN101696323A (en) * 2009-10-30 2010-04-21 华南师范大学 Method for preparing polyaniline/manganese dioxide composite material for super capacitor

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101281821A (en) * 2008-05-20 2008-10-08 中山大学 Nano thread-shaped manganese dioxide load carbon silica aerogel as well as preparation method and application thereof
CN101696323A (en) * 2009-10-30 2010-04-21 华南师范大学 Method for preparing polyaniline/manganese dioxide composite material for super capacitor

Non-Patent Citations (3)

* Cited by examiner, † Cited by third party
Title
《功能材料》 20081231 邓梅根 基于阴离子还原剂制备的超级电容器用中孔MnO2研究 2002-2004 1 第39卷, 第12期 2 *
《功能材料与器件学报》 20070831 王珏 等 阴离子还原剂对超级电容器材料MnO2的物性及电容特性的影响 351-356 1 第13卷, 第4期 2 *
《功能材料与器件学报》 20091031 邓梅根 等 超级电容器用MnO2纳米棒的水热法合成和表征 503-506 1 第15卷, 第5期 2 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104803420A (en) * 2015-04-17 2015-07-29 同济大学 Method for preparing manganese dioxide nano-material with high ammonia gas specific response
CN112588302A (en) * 2020-12-22 2021-04-02 河池学院 alpha-MnO-containing2Photocatalytic system, preparation method and application thereof

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