CN103578785A - Multi-hole nanometer copper oxide composite material, method for preparing same, supercapacitor electrodes and supercapacitor - Google Patents

Multi-hole nanometer copper oxide composite material, method for preparing same, supercapacitor electrodes and supercapacitor Download PDF

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Publication number
CN103578785A
CN103578785A CN201310485740.4A CN201310485740A CN103578785A CN 103578785 A CN103578785 A CN 103578785A CN 201310485740 A CN201310485740 A CN 201310485740A CN 103578785 A CN103578785 A CN 103578785A
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composite material
cupric oxide
oxide composite
porous nano
preparation
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张小俊
南红红
马文勤
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Anhui Normal University
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Anhui Normal University
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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
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    • Y02E60/13—Energy storage using capacitors

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Abstract

The invention relates to a multi-hole nanometer copper oxide composite material, a method for preparing the multi-hole nanometer copper oxide composite material, supercapacitor electrodes and a supercapacitor. Multi-hole nanometer copper oxide materials directly grow on a copper substrate according to a hydrothermal method to acquire the multi-hole nanometer copper oxide composite material capable of being directly used for making the supercapacitor electrodes. Good conductivity of the metal copper substrate is combined with the superhigh capacitance performance of the nano copper oxide materials to improve the specific capacity of the supercapacitor and prolong the cycle life of the supercapacitor.

Description

A kind of porous nano cupric oxide composite material and preparation method thereof, electrode of super capacitor and ultracapacitor
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of porous nano cupric oxide composite material and preparation method thereof, electrode of super capacitor and ultracapacitor.
Background technology
Along with ultracapacitor the continuous application in the fields such as mobile communication, information technology, Aero-Space and science and techniques of defence with and unique large capacity, large electric current fast charging and discharging and the high features such as service life cycle, be subject to common people's extensive favor, cause many novel electrode material for super capacitor be in succession found and apply.At present, conventional electrode material for super capacitor comprises: material with carbon element class electrode material, conducting polymer class electrode material, metal oxide electrode material etc.Because various single electrode materials have shortcoming separately, as poorly conductive, capacity is little, and electrode of super capacitor preparation difficulty waits and is difficult to the application requirements that reaches higher.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of porous nano cupric oxide composite material and preparation method thereof, electrode of super capacitor and ultracapacitor, the present invention uses hydro thermal method directly to make porous nano copper oxide material be grown in copper substrate, obtain a kind of porous nano cupric oxide composite material, can be directly used in structure electrode of super capacitor, the good conductive ability of oxide array on metallic copper substrate is combined with the ultra-high capacity type of copper oxide nano material, realize the raising of ultracapacitor specific capacity, the prolongation of cycle life.
The technical solution used in the present invention is:
A cupric oxide composite material, consists of the porous nano cupric oxide of growing in copper substrate, and porous nano cupric oxide is three-dimensional network shape and is laid in copper substrate.
A preparation method for porous nano cupric oxide composite material, step comprises:
A, base material copper is cleaned up; Cleaning method, for base material copper is put into acetone, ethanol, watery hydrochloric acid, water successively, carries out Ultrasonic Cleaning; The ultrasonic cleaning time is respectively 10-15min, described watery hydrochloric acid concentration >=2mol/L;
B, liquor potassic permanganate is added in reactor, then base material copper is immersed in liquor potassic permanganate to closed reactor, at 50-150 ℃, react 2-8h, be cooled to room temperature, take out reacted base material copper and cleaned up, drying at room temperature, makes porous nano cupric oxide composite material; Described liquor potassic permanganate concentration is 0.001-0.01mol/L; Described cleaning is cleaned water and absolute ethyl alcohol.
, use the preparation of porous nano cupric oxide composite material.
, use the electrode preparation that comprises porous nano cupric oxide composite material.
Porous nano cupric oxide composite material of the present invention under potassium permanganate strong oxidizing property environment, adopts water to do reaction dissolvent based on base material copper, and hyperbaric heating makes to be prepared at the porous nano cupric oxide of copper sheet Surface Creation three-dimensional network shape.
Preparation method of the present invention compared with prior art, has reappearance high, easy and simple to handle, consumes energy low, and synthetic cost is low, and product purity is high, good dispersion, good crystalline and can control, and is suitable for industrial extensive preparation; Prepared porous copper oxide nano composite material has larger specific area, capacity is large, decay little, as electrode of super capacitor, can make capacitor have high power density, long charge and discharge circulation life, short time that discharges and recharges, special power density and the energy density of appropriateness, long storage life, wide working range.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of the porous nano cupric oxide composite material of embodiment 1 preparation.
Fig. 2 is the electron scanning micrograph (SEM) of the porous nano cupric oxide composite material of embodiment 1 preparation.
Fig. 3 is the porous nano cupric oxide composite material of embodiment 1 preparation carries out Electrochemical Detection in alkaline solution cyclic voltammogram (CV) as electrode of super capacitor.
In figure:
1 is that electrode is swept speed for 5mV s in the sodium hydroxide solution of 0.1M -1cyclic voltammetry curve.
2 is that electrode is swept speed for 10mV s in the sodium hydroxide solution of 0.1M -1cyclic voltammetry curve.
3 is that electrode is swept speed for 20mV s in the sodium hydroxide solution of 0.1M -1cyclic voltammetry curve.
4 is that electrode is swept speed for 50mV s in the sodium hydroxide solution of 0.1M -1cyclic voltammetry curve.
5 is that electrode is swept speed for 100mV s in the sodium hydroxide solution of 0.1M -1cyclic voltammetry curve.
Fig. 4 is that the porous copper oxide nano composite material of embodiment 1 preparation is carried out the electrograph that charges and discharge of Electrochemical Detection in alkaline solution kind as electrode of super capacitor.
In figure:
1 is electrode 1A g in the sodium hydroxide solution of 0.1M -1charging and discharging curve.
2 is electrode 2A g in the sodium hydroxide solution of 0.1M -1charging and discharging curve.
3 is electrode 5A g in the sodium hydroxide solution of 0.1M -1charging and discharging curve.
4 is electrode 10A g in the sodium hydroxide solution of 0.1M -1charging and discharging curve.
5 is electrode 20A g in the sodium hydroxide solution of 0.1M -1charging and discharging curve.
Fig. 5 is the electron scanning micrograph (SEM) of the porous nano cupric oxide composite material of embodiment 2 preparations.
Fig. 6 is the electron scanning micrograph (SEM) of the porous nano cupric oxide composite material of embodiment 3 preparations.
Fig. 7 is the electron scanning micrograph (SEM) of the porous nano cupric oxide composite material of embodiment 4 preparations.
Specific implementation method
Embodiment 1
A cupric oxide composite material, consists of the porous nano cupric oxide of growing in copper substrate, and porous nano cupric oxide is three-dimensional network shape and is laid in copper substrate.
A preparation method for porous nano cupric oxide composite material, step comprises:
A, copper sheet is put into acetone, ethanol, watery hydrochloric acid, water successively, carry out Ultrasonic Cleaning; In acetone, ethanol, watery hydrochloric acid, water the ultrasonic cleaning time be respectively 12,15,12,10min, described watery hydrochloric acid concentration is 3mol/L;
B, the liquor potassic permanganate of 20mL0.005mol/L being added in reactor, is then 2.5mm by cross-sectional area 2, length is that 4cm copper sheet immerses in liquor potassic permanganate, tightens reaction kettle cover, at 100 ℃, reacts 4h, is cooled to room temperature, takes out reacted copper sheet and cleans up with distilled water and absolute ethyl alcohol, drying at room temperature, makes porous copper oxide nano composite material.
, use the how empty cupric oxide composite material preparation of nanometer.
, use the electrode preparation that comprises porous nano cupric oxide composite material.
As shown in Figure 2, cupric oxide is the surface that three-dimensional network shape is laid in copper sheet to the pattern of made porous nano cupric oxide composite material.
Get 10mL0.1M NaOH solution and put into electrolysis tank as electrolyte solution, using the porous nano cupric oxide composite material of preparation in embodiment 1 as work electrode, sweeping speed for 5mV s -1time survey cyclic voltammetry curve (in Fig. 3, curve 1), then sweeping speed for 10mV s -1time survey cyclic voltammetry curve (in Fig. 3, curve 2), the like obtain sweeping speed for 20mV s -1(in Fig. 3, curve 3), 50mV s -1(in Fig. 3, curve 4), 100mV s -1(in Fig. 3, curve 5), can find out from the CV figure obtaining, fast increase voltage is linear along with sweeping.
Get 10ml0.1M NaOH solution and put into electrolysis tank as electrolyte solution, using the porous copper oxide nano composite material of preparation in embodiment 1 as work electrode, at 1A g -1time obtain charging and discharging curve (in Fig. 4, curve 1), at 2A g -1time obtain charging and discharging curve (in Fig. 4, curve 2), at 5A g -1time obtain charging and discharging curve (in Fig. 4, curve 3), at 10A g -1time obtain charging and discharging curve (in Fig. 4, curve 4), at 20A g -1time obtain charging and discharging curve (in Fig. 4, curve 5), from charging and discharging curve, can show that porous copper oxide nano composite material compares other material capacity more greatly as electrode, by calculating electrode capacity, be 709F g -1.
Embodiment 2
A cupric oxide composite material, consists of the porous nano cupric oxide of growing in copper substrate, and porous nano cupric oxide is three-dimensional network shape and is laid in copper substrate.
A preparation method for porous nano cupric oxide composite material, step comprises:
A, copper sheet is put into acetone, ethanol, watery hydrochloric acid, water successively, carry out Ultrasonic Cleaning; In acetone, ethanol, watery hydrochloric acid, water the ultrasonic cleaning time be respectively 15,10,10,15min, described watery hydrochloric acid concentration is 5mol/L;
B, the liquor potassic permanganate of 20mL0.001mol/L being added in reactor, is then 2.5mm by cross-sectional area 2, length is that 4cm copper sheet immerses in liquor potassic permanganate, tightens reaction kettle cover, at 150 ℃, reacts 8h, is cooled to room temperature, takes out reacted copper sheet and cleans up with distilled water and absolute ethyl alcohol, drying at room temperature, makes porous copper oxide nano composite material.
, directly use porous copper oxide nano composite material as electrode.
, use the electrode preparation that comprises porous nano cupric oxide composite material.
Embodiment 3
A nano composite material, consists of the porous copper oxide nano material of growing in copper substrate.
A preparation method for porous copper oxide nano composite material, step comprises:
A, copper sheet is put into acetone, ethanol, watery hydrochloric acid, water successively, carry out Ultrasonic Cleaning; In acetone, ethanol, watery hydrochloric acid, water the ultrasonic cleaning time be respectively 15,10,15,15min, described watery hydrochloric acid concentration is 4mol/L;
B, the liquor potassic permanganate of 20mL0.01mol/L being added in reactor, is then 2.5mm by cross-sectional area 2, length is that 4cm copper sheet immerses in liquor potassic permanganate, tightens reaction kettle cover, at 50 ℃, reacts 2h, is cooled to room temperature, takes out reacted copper sheet and cleans up with distilled water and absolute ethyl alcohol, drying at room temperature, makes porous copper oxide nano composite material.
, directly use porous copper oxide nano composite material as electrode.
, use the electrode preparation that comprises porous nano cupric oxide composite material.
Embodiment 4
A nano composite material, consists of the porous copper oxide nano material of growing in copper substrate.
A preparation method for porous copper oxide nano composite material, step comprises:
A, copper sheet is put into acetone, ethanol, watery hydrochloric acid, water successively, carry out Ultrasonic Cleaning; In acetone, ethanol, watery hydrochloric acid, water the ultrasonic cleaning time be respectively 10,10,15,15min, described watery hydrochloric acid concentration is 3mol/L;
B, the liquor potassic permanganate of 20mL0.01mol/L being added in reactor, is then 2.5mm by cross-sectional area 2, length is that 4cm copper sheet immerses in liquor potassic permanganate, tightens reaction kettle cover, at 120 ℃, reacts 4h, is cooled to room temperature, takes out reacted copper sheet and cleans up with distilled water and absolute ethyl alcohol, drying at room temperature, makes porous copper oxide nano composite material.
, directly use porous copper oxide nano composite material as electrode.
, use the electrode preparation that comprises porous nano cupric oxide composite material.

Claims (6)

1. a porous nano cupric oxide composite material, consists of the porous nano cupric oxide of growing in copper substrate, and porous nano cupric oxide is three-dimensional network shape and is laid in copper substrate.
2. a preparation method for porous nano cupric oxide composite material, step comprises:
A, base material copper is cleaned up;
B, liquor potassic permanganate is added in reactor, then base material copper is immersed in liquor potassic permanganate to closed reactor, at 50-150 ℃, react 2-8h, be cooled to room temperature, take out reacted base material copper and cleaned up, drying at room temperature, makes porous nano cupric oxide composite material; Described liquor potassic permanganate concentration is 0.001-0.01mol/L; Described cleaning is cleaned water and absolute ethyl alcohol.
3. preparation method as claimed in claim 2, is characterized in that: in described step a, cleaning method, for base material copper is put into acetone, ethanol, watery hydrochloric acid, water successively, carries out Ultrasonic Cleaning; The ultrasonic cleaning time is respectively 10-15min, described watery hydrochloric acid concentration >=2mol/L.
4. preparation method as claimed in claim 2, is characterized in that: described step b cleans and uses distilled water and absolute ethyl alcohol to clean.
5. an electrode of super capacitor, is used the preparation of porous nano cupric oxide composite material.
6. a super capacitor, is used the electrode preparation that comprises porous nano cupric oxide composite material.
CN201310485740.4A 2013-10-16 2013-10-16 Multi-hole nanometer copper oxide composite material, method for preparing same, supercapacitor electrodes and supercapacitor Pending CN103578785A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103871752A (en) * 2014-03-19 2014-06-18 山东大学 Copper-oxide-based asymmetric super capacitor and manufacturing method thereof
CN105206432A (en) * 2015-09-29 2015-12-30 南京绿索电子科技有限公司 Polyaniline nanometer tube array/copper oxide/manganese dioxide composite material electrode and manufacturing method and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102706936A (en) * 2012-03-15 2012-10-03 安徽师范大学 Preparation method of copper-copper oxide composite electrode

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102706936A (en) * 2012-03-15 2012-10-03 安徽师范大学 Preparation method of copper-copper oxide composite electrode

Non-Patent Citations (4)

* Cited by examiner, † Cited by third party
Title
JIANG ZHI-ANG等: "CuO Nanosheets Synthesized by Hydrothermal Process", 《CHIN. PHYS. LETT.》 *
LIUTAO YU等: "3D porous gear-like copper oxide and their high electrochemical performance as supercapacitors", 《CRYSTENGCOMM》 *
XIAOJUN ZHANG等: "High electrochemical performance based on ultrathin porous CuO nanobelts grown on Cu substrate as integrated electrode", 《PHYSICAL CHEMISTRY CHEMICAL PHYSICS》 *
XIAOJUN ZHANG等: "High electrochemical performance based on ultrathin porous CuO nanobelts grown on Cu substrate as integrated electrode", 《PHYSICAL CHEMISTRY CHEMICAL PHYSICS》, vol. 15, no. 2, 5 November 2012 (2012-11-05), pages 521 - 525 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103871752A (en) * 2014-03-19 2014-06-18 山东大学 Copper-oxide-based asymmetric super capacitor and manufacturing method thereof
CN103871752B (en) * 2014-03-19 2016-08-31 山东大学 A kind of oxidation cuprio asymmetric type supercapacitor and preparation method thereof
CN105206432A (en) * 2015-09-29 2015-12-30 南京绿索电子科技有限公司 Polyaniline nanometer tube array/copper oxide/manganese dioxide composite material electrode and manufacturing method and application thereof
CN105206432B (en) * 2015-09-29 2017-11-03 南京绿索电子科技有限公司 Polyaniline nanotube array/cupric oxide/manganese dioxide composite material electrode and its preparation method and application

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Application publication date: 20140212