CN107871627A - Foam copper supports high capacitance flexible electrode material of CuO nanometer sheet and preparation method thereof - Google Patents

Foam copper supports high capacitance flexible electrode material of CuO nanometer sheet and preparation method thereof Download PDF

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Publication number
CN107871627A
CN107871627A CN201610877849.6A CN201610877849A CN107871627A CN 107871627 A CN107871627 A CN 107871627A CN 201610877849 A CN201610877849 A CN 201610877849A CN 107871627 A CN107871627 A CN 107871627A
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foam copper
cuo
preparation
nanometer sheet
electrode
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CN201610877849.6A
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唐少春
史曦伶
吴娟
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Nanjing University
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Nanjing University
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    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B82NANOTECHNOLOGY
    • B82YSPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00Nanotechnology for materials or surface science, e.g. nanocomposites
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes 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
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/26Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • H01G11/28Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
    • HELECTRICITY
    • H01ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their material
    • H01G11/46Metal oxides
    • 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
    • Y02E60/13Energy storage using capacitors

Abstract

The present invention proposes the preparation method that a kind of foam copper supports the high capacitance flexible electrode material of CuO nanometer sheet, and introduces its application in terms of electrode of super capacitor.Using ammonium persulfate and sodium hydroxide as raw material, oxide etch is carried out to copper surface by one step hydro thermal method, so as to which top layer copper is converted into cupric oxide nano structure.CuO is laminated structure, thickness about 20nm, width about 200nn, and nanometer sheet intersects the surface for being covered in foam copper three-dimensional framework of uniform close, so as to form cellular CuO clads;And the thickness of CuO clads can accurately be controlled by the concentration of reaction time and mixed solution;Prepared foam copper supports CuO nanometer sheet material and may be directly applied to electrode of super capacitor, without binding agent, the characteristics of it has both high specific capacitance, high circulation stability and excellent flexibility;In addition, the preparation method is simple to operate, cost is low, and easily controllable and scale.

Description

Foam copper supports high capacitance flexible electrode material of CuO nanometer sheet and preparation method thereof
Technical field
The present invention relates to a kind of preparation method of flexible super capacitor material, it is characterized in that, by one step hydro thermal method, The thin layer that cupric oxide nanometer sheet is formed is grown in foam copper substrate, has both high specific capacitance, high circulation stability and excellent so as to obtain Different flexible electrode material for super capacitor.The preparation method has simple to operate, and cost is cheap, reproducible and easily controllable The advantages of.
Background technology
With the continuous consumption of the non-renewable energy resources such as natural gas, oil, and the day that the unclean energy is brought to environment Beneficial obvious negative effect, the environmentally friendly type of the mankind, the pursuit enthusiasm of clean energy resource grow to even greater heights.Ultracapacitor has height concurrently The advantages that power density, long, safe high circulation stability and service life, it is a kind of new type of energy storage device.Electrode material is to determine Determine the key of performance of the supercapacitor and cost, selection, design and the preparation of electrode material are high-performance super capacitor research and development Emphasis.
Electrode material for super capacitor mainly has:Carbon material, metal oxide and conducting polymer.Due to oxo transition metal Compound has very high theoretical capacitance and relatively low cost, and lasting emerging of researchers is caused as electrode material Interest.RuO2、NiO、MnO2、Co3O4It is counted as very promising electrode material with CuO.Wherein, CuO is due to its non-toxic, reserves It is high, cost is low, easy preparation, paid close attention to by researchers.Especially, CuO fake capacitance characteristic carries for it as electrode material Having supplied may.Its electric property is strongly depend on pattern and size.
Traditional electrode material is to be powdered, it is necessary to binding agent and conductive additive bonding.Because electrode is that bonding forms, Therefore it is readily formed " dead volume " (Void or dead volume);It has blocked the transmission of electronics and electrolyte to electrode The diffusion of material surface, reduce the utilization rate of active material.Using porous metals as matrix, physics or chemical deposition fake capacitance Metal oxide nanostructure is to obtain high-performance, the new way of flexible super capacitor electrode.However, existing report is often In porous noble metal gold, silver superficial growth oxide, not only preparation process is cumbersome, cost is higher, and nanostructured and current collection Interface binding power between the matrix of pole is often weaker, and electric conductivity can also be affected, and is difficult to meet multiple charge and discharge cycles.Such as Electrode material growth in situ on collector, just can effectively be optimized electrode structure by fruit, make electrolyte more preferable with electrode material Ground contacts, so as to lift the utilization rate of active material.This design evaded such as production time cost long, " dead volume " and The problems such as active material and weak inter-collector adhesion.Commercial foam metal (such as foam copper) can provide a porous, connection Electrode electrolyte interface, be easy to electrolyte permeability to improve electrochemical efficiency.At present, mostly for 3-D nano, structure electricity The compounding design of pole all relies on vapor deposition, high annealing and electrochemical deposition method etc., and these methods are required for such as high The harsh experiment condition such as temperature, high pressure, complicated instrument and equipment, the raw material of high request and the problems such as be difficult to large-scale production Limitation.
The present invention, which proposes, prepares the method that CuO nanometer sheet uniformly coats foam copper electrode under a kind of temperate condition.With bubble Foam copper is matrix, oxide etch is carried out to copper surface by one step hydro thermal method, so as to which top layer copper is converted into cupric oxide nano knot Structure, and influence of the concentration of system research oxidant ammonium persulfate and sodium hydroxide to its surface topography and chemical property.
The content of the invention
The purpose of the present invention:A kind of novel preparation method of the growth copper oxide material in foam copper substrate is proposed, and is introduced Its application in terms of electrode of super capacitor.This method in foam copper substrate surfaces growth in situ cupric oxide causes electrode Active material is tightly combined with substrate, to improving stability of material important in inhibiting;Meanwhile cupric oxide sheet even structure point Cloth forms loose structure on three-dimensional substrates surface;Electrode material can directly apply to capacitor assembling, without binding agent;This A little advantages ensure that the high capacitance performance of material.In addition, the preparation method is simple to operate, cost is low, easily controllable and scale.
The technical scheme is that:The present invention passes through control surface oxygen using the foam copper of three-dimensional porous structure as matrix Change the growth for realizing CuO nanometer sheet, the flexibility of whole electrode is kept while high specific capacitance is obtained;Specifically preparation process is: Appropriate ammonium persulfate and sodium hydroxide are dissolved in deionized water successively and obtain certain density mixed solution, 30mL is mixed Close solution and one piece of rectangle foam copper foil cleaned is transferred in 50mL reactors;Reactor is put into baking oven constant At a temperature of react 15~60min;Foam copper is taken out after natural cooling, dried after being washed repeatedly with deionized water, is obtained final Product.
As preferred plan, in mixed solution the concentration range of ammonium persulfate and sodium hydroxide be respectively 30~50mM and 500~1000mM.
As preferred plan, take out 30mL mixed solutions and one piece of rectangle foam copper foil cleaned is transferred to 50mL In reactor;Foam copper substrate before the reaction successively with deionized water, absolute ethyl alcohol and 1M dilute sulfuric acids be cleaned by ultrasonic 15min with On, to remove surface and oil contaminant and oxide layer.
As preferred plan, reactor is put into baking oven and carries out hydro-thermal reaction at a constant temperature, temperature range be 100~ 160 DEG C, 15~60min of reaction time.
This new electrode material produced by the present invention, CuO are laminated structure, thickness about 20nm, width about 200nm, nanometer Piece intersects the surface for being covered in foam copper three-dimensional framework of uniform close, so as to form cellular CuO clads;And CuO The thickness of clad can accurately be controlled by the concentration of reaction time and mixed solution;Prepared foam copper supports CuO nanometer sheet material may be directly applied to electrode of super capacitor;Without binding agent, it is stable that it has both high specific capacitance, high circulation The characteristics of property and excellent flexibility;Compared with other methods, preparation method proposed by the present invention without any additive or template, into This low and easily controllable and scale.
Beneficial effects of the present invention:
(1) present invention proposes a kind of new method for preparing high capacitance flexible super capacitor electrode.
(2) template or additive need not be used, the material of specific morphology can be prepared by a step hydro-thermal reaction.
(3) compared with other method, the preparation method has advantages below:
1. preparation process is simple, easy to operate, the reaction time is short, and repeatability is high;
2. controllability is good, the thickness of CuO clads can accurately be controlled by reaction time and mixed solution concentration;
3. cost is relatively low, there is good industrial applications prospect;
4. it may extend to other preparations and large-scale production in growth in situ metal oxide materials in metallic substrates.
Brief description of the drawings:
Fig. 1 is (a) SEM and (b) XRD spectrum that embodiment 1 prepares product.
Fig. 2 is high-resolution XPS collection of illustrative plates (a) Cu2p that embodiment 1 prepares product;(b)O1s.
Fig. 3 is ammonium persulfate and naoh concentration is respectively (a) 6mM and 156mM;(b) 13mM and 313mM;(c)25mM And 625mM;(d) the SEM figures of CuO products are obtained during 50mM and 1250mM.
Fig. 4 is (a) cyclic voltammetry curve that embodiment 1 prepares electrode material;(b) constant current charge-discharge curve;(c) it is different Face capacitance under current density;(d) the capacitance conservation rate after charge and discharge cycles is repeated.
Fig. 5 is the bending performance test that embodiment 1 prepares electrode material.
Specific embodiment
The embodiment that foam copper supports CuO nanometer sheet electrode material is prepared using a step hydro-thermal reaction in the present invention It is as follows:
Embodiment 1
Foam copper carries CuO thin slice super capacitor materials:256.8mg sodium peroxydisulfates and 1.125g sodium hydroxides is molten successively For solution in deionized water, its concentration is respectively 37.5mM and 937.5mM;By 30mL mixed solutions and one piece of rectangle cleaned Foam copper foil (1 × 3cm of size2) be transferred in 50mL reactors;It is put into after reactor is tightened constant at 120 DEG C in baking oven At a temperature of react 20min.Reactor cooling is waited after completion of the reaction, sample is taken out, at 60 DEG C after being washed repeatedly with deionized water Dried under air atmosphere, obtain final product.
Fig. 1 a are the SEM figures that embodiment 1 prepares product.Foam copper is porous tridimensional network, even aperture distribution, Product is laminated structure, is uniformly distributed in foam copper substrate, is distributed independently of each other between piece, forms sheet-like array, constitutes Stable loose structure.Fig. 1 b are the XRD of product, and in addition to the three strong peak as caused by foam copper substrate, remaining diffraction maximum is all Corresponding to CuO characteristic peak, it was demonstrated that final product CuO.
Fig. 2 is product X PS spectrograms.Cu2p high-resolution XPS collection of illustrative plates (Fig. 2 a) shows that the position at three peaks is located at respectively At 961.9eV, 954.4eV and 933.6eV, it follows that the valence state of Cu elements is divalence Cu.
Embodiment 2
Ammonium persulfate, naoh concentration are respectively 6mM and 156mM, and other conditions and embodiment 1 are identical.
Embodiment 3
Ammonium persulfate, naoh concentration are respectively 13mM and 313mM, and other conditions and embodiment 1 are identical.
Embodiment 4
Ammonium persulfate, naoh concentration are respectively 25mM and 625mM, and other conditions and embodiment 1 are identical.
Embodiment 5
Ammonium persulfate, naoh concentration are respectively 50mM and 1250mM, and other conditions and embodiment 1 are identical.
Fig. 3 is that using differential responses solution concentration, (ammonium persulfate is proportional to naoh concentration to be changed embodiment 2-5 kinds Become) obtained product.Fig. 3 a are grown in foam copper substrate it can be found that product presentation sheet and the bar-shaped structure being mingled with;Figure Product is tentatively presented laminated structure in 3b, 3c, but grows and uneven;Increase with reactant concentration, obtain shown in Fig. 4 c by The flower-shape structure of CuO pieces composition, but due to the stacking of piece so that electrode " dead volume " increases, and porous reduces.From sheet with The bar-shaped uniform sheet that is mingled with shows that reactant concentration plays the role of important to product morphology to the flower-like structure stacked.
Embodiment 6
Fig. 4 a are that ammonium persulfate and naoh concentration are product under the conditions of 37.5mM and 937.5M in mixed reaction solution Scan round (CV) curve map under different scanning rates.With the increase of sweep speed, peak point current is in rising trend, and Curve shape is basically unchanged.It is worth noting that, the CV figure lines of sample are the curve close to rectangle, without obvious oxidation also Parent peak.Its reason is probably that the redox reaction that CuO/ foams copper electrode occurs is more complicated, multiple small redox peaks More blunt redox peaks have been synthesized, therefore more obvious peak is can't see in figure.When sweep speed is 20mV/s, due to electricity The reaction of pole surface is more abundant, it can be seen that slightly obvious redox peaks.Fig. 4 b are electrode constant current charge-discharge curve map, same Under one current density, the charging and discharging time is essentially identical, illustrates that the electrochemical reaction on the electrode has good invertibity. Curve is not that rectilinear form is presented, but has obvious bending, it was confirmed that the electrode shows Faraday pseudo-capacitance behavior.Fig. 4 c For the specific capacitance value under different current densities, electrode is 1mA/cm in current density2When reached 1.2F/cm2Face capacitance; 10mA/cm is increased in current density2When, capacity retention reaches 62.5%.Fig. 4 d are electrode material cycle life, and circulation is filled After the circle of electric discharge 4000, material specific capacitance value is floated near the 95% of initial value.Fig. 5 tests for electrode material bending performance, will CuO/ foam copper electrodes 45-degree-buckling, 90 °, compare its discharge curve after 135 °, electrode is after wide-angle bends 135 °, capacitance 108% before about bending, there is excellent flexibility.

Claims (7)

1. a kind of foam copper supports the preparation method of the high capacitance flexible electrode material of CuO nanometer sheet, it is characterised in that with three-dimensional The foam copper of loose structure is matrix, and the growth of CuO nanometer sheet is realized by control surface oxidation, is obtaining the same of high specific capacitance When keep the flexibility of whole electrode;Specifically preparation process is:By appropriate ammonium persulfate and sodium hydroxide be dissolved in successively from Certain density mixed solution is obtained in sub- water, the rectangle foam copper foil that 30mL mixed solutions and one piece were cleaned shifts Into 50mL. reactors;Reactor is put into baking oven reacts 15~60min at a constant temperature;By foam copper after natural cooling Take out, dried after being washed repeatedly with deionized water, obtain final product.
2. preparation method according to claim 1, it is characterised in that dissolve appropriate ammonium persulfate and sodium hydroxide successively Prepare solution in deionized water, in mixed solution the concentration range of ammonium persulfate and sodium hydroxide be respectively 30~50mM and 500~1000mM.
3. preparation method according to claim 1, it is characterised in that take out 30mL mixed solutions and one piece of length cleaned Square foam copper foil is transferred in 50mL reactors, and rectangle foam copper size of foundation base is 3cm × 1cm;Foam copper substrate exists It is cleaned by ultrasonic more than 15min with deionized water, absolute ethyl alcohol and 1M dilute sulfuric acids successively before reaction, to remove surface and oil contaminant and oxidation Layer.
4. preparation method according to claim 1, it is characterised in that reactor is put into baking oven that hydro-thermal is anti-at a constant temperature Should, temperature range is 100~160 DEG C, 15~60min of reaction time.
5. preparation method according to claim 1, it is characterised in that after reactor is cooled to room temperature, foam copper is taken out, Through washing repeatedly, then dried at 60 DEG C, obtain final product.
6. foam copper according to claim 1 supports the high capacitance flexible electrode material of CuO nanometer sheet, it is characterised in that; The sheet CuO of generation thickness about 20nm, width about 200nm, nanometer sheet intersect homoepitaxial foam copper three-dimensional framework Surface, so as to form cellular CuO clads;And the thickness of CuO clads is controllable.
7. foam copper prepared by supports CuO nanometer sheet material and may be directly applied to electrode of super capacitor, and it has both high than electricity The characteristics of appearance, high circulation stability and excellent flexibility.
CN201610877849.6A 2016-09-28 2016-09-28 Foam copper supports high capacitance flexible electrode material of CuO nanometer sheet and preparation method thereof Pending CN107871627A (en)

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CN108889264A (en) * 2018-07-13 2018-11-27 北京京盛国泰科技有限公司 A kind of preparation method of the foam copper of adsorption-decomposition function formaldehyde
CN108950585A (en) * 2018-08-03 2018-12-07 武汉工程大学 A kind of MoS2@Cu2S@foam copper composite nano materials and its preparation method and application
CN109888167A (en) * 2019-02-21 2019-06-14 三峡大学 A kind of copper-based self-supporting CuO-Cu2The preparation method of O composite array sodium ion negative electrode material
CN110504107A (en) * 2019-08-20 2019-11-26 吉林大学 A kind of nanometer combined electrode material and preparation method thereof and supercapacitor
CN110963523A (en) * 2018-09-29 2020-04-07 清华大学 Nano porous copper loaded copper oxide nanosheet array composite material and preparation method thereof
CN112897567A (en) * 2021-03-31 2021-06-04 江南大学 Preparation method of copper oxide with nanometer flower-like structure

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Publication number Priority date Publication date Assignee Title
CN108889264A (en) * 2018-07-13 2018-11-27 北京京盛国泰科技有限公司 A kind of preparation method of the foam copper of adsorption-decomposition function formaldehyde
CN108950585A (en) * 2018-08-03 2018-12-07 武汉工程大学 A kind of MoS2@Cu2S@foam copper composite nano materials and its preparation method and application
CN108950585B (en) * 2018-08-03 2020-04-17 武汉工程大学 MoS2@ Cu2S @ foam copper composite nano material and preparation method and application thereof
CN110963523A (en) * 2018-09-29 2020-04-07 清华大学 Nano porous copper loaded copper oxide nanosheet array composite material and preparation method thereof
CN110963523B (en) * 2018-09-29 2021-11-05 清华大学 Nano porous copper loaded copper oxide nanosheet array composite material and preparation method thereof
CN109888167A (en) * 2019-02-21 2019-06-14 三峡大学 A kind of copper-based self-supporting CuO-Cu2The preparation method of O composite array sodium ion negative electrode material
CN110504107A (en) * 2019-08-20 2019-11-26 吉林大学 A kind of nanometer combined electrode material and preparation method thereof and supercapacitor
CN112897567A (en) * 2021-03-31 2021-06-04 江南大学 Preparation method of copper oxide with nanometer flower-like structure

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Application publication date: 20180403