CN107887178A - A kind of nanoporous nickel vanadium manganese/oxide combination electrode and preparation method thereof - Google Patents

A kind of nanoporous nickel vanadium manganese/oxide combination electrode and preparation method thereof Download PDF

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CN107887178A
CN107887178A CN201711007381.6A CN201711007381A CN107887178A CN 107887178 A CN107887178 A CN 107887178A CN 201711007381 A CN201711007381 A CN 201711007381A CN 107887178 A CN107887178 A CN 107887178A
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preparation
combination electrode
nickel vanadium
vanadium manganese
electrode
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CN107887178B (en
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康建立
王知常
张志佳
于镇洋
乔志军
黄钦
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Tianjin Polytechnic University
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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
    • 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
    • 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
    • H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
    • 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
    • H01G11/46—Metal oxides
    • 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 discloses a kind of nanoporous nickel vanadium manganese/oxide combination electrode and preparation method thereof.The ternary composite electrode is that alloy strip is first prepared into by way of getting rid of band, go alloyage that alloy strip is made into classifying porous nano metal by electrochemistry again, the oxide layer of doping hydroxyl is produced on nano metal surface finally by the method for electrochemical oxidation, is prepared into ternary nano porous composite electrode.The combination electrode measures cyclic voltammetry curve and constant current charge-discharge curve etc. under three-electrode system, properties is calculated, wherein specific capacitance is in 100 1500F/cm3, specific capacitance conservation rate is 60% 75%, and the specific capacitance of ternary composite electrode system of the present invention is greatly improved, and specific capacitance conservation rate obtains larger raising.

Description

A kind of nanoporous nickel vanadium manganese/oxide combination electrode and preparation method thereof
Technical field
The invention belongs to the electrode material technical field for fake capacitance, more particularly to a kind of nanoporous nickel vanadium manganese/oxygen Compound combination electrode, further relate to a kind of preparation method of above-mentioned electrode.
Background technology
Ultracapacitor (supercapacitor), also commonly known as electrochemical capacitor (electrochemical Capacitor), different from classic flat-plate capacitor, it is mainly double by being formed in Cathode/Solution Interface generation Electrostatic Absorption Electric layer (double layer capacitor) or solution electrode interface occur underpotential deposition include quick redox reaction and The device that doping (pseudocapacitors) carries out energy storage is adulterated/gone, belongs to a kind of emerging high-efficiency energy-storage device.
Pseudocapacitors are called Faradic pseudo-capacitor, and its development is more later with respect to double layer capacitor, initially by Conwey seminars research and develop to ru oxide and propose and concept is set forth：Different from double layer capacitor but it is to electricity One supplement of container development, it can be by occurring quick redox reaction or doping/go to mix in Cathode/Solution Interface Miscellaneous process carries out the storage of energy.Compared with double layer capacitor, pseudocapacitors not only occur on electrode material due to faraday's reaction Surface is also carried out in material internal, and the energy density and specific capacitance that can effectively improve capacitor (are the 10- of double layer capacitor 100 times).Pseudocapacitors electrode material multiselect transition metal oxide, wherein, ru oxide has high specific capacitance, long circulating The feature performance benefits such as life-span, high conductivity, good electrochemical reversibility and high efficiency, but price is prohibitively expensive and use by Limitation.
Bibliography Self-GrownOxy-Hydroxide@NanoporousMetal Electrode for High- PerformanceSupercapacitors (JianLiKang, AkihikoHirata, H.-J.Qiu, Lu YangChen, XingBoGe, Takeshi Fujita and MingWei Chen, Advanced Materials Volume26, Issue2, P269-272, January) in disclose a kind of autoxidation oxyhydroxide nano porous metal electrode in high-performance super capacitor Application in device, the Ni30Mn70 alloys prepared in document are by going alloyage and electrochemical oxidation to be prepared for nano porous metal Oxide material, there is the electrode material compared with high specific capacitance and energy density.But the material current density is more than 10A/cm3When, Specific capacitance reduces obvious.How further to improve specific capacitance and specific capacitance conservation rate be the development of current super capacitor a big heat Point.
The content of the invention
It is an object of the invention to provide a kind of bulky capacitor, nanoporous nickel vanadium manganese/oxide of high specific capacitance conservation rate Combination electrode.
To achieve the above object, the present invention provides following technical scheme：A kind of nanoporous nickel vanadium manganese/oxide compound electric Pole, comprise the following steps：(1) preparation of alloy strip：Ni, V and Mn metallic particles are prepared into thickness in band machine is got rid of is The atom content percentage of 20-50 μm of alloy strip, wherein each component is：20-30% Ni, 5-20% V, 60%- 70% Mn；(2) removal alloying is handled：Alloy strip made from step (1) is prepared into nanoporous by removal alloying technique Metal, Mn content is 20-40% after removal alloying；(3) autoxidation is handled：Made with nano porous metal made from step (2) For anode, electrochemical oxidation is carried out in alkali hydroxide soln, oxidizing potential is maintained at below 1V, makes nano-porous gold Metal surface produces the oxide layer of doping hydroxyl, obtains nanoporous ternary composite electrode.
Preferably, the diameter of Ni, V and Mn metallic particles is chosen for 1~3mm in step (1).
Preferably, band process is got rid of in step (1) to carry out under argon gas protection, temperature control is at 800~1500 DEG C, when getting rid of band Rotating speed is chosen for 1200rad/s~1800rad/s
Preferably, step (2) chooses electrochemistry removal alloying method, by alloy strip made from step (1), as work Electrode, using three-electrode system in weakly acidic ammonium sulfate removal alloying, removal alloying voltage be chosen for -0.45V~- 0.65V, removal alloying time are 3600~10000s
Preferably, step (3) chooses stepped-up voltage oxidation, and 120- is respectively aoxidized under 0.9V, 0.8V, 0.7V, 0.6V voltage 360s。
Another object of the present invention is to provide a kind of bulky capacitor prepared using the above method, high specific capacitance conservation rate Nanoporous nickel vanadium manganese/oxide combination electrode.
Compared with prior art, the beneficial effects of the invention are as follows：
1) the non-single phase solid solution of NiVMn alloys prepared by the present invention, is triple-phase alloys (Mn, Ni2V3, MnV three-phase), compared with two The single-phase NiMn alloys specific capacitance of member is highly improved, and triple-phase alloys are kept compared with the NiCoMn single-phase alloys specific capacitance of ternary Rate has obtained larger lifting.
2) electrode material for preparing of the present invention is the three-D nano-porous structure that duplex is led to, spontaneous in electrode surface and duct Long one layer of mixed valency doping oxide thin layer thing, electric conductivity is good, and its aperture can pass through different corrosive liquids in alloy process is removed Concentration and etching time are adjusted.
3) ternary nano porous metal oxide electrode specific capacitance prepared by the present invention is in 1A/cm3When, specific capacitance is up to 1500F/cm3；Current density rises to 10A/cm3When, specific capacitance conservation rate is more than 64%, wherein Ni20V20Mn60 specific capacitances Conservation rate is up to 75%, and specific capacitance is greatly improved, and specific capacitance conservation rate obtains larger raising.
Brief description of the drawings
Fig. 1 is that the EDX of Ni25V15Mn60 ternary alloy three-partalloy bands schemes；
Fig. 2 is the XRD of Ni25V15Mn60 ternary alloy three-partalloy bands；
Fig. 3 A and Fig. 3 B are Ni25V15Mn60 nanoporous nickel vanadium manganese/oxide combination electrode under different amplification SEM schemes；
Fig. 4 is the cyclic voltammetry curve figure of Ni25V15Mn60 nanoporous nickel vanadium manganese/oxide combination electrode；
Fig. 5 is the constant current charge-discharge diagram of Ni25V15Mn60 nanoporous nickel vanadium manganese/oxide combination electrode；
Fig. 6 is Ni20V20Mn60 nanoporous nickel vanadium manganese/specific capacity of the oxide combination electrode under different current densities Figure.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out clear, complete Site preparation describes.
Embodiment 1：
Preparation method is as follows：
(1) preparation of alloy strip：It is respectively 25% Ni, 15% V, 60% Mn by atom content percentage, uses Get rid of the mode of band under argon gas protection, thickness is made under the rotating speed in 1200rad/s-1800rad/s is 20-30um, width is 2-3mm alloy strip.
(2) removal alloying prepares nanoporous alloy：By alloy strip made from step (1) be made width for 1.5~ 4mm, length are 1~100mm experiment band；Prepare nanometer perforated electrodes by the way of electrochemical corrosion, selection for three Electrode Shanghai Chen Hua electrochemical workstation, using alloy strip as working electrode, platinized platinum is that Ag/Agcl electrodes are reference to electrode Electrode.0.5~2mol/L ammonium sulfate is removal alloying solution, corrodes 3600- under -0.45V~-0.65V voltages 10000s。
(3) Autoxidation Method prepares ternary composite electrode：By the nanoporous alloy that step (2) obtains 1mol/L hydrogen-oxygen Change in potassium solution and carry out electrochemical oxidation, oxidation voltage is respectively that the next oxidation 120s of 0.9V, 0.8V, 0.7V, 0.6V (uses Shanghai Occasion China electrochemical workstation, using nanoporous alloy strip as working electrode, platinized platinum is that Ag/Agcl electrodes are reference to electrode Electrode).
(4) measure of chemical property：The nano porous metal oxide strips prepared to step (3) are carried out at activation Reason.Speed -0.6V is swept in the 50mv/s circle of progress cyclic voltammetric activation 100 under sweeping speed -0.6V~0.6V voltages, then in 40mv/s The circle of cyclic voltammetric activation 50 is carried out under~0.6V voltages, finally measures 30mv/s, 20mv/s, 10mv/s respectively, 5mv/s is swept under speed Cyclic voltammetry curve.It is respectively again 10A/cm in current density3, 7A/cm3, 5A/cm3, 3A/cm3, 1A/cm3Current density Lower survey constant current charge-discharge curve.
The EDX figures that Fig. 1 is Ni25V15Mn60 ternary alloy three-partalloy bands in the present embodiment are referred to, system can be seen that by this figure Standby alloy strip composition is consistent with theoretical content.
Refer to the XRD that Fig. 2 is Ni25V15Mn60 ternary alloy three-partalloy bands in the present embodiment, it can be seen that the conjunction of the component The non-single phase solid solution of gold bar band, but by the phase composition of Mn, Ni2V3, MnV tri-.NiMn alloys specific capacitance single-phase compared with binary obtain compared with Big lifting, and triple-phase alloys have obtained larger lifting compared with the NiCoMn single-phase alloy specific capacitance conservation rates of ternary.
It is that Ni25V15Mn60 ternary alloy three-partalloys band removes alloy through step (2) (3) in the present embodiment to refer to Fig. 3 A and Fig. 3 B The SEM figures of the nanoporous nickel vanadium manganese/oxide combination electrode change, obtained after autoxidation, corrosion, oxidation is can be seen that by this figure Process is uniform, corrodes whole alloy strip and thoroughly, forms the logical three-D nano-porous structure of duplex.
It is Ni25V15Mn60 nanoporous nickel vanadium manganese/oxide combination electrode in the present embodiment to refer to Fig. 4 and Fig. 5 Cyclic voltammetry curve figure and constant current charge-discharge diagram, it is consistent that the control of two figures can be seen that redox peaks correspond to, and passes through constant current charge-discharge The discharge time of curve and specific capacitance calculation formula can calculate specific capacitance.
Embodiment 2：
With the difference is that only for embodiment 1, the atom content percentage of each component is in step (1)：20% Ni, 20% V, 60% Mn.
It is Ni20V20Mn60 nanoporous nickel vanadium manganese/oxide combination electrode in the present embodiment in different electricity to refer to Fig. 6 Specific volume spirogram under current density, specific capacitance conservation rate can be calculated by being compared according to the specific capacitance under different current densities.
Embodiment 3：
With the difference is that only for embodiment 1, the atom content percentage of each component is in step (1)：20% Ni, 10% V, 70% Mn.
The chemical property measure knot of nanoporous nickel vanadium manganese/oxide combination electrode made from embodiment 1- embodiments 3 Fruit is as shown in table 1.
The chemical property measurement result of table 1
The electrode is that alloy strip is first prepared into by way of getting rid of band, then goes alloyage by alloy strip by electrochemistry Classifying porous nano metal is made, the oxidation of doping hydroxyl is produced on nano metal surface finally by the method for electrochemical oxidation Layer, is prepared into ternary nano porous composite electrode.The combination electrode measures cyclic voltammetry curve and constant current under three-electrode system Charging and discharging curve etc., properties are calculated, wherein specific capacitance is in 100-1500F/cm3, specific capacitance conservation rate is in 60%- 75%, and possess less internal resistance, higher energy density and power density.
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding And modification, the scope of the present invention is defined by the appended.

Claims (6)

  1. A kind of 1. preparation method of nanoporous nickel vanadium manganese/oxide combination electrode, it is characterised in that：Comprise the following steps,
    (1) preparation of alloy strip：Ni, V and Mn metallic particles are prepared into the conjunction that thickness is 20~50 μm in getting rid of with machine The atom content percentage of gold bar band, wherein each component is：20~30% Ni, 5~20% V, 60%~70% Mn；
    (2) removal alloying is handled：Alloy strip made from step (1) is prepared into nano porous metal by removal alloying technique, Mn content is 20~40% after removal alloying；
    (3) autoxidation is handled：So that nano porous metal is as anode made from step (2), in alkali hydroxide soln Electrochemical oxidation is carried out, oxidizing potential is maintained at below 1V, nano-porous gold metal surface is produced the oxide layer of doping hydroxyl, obtains To nanoporous ternary composite electrode.
  2. 2. the preparation method of nanoporous nickel vanadium manganese/oxide combination electrode according to claim 1, it is characterised in that： The diameter of Ni, V and Mn metallic particles is chosen for 1~3mm in step (1).
  3. 3. the preparation method of nanoporous nickel vanadium manganese/oxide combination electrode according to claim 1, it is characterised in that： Get rid of band process in step (1) to carry out under argon gas protection, temperature control is at 800~1500 DEG C, and rotating speed is chosen for when getting rid of band 1200rad/s~1800rad/s.
  4. 4. the preparation method of nanoporous nickel vanadium manganese/oxide combination electrode according to claim 1, it is characterised in that： Step (2) chooses electrochemistry removal alloying method, by alloy strip made from step (1), as working electrode, using three electrodes System removal alloying in weakly acidic ammonium sulfate, removal alloying voltage are chosen for -0.45V~-0.65V, removal alloying Time is 3600~10000s.
  5. 5. the preparation method of nanoporous nickel vanadium manganese/oxide combination electrode according to claim 1, it is characterised in that： Step (3) chooses stepped-up voltage oxidation, and 120-360s is respectively aoxidized under 0.9V, 0.8V, 0.7V, 0.6V voltage.
  6. 6. the preparation method of nanoporous nickel vanadium manganese/oxide combination electrode according to claim any one of 1-5 is made Electrode.
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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108807890A (en) * 2018-05-24 2018-11-13 天津工业大学 A kind of ternary nano porous nickel vanadium manganese oxide electrode material and preparation method thereof
CN112062166A (en) * 2020-08-29 2020-12-11 渤海大学 Ternary composite electrode material for hybrid capacitor and application thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104051161A (en) * 2014-07-11 2014-09-17 天津工业大学 Self oxide nanometer porous nickel cobalt manganese/hydroxyl oxide composite ternary electrode

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104051161A (en) * 2014-07-11 2014-09-17 天津工业大学 Self oxide nanometer porous nickel cobalt manganese/hydroxyl oxide composite ternary electrode

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
JIANLI KANG等: ""Extraordinary Supercapacitor Performance of a Multicomponent and Mixed‐Valence Oxyhydroxide"", 《ANGEWANDTE CHEMIE INTERNATIONAL EDITION》 *
张少飞: ""多元纳米多孔复合电极的制备与性能研究"", 《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》 *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108807890A (en) * 2018-05-24 2018-11-13 天津工业大学 A kind of ternary nano porous nickel vanadium manganese oxide electrode material and preparation method thereof
CN112062166A (en) * 2020-08-29 2020-12-11 渤海大学 Ternary composite electrode material for hybrid capacitor and application thereof

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