CN104051161B - Self oxide nanometer porous nickel cobalt manganese/hydroxyl oxide composite ternary electrode - Google Patents
Self oxide nanometer porous nickel cobalt manganese/hydroxyl oxide composite ternary electrode Download PDFInfo
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Abstract
The invention provides a self oxide nanometer porous nickel cobalt manganese/hydroxyl oxide composite ternary electrode. The preparation method of the ternary composite electrode includes the following steps of (1) preparing alloy, wherein nickel cobalt manganese alloy is prepared, and the alloy is machined to be alloy strips or alloy plates with the thickness ranging from 20 microns to 100 microns, and (2) preparing nanometer porous metal through dealloying, wherein the nanometer porous metal (3) is prepared by conducting dealloying on the alloy obtained in the step (1), the ternary composite electrode is prepared through a self oxide method, the nanometer porous metal obtained in the step (2) serves as the anode, and electrochemical oxidation is conducted in an alkali metal hydroxide solution, so that an oxide layer mixed with hydroxy is generated on the surface of the nanometer metal.
Description
Technical field
The present invention relates to a kind of electrochemical capacitor electrode and preparation method thereof.
Background technology
Electrochemical capacitor (Electrochemical Capacitor, abbreviation EC), is a kind of Jie also known as ultracapacitor
New type of energy storage device between traditional capacitor and battery.There is high power density, high invertibity, long life and have concurrently
The advantages of storage of battery high energy amount and traditional capacitor high-output power, EC can be divided into electric double layer electricity according to its charge-storage mechanism
Container and Faradic pseudo-capacitor, and the latter is also called fake capacitance (Pseudocapacitance).Adopting double layer capacitor more
Material with carbon element, as electrode material, adopts transition metal oxide to make electrode material, existing oxo transition metal more in fake capacitance
In compound, although ru oxide has high specific capacitance, long circulation life, high conductivity, good electrochemical reversibility and height
The feature performance benefits such as efficiency, but prohibitively expensive and using being restricted.And the oxidation of other metals such as the nickel of low price, cobalt, manganese
Thing is used for making although theory is higher than electric capacity during electrode material, but because of reasons such as electric conductivity differences, causes its practical application to be subject to
To limiting, how next by the way of conducting polymer or material with carbon element and metal oxide are made composite in prior art
Improve electrode material performance, bibliography 1 Self-Grown Oxy-Hydroxide@Nanoporous Metal
Electrode for High-Performance Supercapacitors (JianLi Kang, Akihiko Hirata, H.-
J.Qiu, LuYang Chen, XingBo Ge, Takeshi Fujita and MingWei Chen, Advanced
Materials Volume26, Issue2, p269 272, January15,2014) in disclose a kind of oxidation of autoxidation hydroxyl
Application in high-performance super capacitor for the thing nano porous metal electrode, provides oxyhydroxide in bibliography 1 and receives
The preparation method of rice porous metal electrode, that is, adopt nickel-manganese (Ni30Mn70) after removal alloying is processed, to obtain nanometer many
Mesoporous metal, then using electrochemical method carry out autoxidation process make nano porous metal top layer occur automatic oxidation reaction produce gold
The oxyhydroxide belonging to, unexpectedly obtains a kind of electrode material having compared with high specific capacitance and energy density.But grinding further
Although studying carefully it was found that the electrode material obtaining in bibliography 1 is in 0.5-10A/cm3Current density under can maintain relatively
High ratio electric capacity (300-500F/cm3) but we find in testing further, when current density improves further, it compares
Electric capacity declines obvious.How to improve the ratio electric capacity of electrode and power density further is the significant challenge facing at present.And
Existing research is it has been found that gold atom doping can improve conductance and the chemical property of oxide, bibliography 2
Enhanced Supercapacitor Performance of MnO2By Atomic Doping. (Dr.Jianli Kang,
Dr.Akihiko Hirata, Lijing Kang, Dr.Xianmin Zhang, Ying Hou, Dr.Luyang Chen, Cheng
Li, Dr.Takeshi Fujita, Dr.Kazuto Akagi and Prof.Mingwei Chen, Angewandte Chemie
Volume125, Issue6, pages1708 1711, February4,2013.)) in disclose one kind and adopt physical vapour deposition (PVD)
The method (being golden particulate in bibliography 2) of method doping oxide electrode material.But the method process is complicated, high cost, and mixes
Miscellaneous element is noble metal gold, and this can improve the cost of electrode material further and promote difficulty.
Content of the invention
It is found surprisingly that under study for action, process preparation when the nickel cobalt manganese alloy using certain proportion scope carries out removal alloying
Nano porous metal and carry out further autoxidation process obtain make its surface autoxidation produce oxyhydroxide layer after obtain
Electrode, be used for preparing during super capacitor and compare binary system (Ni-Mn), this invent described ternary composite electrode system ratio electricity
Hold acquisition and (400-1000F/cm is greatly improved3),
The present invention provide a kind of autoxidation nanoporous nickel cobalt manganese/oxyhydroxide ternary composite electrode it is characterised in that
The preparation method of described ternary composite electrode comprises the steps：
(1) alloy preparation, prepares nickel cobalt manganese alloy, described alloy, and the amount percentage of the material of manganese is 60-75%, nickel
The amount percentage of material is 5%-25%, balance of cobalt；Described alloy be processed to thickness 20～100 μm alloy strip or
Alloy sheets；
(2) removal alloying prepares nano porous metal, and the alloy obtaining prepared by step (1) adopts removal alloying method
Prepare nano porous metal, the pore-size distribution of described nano porous metal is 1-20nm, and specific surface area is 30-100m2/g；Institute
State in nano porous metal, the amount percentage of the material of manganese is 10-30%
(3) Autoxidation Method prepares ternary composite electrode, using the prepared nano porous metal of step (2) as anode, in alkali
Carry out electrochemical oxidation in metal hydroxide solutions, make nano metal surface produce the oxide layer of doping hydroxyl, oxidizing potential
In below 1v, control oxidated layer thickness and the structure of doping hydroxyl by controlling oxidization time and oxidizing potential；
Described ternary composite electrode, is characterized in that the removal alloying method in described preparation method preferred steps (2) is
Chemical removal alloying method or electrochemistry removal alloying method, more preferably electrochemistry removes alloy approach.
Described chemistry removal alloying method is step (1) to be prepared alloy strip or alloy sheets are dipped in concentration and are
Corroded in the hydrochloric acid solution of 0.05mol/L～1mol/L, complete and then be vacuum dried.
Described electrochemistry removal alloying method be with step (1) be obtained alloy strip or alloy sheets work electrode,
It is placed in faintly acid salting liquid, do to electrode with platinized platinum, alternative selects Ag/Agcl electrode as reference electrode, using three electrode body
It is removal alloying.Removal alloying is chosen by the relation of open-circuit voltage and nickel, the pH of cobalt, manganese corrosion potential and faintly acid salting liquid
Voltage, removal alloying voltage be -0.45V～-0.75V (vs.Ag/AgCl reference electrode), the removal alloying time be 1200s～
8000s, by adjusting corrosion potentials and etching time, concentration of electrolyte accomplish to nano porous metal aperture control；
Described faintly acid salting liquid is ammonium sulfate, and its concentration is 0.5mol/L～3mol/L.
Described corrosion potentials are reference electrode and the relation of working electrode and the relation according to corrosion of metal current potential and PH
Choose most suitable relation.
Described ternary composite electrode, is characterized in that in the step (3) of described preparation method, alkali hydroxide soln
, in the KOH solution of 0.5mol/L～3mol/L, (vs.Ag/AgCl reference is electric for the preferred 0.1V-1V of oxidizing potential for preferred concentration range
Pole), oxidization time 20s～300s.
Described ternary composite electrode, is characterized in that the tri compound that in described preparation method, preferred pair step (3) is obtained
Electrode is made annealing treatment in annealing atmosphere.Described annealing atmosphere is selected from one or more of air, nitrogen, annealing temperature
For 200-400 DEG C.
Described ternary composite electrode, is characterized in that described oxide layer chemical formula is (Ni2+ aCo2+ bCo4+ cMn2+ dMn4+ e)Of
(OH)g(H2O)h, a is 0.02-0.15, and b is 0.05-0.20, and c is 0.05-0.20, and d is 0.04-0.15, and e is 0.01-0.15, f
For 0.20-0.50, g is 0.20-0.50, and H is 0.01-0.10.In described oxide layer chemical formula, preferred a is 0.11 for 0.035, b,
C be 0.09, d be 0.071, e be 0.04, f be 0.34, g be 0.29, h be 0.024.
The present invention also provides a kind of autoxidation nanoporous nickel cobalt manganese/oxyhydroxide ternary composite electrode, and its feature exists
Lead to nanoporous core shell structure in having three-dimensional duplex, aperture 1-20nm is adjustable, oxide shells and metallic core have lattice
Matching relationship, described ternary composite electrode is prepared with any method aforementioned.
Autoxidation nanoporous/nickel cobalt manganese oxyhydroxide ternary composite electrode that the present invention provides, has three-dimensional duplex
Logical nanoporous core shell structure, aperture 1-20nm is adjustable, and oxide shells and metallic core have Lattice Matching relation.The present invention
There is provided ternary composite electrode, in the preparation first by these three metals of Ni, Co, Mn by certain material amount proportioning system
Standby obtain alloy strip, and further nano porous metal is prepared into using removal alloying method, then is adopted with nano porous metal
Prepare ternary composite electrode with Autoxidation Method, the electricity prepared with the employing Ni-Mn alloy disclosed in bibliography for raw material
Pole is compared, the ternary composite electrode that the present invention provides, and due to increased cobalt element, is found surprisingly that and can be effectively increased its conduction
Property, the electrode obtaining all increases than electric capacity and energy density under low current and two kinds of more extreme operating modes of high current.
Specifically, by embodiment, comparative example be obtained in the middle of and final products detection find, provided in an embodiment of the present invention annealing and
Unannealed electrode, it is in relatively low discharge current (0.5～1A/cm3) under, it is all significantly higher than than electric capacity and specific energy and is added without
The comparative example of cobalt element, in higher discharge current (20A/cm3) under it also increases than electric capacity and specific energy, and detection data
Show, the raising of electrode performance is not to be stepped up with the increase of cobalt addition merely, but in a proportion
Increase more, when cobalt continues to increase, the performance of electrode occurs in that decline on the contrary.The nickel-cobalt-manganese ternary compound electric that the present invention provides
Pole, compared with existing nickel violent binary combination electrode, significantly improves its performance.
Brief description：
Fig. 1 is obtained the EDX energy spectrum analysis figure of electrode for embodiment 1-1；
Fig. 2 is obtained the CV curve map of electrode for embodiment 1-1；
Fig. 3 is obtained the charging and discharging curve figure of electrode for embodiment 1-1, and wherein (a) is current density 1A/cm3Under charge and discharge
Electric curve map, (b) is current density 20A/cm3Under charging and discharging curve figure
Specific embodiment
Following examples can make this professional technique technical staff be more fully appreciated by the present invention, but never in any form
Limit the present invention.Embodiment preparation method is as follows
(1) alloy preparation, prepares nickel cobalt manganese alloy, three kinds of metal vacuum is got rid of band machine and forms conjunction in low vacuum melting
Gold；And then get rid of band and obtain alloy strip, described strip width is 3mm, and length is 2.8mm, and thickness is H μm
(2) removal alloying prepares nano porous metal,
Using electrochemistry removal alloying method：
The alloy obtaining prepared by step (1) prepares nano porous metal using electrochemistry removal alloying method, goes to close
Aurification step is：As removal alloying solution, instrument is occasion China electrochemical workstation to 1mol/L ammonium sulfate, the test of employing
System is three-electrode system, and, as working electrode, as to electrode, Ag/Agcl electrode is as reference for platinized platinum for wherein alloy strip
Electrode.Corrosion potentials are -0.65v (vs.Ag/AgCl reference electrode), and etching time controlled at 1800 seconds.
(3) Autoxidation Method prepares ternary composite electrode (prepare in comparative example for combination electrode)
The nano porous metal that step (2) is prepared is placed in the potassium hydroxide solution of 1mol/L as anode and carries out
Electrochemical oxidation, oxidation voltage and time are respectively 0.9v20s, 0.8v20s, 0.6v20s (vs.Ag/AgCl reference electrode).
Annealing, annealing atmosphere is selected from air or nitrogen, and annealing temperature is T DEG C.
Embodiment, comparative example are obtained middle and final products detection project
The nickel cobalt manganese alloy that step (1) obtains, the amount proportioning of the material of its nickel cobalt manganese is Ni：Co：Mn, the thickness of alloy strip
Spend for H μm
Step (2) obtains nano porous metal, and its pore-size distribution is Rnm, and specific surface area is Sm2/g；Described nanoporous
In metal, the amount percentage of the material of manganese is Mn%
Ternary composite electrode that step (3) obtains (prepare in comparative example for combination electrode),
1) xps energy spectrum analysis,
The oxide layer obtaining ternary composite electrode to step (3) is detected using EDX energy spectrum analysis, obtains aoxidizing stratification
Formula (Ni2+ aCo2+ bCo4+ cMn2+ dMn4+ e)Of(OH)g(H2O)h, and show through detection, oxide layer chemical formula is before and after annealing
It is basically unchanged.The EDX energy spectrum analysis figure of the wherein prepared ternary composite electrode of embodiment 1-1 is shown in Fig. 1.
2) performance test,
Step is：First with cyclic voltammetry curve method, electrode is carried out with activation process, described activation method is：Sweeping first
Retouch speed and be circulated volt-ampere activation for setting voltage window under conditions of 50mv/s for 0V-0.6V, the activation number of turns is 100 circles,
Then under conditions of 50mv/s, voltage window is circulated volt-ampere activation 100 circle for -0.4V-0.6V, finally 100mv/s's
Under the conditions of voltage window for -0.4V-0.6V be circulated volt-ampere activation 100 circle.After the completion of activation, electrode is obtained to embodiment 1-1
Carry out testing its CV curve (see Fig. 2) respectively under the sweep speed of 5mv/s, 10mv/s, 20mv/s, 30mv/s, 40mv/s, then
Testing all embodiments and comparative example the electrode obtained respectively in current density is 1A/cm3And 20A/cm3When charging and discharging curve (its
The charging and discharging curve of middle embodiment 1-1 is shown in Fig. 3), and 1., 2. the ratio electric capacity under its two kinds of test conditions is calculated respectively according to formula
And energy density.Each embodiment (comparative example) respectively test annealing before and after electrode than electric capacity C and energy density E.
1A/cm3Before annealing under test condition, electrode is C than electric capacityL, energy density is EL；Annealing rear electrode material, energy
Density is E 'L.
20A/cm3Before annealing under test condition, electrode is C than electric capacityH, energy density is EH；Annealing rear electrode C 'H, energy
Density is E 'H.
Compare electric capacity(F/cm3)①
Energy density(mwh/cm3)②
Power density((W/cm3)③
Wherein, vsingleRepresent working electrode volume, V represents operating voltage window.ω represents current density, and t represents electric discharge
Time, P represents power density, and E represents energy density.
Wherein, employ aforesaid electrochemistry removal alloying method in the step (2) of all embodiments and comparative example,
Embodiment 1-1～embodiment 5-2, and the technological parameter of D1 as a comparison case and product see table：
Additionally, other performance parameters that detection embodiment 1-1 the electrode obtained obtains when being tested before being annealed
As following table：
In performance test it was found that reducing with current density, can increase than electric capacity, embodiment 1-1 is obtained
For electrode, in 0.5A/cm3When can reach 901F/cm than electric capacity3, after annealing, it more may be up to 1000F/cm than electric capacity3.
Claims (8)
1. a kind of autoxidation nanoporous nickel cobalt manganese/oxyhydroxide ternary composite electrode is it is characterised in that described ternary is multiple
Composite electrode preparation method comprises the steps：
（1）Prepared by alloy, prepare nickel cobalt manganese alloy, described alloy, and the amount percentage of the material of manganese is 60-75%, the material of nickel
Amount percentage is 5%-25%, balance of cobalt；Described alloy is processed to thickness in 20 ~ 100 μm of alloy strip or alloy sheets；
（2）Removal alloying prepares nano porous metal, by step（1）The alloy obtaining of preparation adopts removal alloying method to prepare
Nano porous metal, the pore-size distribution of described nano porous metal is 1-20nm, and specific surface area is 30-100m2/g；Described receive
In rice porous metals, the amount percentage of the material of manganese is 10-30%；
（3）Autoxidation Method prepares ternary composite electrode, with step（2）Prepared nano porous metal as anode, in alkali metal
Carry out electrochemical oxidation in hydroxide solution, make nano metal surface produce the oxide layer of doping hydroxyl, oxidizing potential is in 1V
Hereinafter, oxidated layer thickness and the structure of doping hydroxyl, described oxidation stratification are controlled by controlling oxidization time and oxidizing potential
Formula is (Ni2+ aCo2+ bCo4+ cMn2+ dMn4+ e) Of(OH)g(H2O)h, a is 0.02-0.15, and b is 0.05-0.20, and c is
0.05-0.20, d are 0.04-0.15, and e is 0.01-0.15, and f is 0.20-0.50, and g is 0.20-0.50, and h is 0.01-0.10.
2. ternary composite electrode as claimed in claim 1, is characterized in that, in described oxide layer chemical formula, a for 0.035, b is
0.11, c be 0.09, d be 0.071, e be 0.04, f be 0.34, g be 0.29, h be 0.024.
3. ternary composite electrode as claimed in claim 1 or 2, is characterized in that described preparation method step（2）In go close
Aurification method is chemical removal alloying method or electrochemistry removal alloying method.
4. ternary composite electrode as claimed in claim 3, is characterized in that described chemistry removal alloying method is by step（1）System
Standby obtain alloy strip or alloy sheets are dipped in the hydrochloric acid that concentration is 0.005mol/L ~ 0.1mol/L and are corroded, after the completion of true
Empty dry.
5. ternary composite electrode as claimed in claim 3, is characterized in that described preparation method step（2）In removal alloying side
Method is electrochemistry removal alloying method.
6. ternary composite electrode as claimed in claim 5, is characterized in that described electrochemistry removal alloying method is with step（1）
Prepared alloy strip or alloy sheets are worked electrode, are placed in faintly acid salting liquid, do to electrode with platinized platinum, alternative is selected
Ag/AgCl electrode as reference electrode, using three-electrode system removal alloying；By open-circuit voltage and nickel, cobalt, manganese corrosion potential
Choose removal alloying voltage with the relation of the pH of faintly acid salting liquid, removal alloying voltage is -0.45V ~ -0.75V, removal alloying
Time is 1200s ~ 8000s, and described faintly acid salting liquid is the ammonium sulfate of 0.5mol/L ~ 3mol/L for concentration.
7. ternary composite electrode as claimed in claim 1 or 2, is characterized in that step in described preparation method（3）In, alkali metal
Hydroxide solution is the KOH solution in 0.5mol/L ~ 3mol/L for the concentration range, and oxidizing potential is 0.1V-1V, oxidization time
20s~300s.
8. ternary composite electrode as claimed in claim 1 or 2, is characterized in that to step（3）Prepared electrode is in annealing atmosphere
In made annealing treatment, described annealing atmosphere is selected from one of air, nitrogen or two kinds, and annealing temperature is 200-400 DEG C.
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| CN105016397B (en) * | 2015-07-10 | 2016-10-12 | 济南大学 | A kind of AB2o4the preparation method of spinel structure nano-metal-oxide |
| CN106531449B (en) * | 2016-10-24 | 2018-04-06 | 上海应用技术大学 | A kind of preparation method of nanometer sheet core shell structure |
| CN107887178B (en) * | 2017-10-16 | 2019-11-22 | 天津工业大学 | A kind of nanoporous nickel vanadium manganese/oxide combination electrode and preparation method thereof |
| CN107863253A (en) * | 2017-10-16 | 2018-03-30 | 天津工业大学 | A kind of nanoporous nickel-iron-manganese alloys/oxides combination electrode and preparation method thereof |
| CN107910193B (en) * | 2017-11-13 | 2020-04-28 | 吉科猛 | Nano porous metal/metal oxide hybrid structure material, preparation and energy storage application |
| CN110635103B (en) * | 2019-08-29 | 2022-04-01 | 宁波杰士兄弟工具有限公司 | Flexible nano porous metal oxide cathode for secondary battery and preparation method thereof |
| CN113496823B (en) * | 2020-03-18 | 2023-04-11 | 天津理工大学 | Symmetric hybrid supercapacitor and application thereof |
| CN114530333B (en) * | 2020-11-23 | 2024-04-19 | 南京理工大学 | Nano porous cobalt electrode material and preparation method thereof |
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Effective date of registration: 20210427 Address after: 315803 No.1, building 1, No.12, Zhenxing Road, qijiashan, Beilun District, Ningbo City, Zhejiang Province Patentee after: NINGBO JIESHI BROTHER TOOLS Co.,Ltd. Address before: 300387 Tianjin city Xiqing District West Binshui Road No. 399, Tianjin University of Technology Patentee before: TIANJIN POLYTECHNIC University |