CN106449158A - Nickel-manganese composite oxide nano prism array electrode on titanium substrate and preparation method of nickel-manganese composite oxide nano prism array electrode - Google Patents
Nickel-manganese composite oxide nano prism array electrode on titanium substrate and preparation method of nickel-manganese composite oxide nano prism array electrode Download PDFInfo
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- CN106449158A CN106449158A CN201610817064.XA CN201610817064A CN106449158A CN 106449158 A CN106449158 A CN 106449158A CN 201610817064 A CN201610817064 A CN 201610817064A CN 106449158 A CN106449158 A CN 106449158A
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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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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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
- H01G11/22—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
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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
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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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
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G11/28—Electrodes 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
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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
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- 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 belongs to the field of inorganic material preparation and electrochemical application, and particularly relates to a nickel-manganese composite oxide nano prism array electrode on a titanium substrate and a preparation method of the nickel-manganese composite oxide nano prism array electrode. The electrode comprises a titanium metal substrate and a nickel-manganese composite oxide nano prism array growing on the titanium metal substrate; nickel-manganese composite oxide nano prisms are vertically, uniformly and densely distributed on the surface of the titanium metal substrate and are in an array form; and the diameter of the single nickel-manganese composite oxide nano prism is 200-500nm. According to the nickel-manganese composite oxide nano prism array electrode on the titanium substrate, in a three-electrode system, the working voltage range can reach 0-1.4V; obvious water electrolysis is avoided; and the nickel-manganese composite oxide nano prism array electrode is a rare material with a wide working voltage range, can be used as a positive electrode material of a super-capacitor, has good electrochemical properties and has widespread application value.
Description
Technical field
The invention belongs to inorganic material preparation and electrochemical applications field are and in particular to nickel manganese composite oxygen in a kind of titanium substrate
Compound nanometer water chestnut post array electrode and preparation method thereof.
Background technology
Ultracapacitor, also known as electrochemical capacitor, is a kind of novel energy-storing between traditional capacitor and battery
Element, has that power density is high, has extended cycle life, operating temperature width and the features such as environmental protection.But compared with lithium ion battery, surpass
The energy density of level capacitor is less than normal.Accordingly, it would be desirable to improve the energy density of super capacitor, important means are raising
The operating voltage of positive and negative electrode material is interval.
Commonly use the interval only 0~1V of the operating voltage (calomel electrode relatively) of the positive electrode of ultracapacitor at present, such as
Fruit can widen positive electrode operating potential interval it is possible to arrange in pairs or groups with the negative material of existing wide operating voltage, is assembled into super
Capacitor, thus the operating voltage improving ultracapacitor device is interval, thus to improve the energy density of ultracapacitor.
Content of the invention
The present invention is directed to the deficiencies in the prior art it is therefore intended that providing nickel manganese composite oxide in a kind of titanium substrate
Nanometer water chestnut post array electrode and preparation method thereof.
For achieving the above object, the technical solution adopted in the present invention is:
Nickel manganese composite oxide nanometer water chestnut post array electrode in a kind of titanium substrate, described electrode is by titanium metal substrate and titanium
The nickel manganese composite oxide nanometer water chestnut post array belonging to growth in substrate is constituted, described nickel manganese composite oxide nanometer water chestnut post is vertical,
Uniformly, densely it is distributed in titanium metal substrate surface, assume array format.
In such scheme, a diameter of 200~500nm of single nickel manganese composite oxide nanometer water chestnut post.
In such scheme, described nickel manganese composite oxide is the nickel manganese composite oxide of carbon containing, and molecular formula is
Ni0.25Mn0.75O@C, nickel manganese atom content is than for 1:3.
In above-mentioned titanium substrate, the preparation method of nickel manganese composite oxide nanometer water chestnut post array electrode, comprises the steps:
(1) urea, ammonium fluoride, nickel acetate, manganese acetate, glucose are dissolved in deionized water, after being sufficiently mixed uniformly
To mixed solution;
(2) titanium metal plate that HCl treatment is crossed is placed in the described mixed solution of step (1), puts into sealing in reactor and add
Heat carries out hydro-thermal reaction;After reaction terminates, after solution natural cooling to be mixed, take out titanium metal plate, cleaning, dry;
(3) titanium metal plate after step (2) drying is made annealing treatment under argon atmosphere, after annealing terminates,
Obtain nickel manganese composite oxide nanometer water chestnut post array electrode in titanium substrate.
In such scheme, in described mixed solution, the amount of the material of nickel acetate and manganese acetate is than for 1:3.
In such scheme, in described mixed solution, the molar concentration of glucose is 0.034~0.05mol/L.
In such scheme, the mass ratio of described urea, ammonium fluoride, nickel acetate, manganese acetate and glucose is 1500:370:
221:649:250.
In such scheme, the temperature of the described hydro-thermal reaction of step (2) is 110~140 DEG C, and the time is 6~8h.Preferably,
The temperature of described hydro-thermal reaction is 125 DEG C, and the time is 6h.
In such scheme, the temperature of the described annealing of step (3) is 450~500 DEG C, and the time is 1~2h.Preferably,
The temperature of described annealing is 450 DEG C, and the time is 1h.
In such scheme, the temperature of the described drying of step (2) is 60 DEG C.
Application in ultracapacitor for the nickel manganese composite oxide nanometer water chestnut post array electrode in above-mentioned titanium substrate.
In electrode of the present invention, titanium substrate vertically, uniformly, is densely distributed ground nickel manganese composite oxide nanometer water chestnut post
Array, can make electrolyte be fully contacted with it in the presence of skin effect, reduce interface resistance;It is simultaneously based on nickel manganese to be combined
The nanometer-sized diameter of oxidate nano water chestnut post makes ion embed/diffusion under the effect of small-size effect, quantum size effect
It is shorter that path becomes, and provides one-dimensional electron propagation ducts;Additionally, titanium substrate as electrode current collecting body in electrochemical process
Chemical stability is good;Nickel manganese composite oxide nanometer water chestnut post array has good electrochemical capacitance as supercapacitor positive electrode
Energy.
Beneficial effects of the present invention:
(1) nickel manganese composite oxide nanometer water chestnut post array electrode in titanium substrate of the present invention, in three-electrode system, its
Operating voltage interval can reach 0~1.4V, and does not have obvious water electrolysis to occur, and is that rare to have wide operating voltage interval
Material, can be used as the positive electrode of ultracapacitor.
(2) preparation method of the present invention is simple and easy to control, energy consumption and low cost, it is possible to achieve nickel manganese composite oxide is received
Rice large area in titanium substrate for the water chestnut post array equably grows, nickel manganese composite oxide nanometer water chestnut post battle array in the titanium substrate obtaining
Row electrode can be used as supercapacitor positive electrode and shows good chemical property, is with a wide range of applications.
Brief description
Fig. 1 is the electron microscope of nickel manganese composite oxide nanometer water chestnut post array electrode in the titanium substrate of embodiment 1 preparation
(wherein (a) is the nickel manganese composite oxide nanometer water chestnut post array shape appearance figure of 10000 times of amplification to figure, and (b) is to amplify 100000 times
Nickel manganese composite oxide nanometer water chestnut post array shape appearance figure), X-ray diffractogram (c), EDS quantitative analysis figure (d), constituent content divides
Analysis figure (e).
Fig. 2 is the capacitive property figure of nickel manganese composite oxide nanometer water chestnut post array electrode in the titanium substrate of embodiment 1 preparation,
A is cyclic voltammetry curve figure, and b is constant current charge-discharge diagram, and c is multiplying power figure, and d is impedance diagram, and e is circulation figure.
Fig. 3 is nickel manganese composite oxide nanometer water chestnut post array Ni in the titanium substrate of embodiment 2 preparation0.25Mn0.75O@C section
SEM schemes, and wherein (a) schemes for section SEM, and (b) is enlarged drawing.
Specific embodiment
For a better understanding of the present invention, it is further elucidated with present disclosure with reference to embodiment, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
In a kind of titanium substrate, nickel manganese composite oxide nanometer water chestnut post array electrode, is prepared via a method which to obtain:
(1) 1.5g urea, 0.37g ammonium fluoride, 0.221g nickel acetate, 0.649g manganese acetate, 0.25g glucose are dissolved in
In 50mL deionized water, the amount of the material of nickel acetate and manganese acetate is than for 1:3, urea, ammonium fluoride, nickel acetate, manganese acetate material
Amount concentration be respectively 0.5mol/L, 0.2mol/L, 0.025mol/L, 0.075mol/L, with magnetic stirrer so as to fill
Divide dissolving, mix, be configured to mixed solution;
(2) titanium sheet crossed with HCl treatment is placed in the mixed solution that step (1) is prepared as substrate;Then poly- four
It is heated to seal to 125 DEG C in the autoclave of PVF inner bag (100 milliliters), keep 6 hours;After natural cooling, titanium metal plate is taken
Go out, be placed in quartz tube furnace and be heated to 450 DEG C of annealing 1 hour under argon atmosphere, obtain nickel manganese composite oxide in titanium substrate
Nanometer water chestnut post array electrode.
Nickel manganese composite oxide nanometer water chestnut post array electrode in titanium substrate described in the present embodiment is done SEM
Observe, result is shown in Fig. 1 (a) and (b).The result of Fig. 1 (a) and (b) shows, nickel manganese composite oxide nanometer water chestnut post is uniform, intensive
Be distributed in surface of metal titanium, assume array format, its single nickel manganese composite oxide nanometer water chestnut post a diameter of 300~
400nm.Fig. 1 (c) is the X-ray diffractogram of nickel manganese composite oxide nanometer water chestnut post array electrode in titanium substrate, permissible from figure
Find out:In addition to the diffraction maximum of titanium substrate, prepared electrode is mainly reflected in MnO structure and a small amount of MnF;Fig. 2 (d) is EDS
Quantitative analysis results, Fig. 2 (e) is constituent content analysis result, it can be seen that:A certain amount of Ni is also contained in described electrode
And carbon, form Ni0.25Mn0.75O@component C, and nickel manganese atom content is than for 1:3.
Using nickel manganese composite oxide nanometer water chestnut post array electrode in the titanium substrate that the present embodiment prepares as work electricity
Pole, as to electrode, calomel electrode (SCE) is reference electrode to Pt, carries out three electricity in lithium chloride (LiCl) solution of 2mol/L
Pole performance of the supercapacitor test, result is shown in Fig. 2, and wherein a is sweep speed 5mV/s respectively, 10mV/s, 25mV/s, 50mV/s
Cyclic voltammetry curve figure, as can be seen from Figure:In described titanium substrate, nickel manganese composite oxide nanometer water chestnut post array electrode shows
Compare the cyclic voltammetry curve of rectangle, illustrate that it has good capacitive characteristics, potential region is up to 1.4V and not obvious
Water electrolysis reaction occurs;B is the constant current charge-discharge curve map under different current densities, and c is high rate performance figure, in current density
It is respectively 1 milliamps per square centimeter, 2 milliamps per square centimeter, 4 milliamps per square centimeter, 8 milliamps per square centimeter and 16 milliamperes/flat
In the case of square centimetre during constant current charge-discharge, its electric capacity respectively 185.6 millifarads/square centimeter, 160.3 millifarads/square centimeter,
143.6 millifarads/square centimeter, 136.8 millifarads/square centimeter and 135.2 millifarads/square centimeter.Can obtain from high rate performance figure
Go out, current density is respectively 2 milliamps per square centimeter, 4 milliamps per square centimeter, 8 milliamps per square centimeter and 16 milliamperes/square li
Rice, its capacity maintenance dose is respectively (compared with being electric capacity when 1 milliamps per square centimeter with current density) 86.4%, 77.4%,
73.7% and 72.8%;D is impedance diagram, and solution resistance is 8.1ohm, and load transfer impedance is 9.2ohm, and the inside illustration is enlarged drawing;e
For circulation figure, with the volt-ampere round-robin method test of 25mV/s, after 4800 circulations, capacitance size is first circulation capacitance size
73%.The above results illustrate, in the titanium substrate that the present embodiment prepares, nickel manganese composite oxide nanometer water chestnut post array electrode is made
For supercapacitor positive electrode, there is good electrochemical capacitance performance.
Embodiment 2
In a kind of titanium substrate, nickel manganese composite oxide nanometer water chestnut post array electrode, is prepared via a method which to obtain:
(1) 1.5g urea, 0.37g ammonium fluoride, 0.221g nickel acetate, 0.649g manganese acetate, 0.25g glucose are dissolved in
In 50mL deionized water, the amount of the material of nickel acetate and manganese acetate is than for 1:3, urea, ammonium fluoride, nickel acetate, manganese acetate material
Amount concentration be respectively 0.5mol/L, 0.2mol/L, 0.025mol/L, 0.075mol/L, with magnetic stirrer so as to fill
Divide dissolving, mix, be configured to mixed solution;
(2) titanium sheet crossed with HCl treatment is placed in the mixed solution that step (1) is prepared as substrate;Then poly- four
It is heated to seal to 140 DEG C in the autoclave of PVF inner bag (100 milliliters), keep 8 hours;After natural cooling, titanium metal plate is taken
Go out, be placed in quartz tube furnace and be heated to 450 DEG C of annealing 1 hour under argon atmosphere, obtain nickel manganese composite oxide in titanium substrate
Nanometer water chestnut post array electrode.
Nickel manganese composite oxide nanometer water chestnut post array electrode in titanium substrate described in the present embodiment is done SEM
Observe, result is shown in Fig. 3.Fig. 3 (a) is Ni0.25Mn0.75O@C section SEM schemes, as can be seen from the figure:Array being capable of compact growth
In titanium sheet, straight uniform;B () is enlarged drawing, amplified find that prismatic surface has substantial amounts of carbon char particle and nano-pore, should
Nanoprisms have loose structure and show highly porous form, and this transports highly beneficial to ion.
Embodiment 3
In a kind of titanium substrate, nickel manganese composite oxide nanometer water chestnut post array electrode, is prepared via a method which to obtain:
(1) 1.5g urea, 0.37g ammonium fluoride, 0.221g nickel acetate, 0.649g manganese acetate, 0.25g glucose are dissolved in
In 50mL deionized water, the amount of the material of nickel acetate and manganese acetate is than for 1:3, urea, ammonium fluoride, nickel acetate, manganese acetate material
Amount concentration be respectively 0.5mol/L, 0.2mol/L, 0.025mol/L, 0.075mol/L, with magnetic stirrer so as to fill
Divide dissolving, mix, be configured to mixed solution;
(2) titanium sheet crossed with HCl treatment is placed in the mixed solution that step (1) is prepared as substrate;Then poly- four
It is heated to seal to 110 DEG C in the autoclave of PVF inner bag (100 milliliters), keep 8 hours;After natural cooling, titanium metal plate is taken
Go out, be placed in quartz tube furnace and be heated to 500 DEG C of annealing 2 hours under argon atmosphere, obtain nickel manganese composite oxide in titanium substrate
Nanometer water chestnut post array electrode.
Obviously, above-described embodiment is only intended to clearly illustrate made example, and the not restriction to embodiment.Right
For those of ordinary skill in the art, can also make on the basis of the above description other multi-forms change or
Change.There is no need to be exhaustive to all of embodiment.And the obvious change therefore amplified or change
Move within still in the protection domain of the invention.
Claims (10)
1. in a kind of titanium substrate nickel manganese composite oxide nanometer water chestnut post array electrode it is characterised in that described electrode is by titanium
In substrate and titanium metal substrate, the nickel manganese composite oxide nanometer water chestnut post array of growth is constituted, described nickel manganese composite oxide nanometer
Water chestnut post is vertical, uniform, be densely distributed in titanium metal substrate surface, assumes array format.
2. in titanium substrate according to claim 1 nickel manganese composite oxide nanometer water chestnut post array electrode it is characterised in that list
A diameter of 200 ~ 500nm of root nickel manganese composite oxide nanometer water chestnut post.
3. in titanium substrate according to claim 1 nickel manganese composite oxide nanometer water chestnut post array electrode it is characterised in that institute
State the nickel manganese composite oxide that nickel manganese composite oxide is carbon containing, molecular formula is Ni0.25Mn0.75O@C, nickel manganese atom content ratio is
1:3.
4. in the arbitrary described titanium substrate of claim 1 ~ 3 nickel manganese composite oxide nanometer water chestnut post array electrode preparation method, its
It is characterised by, comprise the steps:
(1)Urea, ammonium fluoride, nickel acetate, manganese acetate, glucose are dissolved in deionized water, are mixed after being sufficiently mixed uniformly
Close solution;
(2)The titanium metal plate that HCl treatment is crossed is placed in step(1)In described mixed solution, put into heated sealed in reactor and enter
Row hydro-thermal reaction;After reaction terminates, after solution natural cooling to be mixed, take out titanium metal plate, cleaning, dry;
(3)By step(2)Titanium metal plate after drying is made annealing treatment under argon atmosphere, after annealing terminates, obtains
Nickel manganese composite oxide nanometer water chestnut post array electrode in titanium substrate.
5. preparation method according to claim 4 it is characterised in that in described mixed solution nickel acetate and manganese acetate thing
The amount of matter is than for 1:3.
6. preparation method according to claim 4 it is characterised in that in described mixed solution the molar concentration of glucose be
0.042 mol/L.
7. preparation method according to claim 4 it is characterised in that described urea, ammonium fluoride, nickel acetate, manganese acetate and
The mass ratio of glucose is 1500:370:221:649:250.
8. preparation method according to claim 4 is it is characterised in that step(2)The temperature of described hydro-thermal reaction be 110 ~
140 DEG C, the time is 6 ~ 8h.
9. preparation method according to claim 4 is it is characterised in that step(3)The temperature of described annealing be 450 ~
500 DEG C, the time is 1 ~ 2h.
10. in titanium substrate described in any one of claim 1 ~ 3 nickel manganese composite oxide nanometer water chestnut post array electrode in super capacitor
Application in device.
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CN107633952A (en) * | 2017-09-21 | 2018-01-26 | 北京化工大学 | A kind of nickel manganese composite oxide nano sheet film materials and its preparation method and application |
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CN103896208A (en) * | 2014-02-19 | 2014-07-02 | 华中师范大学 | Manganese dioxide nanowire array electrode on titanium substrate and preparation method thereof |
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