CN106449158B - Nickel manganese composite oxide nanometer water chestnut column array electrode and preparation method thereof in titanium substrate - Google Patents
Nickel manganese composite oxide nanometer water chestnut column array electrode and preparation method thereof in titanium substrate Download PDFInfo
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- CN106449158B CN106449158B CN201610817064.XA CN201610817064A CN106449158B CN 106449158 B CN106449158 B CN 106449158B CN 201610817064 A CN201610817064 A CN 201610817064A CN 106449158 B CN106449158 B CN 106449158B
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
Abstract
It is prepared the invention belongs to inorganic material and electrochemical applications field, and in particular to nickel manganese composite oxide nanometer water chestnut column array electrode and preparation method thereof in a kind of titanium substrate.The electrode is made of the nickel manganese composite oxide nanometer water chestnut column array grown in titanium metal substrate and titanium metal substrate, the nickel manganese composite oxide nanometer water chestnut column is vertical, uniformly, be densely distributed in titanium metal substrate surface, array format is presented；A diameter of 200~500nm of single nickel manganese composite oxide nanometer water chestnut column.Nickel manganese composite oxide nanometer water chestnut column array electrode in titanium substrate of the present invention, in three-electrode system, its operating voltage section can reach 0~1.4V, and there is no apparent water electrolysis, it is the rare material with wide operating voltage section, it can be used as the positive electrode of ultracapacitor and show good chemical property, be with a wide range of applications.
Description
Technical field
It is prepared the invention belongs to inorganic material and electrochemical applications field, and in particular to nickel manganese composite oxygen in a kind of titanium substrate
Compound nanometer water chestnut column array electrode and preparation method thereof.
Background technology
Ultracapacitor, also known as electrochemical capacitor are a kind of novel energy-storings between traditional capacitor and battery
Element has the characteristics that power density is high, has extended cycle life, operating temperature is wide and environmentally friendly.But compared with lithium ion battery, surpass
The energy density of grade capacitor is less than normal.Therefore, it is necessary to improve the energy density of super capacitor, an important means are to improve
The operating voltage section of positive and negative electrode material.
The operating voltage section of the positive electrode of common ultracapacitor only has 0~1V (opposite calomel electrode) at present, such as
Fruit can widen positive electrode operating potential section, so that it may to arrange in pairs or groups with the negative material of existing wide operating voltage, be assembled into super
Thus capacitor improves the energy density of ultracapacitor to improving the operating voltage section of ultracapacitor device.
Invention content
The present invention is directed to the deficiencies in the prior art, and it is an object of the present invention to provide nickel manganese composite oxide in a kind of titanium substrate
Nanometer water chestnut column 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 column array electrode in a kind of titanium substrate, the electrode is by titanium metal substrate and titanium
Belong to the nickel manganese composite oxide nanometer water chestnut column array that grows in substrate to constitute, the nickel manganese composite oxide nanometer water chestnut column is vertical,
Uniformly, it is densely distributed in titanium metal substrate surface, array format is presented.
In said program, a diameter of 200~500nm of single nickel manganese composite oxide nanometer water chestnut column.
In said program, the nickel manganese composite oxide is carbon containing nickel manganese composite oxide, and molecular formula is
Ni0.25Mn0.75O@C, nickel manganese atom content ratio are 1:3.
The preparation method of nickel manganese composite oxide nanometer water chestnut column array electrode, includes the following steps in above-mentioned titanium substrate：
(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 step (1) described mixed solution, is put into sealing in reaction kettle and adds
Heat carries out hydro-thermal reaction；After reaction, after solution natural cooling to be mixed, titanium metal plate is taken out, is cleaned, drying；
(3) titanium metal plate after drying step (2) makes annealing treatment under argon atmosphere, after annealing,
Obtain nickel manganese composite oxide nanometer water chestnut column array electrode in titanium substrate.
In said program, the amount ratio of the substance of nickel acetate and manganese acetate is 1 in the mixed solution:3.
In said program, the molar concentration of glucose is 0.034~0.05mol/L in the mixed solution.
In said program, the urea, ammonium fluoride, nickel acetate, manganese acetate and glucose mass ratio be 1500:370:
221:649:250。
In said program, the temperature of step (2) described hydro-thermal reaction is 110~140 DEG C, and the time is 6~8h.Preferably,
The temperature of the hydro-thermal reaction is 125 DEG C, time 6h.
In said program, the temperature of step (3) described annealing is 450~500 DEG C, and the time is 1~2h.Preferably,
The temperature of the annealing is 450 DEG C, time 1h.
In said program, the temperature of step (2) described drying is 60 DEG C.
Application of the nickel manganese composite oxide nanometer water chestnut column array electrode in ultracapacitor in above-mentioned titanium substrate.
In electrode of the present invention, ground nickel manganese composite oxide nanometer water chestnut column vertically, uniformly, is densely distributed in titanium substrate
Array can be such that electrolyte is come into full contact with it under the action of skin effect, reduce interface resistance；It is compound based on nickel manganese simultaneously
The nanometer-sized diameter of oxidate nano water chestnut column makes ion insertion/diffusion under the effect of small-size effect, quantum size effect
Path becomes shorter, and provides one-dimensional electron propagation ducts；In addition, titanium substrate as electrode current collecting body in electrochemical process
Chemical stability is good；Nickel manganese composite oxide nanometer water chestnut column array, which is used as supercapacitor positive electrode, has good electrochemical capacitance
Energy.
Beneficial effects of the present invention：
(1) nickel manganese composite oxide nanometer water chestnut column array electrode in titanium substrate of the present invention, in three-electrode system,
Operating voltage section can reach 0~1.4V, and not have apparent water electrolysis, be rare to have wide operating voltage section
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 at low cost, and nickel manganese composite oxide may be implemented and receive
Large area of the rice water chestnut column array in titanium substrate is equably grown, nickel manganese composite oxide nanometer water chestnut column battle array in obtained titanium substrate
Row electrode can be used as supercapacitor positive electrode and show good chemical property, be with a wide range of applications.
Description of the drawings
Fig. 1 is the electron microscope of nickel manganese composite oxide nanometer water chestnut column array electrode in the titanium substrate of the preparation of embodiment 1
(wherein (a) is the nickel manganese composite oxide nanometer water chestnut column array shape appearance figure for amplifying 10000 times to figure, is (b) 100000 times of amplification
Nickel manganese composite oxide nanometer water chestnut column array shape appearance figure), X-ray diffractogram (c), EDS quantitative analysis figures (d), constituent content point
Analysis figure (e).
Fig. 2 is the capacitive property figure of nickel manganese composite oxide nanometer water chestnut column array electrode in the titanium substrate of the preparation of embodiment 1,
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 that cycle is schemed.
Fig. 3 is nickel manganese composite oxide nanometer water chestnut column array Ni in the titanium substrate of the preparation of embodiment 20.25Mn0.75The sections O@C
SEM schemes, wherein (a) schemes for section SEM, it is (b) enlarged drawing.
Specific implementation mode
For a better understanding of the present invention, with reference to the embodiment content that the present invention is furture elucidated, but the present invention
Content is not limited solely to the following examples.
Embodiment 1
Nickel manganese composite oxide nanometer water chestnut column array electrode in a kind of titanium substrate, is prepared via a method which to obtain：
(1) 1.5g urea, 0.37g ammonium fluorides, 0.221g nickel acetates, 0.649g manganese acetates, 0.25g glucose are dissolved in
In 50mL deionized waters, the amount ratio of the substance of nickel acetate and manganese acetate is 1：3, urea, ammonium fluoride, nickel acetate, manganese acetate substance
Amount concentration to be respectively 0.5mol/L, 0.2mol/L, 0.025mol/L, 0.075mol/L make it fill with magnetic stirrer
Divide dissolving, is uniformly mixed, is configured to mixed solution；
(2) titanium sheet that HCl treatment is crossed will be used to be placed in the mixed solution of step (1) preparation as substrate；Then poly- four
It is heated to seal to 125 DEG C in the autoclave of vinyl fluoride liner (100 milliliters), is kept for 6 hours；Titanium metal plate is taken after natural cooling
Go out, be placed in quartz tube furnace under argon atmosphere be heated to 450 DEG C anneal 1 hour, obtain nickel manganese composite oxide in titanium substrate
Nanometer water chestnut column array electrode.
Nickel manganese composite oxide nanometer water chestnut column array electrode in titanium substrate described in the present embodiment is done into scanning electron microscope
It observes, the result is shown in Figure 1 (a) and (b).Fig. 1 (a) and (b) the result shows that, nickel manganese composite oxide nanometer water chestnut column is uniform, intensive
Ground is distributed in surface of metal titanium, is presented array format, single nickel manganese composite oxide nanometer water chestnut column a diameter of 300~
400nm.Fig. 1 (c) is the X-ray diffractogram of nickel manganese composite oxide nanometer water chestnut column array electrode in titanium substrate, can be with from figure
Find out：Other than the diffraction maximum of titanium substrate, prepared electrode is mainly reflected in MnO structures and a small amount of MnF；Fig. 2 (d) is EDS
Quantitative analysis results, Fig. 2 (e) be constituent content analysis as a result, it can be seen that：Also contain a certain amount of Ni in the electrode
And carbon, form Ni0.25Mn0.75O@component Cs, and nickel manganese atom content ratio is 1:3.
Using nickel manganese composite oxide nanometer water chestnut column array electrode in the titanium substrate that the present embodiment is prepared as work electricity
Pole, Pt are used as to electrode, and calomel electrode (SCE) is reference electrode, and three electricity are carried out in lithium chloride (LiCl) solution of 2mol/L
As a result pole performance of the supercapacitor test is shown in that Fig. 2, wherein a are that sweep speed distinguishes 5mV/s, 10mV/s, 25mV/s, 50mV/s
Cyclic voltammetry curve figure, as can be seen from Figure：Nickel manganese composite oxide nanometer water chestnut column array electrode is shown in the titanium substrate
The cyclic voltammetry curve for comparing rectangle, illustrates it with good capacitive characteristics, and potential region is up to 1.4V, and without apparent
Water electrolysis reaction occurs；B is the constant current charge-discharge curve graph under different current densities, and c is high rate performance figure, in current density
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 when constant current charge-discharge, capacitance is 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.It can be obtained 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, capacity maintenance dose are respectively (compared with capacitance when current density is 1 milliamps per square centimeter) 86.4%, 77.4%,
73.7% and 72.8%；D is impedance diagram, and solution resistance 8.1ohm, load transfer impedance is 9.2ohm, and the inside illustration is enlarged drawing；e
Scheme for cycle, tested with the volt-ampere round-robin method of 25mV/s, capacitance size is first cycle capacitance size after 4800 cycles
73%.The above results illustrate that nickel manganese composite oxide nanometer water chestnut column array electrode is made in the titanium substrate that the present embodiment is prepared
There is good electrochemical capacitance performance for supercapacitor positive electrode.
Embodiment 2
Nickel manganese composite oxide nanometer water chestnut column array electrode in a kind of titanium substrate, is prepared via a method which to obtain：
(1) 1.5g urea, 0.37g ammonium fluorides, 0.221g nickel acetates, 0.649g manganese acetates, 0.25g glucose are dissolved in
In 50mL deionized waters, the amount ratio of the substance of nickel acetate and manganese acetate is 1：3, urea, ammonium fluoride, nickel acetate, manganese acetate substance
Amount concentration to be respectively 0.5mol/L, 0.2mol/L, 0.025mol/L, 0.075mol/L make it fill with magnetic stirrer
Divide dissolving, is uniformly mixed, is configured to mixed solution；
(2) titanium sheet that HCl treatment is crossed will be used to be placed in the mixed solution of step (1) preparation as substrate；Then poly- four
It is heated to seal to 140 DEG C in the autoclave of vinyl fluoride liner (100 milliliters), is kept for 8 hours；Titanium metal plate is taken after natural cooling
Go out, be placed in quartz tube furnace under argon atmosphere be heated to 450 DEG C anneal 1 hour, obtain nickel manganese composite oxide in titanium substrate
Nanometer water chestnut column array electrode.
Nickel manganese composite oxide nanometer water chestnut column array electrode in titanium substrate described in the present embodiment is done into scanning electron microscope
Observation, is as a result shown in Fig. 3.Fig. 3 (a) is Ni0.25Mn0.75O@C section SEM figures, as can be seen from the figure：Array being capable of compact growth
In titanium sheet, straight uniform；(b) it is enlarged drawing, it is amplified to find that prismatic surface has a large amount of carbon char particle and nano-pore, it should
There is nanoprisms loose structure to show highly porous form, this transports ion highly beneficial.
Embodiment 3
Nickel manganese composite oxide nanometer water chestnut column array electrode in a kind of titanium substrate, is prepared via a method which to obtain：
(1) 1.5g urea, 0.37g ammonium fluorides, 0.221g nickel acetates, 0.649g manganese acetates, 0.25g glucose are dissolved in
In 50mL deionized waters, the amount ratio of the substance of nickel acetate and manganese acetate is 1：3, urea, ammonium fluoride, nickel acetate, manganese acetate substance
Amount concentration to be respectively 0.5mol/L, 0.2mol/L, 0.025mol/L, 0.075mol/L make it fill with magnetic stirrer
Divide dissolving, is uniformly mixed, is configured to mixed solution；
(2) titanium sheet that HCl treatment is crossed will be used to be placed in the mixed solution of step (1) preparation as substrate；Then poly- four
It is heated to seal to 110 DEG C in the autoclave of vinyl fluoride liner (100 milliliters), is kept for 8 hours；Titanium metal plate is taken after natural cooling
Go out, be placed in quartz tube furnace under argon atmosphere be heated to 500 DEG C anneal 2 hours, obtain nickel manganese composite oxide in titanium substrate
Nanometer water chestnut column array electrode.
Obviously, above-described embodiment be only intended to clearly illustrate made by example, and not limitation to embodiment.It is right
For those of ordinary skill in the art, can also make on the basis of the above description it is other it is various forms of variation or
It changes.There is no necessity and possibility to exhaust all the enbodiments.And the obvious variation or change therefore amplified
It moves within still in the protection domain of the invention.
Claims (9)
1. nickel manganese composite oxide nanometer water chestnut column array electrode in a kind of titanium substrate, which is characterized in that the electrode is by titanium
The nickel manganese composite oxide nanometer water chestnut column array grown in substrate and titanium metal substrate is constituted, the nickel manganese composite oxide nanometer
Water chestnut column is vertical, uniformly, be densely distributed in titanium metal substrate surface, array format is presented；The nickel manganese composite oxide be containing
The nickel manganese composite oxide of carbon, molecular formula Ni0.25Mn0.75O@C, nickel manganese atom content ratio are 1:3.
2. nickel manganese composite oxide nanometer water chestnut column array electrode in titanium substrate according to claim 1, which is characterized in that single
A diameter of 200 ~ 500nm of root nickel manganese composite oxide nanometer water chestnut column.
3. the preparation method of nickel manganese composite oxide nanometer water chestnut column array electrode in any titanium substrate of claim 1 ~ 2,
It is characterized in that, includes the following steps：
（1）Urea, ammonium fluoride, nickel acetate, manganese acetate, glucose are dissolved in deionized water, mixed after being sufficiently mixed uniformly
Close solution；
（2）The titanium metal plate that HCl treatment is crossed is placed in step（1）In the mixed solution, be put into reaction kettle heated sealed into
Row hydro-thermal reaction；After reaction, after solution natural cooling to be mixed, titanium metal plate is taken out, is cleaned, drying；
（3）By step（2）Titanium metal plate after drying is made annealing treatment under argon atmosphere, after annealing, is obtained
Nickel manganese composite oxide nanometer water chestnut column array electrode in titanium substrate.
4. preparation method according to claim 3, which is characterized in that the object of nickel acetate and manganese acetate in the mixed solution
The amount ratio of matter is 1:3.
5. preparation method according to claim 3, which is characterized in that the molar concentration of glucose is in the mixed solution
0.042 mol/L。
6. preparation method according to claim 3, which is characterized in that the urea, ammonium fluoride, nickel acetate, manganese acetate and
The mass ratio of glucose is 1500:370:221:649:250.
7. preparation method according to claim 3, which is characterized in that step（2）The temperature of the hydro-thermal reaction
Degree is 110 ~ 140 DEG C, and the time is 6 ~ 8h.
8. preparation method according to claim 3, which is characterized in that step（3）The temperature of the annealing
Degree is 450 ~ 500 DEG C, and the time is 1 ~ 2h.
9. nickel manganese composite oxide nanometer water chestnut column array electrode is in ultracapacitor in titanium substrate described in claim 1
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| CN103098160A (en) * | 2010-09-07 | 2013-05-08 | 国际商业机器公司 | Nanostructure electrode for pseudocapacitive energy storage |
| CN103606467A (en) * | 2013-11-21 | 2014-02-26 | 东华大学 | Preparation method for NiCo2O4/MnO2/AC water system asymmetric super capacitor |
| WO2014085784A1 (en) * | 2012-11-30 | 2014-06-05 | The Regents Of The University Of California | Low-temperature continuous process to derive size-controlled lithium ion anodes and cathodes |
| 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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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103098160A (en) * | 2010-09-07 | 2013-05-08 | 国际商业机器公司 | Nanostructure electrode for pseudocapacitive energy storage |
| WO2014085784A1 (en) * | 2012-11-30 | 2014-06-05 | The Regents Of The University Of California | Low-temperature continuous process to derive size-controlled lithium ion anodes and cathodes |
| CN103606467A (en) * | 2013-11-21 | 2014-02-26 | 东华大学 | Preparation method for NiCo2O4/MnO2/AC water system asymmetric super capacitor |
| 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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