CN103545116A - Foamed nickel-nanometer eight-vulcanization and nine-cobalt composite material, preparation method for same and super-capacitor electrode - Google Patents
Foamed nickel-nanometer eight-vulcanization and nine-cobalt composite material, preparation method for same and super-capacitor electrode Download PDFInfo
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- CN103545116A CN103545116A CN201310438808.3A CN201310438808A CN103545116A CN 103545116 A CN103545116 A CN 103545116A CN 201310438808 A CN201310438808 A CN 201310438808A CN 103545116 A CN103545116 A CN 103545116A
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- 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
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- 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 relates to a foamed nickel-nanometer eight-vulcanization and nine-cobalt composite material, a preparation method for the same and a super-capacitor electrode. The composite material is formed by adhering tubular nanometer eight-vulcanization and nine-cobalt to the surface of foamed nickel. The preparation method comprises the following steps of directly forming precursor on the foamed nickel by using cobalt salt and urea; and preparing the foamed nickel-nanometer eight-vulcanization and nine-cobalt composite material by using sulphur source water heat. The composite nanometer material is stable in performance; and the super-capacitor electrode manufactured by using the composite nanometer material is excellent in performance.
Description
Technical field
The invention belongs to technical field of nano material, be specifically related to a kind of nickel foam-nanometer eight sulfuration nine cobalt composite materials and preparation method thereof, super capacitor electrode.
Background technology
Ultracapacitor is a kind of novel energy device occurring in recent years, ultracapacitor is a kind of novel energy device between physical capacitor and secondary cell, can provide the energy density higher than lithium battery, than the power density of the high nearly order of magnitude of battery and longer cycle life.It is fast that ultracapacitor has charging rate than traditional capacitor, have extended cycle life, discharge power is high, capacity is large, working temperature is wide, prepare pollution-free, the advantages such as long shelf-life, the application of all having succeeded in a lot of fields, the little power supply to electronic toy, large to Aero-Space startup system, all instrument and equipment systems relevant to energy work rate such as the energy work rate system of electric automobile all have the figure of ultracapacitor, super capacitor energy storage system is by the energy and the unified green technology of environmental protection, it is to the environment of preserving our planet, air conservation is a positive feasible strategy.Therefore be subject in recent years people's extensive concern.
Chinese patent CN102509627A discloses a kind of method of preparing carbon particulate supercapacitor electrode in situ by adopting foamed nickel.But the electrochemical capacitor of the prepared electrode of the method only only has 20～60F g
-1, be not suitable for the demand of Future New Energy Source.
Summary of the invention
For the deficiencies in the prior art, the invention provides a kind of nickel foam-nanometer eight sulfuration nine cobalt composite material super capacitor electrodes and preparation method thereof, utilize cobalt salt and urea directly in nickel foam, to form predecessor, by sulphur source hydro-thermal, prepare nickel foam-nanometer eight sulfuration nine cobalt composite materials again, this composite nano materials stable performance, the ultracapacitor excellent performance that uses this composite nano materials to prepare.
The technical solution used in the present invention is:
-nanometer eight sulfuration nine cobalt composite materials, consist of nickel foam surface attachment tubular nanometer eight sulfuration nine cobalts;
Pipe range 10～25 μ m of described tubular nanometer eight sulfuration nine cobalts, tube outer diameter 100～280nm.
A preparation method for nickel foam-nanometer eight sulfuration nine cobalt composite materials, step comprises:
A, by cobalt salt and the urea mixed solution of preparing soluble in water, in mixed solution, cobalt salt concentration is 0.02～0.1 mol/L, urea concentration is 0.1～0.4 mol/L, clean nickel foam is immersed in mixed solution, at 95-140 ℃, react 2-10h, cooling, take out washes clean, the dry predecessor that makes; Described cobalt salt is selected from one or both in cobalt chloride, cobalt nitrate;
B, the predecessor that steps A is made are put into reactor, add 0.02～0.1 mol/L containing S
2-the solution of the salt of ion, to submergence predecessor, is heated to 100-140 ℃, more than reaction 2h, takes out washing, dry, makes nickel foam-nanometer eight sulfuration nine cobalt composite materials; Described containing S
2-the salt of ion is selected from one or both in vulcanized sodium, potassium sulfide.
, use the eight sulfuration nine cobalt composite material preparations of nickel foam-nanometer.
The present invention utilizes cobalt salt and urea directly in nickel foam, to form predecessor, utilize Kinkendal Effect, by sulphur source hydro-thermal, preparing Ni-based eight sulfuration nine cobalt nano-tube arrays is nickel foam-nanometer eight sulfuration nine cobalt composite materials, this composite property is stable, and the ultracapacitor excellent performance that uses this composite material to prepare, has good capacitance characteristic, energy density is high, the features such as the conservation rate after 2,000 times that circulates reaches 90% left and right, has good stability, and the high and Applicable temperature of electric capacity is wide; Preparation method is simple to operate, is easy to promote.
Accompanying drawing explanation
Fig. 1 and Fig. 2 are the scanning electron microscope (SEM) photograph of nickel foam-nanometer eight sulfuration nine cobalt composite materials of embodiment 1 preparation;
Fig. 3 for nickel foam-nanometer eight sulfuration nine cobalt composite materials of using embodiment 1,2,3 preparations as the three-electrode system of electrode of super capacitor the cyclic voltammogram in the KOH of 3mol/L solution;
Fig. 4 be nickel foam-nanometer eight sulfuration nine cobalt composite materials of embodiment 1,2,3 preparation as the three-electrode system of electrode of super capacitor the constant current charge electric discharge figure in the KOH of 3mol/L solution;
Fig. 5 is the scanning electron microscope (SEM) photograph of nickel foam-nanometer eight sulfuration nine cobalt composite materials of embodiment 2 preparations;
Fig. 6 is the scanning electron microscope (SEM) photograph of nickel foam-nanometer eight sulfuration nine cobalt composite materials of embodiment 3 preparations;
Embodiment
Embodiment 1
-nanometer eight sulfuration nine cobalt composite materials, consist of nickel foam surface attachment tubular nanometer eight sulfuration nine cobalts; Pipe range 10～20 μ m of described tubular nanometer eight sulfuration nine cobalts, tube outer diameter 120～250nm.
A preparation method for nickel foam-nanometer eight sulfuration nine cobalt composite materials, step comprises:
A, by cobalt chloride and the urea mixed solution of preparing soluble in water, in mixed solution, cobalt chloride concentration is 0.08mol/L, urea concentration is 0.3mol/L, clean nickel foam is immersed in mixed solution, at 95 ℃, react 10h, cooling, after taking out, use deionized water and absolute ethanol washing, 50 ℃ dry, makes predecessor;
B, the predecessor that steps A is made are put into reactor, add 0.02mol/L sodium sulfide solution to submergence predecessor, are heated to 100 ℃, and reaction 6h takes out and washes with water totally, and vacuumize make nickel foam-nanometer eight sulfuration nine cobalt composite materials.
, use the eight sulfuration nine cobalt composite material preparations of nickel foam-nanometer.
Fig. 1 is the low power field emission scanning electron microscope picture (FESEM) of nickel foam-nanometer eight sulfuration nine cobalt composite materials of embodiment 1 preparation, as shown is eight sulfuration nine cobalt products and is grown in nickel foam completely.
Fig. 2 is the high power field emission scanning electron microscope picture (FESEM) of nickel foam-nanometer eight sulfuration nine cobalt composite materials of embodiment 1 preparation, and nanometer eight sulfuration nine cobalts are hollow structure as shown in the figure.
In order to test the chemical property of prepared electrode, with Hg/Hg
2cl
2electrode is as reference electrode, using platinum electrode as electrode and Ni-based eight sulfuration nine cobalt nano-tube arrays are formed to three-electrode system, in the KOH of 3mol/L electrolyte aqueous solution, carry out the test of chemical property, test electrode is at the cyclic voltammetry curve of 50mV/s, test result is as Fig. 3, curve is the closed figures that has redox peak, illustrate that its capacity is mainly from the redox reaction of eight sulfuration nine cobalts and electrolyte, can find out that charging and discharging curve presents typical symmetrical and linear change in time, the voltage that capacitor in charge and discharge process is described is linear change in time, can there is good capacitance characteristic.
As the three-electrode system of electrode of super capacitor, the constant current charge electric discharge figure in the KOH of 3mol/L solution, as Fig. 4, show that according to following formula electric capacity is 1245F/g to nickel foam-nanometer eight sulfuration nine cobalt composite materials of embodiment 1 preparation.
Wherein C is electric capacity, and I is electric current, and m is active material quality, and Δ t is discharge time, and Δ v is electromotive force window.
Embodiment 2
-nanometer eight sulfuration nine cobalt composite materials, consist of nickel foam surface attachment tubular nanometer eight sulfuration nine cobalts; Pipe range 15～25 μ m of described tubular nanometer eight sulfuration nine cobalts, tube outer diameter 120～280nm.
A preparation method for nickel foam-nanometer eight sulfuration nine cobalt composite materials, step comprises:
A, by cobalt chloride and the urea mixed solution of preparing soluble in water, in mixed solution, cobalt salt concentration is 0.1mol/L, urea concentration is 0.4mol/L, clean nickel foam is immersed in mixed solution, at 140 ℃, react 2h, cooling, after taking out, use deionized water and absolute ethanol washing, 50 ℃ dry, makes predecessor;
B, the predecessor that steps A is made are put into reactor, add 0.04mol/L sodium sulfide solution to submergence predecessor, are heated to 140 ℃, and reaction 4h takes out and washes with water totally, and vacuumize make nickel foam-nanometer eight sulfuration nine cobalt composite materials.
, use the eight sulfuration nine cobalt composite material preparations of nickel foam-nanometer.
The electric capacity that goes out to use the present embodiment to prepare ultracapacitor prepared by nickel foam-nanometer eight sulfuration nine cobalt composite materials according to Fig. 4 constant current charge electric discharge graphic calculation is 1775F/g.
Embodiment 3
-nanometer eight sulfuration nine cobalt composite materials, consist of nickel foam surface attachment tubular nanometer eight sulfuration nine cobalts; Pipe range 10～18 μ m of described tubular nanometer eight sulfuration nine cobalts, tube outer diameter 100～200nm.
A preparation method for nickel foam-nanometer eight sulfuration nine cobalt composite materials, step comprises:
A, by cobalt nitrate and the urea mixed solution of preparing soluble in water, in mixed solution, cobalt nitrate concentration is 0.02mol/L, urea concentration is 0.1mol/L, clean nickel foam is immersed in mixed solution, at 120 ℃, react 6h, cooling, after taking out, use deionized water and absolute ethanol washing, 50 ℃ dry, makes predecessor;
B, the predecessor that steps A is made are put into reactor, add 0.1mol/L potassium sulfide solution to submergence predecessor, are heated to 120 ℃, and reaction 2h takes out and washes with water totally, and vacuumize make nickel foam-nanometer eight sulfuration nine cobalt composite materials.
, use the eight sulfuration nine cobalt composite material preparations of nickel foam-nanometer.
The electric capacity that goes out to use the present embodiment to prepare ultracapacitor prepared by nickel foam-nanometer eight sulfuration nine cobalt composite materials according to Fig. 4 constant current charge electric discharge graphic calculation is 1306F/g.
Claims (6)
1. nickel foam-nanometer eight sulfuration nine cobalt composite materials, consist of nickel foam surface attachment tubular nanometer eight sulfuration nine cobalts.
2. composite material as claimed in claim 1, is characterized in that, pipe range 10～25 μ m of described tubular nanometer eight sulfuration nine cobalts, tube outer diameter 100～280nm.
3. nickel foam-nanometer eight is vulcanized a preparation method for nine cobalt composite materials, and step comprises:
A, by cobalt salt and the urea mixed solution of preparing soluble in water, in mixed solution, cobalt salt concentration is 0.02～0.1mol/L, urea concentration is 0.1～0.4mol/L, clean nickel foam is immersed in mixed solution, at 95-140 ℃, react 2-10h, cooling, take out washes clean, the dry predecessor that makes;
B, the predecessor that steps A is made are put into reactor, add containing S
2-the solution of the salt of 0.02～0.1mol/L, to submergence predecessor, is heated to 100-140 ℃, more than reaction 2h, takes out washing, dry, makes nickel foam-nanometer eight sulfuration nine cobalt composite materials.
4. preparation method as claimed in claim 3, is characterized in that, described cobalt salt is selected from one or both in cobalt chloride, cobalt nitrate.
5. preparation method as claimed in claim 3, is characterized in that, described containing S
2-the salt of ion is selected from one or both in vulcanized sodium, potassium sulfide.
6. a super capacitor electrode, is used the eight sulfuration nine cobalt composite material preparations of nickel foam-nanometer.
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104538586A (en) * | 2014-12-09 | 2015-04-22 | 三峡大学 | In-situ electrode and preparation method thereof |
| CN104795245A (en) * | 2015-05-14 | 2015-07-22 | 安徽师范大学 | Wire-shaped nickel cobalt oxide@nickel cobalt sulfide hetero-structure composite, and preparation method and purpose thereof |
| CN104876282A (en) * | 2015-04-27 | 2015-09-02 | 浙江大学 | CoSx nanomaterial used as super capacitor electrode and preparation method of CoSx nanomaterial |
| CN106783234A (en) * | 2017-01-13 | 2017-05-31 | 安徽师范大学 | A kind of preparation method and application of cobalt sulfide/cobalt basic salt nano composite material |
| CN107195482A (en) * | 2017-05-04 | 2017-09-22 | 华侨大学 | A kind of nanometer rods array composite and its preparation method and application |
| CN107213908A (en) * | 2017-07-04 | 2017-09-29 | 安徽师范大学 | A kind of trisulfides four cobalts nano-hollow pipe@nickel foam composite arrays material, preparation method and applications |
| CN107326384A (en) * | 2017-06-02 | 2017-11-07 | 浙江大学 | Composite of eight nine cobalts of vulcanization and titanium dioxide and its preparation method and application |
| CN108538622A (en) * | 2018-06-14 | 2018-09-14 | 长沙理工大学 | The preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials |
| CN108677191A (en) * | 2018-05-30 | 2018-10-19 | 大连交通大学 | A kind of nano wire skeleton three-dimensional porous foams nickel and preparation method thereof |
| CN109161925A (en) * | 2018-11-09 | 2019-01-08 | 天津工业大学 | A kind of preparation and Hydrogen Evolution Performance research of 3D structure Zn-Co-S nanocomposite |
| CN109786725A (en) * | 2019-03-25 | 2019-05-21 | 江苏大学 | Independent self-supporting positive electrode and preparation method thereof and aluminium ion battery and preparation method thereof |
| CN110459744A (en) * | 2019-08-01 | 2019-11-15 | 华南师范大学 | A kind of silicon-carbon cobalt sulfide compound, lithium ion battery negative material and preparation method thereof |
| CN111682180A (en) * | 2020-06-19 | 2020-09-18 | 西安建筑科技大学 | Preparation and application of porous foamy graphene oxide coated Co9S8@ S composite material |
| CN112023942A (en) * | 2020-09-03 | 2020-12-04 | 广州大学 | NiMoO3S/foam nickel composite material and preparation method and application thereof |
| CN112410816A (en) * | 2020-11-20 | 2021-02-26 | 武汉金特明新材料科技有限公司 | Electrocatalyst and preparation method thereof |
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Cited By (18)
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| CN104538586B (en) * | 2014-12-09 | 2017-02-22 | 三峡大学 | In-situ electrode and preparation method thereof |
| CN104538586A (en) * | 2014-12-09 | 2015-04-22 | 三峡大学 | In-situ electrode and preparation method thereof |
| CN104876282A (en) * | 2015-04-27 | 2015-09-02 | 浙江大学 | CoSx nanomaterial used as super capacitor electrode and preparation method of CoSx nanomaterial |
| CN104795245A (en) * | 2015-05-14 | 2015-07-22 | 安徽师范大学 | Wire-shaped nickel cobalt oxide@nickel cobalt sulfide hetero-structure composite, and preparation method and purpose thereof |
| CN106783234A (en) * | 2017-01-13 | 2017-05-31 | 安徽师范大学 | A kind of preparation method and application of cobalt sulfide/cobalt basic salt nano composite material |
| CN107195482A (en) * | 2017-05-04 | 2017-09-22 | 华侨大学 | A kind of nanometer rods array composite and its preparation method and application |
| CN107326384B (en) * | 2017-06-02 | 2019-04-05 | 浙江大学 | The composite material and preparation method and application of eight vulcanization nine cobalts and titanium dioxide |
| CN107326384A (en) * | 2017-06-02 | 2017-11-07 | 浙江大学 | Composite of eight nine cobalts of vulcanization and titanium dioxide and its preparation method and application |
| CN107213908A (en) * | 2017-07-04 | 2017-09-29 | 安徽师范大学 | A kind of trisulfides four cobalts nano-hollow pipe@nickel foam composite arrays material, preparation method and applications |
| CN108677191A (en) * | 2018-05-30 | 2018-10-19 | 大连交通大学 | A kind of nano wire skeleton three-dimensional porous foams nickel and preparation method thereof |
| CN108538622A (en) * | 2018-06-14 | 2018-09-14 | 长沙理工大学 | The preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials |
| CN109161925A (en) * | 2018-11-09 | 2019-01-08 | 天津工业大学 | A kind of preparation and Hydrogen Evolution Performance research of 3D structure Zn-Co-S nanocomposite |
| CN109786725A (en) * | 2019-03-25 | 2019-05-21 | 江苏大学 | Independent self-supporting positive electrode and preparation method thereof and aluminium ion battery and preparation method thereof |
| CN110459744A (en) * | 2019-08-01 | 2019-11-15 | 华南师范大学 | A kind of silicon-carbon cobalt sulfide compound, lithium ion battery negative material and preparation method thereof |
| CN110459744B (en) * | 2019-08-01 | 2021-01-08 | 华南师范大学 | Silicon-carbon cobalt sulfide compound, lithium ion battery cathode material and preparation method thereof |
| CN111682180A (en) * | 2020-06-19 | 2020-09-18 | 西安建筑科技大学 | Preparation and application of porous foamy graphene oxide coated Co9S8@ S composite material |
| CN112023942A (en) * | 2020-09-03 | 2020-12-04 | 广州大学 | NiMoO3S/foam nickel composite material and preparation method and application thereof |
| CN112410816A (en) * | 2020-11-20 | 2021-02-26 | 武汉金特明新材料科技有限公司 | Electrocatalyst and preparation method thereof |
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Application publication date: 20140129 |