CN106783234B - A kind of preparation method and application of cobalt sulfide/cobalt basic salt nanocomposite - Google Patents
A kind of preparation method and application of cobalt sulfide/cobalt basic salt nanocomposite Download PDFInfo
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- CN106783234B CN106783234B CN201710025907.7A CN201710025907A CN106783234B CN 106783234 B CN106783234 B CN 106783234B CN 201710025907 A CN201710025907 A CN 201710025907A CN 106783234 B CN106783234 B CN 106783234B
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- 239000010941 cobalt Substances 0.000 title claims abstract description 74
- 229910017052 cobalt Inorganic materials 0.000 title claims abstract description 74
- -1 cobalt basic salt Chemical class 0.000 title claims abstract description 71
- INPLXZPZQSLHBR-UHFFFAOYSA-N cobalt(2+);sulfide Chemical compound [S-2].[Co+2] INPLXZPZQSLHBR-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000007772 electrode material Substances 0.000 claims abstract description 13
- 239000002070 nanowire Substances 0.000 claims abstract description 13
- 239000003990 capacitor Substances 0.000 claims abstract description 11
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 8
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 56
- 239000006260 foam Substances 0.000 claims description 28
- 229910052759 nickel Inorganic materials 0.000 claims description 28
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 14
- 239000004202 carbamide Substances 0.000 claims description 14
- 150000001868 cobalt Chemical class 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 8
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical group [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 150000002500 ions Chemical class 0.000 claims description 6
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 5
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 4
- 238000009938 salting Methods 0.000 claims description 4
- 230000008859 change Effects 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 150000003839 salts Chemical class 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 239000005864 Sulphur Substances 0.000 claims 1
- 238000006243 chemical reaction Methods 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 229910052700 potassium Inorganic materials 0.000 claims 1
- 239000011591 potassium Substances 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 8
- 238000012983 electrochemical energy storage Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 18
- 229920006362 Teflon® Polymers 0.000 description 15
- 239000004809 Teflon Substances 0.000 description 14
- 229910001220 stainless steel Inorganic materials 0.000 description 10
- 239000010935 stainless steel Substances 0.000 description 10
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 description 6
- 239000012467 final product Substances 0.000 description 5
- 239000002086 nanomaterial Substances 0.000 description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 4
- 230000005611 electricity Effects 0.000 description 4
- DPLVEEXVKBWGHE-UHFFFAOYSA-N potassium sulfide Chemical compound [S-2].[K+].[K+] DPLVEEXVKBWGHE-UHFFFAOYSA-N 0.000 description 4
- 229910052979 sodium sulfide Inorganic materials 0.000 description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 3
- 241000209094 Oryza Species 0.000 description 2
- 235000007164 Oryza sativa Nutrition 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- NUJOXMJBOLGQSY-UHFFFAOYSA-N manganese dioxide Chemical compound O=[Mn]=O NUJOXMJBOLGQSY-UHFFFAOYSA-N 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 235000009566 rice Nutrition 0.000 description 2
- 238000004073 vulcanization Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 229910019897 RuOx Inorganic materials 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000002322 conducting polymer Substances 0.000 description 1
- 229920001940 conductive polymer Polymers 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 229910000000 metal hydroxide Inorganic materials 0.000 description 1
- 150000004692 metal hydroxides Chemical class 0.000 description 1
- 229910052976 metal sulfide Inorganic materials 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 235000012149 noodles Nutrition 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 229920000767 polyaniline Polymers 0.000 description 1
- 229920000123 polythiophene Polymers 0.000 description 1
- 238000000634 powder X-ray diffraction Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- VRRFSFYSLSPWQY-UHFFFAOYSA-N sulfanylidenecobalt Chemical class [Co]=S VRRFSFYSLSPWQY-UHFFFAOYSA-N 0.000 description 1
- 238000010301 surface-oxidation reaction Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
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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
- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Power Engineering (AREA)
- Nanotechnology (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
- Composite Materials (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention discloses a kind of preparation method and applications of cobalt sulfide/cobalt basic salt nanocomposite.First, it is prepared for cobalt basic salt nano wire by hydro-thermal method, then cobalt basic salt nano wire is converted to by gas phase hydro-thermal method cobalt sulfide/cobalt basic salt nanocomposite of hierarchical structure, in the hierarchical structure, cobalt sulfide nanometer sheet is supported on the surface of cobalt basic salt nano wire, thin nanometer sheet has high specific surface area, it is possible to provide more electro-chemical activity sites are for storing electric energy, to obtain high specific capacitance；Nano wire itself is other than participating in electrochemical energy storage, moreover it is possible to provide support for nanometer sheet, prevent the mutual reunion of nanometer sheet and influence chemical property.Therefore, cobalt sulfide disclosed by the invention/cobalt basic salt nanocomposite can be used as electrode material for super capacitor, with excellent chemical property.
Description
Technical field
The present invention relates to a kind of preparation method and applications of cobalt sulfide/cobalt basic salt nanocomposite, and in particular to one
Plant the preparation method of cobalt sulfide/cobalt basic salt nanocomposite of hierarchical structure and its on electrode material for super capacitor
Using.
Background technology
Ultracapacitor can be generally divided into double layer capacitor (EDLC) and fake capacitance capacitor.EDLC passes through in electricity
The ionic adsorption of pole/electrolyte interface stores charge, and fake capacitance capacitor is reacted by quick surface oxidation reduction and stored
Charge.Electrode material is the principal element for the energy stores performance for determining ultracapacitor.
Carbon-based material such as activated carbon, carbon nanotube and graphene are typical EDLC electrode materials.Transition metal oxide
(such as RuOx, MnO2), metal hydroxides, conducting polymer (such as polyaniline, polythiophene) and metal sulfide (such as
Co8S9, NiS) and it is fake capacitance electrode material, the energy density of ultracapacitor still cannot meet the requirement of practical application at present,
Therefore there is still a need for a large amount of effort to improve the capacitive property of electrode material for super capacitor.
Nano material of single structure, such as nanometer sheet, nanometer rods, nanotube etc. are as electrode material for super capacitor
Specific capacitance is often not ideal enough.Recently, the nano material for building hierarchical structure is considered as a kind of super electricity of exploitation high-performance
The available strategy of container electrode material, in the hierarchical structure nano material reported, ultra-thin nanometer sheet is grown in nano wire
Or on the carrier of other large-sizes, ultrathin nanometer piece has high-specific surface area, can provide more electrochemical energy storage activity
Site.Therefore, these hierarchical structure nano materials can obtain excellent chemical property.
Invention content
The present invention provides a kind of preparation methods of cobalt sulfide/cobalt basic salt nanocomposite to pass through hydro-thermal method first
It is prepared for cobalt basic salt nano wire, then converts cobalt basic salt nano wire to by gas phase hydro-thermal method the vulcanization of hierarchical structure
Cobalt/cobalt basic salt nanocomposite.The cobalt sulfide of the hierarchical structure/cobalt basic salt nanocomposite is received by cobalt basic salt
Cobalt sulfide nanometer sheet is loaded on the surface of rice noodles to be constituted.
The present invention also provides cobalt sulfide/application of the cobalt basic salt nanocomposite on ultracapacitor.
The technical solution that the present invention takes is：
A kind of preparation method of cobalt sulfide/cobalt basic salt nanocomposite, the preparation method comprises the following steps：
A, mixed solution is prepared by cobalt salt and urea are soluble in water, 95~140 DEG C of hydro-thermal reactions 2~8 hours are cooling, wash
Wash, dry after be made predecessor；
B, predecessor made from step A is put on holder, frame is in containing S2-Above the salting liquid of ion, at 100~160 DEG C
Hydro-thermal reaction 2~10 hours obtains cobalt sulfide/cobalt basic salt nanocomposite after cooling.
Nickel foam can also be added in step as backing material；Then cobalt sulfide/cobalt basic salt nanocomposite can
It is grown on backing material.
The cobalt sulfide/cobalt basic salt nanocomposite is hierarchical structure, and the hierarchical structure is by cobalt basic salt nanometer
Cobalt sulfide nanometer sheet is loaded on the surface of line to be constituted.Thin nanometer sheet has high specific surface area, it is possible to provide more electrifications
Active site is learned for storing electric energy, to obtain high specific capacitance；Nano wire itself is other than participating in electrochemical energy storage, also
Support can be provided for nanometer sheet, prevent the mutual reunion of nanometer sheet and influence chemical property.
The ratio between molar concentration of the cobalt salt and urea is (0.02~0.1)：(0.08~0.4).
In the step B, contain S2-A concentration of 0.02~0.2 mol/L of the salting liquid of ion.
The cobalt salt is one or more of cobaltous sulfate, cobalt nitrate, cobalt chloride.
It is described to contain S2-The salt of ion is selected from one or both of vulcanized sodium, potassium sulfide.
The cobalt sulfide/cobalt basic salt nanocomposite can be directly used as the working electrode of ultracapacitor.
The present invention also provides the cobalt sulfide being prepared according to above-mentioned preparation method/cobalt basic salt nanocomposites to make
For the application of electrode material for super capacitor.As electrode material, which show higher specific capacitance and rate charge-discharges
Energy.
Compared with the prior art, the present invention has following advantages：
1, cobalt sulfide/cobalt basic salt of hierarchical structure, in this configuration, thin nanometer sheet are prepared for using gas phase hydro-thermal method
It is supported on the nano wire with large-size, the supporting role of nano wire can be to avoid the reunion between nanometer sheet；
2, in the hierarchical structure of the present invention, nanometer sheet has high specific surface area, can be provided more for electrochemical reaction
More active sites, therefore, the hierarchical structure nano material can obtain excellent chemical property；
3, the present invention is easy to operate, easy to spread；
4, the preparation category of the cobalt sulfide of hierarchical structure/cobalt basic salt nanocomposite is reported for the first time.
Description of the drawings
Fig. 1 is the XRD diagram of presoma cobalt basic salt (a) and cobalt sulfide/cobalt basic salt nanocomposite (b)；
Fig. 2 is that the SEM of presoma cobalt basic salt schemes；
Fig. 3 is that the SEM of cobalt sulfide/cobalt basic salt nanocomposite schemes；
Fig. 4 is that the TEM of cobalt sulfide/cobalt basic salt nanocomposite schemes；
Fig. 5 is the cyclic voltammogram that cobalt sulfide/cobalt basic salt nanocomposite electrode obtains under different scanning rates；
The charging and discharging curve figure that Fig. 6 cobalt sulfides/cobalt basic salt nanocomposite electrode obtains under different current densities；
Fig. 7 is the capacity of cobalt sulfide/cobalt basic salt nanocomposite electrode with cycle charge-discharge change curve.
Specific implementation mode
Embodiment 1
A kind of preparation method of cobalt sulfide/cobalt basic salt nanocomposite, includes the following steps：
A, cobalt chloride and urea are added in 40 milliliters of water respectively, stirring is allowed to dissolve, formation clear solution, cobalt in solution
A concentration of 0.08 mol/L of salt, urea concentration are 0.32 mol/L, and it is 50 milliliters of teflon linings that solution, which is transferred to volume,
Stainless steel autoclave in, then the clean nickel foam of a small pieces (2 2 centimetres of cm x) immersed in mixed solution, it is anti-at 95 DEG C
It answers 8 hours, after cooling, takes out foam nickel sheet, washes clean is dry, and predecessor cobalt basic salt is made；
B, 25 milliliters of 0.2 mol/L sodium sulfide solution is added to the stainless steel for the teflon lining that volume is 50 milliliters
In autoclave, then the nickel foam for being loaded with cobalt basic salt is placed on the teflon holder of superjacent, by autoclave 125
It is heated at DEG C 2 hours, then cooled to room temperature, takes out nickel foam and obtain after washed, dry and be supported on nickel foam
On cobalt sulfide/cobalt basic salt nanocomposite.
The sample of final product is characterized by X-ray powder diffraction, as shown in Figure 1, presoma main component is
Cobalt basic salt, final product are cobalt sulfide/cobalt basic salt nanocomposite.
By scanning electron microscope (SEM) and transmission electron microscope (TEM) to the pattern of presoma and final product
It is characterized.Fig. 2 is the SEM figures of presoma cobalt basic salt, shows that it is nano wire.Fig. 3 and Fig. 4 is final product vulcanization respectively
The SEM and TEM of cobalt/cobalt basic salt nanocomposite scheme, it can be seen that final product cobalt sulfide/cobalt basic salt nanocomposite
Pattern be that thin cobalt sulfide nanometer sheet is supported on cobalt basic salt nano wire.
Embodiment 2
A kind of preparation method of cobalt sulfide/cobalt basic salt nanocomposite, includes the following steps：
A, cobalt nitrate and urea are dissolved in 40 milliliters of water respectively, a concentration of 0.02 mol/L of cobalt salt, urea are dense in solution
Degree is 0.08 mol/L, solution is transferred in the stainless steel autoclave that volume is 50 milliliters of teflon linings, then a small pieces are done
Net nickel foam (2 2 centimetres of cm x) immerses in mixed solution, is reacted 2 hours at 140 DEG C, after cooling, takes out foam nickel sheet,
Washes clean, it is dry, predecessor cobalt basic salt is made；
B, the 0.02 mol/L sodium sulfide solution of 25mL is added in the stainless steel autoclave of 50mL teflon linings, so
The foam nickel sheet for being loaded with cobalt basic salt is placed on the teflon holder of superjacent afterwards, autoclave is heated at 100 DEG C
10 hours, then cooled to room temperature, took out foam nickel sheet and obtains after washed, dry and be supported on nickel foam on piece
The cobalt sulfide of hierarchical structure/cobalt basic salt nanocomposite.
Embodiment 3
A kind of preparation method of cobalt sulfide/cobalt basic salt nanocomposite, includes the following steps：
A, cobaltous sulfate and urea are dissolved in respectively in 40 milliliters of water, a concentration of 0.1 mol/L of cobalt salt, urea in solution
Solution is transferred in the stainless steel autoclave that volume is 50 milliliters of teflon linings by a concentration of 0.4 mol/L, then by a small pieces
Clean nickel foam (2 2 centimetres of cm x) immerses in mixed solution, is reacted 4 hours at 120 DEG C, after cooling, takes out nickel foam
Piece, washes clean is dry, and predecessor cobalt basic salt is made；
B, the 0.1 mol/L potassium sulfide solution of 25mL is added in the stainless steel autoclave of 50mL teflon linings, then
The foam nickel sheet for being loaded with cobalt basic salt is placed on the teflon holder of superjacent, it is small that autoclave is heated at 160 DEG C to 2
When, then cooled to room temperature, takes out foam nickel sheet and obtains the classification knot being supported in nickel foam after washed, dry
The cobalt sulfide of structure/cobalt basic salt nanocomposite.
Embodiment 4
A kind of preparation method of cobalt sulfide/cobalt basic salt nanocomposite, includes the following steps：
A, cobaltous sulfate, cobalt chloride and urea are dissolved in respectively in 40 milliliters of water, cobaltous sulfate, the concentration of cobalt chloride are equal in solution
For 0.03 mol/L, urea concentration is 0.3 mol/L, and it is high that solution is transferred to the stainless steel that volume is 50 milliliters of teflon linings
It presses in kettle, then the clean nickel foam of a small pieces (2 2 centimetres of cm x) is immersed in mixed solution, reacted 6 hours at 110 DEG C, it is cold
But after, foam nickel sheet is taken out, washes clean is dry, and predecessor cobalt basic salt is made；
B, 50mL teflons are added in the 0.08 mol/L potassium sulfide solution of 25mL and 0.06 mol/L sodium sulfide solution
In the stainless steel autoclave of lining, then the foam nickel sheet for being loaded with cobalt basic salt is placed on to the teflon holder of superjacent
On, autoclave is heated 4 hours at 150 DEG C, then cooled to room temperature, takes out foam nickel sheet, after washed, dry,
Obtain the cobalt sulfide/cobalt basic salt nanocomposite for the hierarchical structure being supported in nickel foam.
Embodiment 5
A kind of preparation method of cobalt sulfide/cobalt basic salt nanocomposite, includes the following steps：
A, cobaltous sulfate, cobalt nitrate, cobalt chloride and urea are dissolved in respectively in 40 milliliters of water, cobaltous sulfate in solution, cobalt nitrate,
The concentration of cobalt chloride is respectively 0.02 mol/L, 0.06 mol/L, 0.02 mol/L, and urea concentration is 0.4 mol/L, will
Solution is transferred in the stainless steel autoclave that volume is 50 milliliters of teflon linings, then by a small pieces clean nickel foam (2 cm x
2 centimetres) it immerses in mixed solution, it is reacted 5 hours at 130 DEG C, after cooling, takes out foam nickel sheet, washes clean is dry, is made
Predecessor cobalt basic salt；
B, the 0.15 mol/L potassium sulfide solution of 25mL is added in the stainless steel autoclave of 50mL teflon linings, so
The foam nickel sheet for being loaded with cobalt basic salt is placed on the teflon holder of superjacent afterwards, autoclave is heated 8 at 140 DEG C
Hour, then cooled to room temperature, takes out foam nickel sheet and obtains the classification being supported in nickel foam after washed, dry
The cobalt sulfide of structure/cobalt basic salt nanocomposite.
Embodiment 6
Cobalt sulfide/application of the cobalt basic salt nanocomposite as electrode material for super capacitor
The cobalt sulfide being supported in nickel foam/cobalt basic salt nanocomposite that embodiment 1 is prepared is cut into 1 li
Rice × 1 centimetre of size, as working electrode, respectively using platinum plate electrode and Hg/HgO electrodes as to electrode and reference electrode, structure
At three-electrode system, the test of chemical property is carried out in the KOH electrolyte aqueous solutions of 3 mol/Ls.Fig. 5 is in potential model
It encloses for 0~0.7V, the cyclic voltammetry curve obtained under different scanning rates, the redox peaks in figure show the counterfeit electricity of electrode
Hold characteristic.Fig. 6 is the constant current charge-discharge curve of electrode, is 1Ag in current density-1When, the specific capacitance of electrode is 1994Fg-1；
It is increased to 20Ag in current density-1When, the specific capacitance of electrode is 1600Fg-1, it is shown that higher specific capacitance and multiplying power are filled
Discharge performance.Holding current density is 4Ag-1, after 5000 charge and discharge cycles, capacitance still can maintain initial value
90.2%, as shown in Figure 7.The above electrochemical Characterization the result shows that, the cobalt sulfide/cobalt basic salt nanocomposite is a kind of electricity
The excellent electrode material for super capacitor of chemical property.
Above-mentioned reference embodiment carries out the preparation method and application of cobalt sulfide/cobalt basic salt nanocomposite detailed
Description is illustrative without being restrictive, several embodiments can be enumerated according to limited range, therefore do not departing from
Change and modification under present general inventive concept should belong within protection scope of the present invention.
Claims (8)
1. a kind of preparation method of cobalt sulfide/cobalt basic salt nanocomposite, which is characterized in that the preparation method include with
Lower step：
A, mixed solution is prepared by cobalt salt and urea are soluble in water, 95 ~ 140 DEG C of hydro-thermal reactions 2 ~ 8 hours are cooling, washing, dry
Predecessor is made afterwards；
B, predecessor made from step A is put on holder, frame is in containing S2-Above the salting liquid of ion, hydro-thermal at 100 ~ 160 DEG C
Reaction 2 ~ 10 hours obtains cobalt sulfide/cobalt basic salt nanocomposite after cooling；
The cobalt sulfide/cobalt basic salt nanocomposite is hierarchical structure, and the hierarchical structure is by cobalt basic salt nano wire
Cobalt sulfide nanometer sheet is loaded on surface to be constituted.
2. preparation method according to claim 1, which is characterized in that nickel foam can also be added in step as branch
Timbering material.
3. preparation method according to claim 1 or 2, which is characterized in that the ratio between the molar concentration of the cobalt salt and urea
For（0.02~0.1）：（0.08~0.4）.
4. preparation method according to claim 1 or 2, which is characterized in that in the step B, contain S2-The salting liquid of ion
A concentration of 0.02 ~ 0.2 mol/L.
5. preparation method according to claim 1 or 2, which is characterized in that the cobalt salt is cobaltous sulfate, cobalt nitrate, chlorination
One or more of cobalt.
6. preparation method according to claim 1 or 2, which is characterized in that described to contain S2-The salt of ion is selected from vulcanized sodium, sulphur
Change one or both of potassium.
7. preparation method according to claim 2, which is characterized in that the cobalt sulfide/cobalt basic salt nanocomposite
It can be directly used as the working electrode of ultracapacitor.
8. the cobalt sulfide that preparation method according to claim 1 or 2 is prepared/cobalt basic salt nanocomposite conduct
The application of electrode material for super capacitor.
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| CN109797405B (en) * | 2019-02-21 | 2020-11-10 | 三峡大学 | Preparation method of cobalt sulfide and nitrogen-doped carbon composite array electrode |
| CN113380553B (en) * | 2021-05-25 | 2022-10-04 | 三峡大学 | Co 3 S 4 /Co(CO 3 ) 0.5 (OH)·0.11H 2 O-grade nanowire array electrode material |
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| JP5416486B2 (en) * | 2009-06-04 | 2014-02-12 | 一般財団法人電力中央研究所 | Method for producing zeolite-containing cured body |
| CN103545116A (en) * | 2013-09-24 | 2014-01-29 | 安徽师范大学 | Foamed nickel-nanometer eight-vulcanization and nine-cobalt composite material, preparation method for same and super-capacitor electrode |
| CN105845448B (en) * | 2016-03-17 | 2018-06-01 | 安徽师范大学 | A kind of homogeneity nucleocapsid cobaltosic sulfide nano material, its preparation method and its application as electrode material for super capacitor |
| CN105957728B (en) * | 2016-07-21 | 2018-04-13 | 安徽师范大学 | A kind of nickel cobalt double-hydroxide/NiCo2S4Composite nano materials, its preparation method and the application as electrode material for super capacitor |
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