CN108538622A - The preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials - Google Patents
The preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials Download PDFInfo
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- CN108538622A CN108538622A CN201810610394.0A CN201810610394A CN108538622A CN 108538622 A CN108538622 A CN 108538622A CN 201810610394 A CN201810610394 A CN 201810610394A CN 108538622 A CN108538622 A CN 108538622A
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- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 title claims abstract description 140
- 239000006260 foam Substances 0.000 title claims abstract description 70
- 229910052759 nickel Inorganic materials 0.000 title claims abstract description 70
- 239000003990 capacitor Substances 0.000 title claims abstract description 36
- 239000000463 material Substances 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 24
- 239000000126 substance Substances 0.000 claims abstract description 8
- 238000001354 calcination Methods 0.000 claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims description 22
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 15
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims description 12
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 9
- 239000005864 Sulphur Substances 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- 239000004202 carbamide Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000003837 high-temperature calcination Methods 0.000 claims description 8
- 239000011572 manganese Substances 0.000 claims description 8
- 229910052748 manganese Inorganic materials 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 7
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- 238000001816 cooling Methods 0.000 claims description 4
- 229940099596 manganese sulfate Drugs 0.000 claims description 4
- 239000011702 manganese sulphate Substances 0.000 claims description 4
- 235000007079 manganese sulphate Nutrition 0.000 claims description 4
- MIVBAHRSNUNMPP-UHFFFAOYSA-N manganese(2+);dinitrate Chemical compound [Mn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MIVBAHRSNUNMPP-UHFFFAOYSA-N 0.000 claims description 4
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 claims description 4
- 239000012535 impurity Substances 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
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 2
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 2
- XZYZWJQNGFGZRU-UHFFFAOYSA-N azanium urea fluoride Chemical compound [F-].[NH4+].NC(=O)N XZYZWJQNGFGZRU-UHFFFAOYSA-N 0.000 claims description 2
- 229940071125 manganese acetate Drugs 0.000 claims description 2
- 239000011565 manganese chloride Substances 0.000 claims description 2
- 235000002867 manganese chloride Nutrition 0.000 claims description 2
- 229940099607 manganese chloride Drugs 0.000 claims description 2
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 229910052708 sodium Inorganic materials 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims 1
- 206010054949 Metaplasia Diseases 0.000 claims 1
- 238000003682 fluorination reaction Methods 0.000 claims 1
- 230000015689 metaplastic ossification Effects 0.000 claims 1
- 230000014759 maintenance of location Effects 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 230000035484 reaction time Effects 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 3
- 239000007772 electrode material Substances 0.000 description 10
- 239000000243 solution Substances 0.000 description 9
- 238000000034 method Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 4
- 239000011149 active material Substances 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000005611 electricity Effects 0.000 description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M potassium hydroxide Inorganic materials [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 230000008859 change Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- UCKMPCXJQFINFW-UHFFFAOYSA-N Sulphide Chemical compound [S-2] UCKMPCXJQFINFW-UHFFFAOYSA-N 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 1
- 238000003780 insertion Methods 0.000 description 1
- 230000037431 insertion Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 239000000376 reactant Substances 0.000 description 1
- 229910052979 sodium sulfide Inorganic materials 0.000 description 1
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 description 1
- CADICXFYUNYKGD-UHFFFAOYSA-N sulfanylidenemanganese Chemical compound [Mn]=S CADICXFYUNYKGD-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- 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
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
The invention belongs to ultracapacitor fields, and in particular to a kind of preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials.First nickel foam is pre-processed, then uses hydro-thermal and calcining to grow nickel foam self-supporting MnS nanometer sheet presomas in foam nickel surface, then presoma is vulcanized and generates MnS nanometer sheets, obtains the super capacitor material based on nickel foam self-supporting MnS nanometer sheets.The present invention is based on the super capacitor materials of nickel foam self-supporting MnS nanometer sheets, have excellent chemical property.In its preparation process, raw material are cheap and easy to get, and the reaction time is short, at low cost, simple and practicable, and without masterplate and surfactant-free.The electrode of super capacitor of prepared nickel foam self-supporting MnS nanometer sheets has very high specific capacity and cyclical stability.Maximum specific capacity is up to 1.71Fcm‑2, after recycling 1000 times, coulombic efficiency keeps 100%, capacity retention ratio 100%.
Description
Technical field
The invention belongs to ultracapacitor fields, and in particular to a kind of nickel foam self-supporting MnS nanometer sheet ultracapacitors
The preparation method of material.
Background technology
As important novel energy-storing equipment, ultracapacitor is since Acclimation temperature range is wide, environmental-friendly, charge and discharge are fast
The advantages that degree is fast and has extended cycle life has very extensive in the fields such as wind-power electricity generation, electronics industry and new-energy automobile
Application.In transition metal oxide family, for the oxide of manganese metal due to deriving from a wealth of sources, cheap and specific capacity is high
The advantages that and favored by researchers, but itself poor electric conductivity limits further applying as electrode material.
And the sulfide that manganese metal is prepared by ion exchange be report at present raising electrode material electric conductivity effective ways it
One.Wherein, the manganese sulfide with layer structure is very suitable for the insertion and abjection of electrolyte ion, this electricity for improving material
Chemical property has a very important significance.
On the other hand, direct growth activity substance and directly as electrode of super capacitor on the collector developed in recent years
The research of material is more and more, and the elimination of binder and conductive agent can improve the electric conductivity of electrode material to a certain extent
Energy.Wherein, with tridimensional network nickel foam due to large specific surface area uniform load active material, active material with collection
The chemical property for being in direct contact the fast transfer that can promote electronics and then improving material of fluid.Above method is integrated and is made
The MnS electrode materials of standby nickel foam self-supporting have good research significance, mesh for the bad problem of active material electric conductivity
The preceding related patents for not having the MnS nanometer sheet electrode material for super capacitor of nickel foam self-supporting also are reported.
Invention content
The object of the present invention is to provide a kind of systems based on nickel foam self-supporting MnS nanometer sheet electrode material for super capacitor
The MnS nanometer sheets of nickel foam self-supporting are prepared using simple hydro-thermal and calcining and vulcanizing treatment in Preparation Method.The party
Method raw material are cheap and easy to get, and the reaction time is short, at low cost, simple and practicable, and favorable reproducibility is had excellent performance, prepared nickel foam
MnS nanometers of plate electrodes of self-supporting have very high specific capacity and cyclical stability.
To achieve the goals above, the present invention adopts the following technical scheme that：
A kind of preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials, first locates nickel foam in advance
Then reason uses hydro-thermal and high-temperature calcination to grow MnS nanometer sheet presomas in foam nickel surface, then presoma is vulcanized and is generated
MnS nanometer sheets obtain the super capacitor material based on nickel foam self-supporting MnS nanometer sheets.
The preparation method of the nickel foam self-supporting MnS nanometer sheet super capacitor materials, is as follows：
(1) it cleans 1~3h of nickel foam with deionized water and EtOH Sonicate to be pre-processed, removes its surface impurity；
(2) in deionized water by the dissolving of manganese source, urea and ammonium fluoride, it is sufficiently stirred to obtain mixed reaction solution, later
Pretreated nickel foam is put into reaction kettle, be added mixed reaction solution, at 100~200 DEG C carry out hydro-thermal reaction 1~
5h, is completed after reaction and after being cleaned and dried, then is reacted at 200~500 DEG C through high-temperature calcination before 1~4h obtains MnS nanometer sheets
Drive body；
(3) the MnS nanometer sheet presomas after calcining are positioned in reaction kettle and are added sulphur source, the sulphur at 100~200 DEG C
Change 1~8h of reaction, is cleaned after cooling and obtain the MnS nanometer sheets grown in foam nickel surface, i.e., it is described to be based on nickel foam self-supporting
MnS nanometer sheets super capacitor material.
The preparation method of the nickel foam self-supporting MnS nanometer sheet super capacitor materials, in step 2), manganese source plus
It is 0.1~0.2molL to enter amount-1, the addition of urea is 0.1~0.2molL-1, the addition of ammonium fluoride is 0.01~
0.1mol·L-1。
The preparation methods of the nickel foam self-supporting MnS nanometer sheet super capacitor materials, manganese source, urea ammonium fluoride
Molar ratio is 3:3:1.
The preparation method of the nickel foam self-supporting MnS nanometer sheet super capacitor materials, in step 2), manganese source is manganese
Salts substances：Manganese sulfate, manganese nitrate, manganese acetate or manganese chloride.
The preparation method of the nickel foam self-supporting MnS nanometer sheet super capacitor materials, in step 3), sulphur source is sulphur
Change the solution of sodium, thiocarbamide or sulphur powder, a concentration of 0.1~0.3molL-1。
The preparation method of the nickel foam self-supporting MnS nanometer sheet super capacitor materials is grown in foam nickel surface
The mass density of MnS nanometer sheets is 0.5~1.5mgcm-2。
The preparation method of the nickel foam self-supporting MnS nanometer sheet super capacitor materials, MnS nanometer sheets it is a diameter of
1.0~2.0 μm, thickness is 0.2~0.5 μm.
The remarkable advantage and advantageous effect of the present invention is：
The present invention obtains MnS nanometers of plate electrode materials of nickel foam self-supporting using hydro-thermal and high-temperature calcination and vulcanizing treatment
Material, this method raw material are cheap and easy to get, and the reaction time is short, at low cost, simple and practicable, and favorable reproducibility is had excellent performance, and without mould
Version and surfactant-free.Prepared nickel foam self-supporting MnS nanometer sheet electrode of super capacitor has very high specific capacity
And cyclical stability, electrode maximum specific capacity is up to 1.71Fcm-2, after recycling 1000 times, coulombic efficiency keeps 100%, holds
It is 100% to measure conservation rate.
Description of the drawings
Fig. 1 is the X-ray diffractogram of MnS nanometer sheets.In figure, abscissa 2Theta represents the angle of diffraction (degree), indulges and sits
Mark Intensity represents intensity (a.u.).
Fig. 2 is the scanning electron microscope (SEM) photograph of MnS nanometer sheets.Wherein, (b) be (a) enlarged drawing.
Fig. 3 (a)-Fig. 3 (b) is the chemical property figure of MnS nanometer sheets.Wherein, Fig. 3 (a) is under different current densities
Charging and discharging curve figure, abscissa Time represent the time (s), and ordinate Potential represents current potential (V)；Fig. 3 (b) is different electricity
The specific volume spirogram being calculated under current density, abscissa Current density represent current density (Ag-1), ordinate
Areal capacitance represent specific capacity (Fcm-2)。
Fig. 4 is that current density is 2Ag-1When, the cycle performance figure of MnS nanometer sheets.In figure, abscissa Cycles representatives follow
Ring number, left ordinate Capacitance retention represent capacity retention ratio (%), right ordinate Coulombic
Efficiency represents coulombic efficiency (%).
Specific implementation mode
In specific implementation process, the present invention first pre-processes nickel foam, then uses hydro-thermal and calcining in foam
Nickel surface grows nickel foam self-supporting MnS nanometer sheet presomas, then presoma is vulcanized and generates the acquisition of MnS nanometer sheets based on foam
The super capacitor material of nickel self-supporting MnS nanometer sheets.The main function and effect of hydro-thermal reaction be：In high-temperature and high-pressure conditions
Under, reactant can be partially or completely solubilized, and reaction is carried out close to homogeneous, obtain good dispersion, purity height, shape
The controllable super capacitor material of looks.High-temperature calcination processing main function and effect be：The hydroxide that hydro-thermal reaction is obtained
Further oxidation obtains oxide electrode material to object.Present invention exploitation it is new based on the super of nickel foam self-supporting MnS nanometer sheets
Capacitor material has excellent chemical property.
The present invention is further illustrated the present invention with the following example, but protection scope of the present invention is not limited to following reality
Apply example.
The preparation of 1 nickel foam self-supporting MnS nanometer sheet electrode materials of embodiment
In the present embodiment, the specification of nickel foam is long 6cm × wide 3.6cm × thickness 1.1mm, hole count 110PPI, and face is close
Spend 420 ± 25gm-2, clean nickel foam 2h with deionized water and EtOH Sonicate and pre-processed, remove its surface impurity；It will
Manganese nitrate, urea and ammonium fluoride dissolve in deionized water, manganese nitrate 0.15molL-1, urea 0.15molL-1And
Ammonium fluoride 0.05molL-1, it is sufficiently stirred to obtain mixed reaction solution, pretreated nickel foam is put into reaction kettle later,
Mixed reaction solution is added, hydro-thermal reaction 3h is carried out at 150 DEG C, exists after reaction is completed and is cleaned and dried, then through high-temperature calcination
2.5h is reacted at 350 DEG C obtains MnS nanometer sheet presomas；MnS nanometer sheet presomas after calcining are positioned in reaction kettle simultaneously
Sodium sulfide solution, a concentration of 0.25molL is added-1, 4h is reacted at 150 DEG C, is cleaned and is obtained in nickel foam table after cooling
The MnS nanometer sheets for looking unfamiliar long, i.e., the super capacitor material of the described MnS nanometer sheets based on nickel foam self-supporting, in nickel foam
The mass density that surface grows MnS nanometer sheets is 1.0mgcm-2。
As seen from Figure 1, Figure 2, material made from the present embodiment is really MnS nanometer sheets, and specification is as follows：MnS nanometers
A diameter of 1.0 μm of piece, thickness are 0.2 μm.
2 electrochemical property test of embodiment
In the present embodiment, nickel foam self-supporting MnS nanometer sheets made from embodiment 1 are made into electrode of super capacitor and are carried out
Electrochemical property test.Test result is as shown in Figure 3, Figure 4, when electrolyte is concentration 6molL-1Potassium hydroxide aqueous solution
When, MnS nanometers of plate electrode high specific capacity of nickel foam self-supporting are up to 1.71Fcm-2, after recycling 1000 times, coulombic efficiency
100% is kept, capacity retention ratio 100%.
The preparation of 3 nickel foam self-supporting MnS nanometer sheet electrode materials of embodiment
In the present embodiment, cleans nickel foam 1h with deionized water and EtOH Sonicate and pre-processed, it is miscellaneous to remove its surface
Matter；In deionized water by the dissolving of manganese sulfate, urea and ammonium fluoride, manganese sulfate 0.18molL-1, urea 0.18molL-1
And ammonium fluoride 0.06molL-1, it is sufficiently stirred to obtain mixed reaction solution, pretreated nickel foam is put into reaction kettle later
In, mixed reaction solution is added, hydro-thermal reaction 5h is carried out at 100 DEG C, after reaction is completed and is cleaned and dried, then through high-temperature calcination
4h is reacted at 200 DEG C obtains MnS nanometer sheet presomas；MnS nanometer sheet presomas after calcining are positioned in reaction kettle simultaneously
Thiourea solution, a concentration of 0.20molL is added-1, 8h is reacted at 100 DEG C, is cleaned and is obtained in foam nickel surface after cooling
The MnS nanometer sheets of growth, i.e., the super capacitor material of the described MnS nanometer sheets based on nickel foam self-supporting, in nickel foam table
The mass density for long MnS nanometer sheets of looking unfamiliar is 0.8mgcm-2, the specification of MnS nanometer sheets is as follows：The diameter of MnS nanometer sheets
It it is 1.2 μm, thickness is 0.25 μm.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification should all belong to the covering scope of the present invention.
Claims (8)
1. a kind of preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials, which is characterized in that first to nickel foam
It is pre-processed, hydro-thermal and high-temperature calcination is then used to grow MnS nanometer sheet presomas in foam nickel surface, then by presoma sulphur
Metaplasia obtains the super capacitor material based on nickel foam self-supporting MnS nanometer sheets at MnS nanometer sheets.
2. the preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials as described in claim 1, feature exist
In being as follows：
(1) it cleans 1~3h of nickel foam with deionized water and EtOH Sonicate to be pre-processed, removes its surface impurity；
(2) in deionized water by the dissolving of manganese source, urea and ammonium fluoride, it is sufficiently stirred to obtain mixed reaction solution, it later will be pre-
Treated, and nickel foam is put into reaction kettle, and mixed reaction solution is added, and 1~5h of hydro-thermal reaction is carried out at 100~200 DEG C, is waited for
After reaction is completed and is cleaned and dried, then 1~4h is reacted at 200~500 DEG C through high-temperature calcination and obtain MnS nanometer sheet presomas；
(3) the MnS nanometer sheet presomas after calcining are positioned in reaction kettle and are added sulphur source, vulcanize at 100~200 DEG C anti-
It answers 1~8h, is cleaned after cooling and obtain the MnS nanometer sheets grown in foam nickel surface, i.e., the described MnS based on nickel foam self-supporting
The super capacitor material of nanometer sheet.
3. the preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials as claimed in claim 2, feature exist
In in step 2), the addition of manganese source is 0.1~0.2molL-1, the addition of urea is 0.1~0.2molL-1, fluorination
The addition of ammonium is 0.01~0.1molL-1。
4. the preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials as claimed in claim 3, feature exist
In manganese source, the molar ratio of urea ammonium fluoride are 3:3:1.
5. the preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials as claimed in claim 2, feature exist
In in step 2), manganese source is manganese salt substance：Manganese sulfate, manganese nitrate, manganese acetate or manganese chloride.
6. the preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials as claimed in claim 2, feature exist
In in step 3), sulphur source is the solution of vulcanized sodium, thiocarbamide or sulphur powder, a concentration of 0.1~0.3molL-1。
7. the preparation method of the nickel foam self-supporting MnS nanometer sheet super capacitor materials as described in one of claim 1 to 6,
It is characterized in that, the mass density for growing MnS nanometer sheets in foam nickel surface is 0.5~1.5mgcm-2。
8. the preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials as claimed in claim 7, feature exist
In a diameter of 1.0~2.0 μm of MnS nanometer sheets, thickness is 0.2~0.5 μm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810610394.0A CN108538622A (en) | 2018-06-14 | 2018-06-14 | The preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110211812A (en) * | 2019-06-14 | 2019-09-06 | 上海应用技术大学 | A kind of MnS@CoMn-LDH composite material and preparation method and application |
| CN111268734A (en) * | 2020-02-13 | 2020-06-12 | 广州大学 | Transition metal sulfide nanosheet and preparation method and application thereof |
Citations (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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