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 PDF

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Publication number
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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CN
China
Prior art keywords
nickel foam
supporting
mns
super capacitor
nanometer sheet
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CN201810610394.0A
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Chinese (zh)
Inventor
吴春
贾传坤
丁美
楼雪纯
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长沙理工大学
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Priority to CN201810610394.0A priority Critical patent/CN108538622A/en
Publication of CN108538622A publication Critical patent/CN108538622A/en

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    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors [EDLCs]; Processes specially adapted for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/30Electrodes characterised by their materials
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors [EDLCs]; Processes specially adapted for the manufacture thereof or of parts thereof
    • H01G11/22Electrodes
    • H01G11/24Electrodes characterised by structural features, e.g. forms, shapes, surface areas, porosities or dimensions, of the materials making up or comprised in the electrodes; characterised by the structural features of powders or particles used therefor
    • HELECTRICITY
    • H01BASIC ELECTRIC ELEMENTS
    • H01GCAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors [EDLCs]; Processes specially adapted for the manufacture thereof or of parts thereof
    • H01G11/84Processes for the manufacture of hybrid or EDL capacitors, or components thereof
    • H01G11/86Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02EREDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/13Energy storage using capacitors

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

The preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials

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.
CN201810610394.0A 2018-06-14 2018-06-14 The preparation method of nickel foam self-supporting MnS nanometer sheet super capacitor materials CN108538622A (en)

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Application publication date: 20180914