CN110079846A - Nickelous selenide with different-shape/nickel base electrode material electro-deposition preparation method - Google Patents
Nickelous selenide with different-shape/nickel base electrode material electro-deposition preparation method Download PDFInfo
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- CN110079846A CN110079846A CN201910414230.5A CN201910414230A CN110079846A CN 110079846 A CN110079846 A CN 110079846A CN 201910414230 A CN201910414230 A CN 201910414230A CN 110079846 A CN110079846 A CN 110079846A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D5/00—Electroplating characterised by the process; Pretreatment or after-treatment of workpieces
- C25D5/34—Pretreatment of metallic surfaces to be electroplated
- C25D5/38—Pretreatment of metallic surfaces to be electroplated of refractory metals or nickel
- C25D5/40—Nickel; Chromium
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25D—PROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
- C25D9/00—Electrolytic coating other than with metals
- C25D9/04—Electrolytic coating other than with metals with inorganic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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 OR LIGHT-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
Abstract
A kind of high-performance nickelous selenide/nickel-based super capacitor electrode material preparation method with different-shape, (1) foam nickel base working electrode is cleaned with dilute hydrochloric acid, it is respectively for several times with dehydrated alcohol, deionized water ultrasonic cleaning, spare after drying to remove the oxide impurity on surface；(2) a step electro-deposition method is used, using electro-deposition techniques, grows selenizing nickel electrode in nickel foam surface in situ.Avoid the harsh conditions such as high temperature, high pressure, the strong reductant in the other synthesis technologies of nickelous selenide.The method of the present invention simple process, it is easy to operate, it is at low cost, resulting nickelous selenide/nickel electrode electrochemical performance is prepared, is a kind of potential electrode material for super capacitor.
Description
Technical field
The invention belongs to electrode material for super capacitor preparation technical fields, are related to nickelous selenide/nickel base electrode material, specifically
It is related to a kind of electro-deposition preparation method of the nickelous selenide with different-shape/nickel base electrode material.
Background technique
Currently, society increases the consumption of the energy year by year.Conventional fossil fuel is faced with that reserves are limited, endanger environment etc. one
Series of problems.Therefore, exploitation green energy resource is extremely urgent.However, energy conversion efficiency existing for these new energy it is low, by external
Condition influences that big, production capacity is uncontrollable, the problems such as being unevenly distributed limits the universal and application of new energy.In order to solve new energy
There is currently the problem of, the preparation method that we will pay attention to energy storage and conversion equipment is innovated.Supercapacitor is as the energy
A member of storage and conversion art has been used for new energy hair because its charge/discharge is rapid, active time is long, advantages of environment protection
The fields such as electricity, distributed energy storage, new-energy automobile.Research and development supercapacitor critical material and technology are classified as " country by China
Medium-term and long-term scientific and technological development planning outline (2006-2020) " and " national " 11th Five-Year " scientific and technical development program " weight
One of the direction of point development.
Electrode material performance plays critical impact to the energy-storage property of supercapacitor, thus, design green, efficiently,
Cheap electrode material is the research emphasis of current super capacitor system.Transition metal nickelous selenide, because of its higher theoretical ratio
Capacitor, cost performance be high and the favor by researchers.But the electricity of the Ni-based transistion metal compound of selenizing reported at present
Chemical property and its theoretical electrochemistry performance still have larger gap.Since the chemical property of conventional bulk electrode material is limited to
The limited electrochemical reaction active site of crystal itself, therefore designing, there is abundant electro-chemical activity site to improve electrode material
Intrinsic electro-chemical activity be research key points and difficulties.Currently, most electrode material preparation process are complicated, it is unfavorable for material
The large-scale application of material.
Summary of the invention
In order to overcome the above-mentioned deficiencies of the prior art, the object of the present invention is to provide a kind of selenizings with different-shape
Nickel/nickel base electrode material electro-deposition preparation method, the foam nickel base for working electrode are pre-processed to remove surface
Impurity, clean surface.By applying the effect of external electric field in the solution containing nickel ion and plasma selenium, it is dynamic to change chemical reaction
Mechanics realizes the growth in situ nickelous selenide in nickel foam, obtains nickelous selenide/nickel base electrode material.It can be by controlling in solution not
Nickelous selenide/nickel electrode pattern is controlled with the mass ratio of metal ion, and then regulates and controls the chemical property of the electrode material.Its
Simple process, cost is relatively low, functional.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of electro-deposition preparation method of the nickelous selenide with different-shape/nickel-based super capacitor electrode material, including it is following
Step:
1) nickel foam of the cm of diameter d=0.4 is impregnated into 5 ~ 20min in the dilute hydrochloric acid solution of 4 mol/L of concentration, ultrasound 5 ~
10min is cleaned several times respectively with dehydrated alcohol, deionized water after taking-up, is weighed after drying；
2) nickel acetate, selenium dioxide, the lithium chloride matched using Ni/Se=13/7 is electrolysed Compound mixed solution electric depositing solution；
3) the cleaned processed nickel foam of step 1) is used as working electrode, saturated calomel electrode is as reference electrode, platinized platinum
Nickelous selenide/nickel electrode material is prepared using constant potential electro-deposition techniques for electrode, be put into step 2 preparation, voltage is-
0.45 V vs. SCE, electrodeposition time 300-2400 s, obtaining pattern is that nano-pillar, nano particle, micron are octahedra) selenium
Change nickel/nickel base electrode material；
4) after electro-deposition, nickelous selenide/nickel base electrode material obtained by deionized water, washes of absolute alcohol is used respectively, after drying
It weighs, calculates the weight of prepared nickelous selenide/nickel base electrode material.
The parameters adjusting of nickel acetate, selenium dioxide, lithium chloride in the step 2) are as follows: 0.065 M nickel acetate, 0.035
M selenium dioxide, 0.2 M lithium chloride.
The electrodeposition time that the electrodeposition process parameter is respectively as follows: constant potential electro-deposition be divided into 300 s, 1200 s,
2400 s, are respectively designated as NS-1, NS-2, NS-3.
Any strong reductant or surfactant are not added in the deposition process, it is subsequent without subsequent calcination
Etc. heat treatment process.
The beneficial effects of the present invention are:
1) nickelous selenide/nickel nano material is prepared by electro-deposition method, preparation process is simple, products therefrom purity is higher.
2) this method is avoided using the noxious material in the customary preparation methods such as hydrazine hydrate, sodium borohydride or reduction by force
Agent requires Preparation equipment lower.
3) present invention can get nickelous selenide/nickel base electrode material with excellent electrochemical performance.
4) this project is dedicated to synthesizing component, the Ni-based nano-electrode of the selenizing of morphology controllable by simple, efficient method
Material, and ultracapacitor device is prepared based on these different components and the nanostructure of morphology controllable.
Detailed description of the invention
Fig. 1 is nickelous selenide prepared by the present invention/nickel base electrode material XRD diagram.
Fig. 2 is nickelous selenide prepared by the present invention/nickel base electrode material SEM figure.
Fig. 3 is nickelous selenide prepared by the present invention/nickel base electrode material cyclic voltammetry curve.
Fig. 4 is nickelous selenide prepared by the present invention/nickel base electrode material constant current charge-discharge curve.
Fig. 5 is nickelous selenide prepared by the present invention/nickel base electrode material impedance curve.
Specific embodiment
Nickelous selenide of the present invention/nickel base electrode material preparation method is done into one below with reference to specific embodiment
Step explanation, but the scope of protection of the present invention is not limited thereto.
Embodiment 1
(1) nickel foam (cm of d=0.4) is impregnated into 5 ~ 20min, 5 ~ 10min of ultrasound in dilute hydrochloric acid (4 mol/L).Divide after taking-up
It is not cleaned several times with dehydrated alcohol, deionized water, is weighed after drying.
(2) electric depositing solution: 0.065 M nickel acetate, 0.035 M selenium dioxide, 0.2 M lithium chloride is configured.
(3) nickel foam of cleaned processing is used as working electrode, prepares nickelous selenide/nickel using constant potential electro-deposition techniques
Base electrode material.Voltage is -0.45 V vs. SCE, and 300 s of electro-deposition obtains the Ni with nano-pillar pattern0.85Se/Ni electricity
Pole.
(4) after electro-deposition, respectively with deionized water, washes of absolute alcohol gained Ni0.85Se/Ni electrode material dries
It is weighed after dry.
Through detecting, the Ni0.85Specific capacitance of the Se/Ni electrode material in 2 M KOH solutions is that 896F/g(current density is
10 A/g).
Embodiment 2
(1) nickel foam (cm of d=0.4) is impregnated into 5 ~ 20min, 5 ~ 10min of ultrasound in dilute hydrochloric acid (4 mol/L).Divide after taking-up
It is not cleaned several times with dehydrated alcohol, deionized water, is weighed after drying.
(2) electric depositing solution: 0.065 M nickel acetate, 0.035 M selenium dioxide, 0.2 M lithium chloride is configured.
(3) nickel foam of cleaned processing is used as working electrode, prepares nickelous selenide/nickel using constant potential electro-deposition techniques
Base electrode material.Voltage is -0.45 V vs. SCE, and 1200 s of electro-deposition obtains the Ni with nano particle pattern0.85Se/
Ni electrode.
(4) after electro-deposition, respectively with deionized water, washes of absolute alcohol gained Ni0.85Se/Ni electrode material dries
It is weighed after dry.
Through detecting, the Ni0.85Specific capacitance of the Se/Ni electrode material in 2 M KOH solutions is 1126 F/g(current densities
For 10 A/g).
Embodiment 3
(1) nickel foam (cm of d=0.4) is impregnated into 5 ~ 20min, 5 ~ 10min of ultrasound in dilute hydrochloric acid (4 mol/L).Divide after taking-up
It is not cleaned several times with dehydrated alcohol, deionized water, is weighed after drying.
(2) electric depositing solution: 0.065 M nickel acetate, 0.035 M selenium dioxide, 0.2 M lithium chloride is configured.
(3) nickel foam of cleaned processing is used as working electrode, prepares nickelous selenide/nickel using constant potential electro-deposition techniques
Electrode material.Voltage is -0.45 V vs. SCE, and 2400 s of electro-deposition obtains the Ni with micron shape of octahedron0.85Se/
Ni electrode.
(4) after electro-deposition, respectively with deionized water, washes of absolute alcohol gained Ni0.85Se/Ni electrode material dries
It is weighed after dry.
Through detecting, the Ni0.85Specific capacitance of the Se/Ni electrode material in 2 M KOH solutions is 1231F/g(current density
For 10 A/g).
Fig. 1 is prepared nickelous selenide/nickel base electrode material X-ray diffractometer map (XRD).It can by XRD analysis
Know, material prepared by the present invention is hexagonal crystal system nickelous selenide (Ni0.85Se, JCPDF 018-0888) and nickel foam composite wood
Material.
Fig. 2 is nickelous selenide prepared by the present invention/nickel base electrode material SEM figure.As shown in Figure 2, prepared by the present invention
Ni0.85Se/Ni electrode material is respectively provided with nano-pillar, nano particle, micron shape of octahedron.With the tune of electrodeposition time
Control, Ni0.85Se/Ni has different patterns.
Two, Ni0.85Se/Ni electrode material for super capacitor electrochemical Characterization
Fig. 3 is Ni of the invention0.85The cyclic voltammetry curve of Se/Ni electrode material.From the figure 3, it may be seen that in the voltage window of 0 ~ 0.45V
Under mouthful, the Ni with different-shape0.85There are symmetrical redox peaks in Se/Ni electrode material, shows that the material surface can
Typical fake capacitance reaction occurs.
Fig. 4 is Ni of the invention0.85The constant current charge-discharge of Se/Ni electrode material.Ni with different-shape0.85Se/Ni
There is symmetrical charging and discharging curve in electrode material.
Fig. 5 is Ni of the invention0.85The impedance diagram of Se/Ni electrode material.As shown in Figure 5, with different-shape
Ni0.85Se/Ni electrode material has lesser internal resistance, is conducive to the progress of electrochemical reaction.
In conclusion the present invention passes through simple process, easy to operate constant potential electro-deposition techniques, the Ni of preparation0.85Se/
Ni electrode material has the different-shapes such as nano-pillar, nano particle, micron octahedron, and specific capacitance is high, and resistance is small, is a kind of property
The excellent super capacitor material of energy.
Claims (4)
1. a kind of electro-deposition preparation method of the nickelous selenide with different-shape/nickel-based super capacitor electrode material, feature
It is, comprising the following steps:
1) nickel foam of the cm of diameter d=0.4 is impregnated into 5 ~ 20min in the dilute hydrochloric acid solution of 4 mol/L of concentration, ultrasound 5 ~
10min is cleaned several times respectively with dehydrated alcohol, deionized water after taking-up, is weighed after drying；
2) nickel acetate, selenium dioxide, the lithium chloride matched using Ni/Se=13/7 is electrolysed Compound mixed solution electric depositing solution；
3) the cleaned processed nickel foam of step 1) is used as working electrode, saturated calomel electrode is as reference electrode, platinized platinum
Nickelous selenide/nickel electrode material is prepared using constant potential electro-deposition techniques for electrode, be put into step 2 preparation, voltage is-
0.45 V vs. SCE, electrodeposition time 300-2400 s, obtaining pattern is that nano-pillar, nano particle, micron are octahedra) selenium
Change nickel/nickel base electrode material；
4) after electro-deposition, nickelous selenide/nickel base electrode material obtained by deionized water, washes of absolute alcohol is used respectively, after drying
It weighs, calculates the weight of prepared nickelous selenide/nickel base electrode material.
2. a kind of electro-deposition preparation side of the nickelous selenide with different-shape/nickel base electrode material according to claim 1
Method, which is characterized in that the parameters adjusting of nickel acetate, selenium dioxide, lithium chloride in the step 2) are as follows: 0.065 M nickel acetate,
0.035 M selenium dioxide, 0.2 M lithium chloride.
3. a kind of electro-deposition preparation side of the nickelous selenide with different-shape/nickel base electrode material according to claim 1
Method, which is characterized in that the electrodeposition time that the electrodeposition process parameter is respectively as follows: constant potential electro-deposition be divided into 300 s,
1200 s, 2400 s, are respectively designated as NS-1, NS-2, NS-3.
4. a kind of electro-deposition preparation side of the nickelous selenide with different-shape/nickel base electrode material according to claim 1
Method, which is characterized in that any strong reductant or surfactant are not added in the deposition process, it is subsequent without rear
The heat treatment process such as continuous calcining.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910414230.5A CN110079846A (en) | 2019-05-17 | 2019-05-17 | Nickelous selenide with different-shape/nickel base electrode material electro-deposition preparation method |
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| CN201910414230.5A CN110079846A (en) | 2019-05-17 | 2019-05-17 | Nickelous selenide with different-shape/nickel base electrode material electro-deposition preparation method |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113066675A (en) * | 2021-03-26 | 2021-07-02 | 电子科技大学 | Super capacitor electrode material and preparation method thereof |
| CN114420469A (en) * | 2022-02-09 | 2022-04-29 | 陕西科技大学 | 3D flower-shaped nickel zinc selenide flexible composite electrode material and preparation method and application thereof |
| CN115072673A (en) * | 2022-06-14 | 2022-09-20 | 蚌埠学院 | Preparation method and application of nickel selenide nano material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113066675A (en) * | 2021-03-26 | 2021-07-02 | 电子科技大学 | Super capacitor electrode material and preparation method thereof |
| CN114420469A (en) * | 2022-02-09 | 2022-04-29 | 陕西科技大学 | 3D flower-shaped nickel zinc selenide flexible composite electrode material and preparation method and application thereof |
| CN114420469B (en) * | 2022-02-09 | 2024-04-05 | 陕西科技大学 | 3D flower-shaped nickel zinc selenide flexible composite electrode material and preparation method and application thereof |
| CN115072673A (en) * | 2022-06-14 | 2022-09-20 | 蚌埠学院 | Preparation method and application of nickel selenide nano material |
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