CN108796551A - It is supported on sea urchin shape vulcanization Co catalysts in nickel foam and preparation method thereof, as the application of electrolysis water oxygen-separating catalyst - Google Patents
It is supported on sea urchin shape vulcanization Co catalysts in nickel foam and preparation method thereof, as the application of electrolysis water oxygen-separating catalyst Download PDFInfo
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- CN108796551A CN108796551A CN201810564204.6A CN201810564204A CN108796551A CN 108796551 A CN108796551 A CN 108796551A CN 201810564204 A CN201810564204 A CN 201810564204A CN 108796551 A CN108796551 A CN 108796551A
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/04—Electrodes; Manufacture thereof not otherwise provided for characterised by the material
- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/073—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material
- C25B11/075—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of a single catalytic element or catalytic compound
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B1/00—Electrolytic production of inorganic compounds or non-metals
- C25B1/01—Products
- C25B1/02—Hydrogen or oxygen
- C25B1/04—Hydrogen or oxygen by electrolysis of water
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- C—CHEMISTRY; METALLURGY
- C25—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
- C25B11/02—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form
- C25B11/03—Electrodes; Manufacture thereof not otherwise provided for characterised by shape or form perforated or foraminous
- C25B11/031—Porous electrodes
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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
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
Abstract
The present invention relates to a kind of sea urchin shape cobalt sulfide being supported in nickel foam and preparation method thereof, as the application of electrolysis water oxygen-separating catalyst.Wherein preparation method includes the following steps：（1）Nickel foam is positioned over and is cleaned by ultrasonic the greasy dirt for removing its surface in organic washing agent, then nickel foam is placed in ultrasonic cleaning nickel foam surface impurity in dilute acid soln；（2）By cobalt nitrate, thioacetamide is dissolved in the mixed solvent, and stirring obtains Catalyst precursor solutions to dissolving；（3）Catalyst precursor solutions are transferred in the reaction kettle for being placed with processing nickel foam, after hydro-thermal reaction, obtain being supported on the sea urchin shape cobalt sulfide in nickel foam.The catalysis analysis oxygen of sea urchin shape vulcanization Co catalysts is had excellent performance, and can be applied to catalytic electrolysis water electrode material, and the catalyst preparation is at low cost, operating procedure is simple, and catalytic stability is good.
Description
Technical field
The invention belongs to field of nanometer material technology, and in particular to a kind of sea urchin shape cobalt sulfide being supported in nickel foam and its system
Preparation Method, as the application of electrolysis water oxygen-separating catalyst.
Background technology
The fossil energies such as coal, oil, natural gas support the progress of modern times human civilization and the development of economic society.
However, due to huge consumption of the non-renewable and mankind to fossil energy of fossil energy, fossil energy faces exhausted danger
Machine and along with serious environmental problem.Energy resource structure based on fossil energy has apparent unsustainable property.Have
The fossil energy storage of limit forces the mankind to seek renewable and environmentally friendly new energy.Turn of extensive intermittent energy at present
Change, storage is with using being required for high-efficiency cleaning method to solve, and to be then problem above provide one kind to water electrolysis hydrogen production feasible has
The solution of effect, but in water electrolysis hydrogen production, excessively high oxygen overpotential on anode needs to consume higher electric energy so that energy
Transformation efficiency is low.Precious metal anode has both good activity and stability, but because of valence as electrolysis elutriation oxygen catalytic electrode material
Lattice are expensive and rare, are unfavorable for mass production.Traditional electrolyzed alkaline water anode catalyst base metal cobalt compound performance is excellent
Good catalytic activity and cheap, has obtained extensive research.
Invention content
The technical problem to be solved by the present invention is to provide one kind in view of the deficiency of the prior art and be supported on
Sea urchin shape cobalt sulfide in nickel foam and preparation method thereof, as the application of electrolysis water oxygen-separating catalyst, using nickel foam as substrate
Sea urchin shape cobalt sulfide uniform load is exposed more active surfaces by skeleton by hydro-thermal reaction in foam nickel surface, in
The reduction of resistance improves the electric conductivity of catalyst, is integrally improved the catalytic performance of base metal cobalt compound.
The present invention be solve the problems, such as it is set forth above used by technical solution be：
A kind of preparation method for the sea urchin shape cobalt sulfide being supported in nickel foam, mainly includes the following steps that：
(1) pretreatment of carrier foam nickel：Nickel foam is sliced and is cleaned up；
(2) preparation of Catalyst precursor solutions：Cobalt nitrate and thioacetamide are dissolved in solvent, stirring to dissolving,
Obtain Catalyst precursor solutions；
(3) it is supported on the preparation of the sea urchin shape vulcanization Co catalysts in nickel foam：Catalyst precursor solutions are transferred to and are put
In the reaction kettle for having carrier foam nickel, after hydro-thermal reaction, obtain being supported on the sea urchin shape vulcanization Co catalysts in nickel foam；
By said program, the pretreatment of step (1) carrier foam nickel is specially：Nickel foam is sliced, organic washing is placed in
It is cleaned by ultrasonic in agent and removes its surface and oil contaminant, then nickel foam is placed in dilute acid soln and is cleaned by ultrasonic its surface impurity.Wherein, institute
It is preferably acetone or absolute ethyl alcohol etc. to state organic washing agent, and the time of ultrasonic cleaning is preferably 5-15min；The dilute acid soln
Preferred concentration is 2-4molL-1, such as dilute hydrochloric acid, the time of ultrasonic cleaning is preferably 5-15min.
By said program, the cobalt nitrate is cabaltous nitrate hexahydrate, the mass ratio of cabaltous nitrate hexahydrate and thioacetamide
It is 1:3 to 3:1, preferred mass ratio is 3:2.
By said program, step (2) described solvent is water, alcohol or mixed solvent.Wherein, mixed solvent is preferably by distilling
Water and alcohol miscible with water mix in any proportion；It is further preferred that the in the mixed solvent distilled water, miscible with water
Alcohol volume ratio most preferably 1:1.
By said program, the hydrothermal reaction condition described in step (3) is 120-180 DEG C of reaction temperature, reaction time 2-6h；
Most preferably 150 DEG C of reaction temperature, reaction time 4h.
The sea urchin shape cobalt sulfide being supported on obtained by above-mentioned preparation method in nickel foam, wherein sea urchin shape cobalt sulfide uniform load
On foam nickel skeleton, and the mean radius of sea urchin sphere is 2-4 μm or so, sea urchin shape sphere include it is many from center to
The nano wire of outgrowth.
Another object of the present invention is to provide the sea urchin shape cobalt sulfides being supported in nickel foam to urge as electrolysis elutriation oxygen
The application of agent can be applied to the electrode materials such as lithium battery, electrolysis aquatic products hydrogen catalysis electrode material, ultracapacitor.
Compared with prior art, the beneficial effects of the invention are as follows：
First, the present invention is being steeped sea urchin shape cobalt sulfide uniform load by hydro-thermal reaction using nickel foam as substrate skeleton
Foam nickel surface, the sea urchin shape cobalt sulfide being supported in nickel foam are catalyzed compared to the cobalt sulfide that other two-step hydrothermal route methods synthesize
Agent synthesizes large specific surface area, exposes more active surfaces, the reduction of internal resistance improves the electric conductivity of catalyst, whole
Body improves the catalytic performance of base metal cobalt compound.
Second, application of the present invention using the sea urchin shape cobalt sulfide that is supported in nickel foam as electrolysis water oxygen-separating catalyst,
Polymerization catalyst will not occur in catalytic reaction process, it is inexpensive and efficient, stable；And sea urchin shape vulcanization Co catalysts are direct
It is supported in nickel foam, not easily to fall off, as catalyst in reaction, the not presence of adhesive can expose more activity
Surface, while internal resistance is reduced, transfering dynamics and stable in catalytic performance are promoted, catalysis analysis oxygen is had excellent performance.
Third, the preparation method of the sea urchin shape cobalt sulfide of the present invention being supported in nickel foam, at low cost, preparation process
Simply.
Description of the drawings
Fig. 1 is the XRD diagram for the sea urchin shape cobalt sulfide being supported in embodiment 1 in nickel foam；
Fig. 2 (a), Fig. 2 (b) are the scanning electron microscope for the sea urchin shape cobalt sulfide being supported in embodiment 1 in nickel foam
Figure；
Fig. 3 is embodiment 1, be supported in embodiment 3 and embodiment 4 the sea urchin shape cobalt sulfide in nickel foam in 1.0mol
L-1Linear sweep voltammetry curve graph under KaOH electrolyte；
Fig. 4 is the time current curve for the sea urchin shape cobalt sulfide being supported in embodiment 1 in nickel foam, the constant electricity of test
Pressure is 1.55V.
Specific implementation mode
With reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.It should be noted that the combination of the technical characteristic or technical characteristic described in following embodiments is not construed as
Isolated, they can be combined with each other to reach superior technique effect.
Embodiment 1
A kind of preparation method for the sea urchin shape cobalt sulfide being supported in nickel foam, including following steps：
(1) nickel foam is sliced into 3cm × 3cm sizes, is positioned over the ultrasonic cleaning of 40ml absolute ethyl alcohols and removes its surface oil
Then nickel foam is placed in 3molL by dirt-1Hydrochloric acid solution is cleaned by ultrasonic surface impurity；
(2) 0.3g cabaltous nitrate hexahydrates and 0.2g thioacetamides are dissolved in 20mL distilled water and 20mL absolute ethyl alcohols respectively
In the mixed solvent, stirring obtain the Catalyst precursor solutions of pink in 15 minutes to dissolving；
(3) Catalyst precursor solutions are transferred in 100mL polytetrafluoroethyllining lining reaction kettles, are placed in simultaneous reactions kettle
The a piece of nickel foam after step (1) processing, hydro-thermal reaction 4h is then carried out under the conditions of 150 DEG C, is cooled to room temperature, sample is taken out
Product are washed 6 times with water and ethyl alcohol, obtain being supported on the sea urchin shape cobalt sulfide in nickel foam after 60 DEG C of dryings.
Morphology characterization and performance test：The present invention is supported on obtained by embodiment in nickel foam using MSAL-XD2 to characterize
The crystal structure of sea urchin shape cobalt sulfide, the results are shown in Figure 1, in 2 θ=29.7 °, 31.1 °, and 39.5 °, 47.6 °, 54.6 ° of difference
Corresponding to (311) of cobalt sulfide, (222), (331), (511), (531) (JCPDS No.02-1459) diffraction crystal face；In addition, 2 θ
=44.5 °, 51.8 °, 76.4 ° of (111) for corresponding respectively to base foam nickel, (200), (220) (JCPDS No.65-2865)
Diffraction crystal face, it was demonstrated that its cobalt sulfide is successfully supported in nickel foam.
The present invention is vulcanized using SEM-XL30S scanning electron microscope to characterize the sea urchin shape being supported on obtained by embodiment in nickel foam
Cobalt surrounds and watches pattern, as shown in Fig. 2, sea urchin shape cobalt sulfide uniform load is can be seen that on foam nickel skeleton from Fig. 2 (a), and
The mean radius of sea urchin sphere is 3 μm or so；Sea urchin shape sphere includes many receiving from center to outgrowth in Fig. 2 (b)
Rice noodles may provide many active sites for catalysis reaction.
Embodiment 1, embodiment 3,4 gained of embodiment are supported on sea urchin shape cobalt sulfide sample and ruthenium-oxide in nickel foam
It is supported in nickel foam respectively as working electrode, carbon-point is auxiliary electrode, Hg/Hg2Cl2It is first with 1.0mol for reference electrode
L-1KOH is electrolyte, and composition three-electrode system carries out electrochemical property test on occasion China CHI66D electrochemical workstations.Linearly
Scanning curve figure is as shown in Figure 3, it can be seen that the catalysis analysis oxygen performance of embodiment 1 is promoted rapidly with the increase of voltage, wherein in fact
The sea urchin shape cobalt sulfide being supported in example 1 in nickel foam is applied compared to embodiment 3, embodiment 4 and Precious metal oxidation ruthenium in larger electricity
Catalysis analysis oxygen performance under current density is best, and current density is reached for 200mA/cm2When, corresponding voltage value is minimum, is 1.74V.
The sea urchin shape cobalt sulfide sample that 1 gained of embodiment is supported in nickel foam is persistently catalyzed oxygen and stability test knot is precipitated
Fruit as shown in figure 4, to the sea urchin shape cobalt sulfide that is supported in nickel foam after lasting catalysis oxygen is precipitated 14 hours, protect by current density
It is fixed to keep steady, and shows that it has good durability, can be applied to Industrial Catalysis electrolysis water material.
Embodiment 2
The present embodiment difference from Example 1 is：Organic washing agent described in step (1) is acetone, other
Part is same as Example 1.
Embodiment 3
The present embodiment difference from Example 1 is：Solvent described in step (2) be distilled water, other conditions with
Embodiment 1 is identical.
Embodiment 4
The present embodiment difference from Example 1 is：Solvent described in step (2) is absolute ethyl alcohol, and other conditions are equal
It is same as Example 1.
Embodiment 5
The present embodiment difference from Example 1 is：, the mass ratio 1 of cabaltous nitrate hexahydrate and thioacetamide:3；Water
Thermal rection condition is 140 DEG C of reaction temperature, reaction time 6h；Be supported on the sea urchin shape cobalt sulfide in nickel foam in 1.0mol
L-1Linear sweep voltammetry curve under KaOH electrolyte, current density are reached for 100mA/cm2When, corresponding voltage value is 1.72V,
Other conditions are same as Example 1.
Embodiment 6
The present embodiment difference from Example 1 is：The mass ratio 3 of cabaltous nitrate hexahydrate and thioacetamide:1；Water
Thermal rection condition is 160 DEG C of reaction temperature, reaction time 3h；Be supported on the sea urchin shape cobalt sulfide in nickel foam in 1.0mol
L-1Linear sweep voltammetry curve under KaOH electrolyte, current density are reached for 100mA/cm2When, corresponding voltage value is 1.71V；
Other conditions are same as Example 1.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from the spirit and principles of the present invention made by changes, modifications, substitutions, combinations, simplifications,
Equivalent substitute mode is should be, is included within the scope of the present invention.
Claims (10)
1. a kind of preparation method for the sea urchin shape cobalt sulfide being supported in nickel foam, it is characterised in that mainly include the following steps that：
（1）The pretreatment of carrier foam nickel：Nickel foam is sliced and is cleaned up；
（2）The preparation of Catalyst precursor solutions：Cobalt nitrate and thioacetamide are dissolved in solvent, stirring is obtained to dissolving
Catalyst precursor solutions；
（3）It is supported on the preparation of the sea urchin shape vulcanization Co catalysts in nickel foam：Catalyst precursor solutions are transferred to and are placed with load
In the reaction kettle of body nickel foam, after hydro-thermal reaction, obtain being supported on the sea urchin shape vulcanization Co catalysts in nickel foam.
2. a kind of preparation method of sea urchin shape cobalt sulfide being supported in nickel foam according to claim 1, feature exist
It is cabaltous nitrate hexahydrate in the cobalt nitrate, the mass ratio of cabaltous nitrate hexahydrate and thioacetamide is 1:3 to 3:1.
3. a kind of preparation method of sea urchin shape cobalt sulfide being supported in nickel foam according to claim 1, feature exist
In step（3）The hydrothermal reaction condition is 120-180 DEG C of reaction temperature, reaction time 2-6h.
4. a kind of preparation method of sea urchin shape cobalt sulfide being supported in nickel foam according to claim 3, feature exist
In step（3）The hydrothermal reaction condition is 150 DEG C of reaction temperature, 4 h of reaction time.
5. a kind of preparation method of sea urchin shape cobalt sulfide being supported in nickel foam according to claim 1, feature exist
In step（2）The solvent is water, alcohol or mixed solvent.
6. a kind of preparation method of sea urchin shape cobalt sulfide being supported in nickel foam according to claim 5, feature exist
It is mixed in any proportion by distilled water and alcohol miscible with water in the mixed solvent.
7. a kind of preparation method of sea urchin shape cobalt sulfide being supported in nickel foam according to claim 1, feature exist
In step（1）The pretreatment of carrier foam nickel is specially：Nickel foam is sliced, ultrasonic cleaning in organic washing agent is placed in and removes it
Surface and oil contaminant, then nickel foam is placed in dilute acid soln and is cleaned by ultrasonic its surface impurity.
8. a kind of preparation method of sea urchin shape cobalt sulfide being supported in nickel foam according to claim 7, feature exist
It is acetone or absolute ethyl alcohol in the organic washing agent, the time of ultrasonic cleaning is 5-15min；The dilute acid soln is a concentration of
2-4mol·L-1, the time of ultrasonic cleaning is 5-15min.
9. the sea urchin shape cobalt sulfide being supported in nickel foam prepared by any one of claim 1-8 the methods, feature exist
It it is 2-4 μm in the mean radius of the sea urchin sphere of sea urchin shape cobalt sulfide, sea urchin shape sphere includes that several are outside from center
The nano wire of growth.
10. the sea urchin shape cobalt sulfide being supported in nickel foam described in claim 9 is in catalytic electrolysis elutriation Oxygen Electrode Material, lithium
Application in terms of battery electrode material, electrode material for super capacitor.
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| CN201810564204.6A CN108796551B (en) | 2018-06-04 | 2018-06-04 | Sea urchin-shaped cobalt sulfide catalyst loaded on foamed nickel, preparation method thereof and application of catalyst as electrolyzed water oxygen evolution catalyst |
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| CN201810564204.6A CN108796551B (en) | 2018-06-04 | 2018-06-04 | Sea urchin-shaped cobalt sulfide catalyst loaded on foamed nickel, preparation method thereof and application of catalyst as electrolyzed water oxygen evolution catalyst |
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Cited By (9)
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| CN109518207A (en) * | 2018-12-20 | 2019-03-26 | 华中科技大学 | A kind of efficient oxygen evolution reaction elctro-catalyst and preparation method thereof |
| CN109847778A (en) * | 2019-01-04 | 2019-06-07 | 华中师范大学 | A kind of cobalt disulfide for being electrolysed elutriation oxygen/carbon nitrogen composite material and its synthetic method |
| CN110404564A (en) * | 2019-08-16 | 2019-11-05 | 澳门大学 | A kind of difunctional complete solution water power catalyst and the preparation method and application thereof |
| CN111408362A (en) * | 2020-03-23 | 2020-07-14 | 山东鲁北国际新材料研究院有限公司 | Sea urchin-shaped cobalt sulfide-charcoal composite material and preparation method and application thereof |
| CN111686773A (en) * | 2020-07-14 | 2020-09-22 | 南京林业大学 | Sea urchin-like nickel-iron phosphonate photocatalyst and preparation method thereof |
| CN112962115A (en) * | 2021-02-09 | 2021-06-15 | 上海交通大学 | Foamed nickel loaded sulfide electrocatalyst and preparation method and application thereof |
| CN114360919A (en) * | 2021-11-22 | 2022-04-15 | 沈阳工程学院 | Preparation method of high-performance electrode material with nano sea urchin structure |
| CN114990622A (en) * | 2022-06-02 | 2022-09-02 | 蚌埠学院 | Preparation method of sea urchin-shaped iron-doped nickel hydroxide oxygen evolution catalyst |
| CN115786964A (en) * | 2023-02-06 | 2023-03-14 | 北京化工大学 | Cobalt-based spinel Cu 0.7 Co 2.3 O 4 Electrocatalyst and preparation method and application thereof |
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Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109518207A (en) * | 2018-12-20 | 2019-03-26 | 华中科技大学 | A kind of efficient oxygen evolution reaction elctro-catalyst and preparation method thereof |
| CN109847778A (en) * | 2019-01-04 | 2019-06-07 | 华中师范大学 | A kind of cobalt disulfide for being electrolysed elutriation oxygen/carbon nitrogen composite material and its synthetic method |
| CN110404564A (en) * | 2019-08-16 | 2019-11-05 | 澳门大学 | A kind of difunctional complete solution water power catalyst and the preparation method and application thereof |
| CN110404564B (en) * | 2019-08-16 | 2022-12-13 | 澳门大学 | Double-function full-electrolysis water-electricity catalyst and preparation method and application thereof |
| CN111408362A (en) * | 2020-03-23 | 2020-07-14 | 山东鲁北国际新材料研究院有限公司 | Sea urchin-shaped cobalt sulfide-charcoal composite material and preparation method and application thereof |
| CN111686773B (en) * | 2020-07-14 | 2021-11-16 | 南京林业大学 | Sea urchin-like nickel-iron phosphonate photocatalyst and preparation method thereof |
| CN111686773A (en) * | 2020-07-14 | 2020-09-22 | 南京林业大学 | Sea urchin-like nickel-iron phosphonate photocatalyst and preparation method thereof |
| CN112962115A (en) * | 2021-02-09 | 2021-06-15 | 上海交通大学 | Foamed nickel loaded sulfide electrocatalyst and preparation method and application thereof |
| CN112962115B (en) * | 2021-02-09 | 2022-04-01 | 上海交通大学 | Foamed nickel loaded sulfide electrocatalyst and preparation method and application thereof |
| CN114360919A (en) * | 2021-11-22 | 2022-04-15 | 沈阳工程学院 | Preparation method of high-performance electrode material with nano sea urchin structure |
| CN114990622A (en) * | 2022-06-02 | 2022-09-02 | 蚌埠学院 | Preparation method of sea urchin-shaped iron-doped nickel hydroxide oxygen evolution catalyst |
| CN115786964A (en) * | 2023-02-06 | 2023-03-14 | 北京化工大学 | Cobalt-based spinel Cu 0.7 Co 2.3 O 4 Electrocatalyst and preparation method and application thereof |
| CN115786964B (en) * | 2023-02-06 | 2023-12-12 | 北京化工大学 | Cobalt-based spinel Cu 0.7 Co 2.3 O 4 Electrocatalyst, preparation method and application thereof |
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