CN111362320A - Loaded nickel sulfide nanorod material and preparation method and application thereof - Google Patents
Loaded nickel sulfide nanorod material and preparation method and application thereof Download PDFInfo
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- 239000002073 nanorod Substances 0.000 title claims abstract description 56
- 239000000463 material Substances 0.000 title claims abstract description 45
- WWNBZGLDODTKEM-UHFFFAOYSA-N sulfanylidenenickel Chemical compound [Ni]=S WWNBZGLDODTKEM-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title abstract description 10
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 76
- HEMHJVSKTPXQMS-UHFFFAOYSA-M sodium hydroxide Substances [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 37
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 35
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- 239000000758 substrate Substances 0.000 claims abstract description 25
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 13
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 13
- 238000000354 decomposition reaction Methods 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims abstract description 8
- 238000004519 manufacturing process Methods 0.000 claims abstract description 4
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 18
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 229910001220 stainless steel Inorganic materials 0.000 claims description 5
- 239000010935 stainless steel Substances 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000006260 foam Substances 0.000 abstract description 22
- 238000011065 in-situ storage Methods 0.000 abstract description 6
- 230000012010 growth Effects 0.000 abstract description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052739 hydrogen Inorganic materials 0.000 abstract description 3
- 239000001257 hydrogen Substances 0.000 abstract description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 238000002425 crystallisation Methods 0.000 abstract description 2
- 230000008025 crystallization Effects 0.000 abstract description 2
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000010899 nucleation Methods 0.000 abstract description 2
- 230000006911 nucleation Effects 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 239000002086 nanomaterial Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000008367 deionised water Substances 0.000 description 6
- 229910021641 deionized water Inorganic materials 0.000 description 6
- 238000011160 research Methods 0.000 description 5
- 238000003491 array Methods 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- 239000002070 nanowire Substances 0.000 description 3
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000004833 X-ray photoelectron spectroscopy Methods 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000010411 electrocatalyst Substances 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 238000002173 high-resolution transmission electron microscopy Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004502 linear sweep voltammetry Methods 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 239000004005 microsphere Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000000877 morphologic effect Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G53/00—Compounds of nickel
- C01G53/11—Sulfides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
- B01J27/043—Sulfides with iron group metals or platinum group metals
-
- B01J35/23—
-
- B01J35/33—
-
- 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
- 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
-
- 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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
- C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/04—Particle morphology depicted by an image obtained by TEM, STEM, STM or AFM
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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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 invention discloses a loaded nickel sulfide nanorod material as well as a preparation method and application thereof. Control of NiS Using polyvinylpyrrolidone and sodium hydroxide2And in the processes of nucleation, crystallization and growth of the nanocrystalline, the formation of a one-dimensional nanorod structure is realized through one-step hydrothermal reaction, and the loaded nickel sulfide nanorod material is obtained. In the loaded nickel sulfide nanorod material, the nickel sulfide nanorod array is loaded on the foam nickel substrate in situ, and due to the special one-dimensional structure of the nickel sulfide nanorod array, the nickel sulfide nanorod has excellent catalytic performance on hydrogen production and oxygen evolution half reactions of electrocatalytic decomposition of water,is expected to be applied to the field of water decomposition by electrocatalysis in a large scale.
Description
Technical Field
The invention relates to nickel sulfide (NiS)2) Nanometer material, especially nickel sulfide nanometer rod material and its preparation process and application.
Background
With the development of industry and economy, the energy crisis has become one of the problems that must be solved. The method for preparing hydrogen by decomposing water based on an electrochemical method is an effective way for solving the energy problem. Since the water splitting reaction involves two half-reactions, hydrogen production (HER) and Oxygen Evolution (OER), both of which require a catalyst to accelerate the reaction rate. Therefore, the search for highly efficient, inexpensive HER and OER electrocatalysts has become a hotspot of research in recent years.
Compared with the traditional electro-catalyst Pt and Ru/Ir-based material, the cubic phase NiS2The material has the advantages of low cost, rich sources and the like, and is an electrocatalytic material which is widely researched. Overall, however, currently NiS2The problem of high electrocatalytic overpotentials of the base materials still remains. In order to solve the problems, the electro-catalytic performance of the catalyst is improved by optimizing the shape and the structure of the catalyst. NiS currently applied to electrocatalytic water splitting reaction2The material comprises various nano structures such as nano particles, nano sheets, nano wires, nano hollow microspheres and the like. Among them, the one-dimensional nanostructures have attracted much attention in recent years due to their higher specific surface area and richer surface active sites, and shorter ion and electron transport paths, compared to other nanostructures. Recent reports indicate that NiS grown in situ on carbon fiber paper substrates2Nanowire arrays showed good HER and OER activity, and 10mA/cm could be obtained at overpotentials of 165mV and 246mV, respectively2Has a current density of HER and OER which is much lower than that of NiS2Nanosheet arrays (int. j. hydrogeneenergy, 2017,42, 17038-. These results indicate that one-dimensional nanostructures do have unique advantages in the field of electrocatalysis. However, in general, one-dimensional NiS is currently concerned2The research of nanostructures is still very limited. Except that it has been reportedIn addition to the nanowires of (a), there is no other one-dimensional NiS2Reports of nanostructures such as nanorods.
In addition, recent research also finds that besides the morphological structure optimization of the material itself, the in-situ growth of the nano-structure on the substrate in the form of an array (such as foamed nickel, carbon cloth, carbon paper, etc.) is an effective means for improving the electrocatalytic performance. Research shows that the in-situ grown nanometer structure has close interface contact with the substrate and is favorable to the transmission of ions and electrons. In addition, the nanometer material loaded on the substrate can be directly used as a working electrode for electrocatalytic water decomposition reaction, so that the complex process of manufacturing the electrode by using a powder material is avoided, and the method is favorable for actual large-scale production. However, overall, the controlled in-situ growth of nanostructures on a substrate is technically problematic. For example, how can an appropriate substrate be selected to achieve growth of nanostructures? How can the structure of the nanomaterial be controlled? And so on.
Disclosure of Invention
The invention aims to provide a supported nickel sulfide nanorod material and a preparation method thereof, and the material is used for electrocatalytic water decomposition reaction.
The invention provides a loaded nickel sulfide nanorod material, which comprises a substrate and nickel sulfide nanorods loaded on the substrate; the nickel sulfide nanorod is cubic phase nickel sulfide, the diameter of the nickel sulfide nanorod is 30-90nm, and the length of the nickel sulfide nanorod is 150-450 nm.
Preferably, the substrate is foamed nickel.
The preparation method of the loaded nickel sulfide nanorod material comprises the following steps of: nickel nitrate (Ni (NO))3)2·6H2O), thiourea (CN)2H4S), sodium hydroxide (NaOH) and polyvinylpyrrolidone (PVP) are dissolved in water and placed in a reaction kettle; putting a substrate into the reaction kettle, and keeping the reaction kettle at the temperature of 110-; and washing and drying the substrate to obtain the loaded nickel sulfide nanorod material.
Preferably, the molar ratio of the nickel nitrate, the thiourea, the sodium hydroxide and the polyvinylpyrrolidone is 1:3-5:0.02-0.05: 0.002-0.005.
Preferably, the molar ratio of the water to the nickel nitrate is 6-13: 1.
Preferably, the reaction vessel is a stainless steel autoclave.
The loaded nickel sulfide nanorod material can be used as a catalyst for electrocatalytic water decomposition reaction.
The invention has the technical effects that: first, control of NiS using polyvinylpyrrolidone and sodium hydroxide2The nucleation, crystallization and growth process of the nano-crystal is simple in operation, so that NiS is obtained2Forming a one-dimensional rod-shaped structure; one-dimensional NiS of the second2The nano-rod grows on the substrate in situ in an array form, can be directly used as a working electrode for electrocatalytic water decomposition reaction, and is beneficial to practical electrochemical application; thirdly, the one-dimensional NiS has the advantages of one-dimensional loose rod-shaped structure and large specific surface area2The nanorod array shows excellent electrocatalytic performance to HER and OER half reactions of water decomposition, and develops a research idea of electrocatalytic water decomposition reaction.
Drawings
FIG. 1 is an X-ray diffraction profile of the foamed nickel supported nickel sulfide nanorod material prepared in example 1.
Figure 2 is a low power scanning electron micrograph of the foamed nickel supported nickel sulfide nanorod material prepared in example 1 and the original foamed nickel substrate.
Fig. 3 is a scanning electron micrograph and a transmission electron micrograph of the foamed nickel-supported nickel sulfide nanorod material prepared in example 1.
FIG. 4 is an X-ray photoelectron spectroscopy plot of the foamed nickel-supported nickel sulfide nanorod material prepared in example 1.
Figure 5 is a graph of HER performance for different materials.
Figure 6 is a graph of OER performance for different materials.
Detailed Description
The following detailed description will be provided with the advantages of the present invention in conjunction with the embodiments of the drawings, which are intended to help the reader to better understand the spirit of the present invention, but not to limit the scope of the present invention.
Preparation example 1:
2.4mmol of nickel nitrate (Ni (NO)3)2·6H2O), 0.8g of thiourea (CN)2H4S), 0.1mmol of sodium hydroxide (NaOH) and 0.6g of polyvinylpyrrolidone (PVP) are dissolved in 50mL of deionized water to obtain a water solution, the water solution is transferred to a 100mL stainless steel autoclave, a piece of washed foam nickel (1 × 3 cm) is added, the autoclave is kept at 150 ℃ for 10h, after the reaction is finished and the temperature is cooled to the room temperature, the foam nickel is thoroughly washed by the deionized water and ethanol, and then dried at 70 ℃ for 10h to obtain the nickel sulfide nanorod material loaded with the foam nickel.
Preparation example 2:
2.4mmol of nickel nitrate (Ni (NO)3)2·6H2O), 0.8g of thiourea (CN)2H4S), 0.1mmol of sodium hydroxide (NaOH) and 0.65g of polyvinylpyrrolidone (PVP) are dissolved in 50mL of deionized water to obtain a water solution, the water solution is transferred to a 100mL stainless steel autoclave, a piece of washed foam nickel (1 × 3 cm) is added, the autoclave is kept at 160 ℃ for 10h, after the reaction is finished and the temperature is cooled to the room temperature, the foam nickel is thoroughly washed by the deionized water and ethanol, and then dried at 70 ℃ for 10h to obtain the nickel sulfide nanorod material loaded with the foam nickel.
Preparation example 3:
2.4mmol of nickel nitrate (Ni (NO)3)2·6H2O), 0.8g of thiourea (CN)2H4S), 0.1mmol of sodium hydroxide (NaOH) and 0.6g of polyvinylpyrrolidone (PVP) are dissolved in 76mL of deionized water to obtain a water solution, the water solution is transferred to a 100mL stainless steel autoclave, a piece of washed foam nickel (1 × 3 cm) is added, the autoclave is kept at 150 ℃ for 10h, after the reaction is finished and the temperature is cooled to the room temperature, the foam nickel is thoroughly washed by the deionized water and ethanol, and then dried at 70 ℃ for 10h to obtain the nickel sulfide nanorod material loaded with the foam nickel.
Preparation of NiS obtained in examples 1 to 32The material is a one-dimensional nanorod structure, and nanorods are approximately perpendicular in an array formDirectly loaded on a foam nickel substrate, and the phase of the foam nickel substrate is cubic NiS2The diameter is 30-90nm, and the length is 150-450 nm.
The nickel sulfide nanorod material loaded with the foamed nickel is used for a working electrode of electrocatalytic water decomposition reaction, and the electrocatalytic performance test is as follows: testing on a CHI 660E electrochemical workstation by adopting a standard three-electrode system; using platinum foil and saturated calomel electrode as counter electrode and reference electrode, respectively, and using foamed nickel loaded nickel sulfide nano rod material (grown with one-dimensional NiS)2Nanorod array nickel foam) was cut into 3 × 3mm as the working electrode, 1M KOH aqueous solution was used as the electrolyte, the polarization curve was obtained by Linear Sweep Voltammetry (LSV) at a sweep rate of 5 mV/s.
FIG. 1 is the result of characterization of nickel sulfide nanorod material supported by nickel foam using an X-ray diffraction (XRD) instrument. It is evident from this that in addition to the sharp diffraction peak of the nickel foam substrate (marked "#"), there is also a typical cubic phase NiS2The diffraction peak of (JCPDS No.88-1709, marked ""). Cubic phase NiS2The diffraction peak of (A) is less sharp because the diffraction peak of the foamed nickel substrate is too strong to mask the cubic phase NiS to a large extent2。
Figure 2 is a low-power scanning electron micrograph of the nickel foam-supported nickel sulfide nanorod material and the original nickel foam substrate. It can be clearly seen that the original foam nickel surface is a smooth fish scale structure. After the hydrothermal reaction, a layer of uniform and compact nano structure is covered on the surface of the foamed nickel, which shows that the product successfully grows on the surface of the foamed nickel.
Fig. 3 is a scanning electron micrograph and a transmission electron micrograph of a nickel sulfide nanorod material supported by nickel foam. The low-magnification scanning electron microscope image shows that the nanorods are approximately vertically loaded on the surface of the nickel foam. In addition, the size diameter of the nano rod is 30-90nm, and the length is 150-450 nm. In high resolution transmission electron microscopy images, clear lattice fringes with interplanar spacing of 0.28nm can be normalized to cubic NiS2The (200) crystal face of the nano-rod further determines that the phase of the nano-rod is cubic NiS2。
FIG. 4 is an X-ray photoelectron spectroscopy plot of a nickel sulfide nanorod material supported by nickel foam. By comparing with the results reported in the literature (ACSAppl. Mater. interfaces 9(2017)2500-2508), NiS with the cubic phase of the nanorods can be further determined2。
Figure 5 is a graph of HER performance for different materials. It can be found that NiS is loaded on the foamed nickel2The nano-rod array reaches 10mA/cm2The current density required only a small overpotential (185mV), smaller than the original foamed nickel substrate (233mV) (fig. 5 a). At the same time, NiS2The tafel slope of the nanorod arrays was also lower relative to nickel foam alone (fig. 5b), indicating faster surface HER electrochemical reaction kinetics.
Figure 6 is a graph of OER performance for different materials. FIG. 6a shows a signal at 40mA/cm2At a current density of (2), NiS2The nanorod array has a lower overpotential (382 mV). In addition, NiS2The nanorod arrays also had a very small Tafel slope (151mV/dec), much lower than the original nickel foam (179mV/dec), indicating that the OER reaction kinetics for their surfaces are also faster.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solution of the present invention by those skilled in the art should fall within the protection scope defined by the claims of the present invention without departing from the spirit of the present invention.
Claims (8)
1. A loaded nickel sulfide nanorod material is characterized in that: comprises a substrate and nickel sulfide nano rods loaded on the substrate; the nickel sulfide nanorod is cubic phase nickel sulfide, the diameter of the nickel sulfide nanorod is 30-90nm, and the length of the nickel sulfide nanorod is 150-450 nm.
2. The supported nickel sulfide nanorod material of claim 1, wherein: the substrate is foamed nickel.
3. The method of making a supported nickel sulfide nanorod material according to claim 1, comprising the steps of: dissolving nickel nitrate, thiourea, sodium hydroxide and polyvinylpyrrolidone in water, and placing the solution in a reaction kettle; putting a substrate into the reaction kettle, and keeping the reaction kettle at the temperature of 110-; and washing and drying the substrate to obtain the loaded nickel sulfide nanorod material.
4. The method of claim 3, wherein: the molar ratio of the nickel nitrate to the thiourea to the sodium hydroxide to the polyvinylpyrrolidone is 1:3-5:0.02-0.05: 0.002-0.005.
5. The method of claim 4, wherein: the molar ratio of the amount of the water to the amount of the nickel nitrate is 6-13: 1.
6. The method of claim 3, wherein: the reaction kettle is a stainless steel autoclave.
7. Use of the supported nickel sulfide nanorod material according to claim 1.
8. Use according to claim 7, characterized in that: the loaded nickel sulfide nanorod material is used for electrocatalytic water decomposition reaction.
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| CN112723429A (en) * | 2021-01-10 | 2021-04-30 | 齐齐哈尔大学 | Preparation method for synthesizing nickel sulfide nano particles by hydrothermal method |
| CN113789545A (en) * | 2021-09-26 | 2021-12-14 | 中汽创智科技有限公司 | Water electrolysis catalyst and preparation method and application thereof |
| CN114807956A (en) * | 2022-04-11 | 2022-07-29 | 西南石油大学 | Preparation method of in-situ growth nano array catalyst applied to hydrogen sulfide hydrogen production |
| CN115832222A (en) * | 2022-12-29 | 2023-03-21 | 楚能新能源股份有限公司 | Flexible sodium-ion battery cathode, preparation method thereof and flexible sodium-ion battery |
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