CN114774977B - Sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, preparation method and application thereof - Google Patents
Sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, preparation method and application thereof Download PDFInfo
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- CN114774977B CN114774977B CN202210489535.4A CN202210489535A CN114774977B CN 114774977 B CN114774977 B CN 114774977B CN 202210489535 A CN202210489535 A CN 202210489535A CN 114774977 B CN114774977 B CN 114774977B
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- doped nickel
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- 239000010411 electrocatalyst Substances 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 41
- 239000002073 nanorod Substances 0.000 title claims abstract description 41
- -1 nickel hydroxide-cerium dioxide Chemical compound 0.000 title claims abstract description 31
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 54
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 24
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000006260 foam Substances 0.000 claims abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 19
- 239000001301 oxygen Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 16
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims abstract description 11
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims abstract description 11
- 235000019345 sodium thiosulphate Nutrition 0.000 claims abstract description 11
- 239000002243 precursor Substances 0.000 claims abstract description 8
- 239000000758 substrate Substances 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 238000000034 method Methods 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 229910000422 cerium(IV) oxide Inorganic materials 0.000 claims description 8
- 239000003153 chemical reaction reagent Substances 0.000 claims description 7
- 238000001816 cooling Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 239000003054 catalyst Substances 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 2
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000003795 desorption Methods 0.000 claims description 2
- 239000004744 fabric Substances 0.000 claims description 2
- 239000011521 glass Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000005303 weighing Methods 0.000 claims description 2
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- 238000001027 hydrothermal synthesis Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 238000004457 water analysis Methods 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 6
- 229910052739 hydrogen Inorganic materials 0.000 description 6
- 239000001257 hydrogen Substances 0.000 description 6
- 229910018661 Ni(OH) Inorganic materials 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 238000005868 electrolysis reaction Methods 0.000 description 3
- 230000010287 polarization Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000000354 decomposition reaction Methods 0.000 description 2
- HTXDPTMKBJXEOW-UHFFFAOYSA-N dioxoiridium Chemical compound O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical group [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 2
- 229910000510 noble metal Inorganic materials 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000001075 voltammogram Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- CETPSERCERDGAM-UHFFFAOYSA-N ceric oxide Chemical compound O=[Ce]=O CETPSERCERDGAM-UHFFFAOYSA-N 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- 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
- C25B11/091—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the electrocatalyst material consisting of at least one catalytic element and at least one catalytic compound; consisting of two or more catalytic elements or catalytic compounds
-
- 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
Abstract
The invention relates to the technical field of electrocatalysis, in particular to a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, a preparation method and application thereof, which takes nickel nitrate, cerium nitrate and sodium thiosulfate as precursors, and grows the sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array on a foam nickel substrate in situ by a one-step hydrothermal method, wherein the sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst has excellent electrocatalytic water analysis oxygen reaction catalytic activity and is used for 10mA/cm 2 Only 200mV overpotential is required at current density, and has the advantages of good stability and high stability, meets the requirements of large-scale industrial application.
Description
Technical Field
The invention relates to the technical field of electrocatalysis, in particular to a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, a preparation method and application thereof.
Background
The energy and environmental problems promote people to demand a renewable clean energy technology, and hydrogen energy is used as a renewable clean energy with high energy density, so that the method has wide application prospect.
The electrocatalytic decomposition of water to produce hydrogen is an effective technology for obtaining hydrogen energy, however, oxygen evolution half reaction (OER) involves a four-electron transfer process, and the reaction process is slow, so that the efficiency of water electrolysis to produce hydrogen is restricted, and therefore, the improvement of the catalytic efficiency of an electrocatalyst for oxygen evolution reaction is a key for realizing efficient water electrolysis to produce hydrogen.
At present, most of commercial oxygen evolution electrocatalysts are ruthenium dioxide and iridium dioxide based on noble metals, however, the price is high and the earth reserves are rare, so that the development and design of oxygen evolution electrocatalysts based on non-noble metals are required to meet the large-scale industrial application requirements of water electrolysis and hydrogen production.
In view of the above drawbacks, the present inventors have finally achieved the present invention through long-time studies and practices.
Disclosure of Invention
The invention aims to solve the problem of poor oxygen evolution performance and stability of the existing electrocatalyst, and provides a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, a preparation method and application thereof.
In order to achieve the above purpose, the invention discloses a preparation method of a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, which comprises the following steps:
s1: respectively weighing nickel nitrate, cerium nitrate and sodium thiosulfate;
s2: adding the precursor reagent weighed in the step S1 into a reaction kettle containing deionized water and a substrate, and heating;
s3: and cooling to room temperature, removing foam nickel, washing and airing to obtain the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst.
In the step S1, the mass of nickel nitrate is 45-360 mg, the mass of cerium nitrate is 20-180 mg, and the mass of sodium thiosulfate is 10-60 mg.
In the step S2, the deionized water is 60mL.
And the heating temperature in the step S2 is 120 ℃, and the temperature is kept for 12 hours after heating.
The substrate in the step S2 is any one of foam nickel, foam iron, carbon cloth and conductive glass.
The invention also discloses a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst prepared by the preparation method and application of the sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst in electrocatalytic moisture desorption oxygen.
Compared with the prior art, the invention has the beneficial effects that: the invention takes nickel nitrate, cerium nitrate and sodium thiosulfate as raw materials, and a sulfur-doped nickel hydroxide-cerium dioxide composite nano rod array is grown on a foam nickel substrate in situ by a one-step hydrothermal method. The preparation process of the electrocatalyst is simple, and simultaneously, the electrocatalyst shows excellent electrocatalytic activity and stability of the electrocatalytic moisture analysis oxygen reaction;
the sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst prepared by the method has excellent catalytic performance when being applied to electrocatalytic oxygen evolution reaction, and the current density is 10mA/cm 2 Only 200mV overpotential is required. The sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst prepared by the method of the invention is respectively applied with 10mA/cm 2 、20mA/cm 2 、50mA/cm 2 、100mA/cm 2 、300mA/cm 2 、10mA/cm 2 The electric current is 25 hours each, and the electrocatalytic oxygen evolution performance is still stable, so that the electrocatalyst provided by the invention has excellent electrocatalytic activity and stability of the water-resolved oxygen reaction, and meets the requirements of large-scale industrial application.
Drawings
FIG. 1 is an SEM image of a sulfur-doped nickel hydroxide-ceria composite nanorod array prepared according to example 3;
FIG. 2 is an XRD pattern for a sulfur-doped nickel hydroxide-ceria composite nanorod array prepared in example 3;
FIG. 3 is a linear sweep voltammogram of a sample electrocatalytic oxygen evolution reaction prepared in various examples;
FIG. 4 shows the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst prepared in example 3, undoped S and CeO 2 Composite electrocatalyst and commercial RuO 2 Is used for generating an oxygen evolution reaction linear sweep voltammogram;
FIG. 5 is a graph of overpotential statistics for a sulfur-doped nickel hydroxide-ceria composite nanorod array electrocatalyst at different current densities;
fig. 6 is a test result of stability of a sulfur-doped nickel hydroxide-ceria composite nanorod array electrocatalyst.
Detailed Description
The above and further technical features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
Example 1
The embodiment provides a preparation method of a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, which comprises the following steps:
(1) An appropriate amount of 180mg of nickel nitrate and 40mg of sodium thiosulfate were weighed respectively.
(2) The precursor reagents were placed in a 100mL reactor containing 60mL deionized water and nickel foam.
(3) The reaction vessel was heated to 120℃and held for 12h.
(4) And cooling to room temperature, removing foam nickel, washing and airing to obtain the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst.
Example 2
The embodiment provides a preparation method of a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, which comprises the following steps:
(1) An appropriate amount of 180mg of nickel nitrate, 45mg of cerium nitrate and 40mg of sodium thiosulfate were weighed respectively.
(2) The precursor reagents were placed in a 100mL reactor containing 60mL deionized water and nickel foam.
(3) The reaction vessel was heated to 120℃and held for 12h.
(4) And cooling to room temperature, removing foam nickel, washing and airing to obtain the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst.
Example 3
The embodiment provides a preparation method of a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, which comprises the following steps:
(1) An appropriate amount of 180mg of nickel nitrate, 90mg of cerium nitrate and 40mg of sodium thiosulfate were weighed respectively.
(2) The precursor reagents were placed in a 100mL reactor containing 60mL deionized water and nickel foam.
(3) The reaction vessel was heated to 120℃and held for 12h.
(4) And cooling to room temperature, removing foam nickel, washing and airing to obtain the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst.
Example 4
The embodiment provides a preparation method of a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, which comprises the following steps:
(1) An appropriate amount of 180mg of nickel nitrate, 180mg of cerium nitrate and 40mg of sodium thiosulfate were weighed respectively.
(2) The precursor reagents were placed in a 100mL reactor containing 60mL deionized water and nickel foam.
(3) The reaction vessel was heated to 120℃and held for 12h.
(4) And cooling to room temperature, removing foam nickel, washing and airing to obtain the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst.
Example 5
The embodiment provides a preparation method of a sulfur-doped nickel hydroxide-cerium dioxide composite nanorod array electrocatalyst, which comprises the following steps:
(1) An appropriate amount of 180mg of nickel nitrate, 360mg of cerium nitrate and 40mg of sodium thiosulfate were weighed respectively.
(2) The precursor reagents were placed in a 100mL reactor containing 60mL deionized water and nickel foam.
(3) The reaction vessel was heated to 120℃and held for 12h.
(4) And cooling to room temperature, removing foam nickel, washing and airing to obtain the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst.
The SEM image of the sulfur-doped nickel hydroxide-ceria composite nano electrocatalyst prepared in example 3 of fig. 1 shows that the composite nano electrocatalyst is a nanorod array structure, and the XRD image shows that the phase composition of the composite nano electrocatalyst is nickel hydroxide and ceria.
Test of the foam Nickel self-supporting Sulfur-doped Nickel hydroxide-cerium oxide composite nanorod array electrocatalyst (S-Ni (OH)) prepared by different examples 2 /CeO 2 Electrocatalytic oxygen evolution polarization curve of/NF) to compare it with undoped and uncomplexed nickel hydroxide and commercial RuO 2 Is used for the electrocatalytic decomposition of water to oxygen. The specific process is as follows:
the electrocatalytic oxygen evolution polarization curves were tested using the electrocatalysts prepared in the different examples as working electrode, platinum sheet electrode as counter electrode, hg/HgO electrode as reference electrode, and freshly prepared 1M KOH aqueous solution (ph=13.9) as electrolyte (fig. 3). As can be seen from fig. 3, when cerium nitrate was used in an amount of 90mg, the electrocatalytic performance of the resulting catalyst was optimal.
Respectively Ni (OH) 2 /NF、S-Ni(OH) 2 /NF、S-Ni(OH) 2 /CeO 2 /NF、RuO 2 The electrocatalytic oxygen evolution polarization curve was tested using freshly prepared 1M KOH aqueous solution (ph=13.9) as the electrolyte, with a platinum sheet electrode as the working electrode and an Hg/HgO electrode as the reference electrode,/NF (fig. 4). Comparative Ni (OH) 2 /NF、S-Ni(OH) 2 /NF、S-Ni(OH) 2 /CeO 2 /NF、RuO 2 The NF is 10, 20, 50mA/cm 2 The lower overpotential (FIG. 5), S-Ni (OH) 2 /CeO 2 The nano rod array structure of the/NF is 10mA/cm 2 Only 200mV overpotential is needed at current density, which is far superior to undoped and uncomplexed catalysts and commercial RuO 2 Is used for the electrocatalytic performance of the catalyst.
For S-Ni (OH) 2 /CeO 2 Continuous application of 10mA/cm to an array of NF nanorods 2 、20mA/cm 2 、50mA/cm 2 、100mA/cm 2 、300mA/cm 2 、10mA/cm 2 The electrocatalytic stability was tested at 25h for each current and the results are shown in figure 6. The results show S-Ni (OH) 2 /CeO 2 The electrocatalytic oxygen evolution performance of the NF nano rod array is still stable after 150h test, and the method is suitable for industrial application.
The foregoing description of the preferred embodiment of the invention is merely illustrative of the invention and is not intended to be limiting. It will be appreciated by persons skilled in the art that many variations, modifications, and even equivalents may be made thereto without departing from the spirit and scope of the invention as defined in the appended claims.
Claims (6)
1. The preparation method of the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst is characterized by comprising the following steps of:
s1: respectively weighing nickel nitrate, cerium nitrate and sodium thiosulfate;
s2: adding the precursor reagent weighed in the step S1 into a reaction kettle containing deionized water and a substrate, and heating;
s3: and cooling to room temperature, removing foam nickel, washing and airing to obtain the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst.
2. The method for preparing the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst according to claim 1, wherein in the step S1, the mass of nickel nitrate is 180mg, the mass of cerium nitrate is 45-180 mg or 360mg, the mass of sodium thiosulfate is 40mg, and in the step S2, deionized water is 60mL.
3. The method for preparing the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst according to claim 1, wherein the heating temperature in step S2 is 120 ℃, and the catalyst is maintained for 12 hours after heating.
4. The method for preparing the sulfur-doped nickel hydroxide-cerium oxide composite nanorod array electrocatalyst according to claim 1, wherein the substrate in the step S2 is any one of foam nickel, foam iron, carbon cloth and conductive glass.
5. A sulfur-doped nickel hydroxide-ceria composite nanorod array electrocatalyst prepared by the method of any one of claims 1 to 4.
6. Use of the sulfur-doped nickel hydroxide-ceria composite nanorod array electrocatalyst according to claim 5 for electrocatalytic moisture desorption of oxygen.
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