CN111905744B - Nickel-iron hydroxide composite material, catalyst, preparation method and application - Google Patents
Nickel-iron hydroxide composite material, catalyst, preparation method and application Download PDFInfo
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- CN111905744B CN111905744B CN202010720414.7A CN202010720414A CN111905744B CN 111905744 B CN111905744 B CN 111905744B CN 202010720414 A CN202010720414 A CN 202010720414A CN 111905744 B CN111905744 B CN 111905744B
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- QJSRJXPVIMXHBW-UHFFFAOYSA-J iron(2+);nickel(2+);tetrahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[Fe+2].[Ni+2] QJSRJXPVIMXHBW-UHFFFAOYSA-J 0.000 title claims abstract description 80
- 239000003054 catalyst Substances 0.000 title claims abstract description 79
- 239000002131 composite material Substances 0.000 title claims abstract description 79
- 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 117
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 56
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 41
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 41
- 239000001301 oxygen Substances 0.000 claims abstract description 41
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 40
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 40
- 239000004744 fabric Substances 0.000 claims abstract description 33
- 238000000151 deposition Methods 0.000 claims abstract description 27
- 239000000243 solution Substances 0.000 claims abstract description 17
- 238000005406 washing Methods 0.000 claims abstract description 17
- UGKDIUIOSMUOAW-UHFFFAOYSA-N iron nickel Chemical compound [Fe].[Ni] UGKDIUIOSMUOAW-UHFFFAOYSA-N 0.000 claims abstract description 16
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 239000011259 mixed solution Substances 0.000 claims abstract description 13
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 98
- 239000006260 foam Substances 0.000 claims description 21
- 229910052742 iron Inorganic materials 0.000 claims description 20
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 230000008021 deposition Effects 0.000 claims description 11
- 238000000354 decomposition reaction Methods 0.000 claims description 10
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 claims description 7
- 238000004070 electrodeposition Methods 0.000 claims description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 238000004458 analytical method Methods 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 238000005137 deposition process Methods 0.000 claims description 3
- 238000004519 manufacturing process Methods 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 4
- 230000003197 catalytic effect Effects 0.000 abstract description 3
- MVFCKEFYUDZOCX-UHFFFAOYSA-N iron(2+);dinitrate Chemical compound [Fe+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O MVFCKEFYUDZOCX-UHFFFAOYSA-N 0.000 abstract description 3
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 abstract description 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 12
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- 239000003792 electrolyte Substances 0.000 description 6
- 229910052697 platinum Inorganic materials 0.000 description 6
- 238000004502 linear sweep voltammetry Methods 0.000 description 5
- 238000001878 scanning electron micrograph Methods 0.000 description 5
- 239000000758 substrate Substances 0.000 description 5
- 229910000863 Ferronickel Inorganic materials 0.000 description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 239000001257 hydrogen Substances 0.000 description 4
- 235000014413 iron hydroxide Nutrition 0.000 description 4
- NCNCGGDMXMBVIA-UHFFFAOYSA-L iron(ii) hydroxide Chemical compound [OH-].[OH-].[Fe+2] NCNCGGDMXMBVIA-UHFFFAOYSA-L 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 238000001075 voltammogram Methods 0.000 description 4
- BFDHFSHZJLFAMC-UHFFFAOYSA-L nickel(ii) hydroxide Chemical compound [OH-].[OH-].[Ni+2] BFDHFSHZJLFAMC-UHFFFAOYSA-L 0.000 description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 description 2
- 238000003487 electrochemical reaction Methods 0.000 description 2
- 238000005868 electrolysis reaction Methods 0.000 description 2
- 238000001453 impedance spectrum Methods 0.000 description 2
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical group Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 description 2
- 239000002135 nanosheet Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000036632 reaction speed Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
- B01J23/755—Nickel
-
- 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
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/33—Electric or magnetic properties
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- 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
- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
- B01J37/34—Irradiation by, or application of, electric, magnetic or wave energy, e.g. ultrasonic waves ; Ionic sputtering; Flame or plasma spraying; Particle radiation
- B01J37/348—Electrochemical processes, e.g. electrochemical deposition or anodisation
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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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- 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
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Abstract
The invention discloses a nickel-iron hydroxide composite material, a catalyst, a preparation method and application, wherein pretreated foamed nickel is added into an iron nitrate solution or an iron chloride solution according to a nickel-iron molar ratio of 1: 1-10, and ultrasonic treatment is carried out to obtain a nickel-iron mixed solution after the foamed nickel is fully dissolved; putting the nickel-iron mixed solution into an electrolytic cell, using carbon cloth as a working electrode, and depositing a nickel-iron hydroxide composite material on the carbon cloth by using a cathode deposition method; washing the deposited carbon cloth, and naturally airing to obtain the nickel-iron hydroxide composite material catalyst; the preparation process of the nickel-iron hydroxide composite catalyst is simple, the prepared nickel-iron hydroxide composite catalyst has excellent catalytic performance when being applied to the electrocatalytic oxygen production reaction, the oxygen evolution reaction rate of the nickel-iron hydroxide composite catalyst is far superior to that of a nickel-iron-based electrocatalytic material prepared by a traditional solution method, the electrocatalytic oxygen evolution stability is good, and the nickel-iron hydroxide composite catalyst has good industrial application prospect.
Description
Technical Field
The invention relates to the technical field of preparation of electrocatalytic materials, and particularly relates to a nickel-iron hydroxide composite material, a catalyst, a preparation method and application.
Background
Environmental pollution and energy crisis impel people to find a new clean energy to replace fossil energy, and hydrogen energy is popular among people as a renewable clean energy with high energy density.
The electrocatalytic decomposition of water is a common technology for hydrogen production, however, the rate of Hydrogen Evolution Reaction (HER) of water electrolysis is limited by Oxygen Evolution Reaction (OER), so that the improvement of the efficiency of the electrocatalyst for oxygen evolution reaction is the key for improving the hydrogen production of water electrolysis.
Catalysts with high performance oxygen evolution reactions have been reported to include ruthenium dioxide (RuO) 2 ) And iron, cobalt, manganese, nickel-based nano materials and the like, but the electrocatalytic oxygen evolution performance of the catalysts is poorAnd the requirements of industrial application cannot be met.
In view of the above-mentioned drawbacks, the present inventors have finally obtained the present invention through long-term research and practice.
Disclosure of Invention
In order to solve the technical defects, the technical scheme adopted by the invention is to provide a preparation method of a nickel-iron hydroxide composite material catalyst, which comprises the following steps:
s1, adding pretreated foamed nickel into an iron nitrate solution or an iron chloride solution according to a molar ratio of nickel to iron of 1: 1-10, and performing ultrasonic treatment to obtain a nickel-iron mixed solution after the foamed nickel is fully dissolved;
s2, putting the nickel-iron mixed solution into an electrolytic cell, using carbon cloth as a working electrode, and depositing a nickel-iron hydroxide composite material on the carbon cloth by using a cathode deposition method;
and S3, washing and naturally airing the deposited carbon cloth to obtain the nickel-iron hydroxide composite catalyst.
Preferably, in the step S1, the pretreatment of the foamed nickel is acid washing, water washing and ethanol washing.
Preferably, in step S2, the cathode deposition process is performed on the electrochemical workstation of CHI660E, and under a three-electrode system, the carbon cloth is used as a working electrode, the carbon rod is used as a counter electrode, and the saturated calomel electrode is used as a reference electrode.
Preferably, in the step S2, the deposition temperature is at room temperature, and the electrodeposition current density is 20mA/cm 2 The deposition time was 10 min.
Preferably, the nickel-iron hydroxide composite material is prepared through the steps S1 and S2 in the preparation method of the nickel-iron hydroxide composite material catalyst.
Preferably, the nickel-iron hydroxide composite catalyst is prepared by the preparation method of the nickel-iron hydroxide composite catalyst, and comprises a carbon cloth substrate and a nickel-iron hydroxide composite catalyst layer deposited and formed on the carbon cloth substrate.
Preferably, the application of the nickel-iron hydroxide composite material in the water decomposition oxygen analysis reaction is provided.
Preferably, the application of the nickel-iron hydroxide composite material catalyst in the water decomposition oxygen analysis reaction is provided.
Compared with the prior art, the invention has the beneficial effects that: the preparation process of the nickel-iron hydroxide composite catalyst is simple, the prepared nickel-iron hydroxide composite catalyst has excellent catalytic performance when applied to an electrocatalytic oxygen production reaction (OER), the oxygen evolution reaction rate of the nickel-iron hydroxide composite catalyst is far superior to that of a nickel-iron-based electrocatalytic material prepared by a traditional solution method, the electrocatalytic oxygen evolution stability is good, and the nickel-iron hydroxide composite catalyst has good industrial application prospects.
Drawings
FIG. 1 is an SEM image of a nickel iron hydroxide composite material prepared according to example one;
FIG. 2 is an SEM image of a nickel iron hydroxide composite material prepared in example ten;
FIG. 3 is an SEM image of a nickel iron hydroxide composite material prepared according to example eleven;
FIG. 4 is a plot of electrocatalytic oxygen production linear sweep voltammetry for nickel iron hydroxide composite catalysts prepared in examples one-eight and ten;
FIG. 5 is a plot of electrocatalytic oxygen generation linear sweep voltammograms of nickel iron hydroxide composite catalysts prepared in examples one, three, eight and twelve to fourteen;
FIG. 6 is a plot of electrocatalytic oxygen production linear sweep voltammetry for nickel iron hydroxide composite catalysts prepared in examples one and nine to twelve;
FIG. 7 is a statistical chart of overpotential at different current densities for the first, tenth, and twelfth embodiments;
FIG. 8 is Tafel plots of 2 x 1NF-Fe, 3 x 1NF-Fe, 4 x 1NF-Fe, 5 x 1NF-Fe, 8 x 1NF-Fe and Fe;
FIG. 9 is an electrochemical impedance spectrum of 3 x 1NF-Fe, 4 x 1NF-Fe and 5 x 1 NF-Fe;
figure 10 is a graph of the results of the 4 x 1NF-Fe stability test.
Detailed Description
The above and further features and advantages of the present invention are described in more detail below with reference to the accompanying drawings.
The preparation method of the nickel-iron hydroxide composite material catalyst comprises the following steps:
s1, adding pretreated foamed nickel into a ferric nitrate solution according to the molar ratio of 1: 1-10 ferronickel, performing ultrasonic treatment, and fully dissolving to obtain a ferronickel mixed solution;
s2, putting the nickel-iron mixed solution into an electrolytic cell, using carbon cloth as a working electrode, and depositing a nickel-iron hydroxide composite material on the carbon cloth by using a cathode deposition method;
and S3, washing and naturally airing the deposited carbon cloth to obtain the nickel-iron hydroxide composite catalyst.
In step S1, ferric nitrate may be replaced with ferric chloride.
In step S1, the pretreatment of the nickel foam is performed by acid washing, water washing, and ethanol washing.
In step S2, the cathode deposition process is performed on the electrochemical workstation of CHI660E, and in a three-electrode system, the carbon cloth is used as a working electrode, the carbon rod is used as a counter electrode, and the saturated calomel electrode is used as a reference electrode.
In the step S2, the deposition temperature is at room temperature, and the electrodeposition current density is 20mA/cm 2 The deposition time was 10 min.
The nickel-iron hydroxide composite catalyst obtained by the preparation method of the nickel-iron hydroxide composite catalyst comprises a carbon cloth substrate and a nickel-iron hydroxide composite catalyst layer deposited and formed on the carbon cloth substrate.
The preparation method of the nickel-iron hydroxide composite catalyst comprises the steps of dissolving foamed nickel in an iron nitrate solution, and preparing the nickel-iron hydroxide composite catalyst loaded on carbon cloth by adopting a cathode deposition method.
The prepared nickel-iron hydroxide composite catalyst has excellent catalytic performance when applied to electrochemical Oxygen Evolution Reaction (OER), and can be used for catalyzing water decomposition to generate oxygen at current density of 10mA/cm 2 The overpotential of time is 198mV, Tafel slopeIs 46 mV/dec. The nickel-iron hydroxide composite catalyst prepared by the method of the invention is applied with 20mA/cm 2 The electrocatalytic oxygen evolution performance of the catalyst is still kept stable after the current is 24h, so that the nickel-iron hydroxide composite material catalyst is suitable for industrial application.
Example one
In this embodiment, a method for preparing a nickel-iron hydroxide composite catalyst is provided, which includes the following steps:
s1, adding the pretreated 4 x 1cm of foamed nickel into 50ml of 0.1M ferric nitrate solution, performing ultrasonic treatment for 30min, and obtaining a ferronickel mixed solution with the ferronickel molar ratio of 1: 2 after the foamed nickel is fully dissolved.
S2, putting 25ml of nickel-iron mixed solution into an electrolytic cell, using carbon cloth as a working electrode, using a carbon rod as a counter electrode and using a saturated calomel electrode as a reference electrode. Depositing the nickel-iron hydroxide composite material on the carbon cloth by using a cathode deposition method, wherein the electrodeposition current density is 20mA/cm 2 The deposition time was 10 min.
And S3, washing and naturally airing the deposited carbon cloth to obtain the nickel-iron hydroxide composite material catalyst, wherein the nickel-iron ratio is 1: 2 and is marked as 4 x 1 NF-Fe.
The prepared nickel-iron hydroxide composite catalyst comprises a carbon cloth substrate and a catalyst layer, has the functions of both a catalyst and an electrode, is convenient to use, is used for electrolyzing water to prepare oxygen, and can simplify the process flow.
The SEM image of the nickel iron hydroxide composite material prepared in step S3 of this example is shown in fig. 1.
Application of 20mA/cm to 4 x 1NF-Fe 2 The current was 24h, and the stability of 4 x 1NF-Fe was tested, and the results are shown in fig. 10. From the results of FIG. 10, it can be seen that 20mA/cm was applied to 4X 1NF-Fe 2 After the current is 24 hours, the electrocatalytic oxygen evolution performance of the catalyst still keeps stable, and the catalyst is suitable for industrial application.
Example two
This example prepared a nickel iron hydroxide composite catalyst with a nickel to iron ratio of 1: 10, noted as 1 x 1NF-Fe, using 1 x 1cm of nickel foam instead of 4 x 1cm of nickel foam in step S1 of the example.
Other embodiments are as in example one.
EXAMPLE III
This example prepared a nickel iron hydroxide composite catalyst with a nickel to iron ratio of 1: 4, noted as 2 x 1NF-Fe, using 2 x 1cm of nickel foam instead of 4 x 1cm of nickel foam in step S1 of the example.
Other embodiments are as in example one.
Example four
This example prepared a nickel iron hydroxide composite catalyst with a nickel to iron ratio of 1: 2.5, noted as 3 x 1NF-Fe, using 3 x 1cm of nickel foam instead of 4 x 1cm of nickel foam in step S1 of the example.
Other embodiments are as in example one.
EXAMPLE five
This example prepared a nickel iron hydroxide composite catalyst with a nickel to iron ratio of 1: 1.5, noted as 5 x 1NF-Fe, using 5 x 1cm of nickel foam instead of 4 x 1cm of nickel foam in step S1 of the example.
Other embodiments are as in example one.
EXAMPLE six
This example prepared a nickel iron hydroxide composite catalyst, designated 6 x 1NF-Fe, using 6 x 1cm of nickel foam instead of 4 x 1cm of nickel foam in step S1 of the example.
Other embodiments are as in embodiment one.
EXAMPLE seven
This example prepared a nickel iron hydroxide composite catalyst, designated 7 x 1NF-Fe, using 7 x 1cm of nickel foam instead of 4 x 1cm of nickel foam in example step S1.
Other embodiments are as in example one.
Example eight
This example prepared a nickel iron hydroxide composite catalyst with a nickel to iron ratio of 1: 1, noted as 8 x 1NF-Fe, using 8 x 1cm of nickel foam instead of 4 x 1cm of nickel foam in step S1 of the example.
Other embodiments are as in embodiment one.
The performance of the nickel-iron hydroxide composite material catalysts prepared in the first to 8 embodiments was tested for oxygen production by electrocatalytic decomposition using a three-electrode system on an electrochemical workstation, and the specific process was as follows: the electrocatalytic oxygen production linear sweep voltammetry curves of the nickel iron hydroxide composite material catalysts prepared from the nickel iron hydroxide mixed solution with different molar ratios are tested by respectively using 1NF-Fe, 2 NF-Fe, 3 NF-Fe, 4 NF-Fe, 1NF-Fe, 5 NF-Fe, 6 NF-Fe, 7 NF-Fe and 8 NF-Fe as working electrodes, a platinum sheet electrode as a counter electrode, a Hg/HgO electrode as a reference electrode and 1mol/L potassium hydroxide solution as electrolyte, and the electrocatalytic oxygen production linear sweep voltammetry curves are shown in figure 4.
From the results of fig. 4, it is understood that 5 × 1NF-Fe and 8 × 1NF-Fe show oxidation peaks due to the high content of nickel, and thus their linear sweep voltammograms cannot be used as a criterion for judging whether the oxygen analysis performance is excellent or not. And 4 x 1NF-Fe, 3 x 1NF-Fe, 2 x 1NF-Fe and Fe do not have oxidation peaks, so that a sample of 4 x 1NF-Fe with the nickel-iron ratio of 1: 2 has smaller overpotential under the same current density, and the nickel-iron hydroxide composite catalyst prepared from 4 x 1cm of foamed nickel has better electrocatalytic oxygen evolution performance.
Example nine
This example prepared a nickel iron hydroxide composite catalyst, designated 4 x 1NF-FeCl, using 50ml of 0.1M ferric chloride solution instead of 50ml of 0.1M ferric nitrate solution as in one step S1 of the example 3 。
Other embodiments are as in example one.
Example ten
S1, preparing 50ml of 0.1M ferric nitrate solution, putting 25ml of the ferric nitrate solution into an electrolytic cell, using carbon cloth as a working electrode, using a carbon rod as a counter electrode, and using a saturated calomel electrode as a reference electrode. Depositing iron hydroxide on carbon cloth by cathode deposition method with electrodeposition current density of 20mA/cm 2 The deposition time was 10 min.
And S2, washing and naturally airing the deposited carbon cloth to obtain the iron hydroxide catalyst which is marked as Fe.
The SEM photograph of the iron hydroxide prepared in step S2 of this example is shown in FIG. 2.
As can be seen from fig. 2, the Fe catalyst is a radial flower-like nanosheet.
EXAMPLE eleven
S1, preparing 50ml of 0.1M nickel nitrate solution, putting 25ml of nickel nitrate solution into an electrolytic cell, using carbon cloth as a working electrode, using a carbon rod as a counter electrode, and using a saturated calomel electrode as a reference electrode. Depositing nickel hydroxide on carbon cloth by cathode deposition with an electrodeposition current density of 20mA/cm 2 The deposition time was 10 min.
And S2, washing the deposited carbon cloth, and naturally airing to obtain the nickel hydroxide catalyst, which is recorded as Ni.
The SEM image of the nickel hydroxide prepared in step S2 of this example is shown in fig. 3. As can be seen from fig. 3, the Ni catalyst is a bulky nanosheet.
Example twelve
S1, adding nickel nitrate into 50ml of 0.1M ferric nitrate solution to ensure that the concentration of the nickel nitrate is 0.2M, namely the molar ratio of the nickel to the iron is 1: 2, and uniformly mixing.
S2, putting 25ml of the mixed solution into an electrolytic cell, using carbon cloth as a working electrode, using a carbon rod as a counter electrode and using a saturated calomel electrode as a reference electrode. Depositing the nickel-iron hydroxide composite material on the carbon cloth by using a cathode deposition method, wherein the electrodeposition current density is 20mA/cm 2 The deposition time was 10 min.
S3, washing and naturally airing the deposited carbon cloth to obtain the nickel-iron hydroxide composite catalyst, which is marked as Ni 1 Fe 2 。
EXAMPLE thirteen
This example uses 0.4M nickel nitrate in place of the 0.2M nickel nitrate of the twelve step S1 example to prepare a nickel iron hydroxide composite catalyst, denoted Ni 1 Fe 4 。
Other embodiments are as in example twelve.
Example fourteen
In this example, a nickel iron hydroxide composite material was prepared by replacing 0.2M nickel nitrate in the twelve step S1 with 0.1M nickel nitrateCatalyst, denoted as Ni 1 Fe 1 。
Other embodiments are as in example twelve.
The performance of the nickel-iron hydroxide composite material catalyst prepared in the nine-fourteen embodiments is tested for oxygen production by electrocatalytic decomposition by using a three-electrode system on an electrochemical workstation, and the specific process is as follows: are respectively made of Ni 1 Fe 1 、Ni 1 Fe 2 、Ni 1 Fe 4 As a working electrode, a platinum sheet electrode is used as a counter electrode, an Hg/HgO electrode is used as a reference electrode, 1mol/L potassium hydroxide solution is used as an electrolyte, and the electrocatalytic oxygen generation linear sweep voltammetry curve of the nickel-iron hydroxide composite catalyst prepared from the nickel-iron mixed solution with different molar ratios is tested, and is shown in fig. 5.
From the results of fig. 5, it is clear that the oxygen evolution performance of the nickel iron hydroxide composite catalyst prepared from nickel foam as a nickel source is superior to that of the nickel iron hydroxide composite catalyst prepared from nickel nitrate as a nickel source at the same nickel iron molar ratio.
Respectively with 4 x 1NF-FeCl 3 And taking Ni and Fe as working electrodes, taking a platinum sheet electrode as a counter electrode, taking an Hg/HgO electrode as a reference electrode, taking 1mol/L potassium hydroxide solution as electrolyte, and testing the electrocatalytic oxygen generation linear scanning voltammogram of the nickel-iron hydroxide composite material catalyst prepared from the nickel-iron mixed solution with different molar ratios, wherein the electrocatalytic oxygen generation linear scanning voltammogram is shown in figure 6.
From the results of FIG. 6, it can be seen that 4X 1NF-Fe and 4X 1NF-FeCl 3 The electrocatalytic oxygen evolution performance of the catalyst is excellent, and under the condition that the molar ratio of nickel to iron is the same, the oxygen evolution performance of the nickel-iron hydroxide composite catalyst prepared by taking foamed nickel as a nickel source is far superior to that of the nickel-iron hydroxide composite catalyst prepared by taking nickel nitrate as a nickel source and that of pure nickel and pure iron hydroxide catalysts.
Example fifteen
This example tested 2 x 1NF-Fe, 3 x 1NF-Fe, 4 x 1NF-Fe, 5 x 1NF-Fe, 8 x 1NF-Fe, Ni 1 Fe 2 Tafel curves for different current densities with FeAnd overpotential to compare 4 x 1NF-Fe, Ni 1 Fe 2 And the ability of Fe to electrocatalytically decompose water to produce oxygen. The specific process is as follows:
4 x 1NF-Fe is taken as a working electrode, a platinum sheet electrode is taken as a counter electrode, an Hg/HgO electrode is taken as a reference electrode, 1mol/L potassium hydroxide solution is taken as electrolyte, and the current density is respectively set to be 10mA/cm 2 、20mA/cm 2 、50mA/cm 2 And 4, testing the overpotential of the NF-Fe at different current densities, wherein a statistical chart of the overpotential at different current densities is shown in a figure 7.
Ni1Fe2 is used as a working electrode, a platinum sheet electrode is used as a counter electrode, an Hg/HgO electrode is used as a reference electrode, 1mol/L potassium hydroxide solution is used as electrolyte, and the current density is respectively set to be 10mA/cm 2 、20mA/cm 2 、50mA/cm 2 Testing of Ni 1 Fe 2 Overpotential at different current densities, and a statistical chart of overpotential at different current densities is shown in fig. 7.
Fe is taken as a working electrode, a platinum sheet electrode is taken as a counter electrode, an Hg/HgO electrode is taken as a reference electrode, 1mol/L potassium hydroxide solution is taken as electrolyte, and the current density is respectively set to be 10mA/cm 2 、20mA/cm 2 、50mA/cm 2 And testing overpotential of Fe under different current densities, wherein a statistical chart of the overpotential under different current densities is shown in FIG. 7.
FIG. 8 is Tafel plots for 2 x 1NF-Fe, 3 x 1NF-Fe, 4 x 1NF-Fe, 5 x 1NF-Fe, 8 x 1NF-Fe and Fe.
Figure 9 is the electrochemical impedance spectra of 3 x 1NF-Fe, 4 x 1NF-Fe and 5 x 1 NF-Fe.
As is clear from the results in FIG. 7, the current densities were 10mA/cm, respectively 2 、20mA/cm 2 And 50mA/cm 2 When the overpotential is 198mV, 22mV1 and 238mV corresponding to 4 x 1NF-Fe, Ni 1 Fe 2 The corresponding overpotentials are 274mV, 286mV and 301mV respectively, the overpotentials corresponding to Fe are 429mV, 44mV 6 and 465mV respectively, the lower the overpotential is, the faster the reaction speed is, the less the energy consumption is, and the better the oxygen evolution performance is, so that the oxygen evolution performance of the nickel-iron hydroxide composite material catalyst prepared by taking nickel foam as a nickel source is far better than that of the nickel-iron hydroxide composite material prepared by taking nickel nitrate as the nickel sourceSynthesizing a material catalyst.
From the results of fig. 8, it is understood that the Tafel slope of 4 × 1NF-Fe is 46mV/dec, the Tafel slope indicates the difficulty of the electrochemical reaction, and the smaller the slope, the more likely the electrochemical reaction occurs, and therefore, the nickel-iron hydroxide composite catalyst prepared using nickel foam as a nickel source is excellent in oxygen evolution performance.
From the results of fig. 9, it is clear that 4 × 1NF-Fe has the smallest radius and the smallest charge transfer resistance, and therefore, the molar ratio of 4 × 1NF-Fe is 1: the nickel-iron hydroxide composite catalyst of 2 has better conductivity and better oxygen evolution performance than 3X 1NF-Fe and 5X 1 NF-Fe.
The foregoing is merely a preferred embodiment of the invention, which is intended to be illustrative and not limiting. It will be appreciated by those skilled in the art that many variations, modifications, and equivalents may be made thereto without departing from the spirit and scope of the invention as defined in the claims.
Claims (4)
1. The application of the nickel-iron hydroxide composite catalyst in the water decomposition oxygen analysis reaction is characterized in that the preparation method of the nickel-iron hydroxide composite catalyst comprises the following steps:
s1, adding the pretreated nickel foam into ferric nitrate solution, performing ultrasonic treatment, and after the nickel foam is fully dissolved, obtaining the nickel-iron with the molar ratio of 1: 2, mixing the nickel and iron;
s2, putting the nickel-iron mixed solution into an electrolytic cell, using carbon cloth as a working electrode, and depositing a nickel-iron hydroxide composite material on the carbon cloth by using a cathode deposition method;
s3, washing and naturally airing the deposited carbon cloth to obtain the nickel-iron hydroxide composite catalyst.
2. The use of a nickel iron hydroxide composite catalyst in a water decomposition oxygen evolution reaction according to claim 1, wherein in step S1, the pretreatment of the nickel foam is acid washing, water washing and ethanol washing.
3. The use of a nickel iron hydroxide composite catalyst in water decomposition oxygen evolution reaction as claimed in claim 1, wherein in step S2, the cathode deposition process is performed on the electrochemical workstation of CHI660E, under a three-electrode system, carbon cloth as a working electrode, carbon rod as a counter electrode, and saturated calomel electrode as a reference electrode.
4. The use of a nickel iron hydroxide composite catalyst in the water decomposition oxygen evolution reaction according to claim 1, wherein in the step S2, the deposition temperature is performed at room temperature, and the electrodeposition current density is 20mA/cm 2 The deposition time was 10 min.
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| CN112701306B (en) * | 2021-01-30 | 2022-03-22 | 江西理工大学 | Nickel iron/carbon film-nickel integrated composite electrode and preparation method thereof |
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| KR102608113B1 (en) * | 2022-01-27 | 2023-12-01 | 인하대학교 산학협력단 | Nickel-iron hydroxide using in situ precipitation method, manufacturing method thereof and its application for oxygen generating electrode |
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| CN114808014B (en) * | 2022-05-06 | 2024-03-19 | 安徽工业大学 | Novel multilayer metal hydroxide electrocatalyst, preparation method and application thereof |
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