CN111569884A - Ni-Fe catalyst and preparation method and application thereof - Google Patents
Ni-Fe catalyst and preparation method and application thereof Download PDFInfo
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- CN111569884A CN111569884A CN202010459867.9A CN202010459867A CN111569884A CN 111569884 A CN111569884 A CN 111569884A CN 202010459867 A CN202010459867 A CN 202010459867A CN 111569884 A CN111569884 A CN 111569884A
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- 239000003054 catalyst Substances 0.000 title claims abstract description 40
- 229910003271 Ni-Fe Inorganic materials 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 65
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 32
- 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 abstract description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 20
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 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 12
- 239000008367 deionised water Substances 0.000 claims abstract description 10
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 10
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 9
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 9
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 7
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000758 substrate Substances 0.000 claims abstract description 5
- 229910001030 Iron–nickel alloy Inorganic materials 0.000 claims abstract description 4
- 238000005520 cutting process Methods 0.000 claims abstract description 4
- 235000019441 ethanol Nutrition 0.000 claims abstract description 4
- 239000006260 foam Substances 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000001132 ultrasonic dispersion Methods 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 238000005868 electrolysis reaction Methods 0.000 description 8
- 238000004070 electrodeposition Methods 0.000 description 6
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 4
- 239000001301 oxygen Substances 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- HTXDPTMKBJXEOW-UHFFFAOYSA-N iridium(IV) oxide Inorganic materials O=[Ir]=O HTXDPTMKBJXEOW-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002994 raw material Substances 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
- 238000001228 spectrum Methods 0.000 description 2
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 239000007809 chemical reaction catalyst Substances 0.000 description 1
- 239000010411 electrocatalyst Substances 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005562 fading Methods 0.000 description 1
- 238000000349 field-emission scanning electron micrograph Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000012456 homogeneous solution Substances 0.000 description 1
- 229930195733 hydrocarbon Natural products 0.000 description 1
- 150000002430 hydrocarbons Chemical class 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 229910000510 noble metal Inorganic materials 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 238000012876 topography 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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- 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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- C25B11/031—Porous electrodes
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- C25B—ELECTROLYTIC OR ELECTROPHORETIC PROCESSES FOR THE PRODUCTION OF COMPOUNDS OR NON-METALS; APPARATUS THEREFOR
- C25B11/00—Electrodes; Manufacture thereof not otherwise provided for
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- C25B11/051—Electrodes formed of electrocatalysts on a substrate or carrier
- C25B11/055—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material
- C25B11/057—Electrodes formed of electrocatalysts on a substrate or carrier characterised by the substrate or carrier material consisting of a single element or compound
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- 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
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- C25D3/56—Electroplating: Baths therefor from solutions of alloys
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Abstract
The invention discloses a preparation method of a Ni-Fe catalyst, which comprises the following steps: step 1: cutting the foamed nickel substrate and the carbon paper, sequentially cleaning with acetone, ethanol and deionized water, and drying for later use; step 2: respectively preparing ferric nitrate and nickel nitrate solution for later use; and step 3: respectively adding the ferric nitrate solution and the nickel nitrate solution obtained in the step 2 into ethylene glycol, and then adding deionized water and ammonium fluoride; performing ultrasonic dispersion to form a uniform precursor solution; and 4, step 4: putting clean foam nickel as a cathode and carbon paper as an anode into a precursor solution preheated to 40 ℃, and standing; and 5: fixing the cathode and the anode, applying voltage at two ends by using a voltage-stabilized power supply, and maintaining for 5 min; step 6: and taking down the foamed nickel deposited with the black catalyst, soaking the foamed nickel in absolute ethyl alcohol for cleaning, taking out the foamed nickel and drying the foamed nickel to obtain the NiFe catalyst. The NiFe catalyst prepared by the invention has excellent electrolytic water performance, simple preparation method, low cost and excellent industrialization prospect.
Description
Technical Field
The invention relates to a Ni-Fe-based catalyst with high-efficiency water electrolysis, a preparation method and application thereof.
Background
Electrocatalytic oxidation of water (OER) is a crucial reaction in the field of electrochemistry. The method is an anode reaction for preparing hydrogen by electrolyzing water, preparing hydrocarbon by electrochemically reducing carbon dioxide, and synthesizing ammonia by electrochemically reducing nitrogen. Noble metal catalysts represented by IrO2 are considered to be the best oxygen evolution reaction catalysts, but are expensive and have poor stability in alkaline environments, and are not sufficient to stably operate for a long time under large current electrolysis conditions. In addition, since OER is a four-electron process, kinetics are slow and overpotential is high. Therefore, factors such as energy consumption, production efficiency, cost, etc. limit the wide application of such catalysts.
Disclosure of Invention
The invention aims to solve the problems of high manufacturing cost, high overpotential, difficulty in high-efficiency electrolysis for a long time and the like of the existing electrocatalyst, and provides a high-efficiency water electrolysis catalyst and a preparation method for quickly and efficiently preparing the catalyst at low cost.
In order to achieve the above object, the present invention provides a method for preparing a Ni-Fe catalyst, comprising the steps of:
step 1: cutting a foamed nickel substrate (but not limited to foamed nickel) and carbon paper, sequentially cleaning with acetone, ethanol and deionized water, and drying for later use;
step 2: respectively preparing ferric nitrate and nickel nitrate solution for later use;
and step 3: respectively adding the ferric nitrate solution and the nickel nitrate solution obtained in the step 2 into ethylene glycol, and then adding deionized water and ammonium fluoride; performing ultrasonic dispersion to form a uniform precursor solution;
and 4, step 4: putting clean foam nickel as a cathode and carbon paper as an anode into a precursor solution preheated to 40-45 ℃, and standing;
and 5: fixing the cathode and the anode, applying voltage at two ends by using a voltage-stabilized power supply, and preferably selecting the electrodeposition time to be 5 min;
step 6: and taking down the foamed nickel deposited with the black catalyst, soaking the foamed nickel in absolute ethyl alcohol for cleaning, taking out the foamed nickel and drying the foamed nickel to obtain the NiFe catalyst.
Preferably, the concentrations of the ferric nitrate solution and the nickel nitrate solution in the step 2 are both preferably 305-315 mmol/L.
Preferably, the volume ratio of the ferric nitrate solution, the nickel nitrate solution, the deionized water and the ethylene glycol in the step 3 is 0.7:0.7:0.7:100, and the concentration of the ammonium fluoride in the precursor solution is 1.08-1.12 mg/mL.
The invention also provides the Ni-Fe catalyst prepared by the method.
The invention also provides the application of the Ni-Fe catalyst in the alkaline OER reaction.
The invention has the beneficial effects that:
1. the Ni-Fe-based catalyst is applied to alkaline OER reaction, has excellent performance and can efficiently electrolyze water;
2. OER in 1M KOH of the present invention at 10mA/cm2The overpotential of (a) is only 220-230 mV and 100mA/cm2The overpotential of the electrode is 255-266 mV, and the performance is far superior to that of commercial RuO2，IrO2.
3. The catalyst prepared by the invention shows excellent stability at 100mA/cm2And 500mA/cm2Under the condition, the electrolysis is carried out for 55 hours continuously, and no obvious fading phenomenon is shown.
4. The raw materials for preparing the catalyst are all cheap raw materials, the preparation method is simple and efficient, the electrode preparation efficiency is improved, the electrode preparation cost is greatly reduced, and the method is very beneficial to industrial application.
Drawings
FIG. 1 is an XED pattern of a Ni-Fe catalyst prepared in example 1 of the present invention and an XRD pattern of a foamed nickel substrate;
FIG. 2 is an XPS plot of Ni-Fe catalyst prepared in example 1 of the present invention;
FIG. 3 is an SEM image of Ni-Fe catalyst prepared in example 1 of the present invention and an SEM image of foamed nickel;
FIG. 4 is a CV diagram of Ni-Fe catalyst prepared in example 1 of the present invention before and after electrolysis at constant potential, the electrolyte being 1M KOH, the scanning speed being 5 mV/s;
FIG. 5 is a constant current electrolysis curve in 1M KOH electrolyte for Ni-Fe catalyst prepared in example 1 of the present invention.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1
The embodiment provides a preparation method of a Ni-Fe catalyst, which comprises the following specific steps:
step 1: cutting the foamed nickel substrate and the carbon paper into 0.5cm × 3.0cm, sequentially cleaning with acetone, ethanol and deionized water for 30min, and drying at 60 deg.C for use.
Step 2: 309mmol/L ferric nitrate and nickel nitrate solutions are prepared respectively for standby.
And step 3: respectively adding 0.7ml of ferric nitrate and nickel nitrate solution with the concentrations into 100ml of ethylene glycol, and then adding 0.7ml of deionized water and 0.11g of ammonium fluoride; sonicate for a period of time to form a homogeneous solution.
And 4, step 4: clean foamed nickel is used as a cathode, carbon paper is used as an anode, the clean foamed nickel and the carbon paper are parallel to each other and are spaced by about 2cm, and the working area is 2.0cm multiplied by 0.5 cm. Put into the precursor solution preheated to 40 ℃ and stand for a while.
And 5: the cathode and the anode are kept fixed, voltage of 220V is applied to the two ends by a voltage-stabilized power supply, and the maintaining time is 5 min.
Step 6: and taking down the foamed nickel deposited with the black catalyst, soaking the foamed nickel in absolute ethyl alcohol for a period of time, taking out the foamed nickel, and drying the foamed nickel at the temperature of 60 ℃ to obtain the Ni-Fe catalyst.
As shown in figure 1, the XRD pattern of the catalyst prepared by the method is consistent with that of the foamed nickel, and all the XRD patterns are diffraction peaks of metallic nickel. It is shown that the catalyst material prepared by this method does not have good crystallinity and may be amorphous.
The XPS diagram of the catalyst obtained by electrodeposition is shown in FIG. 2, in which FIG. 2.A is the fine spectrum of Ni 2p and FIG. 2.B is the fine spectrum of Fe 2 p. Showing that Ni and Fe elements are deposited on the surface of the electrode by an electrodeposition method.
The FESEM image of the catalyst prepared by electrodeposition is shown in FIG. 3. Fig. 3.a is a smooth nickel foam surface. FIG. 3.B shows the surface topography after electrodeposition at the same magnification, wherein FIG. 3.C is an enlargement of the generally black area and FIG. 3.D is an enlargement of the generally gray area. Indicating that the forest-shaped catalyst is attached to the surface of the foamed nickel.
The CV curve of the catalyst prepared by electrodeposition is shown in fig. 4. The curve was first cycled 50 more times at a sweep rate of 50mV/s until the curve was essentially constant, and then the curve shown in the figure was obtained at a sweep rate of 5 mV/s. Wherein the automatic iR compensation performed during the test is 75%, and the other 20% is the manual calibration completed after the test is completed. From this curve we can obtain 10mA/cm2Has an overpotential of 223mV, 100mA/cm2The overpotential of (a) is 265mV, 300mA/cm2Has an overpotential of 287mV, 500mA/cm2Over-potential of 301 mV.
As shown in FIG. 5, the prepared electrodes were each charged at 100mA/cm under 1M KOH2And 500mA/cm2The electrode showed excellent stability as can be seen from the figure. In addition, at 100mA/cm2During electrolysis, we collected the gas at random points for a suitable period of time by the drainage method and calculated the mean faradaic efficiency of the electrolytically oxidized water obtained at this electrode to be 98.5%.
Example 2
Example 1 was repeated.
The result shows that the current density of the electrolyzed water for generating oxygen reaches 10mA/cm2Over-potential of 230mV, 100mA/cm2Has an overpotential of 266mV, 300mA/cm2Over-potential of 289 mV.
Example 3
Example 1 was repeated.
The result shows that the current density of the electrolyzed water for generating oxygen reaches 10mA/cm2Has an overpotential of 223mV, 100mA/cm2The overpotential of (a) is 255mV, 300mA/cm2The overpotential of (3) is 261 mV.
Examples 2 and 3 show that the process has good reproducibility.
Example 4
The applied voltage in step 5 of the preparation method was 200V, and the rest was the same as in example 1.
The result shows that the current density of the electrolyzed water for generating oxygen reaches 10mA/cm2Has an overpotential of 223mV, 100mA/cm2The overpotential of (a) is 272mV, 300mA/cm2The overpotential of (2) is 298 mV.
Claims (5)
1. A preparation method of a Ni-Fe catalyst is characterized by comprising the following steps:
step 1: cutting the foamed nickel substrate and the carbon paper, sequentially cleaning with acetone, ethanol and deionized water, and drying for later use;
step 2: respectively preparing ferric nitrate and nickel nitrate solution for later use;
and step 3: respectively adding the ferric nitrate solution and the nickel nitrate solution obtained in the step 2 into ethylene glycol, and then adding deionized water and ammonium fluoride; performing ultrasonic dispersion to form a uniform precursor solution;
and 4, step 4: putting clean foam nickel as a cathode and carbon paper as an anode into a precursor solution preheated to 40-45 ℃, and standing;
and 5: keeping the cathode and the anode fixed, applying voltage at two ends by using a voltage-stabilized power supply, and maintaining for 5 min;
step 6: and taking down the foamed nickel deposited with the black catalyst, soaking the foamed nickel in absolute ethyl alcohol for cleaning, taking out the foamed nickel and drying the foamed nickel to obtain the Ni-Fe catalyst.
2. The method for preparing the Ni-Fe catalyst of claim 1, wherein the concentrations of the ferric nitrate solution and the nickel nitrate solution in the step 2 are both 305 to 315 mmol/L.
3. The method for preparing the NiFe catalyst according to claim 1, wherein the volume ratio of the ferric nitrate solution, the nickel nitrate solution, the deionized water and the ethylene glycol in the step 3 is 0.7:0.7:0.7:100, and the concentration of the ammonium fluoride in the precursor solution is 1.08-1.12 mg/mL.
4. A Ni-Fe catalyst prepared by the process of any one of claims 1 to 3.
5. Use of the Ni-Fe catalyst of claim 4 in basic OER reactions.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| KR20220120843A (en) * | 2021-02-24 | 2022-08-31 | 영남대학교 산학협력단 | Hydrogen generating electrode using nickel-iron alloy and manufacturing method thereof |
| CN115786959A (en) * | 2022-12-22 | 2023-03-14 | 大连理工大学 | Electrochemical preparation method of carbon-supported nickel-iron double-metal hydroxide catalyst for synthesizing ammonia by electro-reduction of nitrate |
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