CN110773171A - Layered nickel-iron-copper hydroxide electrocatalyst and preparation method and application thereof - Google Patents

Layered nickel-iron-copper hydroxide electrocatalyst and preparation method and application thereof Download PDF

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CN110773171A
CN110773171A CN201910961054.7A CN201910961054A CN110773171A CN 110773171 A CN110773171 A CN 110773171A CN 201910961054 A CN201910961054 A CN 201910961054A CN 110773171 A CN110773171 A CN 110773171A
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ldh
layered
deionized water
nife
iron
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不公告发明人
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Hangzhou Jingliang New Material Technology Co Ltd
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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
    • B01J35/33—
    • 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
    • C25B11/091—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
    • C25B11/095—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 at least one of the compounds being organic
    • 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 layered nickel-iron-copper hydroxide electrocatalyst, a preparation method and application thereof. The electrocatalyst takes layered NiFe-LDH as a matrix and is obtained by doping Cu metal ions to modify the electrocatalytic performance of the layered NiFe-LDH. In the layered nickel-iron-copper hydroxide electrocatalyst provided by the invention, the crystal structure and the electronic structure of a NiFe-LDH matrix are changed by doping copper metal ions, so that the physical and chemical properties of the material are regulated and controlled, the overpotential of the catalyst is reduced, and the electrocatalytic performance of the doped layered composite material is greatly improved. Experiments show that the overpotential and the current density of the layered nickel-iron-copper hydroxide electrocatalyst provided by the invention are 10mA cm ‑2From 1.53V to 1.39V. In addition, the preparation method and the experimental operation provided by the invention are simple and beneficial toAnd (4) large-scale production.

Description

Layered nickel-iron-copper hydroxide electrocatalyst and preparation method and application thereof
The invention relates to the technical field of electrocatalysts, in particular to a layered nickel-iron-copper hydroxide electrocatalyst and a preparation method and application thereof.
Background
With the rapid development of the global industrial field, the human society has faced severe environmental pollution and energy crisis, and researchers expect to solve the two problems through various methods, and electrolyze H 2O to H 2And O 2Is a feasible method (2H) for effectively relieving the current crisis 2O→2H 2+O 2). The total water decomposition is a research hotspot all over the world at present, and the total reaction can be divided into two parts of Hydrogen Evolution (HER) and Oxygen Evolution (OER). However, since the OER reaction energy barrier of oxygen evolution is high, the reaction rate of the full reaction is slow, which seriously limits the efficiency of water electrolysis, seeking oneThe electrocatalyst with high OER reaction rate becomes a key problem for effectively improving the full-decomposition water performance. While RuO2 and IrO2 have high electrocatalytic activity, their expensive price is not conducive to large-scale applications. Therefore, the research and development of stable, efficient and low-cost non-noble metal electrocatalysts are urgent. Because the transition metal is relatively cheap, the hydroxide thereof has good electrocatalytic performance, thereby receiving wide attention.
Layered Double Hydroxides (LDHs) are layered stacked structures consisting of an atomic layer of double metal ions and interlayer hydroxide anions in charge balance with the double metal ions, which results in unique physical and chemical properties. Meanwhile, due to the flexible and variable chemical composition, the physical and chemical properties of the double metal hydroxide are changed along with the type and proportion of metals in the LDH system, so that different catalyst performances are obtained. As a typical LDH system, nickel iron double metal hydroxide (NiFe-LDH) nanosheets have a large specific surface area, which helps to increase the active sites of the catalyst and transport of gases and electrolytes at the surface. In order to improve the dynamic performance of the NiFe-LDH system in the electric decomposition of water, Cu metal ions are doped to change the atom and electronic structure of the NiFe-LDH system, regulate and control the physical and chemical characteristics of the system, and reduce the dynamic energy barrier of OER reaction, thereby improving the electrocatalytic performance of the material. And no relevant report is found in the aspects of preparing the nickel-iron-copper hydroxide electrode material by a simple hydrothermal method and applying the nickel-iron-copper hydroxide electrode material to electrocatalytic decomposition of water.
Disclosure of Invention
The invention aims to provide a layered nickel-iron-copper hydroxide electrocatalyst. The electrocatalyst prepared by the invention takes layered nickel-iron double metal hydroxide (NiFe-LDH) as a substrate, and the layered nickel-iron-copper hydroxide (NiFeCu-LDH) is obtained by doping part of copper metal ions. The doped system has the advantages of good conductivity, low overpotential required by reaction and the like, and the catalytic efficiency of the electrocatalyst for decomposing water is obviously improved. Therefore, the layered nickel-iron-copper hydroxide material is prepared and applied to the aspect of water electrolysis, and has better application prospect.
In order to achieve the above object, the present invention adopts the following technical solutions.
(1) Nickel iron double metal hydroxide (NiFe-LDH):
weighing Ni (NO) 3) 2·6H 2O、Fe(NO 3) 3·9H 2O、NH 4OH (30 wt%) and deionized water were added to absolute ethanol and stirred until completely dissolved, yielding a translucent orange-yellow solution. Transferring the solution into a reaction kettle, and setting the temperature and time for hydrothermal reaction. Naturally cooling to room temperature, centrifugally collecting, washing with ethanol and deionized water for several times, and drying the sample to obtain the NiFe-LDH.
(2) Nickel iron copper trimetal hydroxide (NiFeCu-LDH):
weighing Ni (NO) 3) 2·6H 2O、Fe(NO 3) 3·9H 2O and Cu (NO) 3) 2·3H 2And adding absolute ethyl alcohol into the O, stirring, and finally obtaining NiFeCu-LDH, wherein the subsequent steps are the same as the preparation of NiFe-LDH.
The raw material Ni (NO) in the step 1) 3) 2·6H 2O、Fe(NO 3) 3·9H 2O、NH 4The molar ratio of OH (30 wt%) to deionized water was 1:2:6: 8. The synthesis method is a hydrothermal method, and the volume of the semitransparent orange yellow liquid is 8/10 of the capacity of the reaction kettle; the hydrothermal reaction temperature is 140 ℃ and 180 ℃, and the reaction time is 2-3 hours. The magnetic stirring time is 20-30 min; each was washed 3 times with ethanol and deionized water, respectively.
Raw material Ni (NO) in step 2) 3) 2·6H 2O、Fe(NO 3) 3·9H 2O and Cu (NO) 3) 3·9H 2The molar ratio of O is preferably 1:2 (0.1 to 2), more preferably 1:2 (0.5 to 1.0).
The experiment adopts a three-electrode system to carry out electrochemical test, a glassy carbon electrode (with the diameter of 3mm) is taken as a working electrode, a carbon rod is taken as a counter electrode, a saturated calomel solution is taken as a Reference Electrode (RE), an electric 1M KOH is taken as an electrolyte, and the pH value is 13.97. And carrying out electrochemical performance test on the product.
After doping metallic Cu ions in nickel iron double metal hydroxide (NiFe-LDH), the metallic Cu ions will replace part of the metallic Ni and Fe ions. However, since the valence (+1 or +2) of the metal Cu ion is lower than the valence of Ni (+2) and Fe (+3), after Cu is doped, the coordination numbers of Ni and Fe in the system are increased, and the electronic structures of Ni and Fe ions are obviously changed. When it is used as surface active site, its chemical activity is obviously changed. The experiment result shows that the nickel-iron-copper trimetal hydroxide (NiFeCu-LDH) provided by the invention has the over-potential of OER and the current density of 10mA cm in a proper molar ratio range -2When the voltage is reduced from 1.53V to 1.39V, the electrocatalytic performance is improved.
In addition, the method provided by the invention can obtain the layered nickel-iron-aluminum hydroxide electrocatalyst under mild conditions, and has the advantages of simple equipment, easy operation, short preparation period, environmental friendliness and strong repeatability, and can be used for large-scale production.
Drawings
Figure 1 is an XRD pattern of a product prepared by an example of the present invention. In the figure, a is NiFe-LDH, and b is NiFeCu-LDH. It can be seen that the diffraction peak after Cu doping is not obviously changed, which proves that Cu should replace Ni and Fe ions in the system.
FIG. 2 is an SEM image of a product prepared by an example of the present invention. In the figure, a is NiFe-LDH, and b is NiFeCu-LDH. The prepared materials are all nanosheets.
FIG. 3 is an XPS plot of products prepared according to examples of the invention. The figure contains Ni, Fe and Cu elements. By comparison, the coordination numbers of Ni and Fe in the system are increased after Cu doping.
FIG. 4 is a linear sweep voltammogram of a product prepared according to an example of the invention. By comparison, it can be seen that the electrochemical performance of all the NiFeCu-LDH samples after Cu doping is improved to different degrees. The current density was 10mA cm -2When the activity is higher, the NiFeCu-LDH-3 has the lowest potential and the best activity.
Detailed Description
For a further understanding of the invention, reference will now be made to the preferred embodiments of the invention in conjunction with the following examples, but it will be understood that the description is intended to illustrate the features and advantages of the invention further and is not intended to limit the invention.
The invention provides a layered nickel-iron-copper hydroxide electrocatalyst and a preparation method thereof, wherein the layered nickel-iron-copper hydroxide electrocatalyst comprises the following components in parts by weight: with Ni (NO) 3) 2·6H 2O、Fe(NO 3) 3·9H 2O、Cu(NO 3) 2·3H 2O、NH 4Taking a mixed liquid of OH (30 wt%), deionized water and absolute ethyl alcohol as a raw material, carrying out hydrothermal reaction in a reaction kettle, naturally cooling to room temperature, centrifugally collecting, washing with ethyl alcohol and deionized water for several times, and drying a sample to obtain NiFeCu-LDH. In the above scheme, raw material Ni (NO) 3) 2·6H 2O、Fe(NO 3) 3·9H 2O and Cu (NO) 3) 2·3H 2The molar ratio of O is a key technology for the preparation of the invention, and the hydrothermal reaction temperature is an important condition influencing the performance of the final product.
The chemical reagents used in the examples of the present invention are commercially available, as described below with reference to specific examples.
Example 1
Weighing 0.3 mmo lNi (NO) 3) 2·6H 2O，0.6 mmol Fe(NO 3) 3·9H 2O，1.8 mL NH 4OH (30 wt%) and 2.4 mL of deionized water were added to 75 with absolute ethanol and stirred for 30 minutes to dissolve completely to give a translucent orange yellow solution. The solution was transferred to a 100mL reaction vessel and reacted at 180 ℃ for 2 hours. Naturally cooling to room temperature, centrifugally collecting, respectively washing with ethanol and deionized water for 3 times, and drying the sample to obtain the NiFe-LDH-1.
Example 2
0.3 mmol of Ni (NO) was weighed 3) 2·6H 2O，0.6 mmol Fe(NO 3) 3·9H 2O，1.8 mL NH 4OH (30 wt%) and 2.4 mL of deionized water 75 mL was added to absolute ethanol and stirred for 30 minutes to dissolve completely to give a translucent orange yellow solution. The solution was transferred to a 100mL reaction vessel and reacted at 140 ℃ for 2 hours. Naturally cooling to roomAfter warming, centrifugally collecting, respectively washing with ethanol and deionized water for 3 times, and drying the sample to obtain the NiFe-LDH-2.
Example 3
0.3 mmol of Ni (NO) was weighed 3) 2·6H 2O，0.6 mmol Fe(NO 3) 3·9H 2O，1.8 mL NH 4OH (30 wt%), 2.4 mL deionized water and 0.03 mmol Cu (NO) 3) 2·3H 2O was added to 75 mL of absolute ethanol and stirred for 30 minutes until completely dissolved to obtain a translucent orange-yellow solution. The solution was transferred to a 100mL reaction vessel and reacted at 180 ℃ for 2 hours. Naturally cooling to room temperature, centrifugally collecting, respectively washing with ethanol and deionized water for 3 times, and drying the sample to obtain NiFeCu-LDH-1.
Example 4
0.3 mmol of Ni (NO) was weighed 3) 2·6H 2O，0.6 mmol Fe(NO 3) 3·9H 2O，1.8 mL NH 4OH (30 wt%), 2.4 mL deionized water and 0.15 mmol Cu (NO) 3) 2·3H 2O was added to 75 mL of absolute ethanol and stirred for 30 minutes until completely dissolved to obtain a translucent orange-yellow solution. The solution was transferred to a 100mL reaction vessel and reacted at 180 ℃ for 2 hours. Naturally cooling to room temperature, centrifugally collecting, respectively washing with ethanol and deionized water for 3 times, and drying the sample to obtain NiFeCu-LDH-2.
Example 5
0.3 mmol of Ni (NO) was weighed 3) 2·6H 2O，0.6 mmol Fe(NO 3) 3·9H 2O，1.8 mL NH 4OH (30 wt%), 2.4 mL deionized water and 0.21 mmol Cu (NO) 3) 2·3H 2O was added to 75 mL of absolute ethanol and stirred for 30 minutes until completely dissolved to obtain a translucent orange-yellow solution. The solution was transferred to a 100mL reaction vessel and reacted at 180 ℃ for 2 hours. Naturally cooling to room temperature, centrifugally collecting, respectively washing with ethanol and deionized water for 3 times, and drying the sample to obtain NiFeCu-LDH-3.
Example 6
0.3 mmol of Ni (NO) was weighed 3) 2·6H 2O，0.6 mmol Fe(NO 3) 3·9H 2O，1.8 mL NH 4OH (30 wt%), 2.4 mL deionized water and 0.3 mmol Cu (NO) 3) 2·3H 2O was added to 75 mL of absolute ethanol and stirred for 30 minutes until completely dissolved to obtain a translucent orange-yellow solution. The solution was transferred to a 100mL reaction vessel and reacted at 180 ℃ for 2 hours. Naturally cooling to room temperature, centrifugally collecting, respectively washing with ethanol and deionized water for 3 times, and drying the sample to obtain NiFeCu-LDH-4.
Example 7
0.3 mmol of Ni (NO) was weighed 3) 2·6H 2O，0.6 mmol Fe(NO 3) 3·9H 2O，1.8 mL NH 4OH (30 wt%), 2.4 mL deionized water and 0.45 mmol Cu (NO) 3) 2·3H 2O was added to 75 mL of absolute ethanol and stirred for 30 minutes until completely dissolved to obtain a translucent orange-yellow solution. The solution was transferred to a 100mL reaction vessel and reacted at 180 ℃ for 2 hours. Naturally cooling to room temperature, centrifugally collecting, respectively washing with ethanol and deionized water for 3 times, and drying the sample to obtain NiFeCu-LDH-5.
The electrocatalysts prepared in examples 1 to 7 were subjected to an electrolytic water activity test:
the experimental conditions were as follows: the testing of the catalyst was carried out on an electrochemical workstation of type CHI660E chenhua. The electrolytic cell is a self-made three-electrode cell, a glassy carbon electrode (with the diameter of 3mm) is a Working Electrode (WE), a carbon rod is a Counter Electrode (CE), and a saturated calomel solution is used as a Reference Electrode (RE). Before use, the working electrode needs to be polished by 0.05 mm of copper oxide powder, ultrasonically treated in deionized water and ethanol, and then dried. The electrolyte was 1M KOH, pH 13.97. Adding 5 mg catalyst into a mixture of 200 μ L water, 300 μ L ethanol, and 25 μ L Nafion solution (0.5 wt%), performing ultrasonic treatment for 60 min, collecting 5 μ L liquid, transferring onto glassy carbon electrode with electrode loading of 0.707 mg/cm 2And drying at room temperature. The OER activity of the catalyst is researched by a linear voltammetry scanning method (LSV), the measurement range is 0.2V-1V, and the sweep rate is 10 mV/s. The present Reversible Hydrogen Electrode (RHE) for measuring potential vs isCalculated by the following formula: e (rhe) = e (sce) +0.0591PH + 0.24.
The layered nickel-iron-copper hydroxide electrocatalyst, the preparation method and the application thereof provided by the present invention are described in detail above, the principle and the embodiment of the present invention are illustrated herein by using specific examples, the description of the above examples is only for assisting understanding of the method and the core concept of the present invention, it should be noted that, for those skilled in the art, the present invention may be modified and adjusted without departing from the principle of the present invention, and the modified and adjusted aspects also fall within the protection scope of the claims of the present invention.

Claims (6)

1. A layered nickel iron copper hydroxide electrocatalyst characterized by the following:
nickel iron double metal hydroxide (NiFe-LDH): mixing Ni (NO) 3) 2·6H 2O、Fe(NO 3) 3·9H 2O、NH 4Adding OH (30 wt%) and deionized water into absolute ethyl alcohol, stirring until the OH and the deionized water are completely dissolved to obtain a semitransparent orange yellow solution, transferring the solution into a reaction kettle, setting the temperature and the time for hydrothermal reaction, naturally cooling to room temperature, centrifugally collecting, washing with the ethanol and the deionized water for several times respectively, and drying a sample to obtain NiFe-LDH; nickel iron copper trimetal hydroxide (NiFeCu-LDH): mixing Ni (NO) 3) 2·6H 2O、Fe(NO 3) 3·9H 2O and Cu (NO) 3) 2·3H 2And adding absolute ethyl alcohol into the O, stirring, and finally obtaining NiFeCu-LDH, wherein the subsequent steps are the same as the preparation of NiFe-LDH.
2. The method for preparing layered ferronickel double hydroxide electrocatalyst according to claim 1, characterized in that in step (1), raw material Ni (NO) is used 3) 2·6H 2O、Fe(NO 3) 3·9H 2O、NH 4The molar ratio of OH (30 wt%) to deionized water is 1:2:6: 8; the synthesis method is a hydrothermal method, and the volume of the semitransparent orange yellow liquid is 8/10 of the capacity of the reaction kettle; the hydrothermal reactionThe temperature is 140 ℃ and 180 ℃, and the reaction time is 2-3 hours.
3. The method for preparing layered ferronickel bimetallic hydroxide electrocatalyst according to claim 1, characterized in that in step (1) the magnetic stirring time is 20-30 min; each was washed 3 times with ethanol and deionized water, respectively.
4. The method for preparing layered ferronickel double hydroxide electrocatalyst according to claim 1, characterized in that in step (2), raw material Ni (NO) is used 3) 2·6H 2O、Fe(NO 3) 3·9H 2O and Cu (NO) 3) 2·3H 2The molar ratio of O is 1:2 (0.1-1.5).
5. A layered nickel iron copper hydroxide electrocatalyst prepared by the process as claimed in any one of claims 1 to 4.
6. A layered nickel iron copper hydroxide electrocatalyst according to claim 5 applied to electrocatalytic decomposition of water.
CN201910961054.7A 2019-10-11 2019-10-11 Layered nickel-iron-copper hydroxide electrocatalyst and preparation method and application thereof Pending CN110773171A (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111197170A (en) * 2020-02-24 2020-05-26 苏州科技大学 Metal organic framework material/nickel-iron alloy composite electro-catalytic electrode and preparation method and application thereof
CN111420680A (en) * 2020-03-10 2020-07-17 江苏大学 CuS2/Na5NiO4High-efficiency oxygen evolution catalyst and preparation method thereof
CN112239262A (en) * 2020-09-07 2021-01-19 南京智汇环境气象产业研究院有限公司 Preparation method of layered double-metal hydroxide Ni-Fe-LDH electro-catalytic Fenton reaction cathode plate
CN113481535A (en) * 2021-06-18 2021-10-08 常州工学院 Iron-nickel-vanadium double metal hydroxide and preparation method and application thereof
CN113774421A (en) * 2021-08-04 2021-12-10 杭州师范大学 Preparation method of Ni-Cu LDH metal nano-layer material electrocatalyst
CN114395765A (en) * 2022-01-20 2022-04-26 苏州大学张家港工业技术研究院 High-stability alkaline solution hydrogen evolution electrocatalyst and preparation method and application thereof

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111197170A (en) * 2020-02-24 2020-05-26 苏州科技大学 Metal organic framework material/nickel-iron alloy composite electro-catalytic electrode and preparation method and application thereof
CN111420680A (en) * 2020-03-10 2020-07-17 江苏大学 CuS2/Na5NiO4High-efficiency oxygen evolution catalyst and preparation method thereof
CN111420680B (en) * 2020-03-10 2023-02-17 江苏大学 CuS 2 /Na 5 NiO 4 High-efficiency oxygen evolution catalyst and preparation method thereof
CN112239262A (en) * 2020-09-07 2021-01-19 南京智汇环境气象产业研究院有限公司 Preparation method of layered double-metal hydroxide Ni-Fe-LDH electro-catalytic Fenton reaction cathode plate
CN113481535A (en) * 2021-06-18 2021-10-08 常州工学院 Iron-nickel-vanadium double metal hydroxide and preparation method and application thereof
CN113774421A (en) * 2021-08-04 2021-12-10 杭州师范大学 Preparation method of Ni-Cu LDH metal nano-layer material electrocatalyst
CN113774421B (en) * 2021-08-04 2022-09-23 杭州师范大学 Preparation method of Ni-Cu LDH metal nano-layer material electrocatalyst
CN114395765A (en) * 2022-01-20 2022-04-26 苏州大学张家港工业技术研究院 High-stability alkaline solution hydrogen evolution electrocatalyst and preparation method and application thereof

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Application publication date: 20200211