CN112593256A - Core-shell FeOOH @ NiFe LDH electro-catalysis material and preparation method thereof - Google Patents
Core-shell FeOOH @ NiFe LDH electro-catalysis material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of new energy material technology and electrochemical catalysis, and particularly relates to a core-shell FeOOH @ NiFe LDH electro-catalysis material and a preparation method thereof. The invention provides a brand-new core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers, aiming at the problems that the existing NiFe LDH can not simultaneously exert the activities of two active sites of ferronickel and the system environment is complex. The invention also provides a preparation method of the material, which only uses a step-by-step hydrothermal method to complete the differentiation control of the proportion of the ferronickel, accurately constructs a ferronickel heterostructure and can reserve two active sites of FeOOH and NiFe LDH to the maximum extent. The material shows excellent OER activity in 1M KOH and 10 mA-cm‑2The overpotential under (a) is as low as 192 mV. Exhibits excellent electrochemical durability after continuous water electrolysis for 20hAnd (4) sex. The preparation method disclosed by the invention has the advantages of good process stability, low cost, low equipment requirement, excellent catalytic performance and stronger market competitiveness.
Description
Technical Field
The invention belongs to the field of new energy material technology and electrochemical catalysis, and particularly relates to a core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers and a preparation method thereof.
Background
In recent years, the problems of energy shortage and environmental pollution are increasingly prominent, and a solution is urgently needed. Hydrogen energy is considered to be the most promising sustainable energy source to replace traditional fossil fuels due to its high energy density and its environmental friendliness. The hydrogen production by water electrolysis is considered to be a simple and effective large-scale clean hydrogen production technology. However, the half-reaction oxygen evolution reaction (OER reaction) of the electrolyzed water reaction greatly reduces the overall efficiency of water splitting due to its slow kinetics, and therefore the OER reaction occurring at the anode is the rate determining step of water electrolysis. In order to increase the reaction rate, there is a strong need in the industry for efficient catalysts to facilitate this process to save production costs. Currently, ruthenium/iridium-based oxides are considered the best OER catalysts in commercial production, but their scarcity and high cost as noble metals limit their broader production applications. Therefore, the preparation of the low-cost non-noble metal-based catalyst with high efficiency and good stability has important significance.
To date, inexpensive transition metal materials (oxides/(hydroxy) hydroxides) are considered promising alternatives to noble metals under alkaline conditions due to their abundant earth resources and significant OER reaction catalytic properties. The layered double hydroxide is also called hydrotalcite-like, is a novel layered material which is widely regarded and researched in the late eighties, and the molecular composition of the layered double hydroxide is [ M ]2+ 1-x M3+ x(OH)2](An-)x/n·mH2O。
Of the layered double hydroxides, nickel-iron layered double hydroxide (NiFe LDH) has been widely noted for its excellent properties, which are mainly coming fromFrom Ni (OH) in the component2And FeOOH. For example, Chinese patent CN110129815A discloses an electrode material of TM-NiFe LDH, which mainly utilizes Ni active sites to achieve the purpose of enhancing the catalytic performance of OER reaction; for another example, chinese patent CN111686736A discloses a preparation method of NiFe LDH/NF water electrolysis catalyst containing high-activity high-valence iron, which mainly uses iron as active phase to perform catalytic reaction. However, since the distribution of ferronickel in NiFe LDH is very uneven and the relative iron content of NiFe LDH itself is less, a means of simultaneously exerting two active sites in NiFe LDH has not been reported.
In order to obtain a catalyst electrode material with better performance, there are many reports that various components are added, more active sites are introduced, and a very complex bulk phase composition structure is constructed, such as NiFe LDH/Ti disclosed in Chinese patent CN201910635219.13C2/Bi2WO6The nano-sheet array gives full play to the performance advantages of each component. However, synthesis is difficult due to excessive raw materials, and the complex components may interfere with the active sites of NiFe LDH itself, thus being unfavorable for the performance, even leading to inferior catalytic performance to LDH itself. In addition, too complicated system also brings about a problem of poor reproducibility.
So far, no oxygen evolution reaction catalyst electrode material has been disclosed which can simultaneously utilize two active sites of ferronickel and can obtain excellent performance without adding other elements. The difficulty in preparing the material lies in that the proportion of ferronickel needs to be adjusted in a gradient manner, and even segregation of two components is promoted, so that the simultaneous existence of two metal active sites is ensured. The heterogeneous material with multiple active sites has excellent catalytic performance of oxygen evolution reaction.
In order to solve the problems, the invention explains that the differentiation control of the ferronickel proportion is realized through step-by-step hydrothermal treatment, the ferronickel heterostructure material is accurately constructed, the ferronickel proportion difference of two parts of structures reaches a necessary range, so that two active sites of FeOOH and NiFe LDH are reserved to the maximum extent, and the core-shell FeOOH @ NiFe LDH heterogeneous microsphere high-activity electrocatalytic material with vertically staggered wafers is obtained. The preparation method disclosed by the invention has the advantages of good process stability, low raw material cost, low equipment requirement, excellent catalytic performance and stronger market competitiveness.
Disclosure of Invention
The invention provides a brand-new core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers, aiming at the problems that the activity of two active sites cannot be exerted simultaneously and the system environment is complex in the existing NiFe LDH. The core-shell structure microscopically comprises an inner core and an outer shell, and is characterized in that:
(1) the inner core part is constructed by first hydrothermal treatment, is rich in high-activity FeOOH, is smooth and spherical in shape, and contains more than 90% of iron ions in the total molar amount of cations.
(2) The shell part is constructed by secondary hydrothermal treatment, the main component is NiFe LDH nano-sheets, and the molar ratio of Ni to Fe is between 2:1 and 3: 1. The nano sheets are tightly combined outside FeOOH in an in-situ growth mode to form a shell part, and specifically comprise a three-level assembly structure:
a first-stage structure: NiFe LDH nano-sheets with the thickness of 10-50 nanometers;
a second-stage structure: NiFe LDH nanosheet micro-clusters formed by parallelly stacking 5-15 layers of nanosheets;
and (3) a third-level structure: the cross-shaped nanometer flower porous shell is formed by vertically interleaving a plurality of groups of nanometer sheet clusters.
The invention also provides a preparation method of the vertically staggered core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material, the method only uses a step-by-step hydrothermal method to complete the differential control of the proportion of the ferronickel, the ferronickel heterogeneous core-shell structure is accurately constructed, and two catalytic active sites can be reserved to the maximum extent. The preparation method comprises the following steps:
(1) mixing ferric salt, urea and ammonium fluoride according to a molar ratio of 1: 10-30: 2-4, adding a certain amount of deionized water to dissolve the mixture, stirring for 1-4 hours, transferring the solution to a closed reaction kettle, and performing hydrothermal treatment at 100-120 ℃ for 1-3 hours; transferring all products in the reaction kettle to a beaker to obtain a microsphere precursor rich in FeOOH;
(2) mixing nickel salt, urea and ammonium fluoride according to a molar ratio of 1: 10-30: 2-4, adding a certain amount of deionized water to dissolve the nickel salt, urea and ammonium fluoride, and uniformly mixing; mixing the product obtained in the step 1 with the product according to a certain proportion to ensure that the ratio of Fe: the molar ratio of Ni is in the range of 1: 2-1: 3, the mixture is placed in a closed reaction kettle after being uniformly stirred, and the mixture is subjected to hydrothermal treatment for 10-16 hours at the temperature of 100-120 ℃; naturally cooling to room temperature, centrifugally washing the obtained precipitate, and drying at 60-80 ℃ for 12-24 hours to obtain the core-shell FeOOH @ NiFe LDH heterogeneous microsphere electrocatalytic material with vertically staggered wafers.
The ferric salt in the step (1) is one of ferric nitrate and hydrate thereof or ferric chloride and hydrate thereof;
the nickel salt in the step (2) is one of nickel nitrate and a hydrate thereof or nickel chloride and a hydrate thereof.
Has the advantages that: the core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers obtains high-efficiency and stable OER performance in alkaline electrolyte. Aiming at the problem that the traditional NiFe LDH cannot simultaneously utilize two active sites on the premise that the system components are relatively simple, the invention provides a synthesis method which can regulate the nickel-iron ratio only by twice hydrothermal processes and ensure that the two active sites are reserved to the maximum extent and has a simpler process. The method can realize differential control of the proportion of ferronickel by a step-by-step hydrothermal method, accurately constructs a ferronickel heterostructure, can reserve two OER catalytic active sites of nickel and iron to the maximum extent, obtains a vertically staggered core-shell heterogeneous microsphere catalytic material with a wafer intersection angle close to 90 degrees, and has obvious difference from the traditional LDH nano flower-like structure. An inner core rich in FeOOH is hydrothermally constructed for the first time, and has an active site of the FeOOH; the shell of the NiFe LDH is constructed by the secondary hydrothermal process, and the shell has the active sites of the NiFe LDH. The electron transfer exists between the two active sites, and the synergistic effect of the two active sites can greatly improve the electrocatalytic activity of the material. In addition, the heterostructure of the NiFe LDH nano-sheets vertically dispersed on the surface of the FeOOH-rich core provides a large amount of interlayer space, can remarkably increase the surface area of electrochemical activity, provides more channels for rapid transfer of ions and electrons and smooth escape of oxygen, can also enhance the mechanical stability and electrochemical stability of the material, and ensures that the material can be subjected to catalytic electrolysis for a long time under high potential, thereby promoting the activity and stability of OER.
Electrochemical tests show that the core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers shows excellent OER activity in 1M KOH electrolyte and 10 mA-cm-2The overpotential of the current density can reach 192mV at the lowest. After continuous water electrolysis for 20h, the catalyst showed excellent electrochemical durability with almost negligible voltage change.
Drawings
FIG. 1 is an X-ray diffraction pattern of the core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers in example 1;
FIG. 2 is a scanning electron micrograph of the core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers in example 1.
Detailed Description
The invention is explained in more detail below with reference to the figures and examples:
example 1
1.8mmol of ferric nitrate nonahydrate solid, 42.7mmol of urea solid and 6.7mmol of ammonium fluoride solid are weighed and dissolved in 22 ml of deionized water, and after the solutions are fully dissolved, a magnetic stirrer is used for stirring for 2 hours, and the solution is filled into a high-pressure lining. The inner liner was placed in a stainless steel reactor vessel, sealed, placed in an oven at 100 ℃ for 2 hours at constant temperature, then allowed to cool naturally to room temperature, and all the contents of the reactor were transferred to a beaker and labeled as solution A.
3.6mmol of nickel nitrate hexahydrate solid, 85.3mmol of urea solid and 13.4mmol of ammonium fluoride solid are weighed and dissolved in 44 ml of deionized water, and stirred for 30 minutes by using a magnetic stirrer to be fully dissolved, and the solution is marked as liquid B.
And dropwise adding the uniformly mixed solution B into the solution A while stirring, completely transferring, stirring for 30 minutes by using a magnetic stirrer to uniformly mix, and filling into a high pressure tank. And (3) putting the lining into a stainless steel reaction kettle container, sealing, putting the stainless steel reaction kettle container into an oven at the temperature of 100 ℃, keeping the temperature for 10 hours, and naturally cooling to room temperature to obtain a reddish brown precipitate. Washing the obtained precipitate with deionized water for 5 times, and drying in an oven at 60 ℃ for 12 hours to obtain the core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers.
At 10 and 100mA cm-2The overpotential is as low as 192 and 347 mV. And after continuous water electrolysis for 20h, excellent electrochemical durability is shown.
Example 2
1.2mmol of ferric nitrate nonahydrate solid, 12mmol of urea solid and 2.4mmol of ammonium fluoride solid are weighed and dissolved in 22 ml of deionized water, and after the solutions are fully dissolved, a magnetic stirrer is used for stirring for 1 hour, and the solution is filled into a high-pressure lining. The inner liner was placed in a stainless steel reactor vessel, sealed, placed in an oven at 100 ℃ for 1 hour at constant temperature, then allowed to cool naturally to room temperature, and all the contents of the reactor were transferred to a beaker and labeled as liquid A.
3.6mmol of nickel nitrate hexahydrate solid, 36mmol of urea solid and 7.2mmol of ammonium fluoride solid were weighed out and dissolved in 44 ml of deionized water, and stirred for 30 minutes by using a magnetic stirrer to be fully dissolved, and the solution was marked as liquid B.
And dropwise adding the uniformly mixed solution B into the solution A while stirring, completely transferring, stirring for 30 minutes by using a magnetic stirrer to uniformly mix, and filling into a high pressure tank. And (3) putting the lining into a stainless steel reaction kettle container, sealing, putting the stainless steel reaction kettle container into an oven at the temperature of 100 ℃, keeping the temperature for 12 hours, and naturally cooling to room temperature to obtain a dark yellow precipitate. Washing the obtained precipitate with deionized water for 5 times, and drying in an oven at 60 ℃ for 12 hours to obtain the core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers.
At 10mA cm-2Under conditions of (a) is lower than the NiFe LDH of the same starting material. And after continuous water electrolysis for 20h, excellent electrochemical durability is shown.
Example 3
Weighing 2mmol ferric nitrate nonahydrate solid, 60mmol urea solid and 8mmol ammonium fluoride solid, dissolving in 22 ml deionized water, stirring for 4 hours by using a magnetic stirrer after fully dissolving, and filling into a high-pressure lining. The inner liner was placed in a stainless steel reactor vessel, sealed, placed in an oven at 120 ℃ for 3 hours at constant temperature, then allowed to cool naturally to room temperature, and all the contents of the reactor were transferred to a beaker and labeled as solution A.
5mmol of nickel nitrate hexahydrate solid, 150mmol of urea solid and 20mmol of ammonium fluoride solid are weighed and dissolved in 44 ml of deionized water, and the solution is stirred for 30 minutes by using a magnetic stirrer to be fully dissolved and marked as solution B.
And dropwise adding the uniformly mixed solution B into the solution A while stirring, completely transferring, stirring for 30 minutes by using a magnetic stirrer to uniformly mix, and filling into a high pressure tank. And (3) placing the lining into a stainless steel reaction kettle container, sealing, placing in an oven at 120 ℃, keeping the temperature for 16 hours, and naturally cooling to room temperature to obtain brick red precipitate. Washing the obtained precipitate with deionized water for 5 times, and drying in an oven at 60 ℃ for 12 hours to obtain the core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers.
At 10mA cm-2Under conditions of (a) is lower than the NiFe LDH of the same starting material. And after continuous water electrolysis for 20h, excellent electrochemical durability is shown.
Example 4
1mmol of ferric nitrate nonahydrate solid, 15mmol of urea solid and 3mmol of ammonium fluoride solid are weighed and dissolved in 22 ml of deionized water, and after the solutions are fully dissolved, the mixture is stirred for 2 hours by using a magnetic stirrer and then is filled into a high-pressure lining. The inner liner was placed in a stainless steel reactor vessel, sealed, placed in an oven at 110 ℃ for 2 hours at constant temperature, then allowed to cool naturally to room temperature, and all the contents of the reactor were transferred to a beaker and labeled as solution A.
2.3mmol of nickel nitrate hexahydrate solid, 34.5mmol of urea solid and 6.9mmol of ammonium fluoride solid were weighed out and dissolved in 44 ml of deionized water, and the solution was stirred for 30 minutes by a magnetic stirrer to be fully dissolved and labeled as solution B.
And dropwise adding the uniformly mixed solution B into the solution A while stirring, completely transferring, stirring for 30 minutes by using a magnetic stirrer to uniformly mix, and filling into a high pressure tank. And (3) putting the lining into a stainless steel reaction kettle container, sealing, putting the stainless steel reaction kettle container into an oven at the temperature of 110 ℃, keeping the temperature for 12 hours, and naturally cooling to room temperature to obtain a reddish brown precipitate. Washing the obtained precipitate with deionized water for 5 times, and drying in an oven at 60 ℃ for 12 hours to obtain the core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers.
At 10mA cm-2Under conditions of (a) is lower than the NiFe LDH of the same starting material. And after continuous water electrolysis for 20h, excellent electrochemical durability is shown.
The working electrode surface modification method comprises the following steps:
firstly, polishing a glassy carbon electrode with the diameter of 3mm to a mirror surface in a special grinding tool, and cleaning the electrode by using ultrapure water. Weighing 4.00 mg of the material and 1.00 mg of conductive carbon black into a penicillin bottle, adding 1 ml of ethanol, performing ultrasonic treatment for 30 minutes, adding 50 microliters of 5 wt% naphthol solution, performing ultrasonic treatment for 30 minutes, using a liquid transfer gun to drop 1 microliter of ink onto a glassy carbon electrode, naturally drying at room temperature, and repeatedly dropping for 5 times.
The core-shell FeOOH @ NiFe LDH heterogeneous catalytic material with vertically staggered wafers is characterized by using a cyclic voltammetry method: a three-electrode system is adopted, a working electrode is a modified glassy carbon electrode, a counter electrode is a 2-by-2-centimeter platinum mesh electrode, a reference electrode is a mercury/mercury oxide electrode, and electrolyte is 1M KOH solution. The experimental test temperature is 25 +/-1 ℃. Electrochemical testing was performed on the Shanghai Chenghua CHI 660E workstation.
Linear sweep voltammetry test: the scanning rate is 10 mV.s-1The electrode potential was iR corrected and converted to the electrode potential for the Reversible Hydrogen Electrode (RHE).
The stability test adopts a timing potential test method: the fixed current density is 10mA cm-2。
Testing of electrochemical impedance: setting the corresponding parameters as follows: 0.01-106The frequency of Hz is changed, the amplitude is 5mV, and the open-circuit voltage is kept under the condition of direct-current voltage.
The core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers described in the embodiment 1 is subjected to structural characterization:
in the XRD diffraction pattern of FIG. 1, the characteristic peaks of FeOOH and NiFe LDH appear simultaneously. The conclusion that the core-shell FeOOH @ NiFe LDH heterogeneous microsphere catalytic material with vertically staggered wafers is successfully synthesized can be obtained.
In the scanning electron micrograph of fig. 2, smooth FeOOH spheres can be seen, constituting the inner core of the material; the NiFe LDH grown in situ outside the FeOOH comprises a tertiary structure, respectively
A first-stage structure: NiFe LDH nano-sheets with the thickness of 20-50 nm;
a second-stage structure: NiFe LDH nano-sheet micro-clusters formed by parallelly stacking 5-15 layers of nano-sheets;
and (3) a third-level structure: the cross nanometer flower-shaped shell is formed by vertically interleaving a plurality of groups of nanometer sheet clusters.
The above specific examples are merely illustrative of the present invention and are not intended to limit the present invention. Variations, modifications, and alterations without departing from the general route and embodiments of the invention are intended to be within the scope of the invention.
Claims (3)
1. The core-shell FeOOH @ NiFe LDH electrocatalytic material is characterized in that the core is a microsphere rich in high-activity FeOOH constructed by first hydrothermal treatment, the shell is a NiFe LDH three-level assembled nano structure constructed by second hydrothermal treatment, and the average Ni ratio of the shell to the core is as follows: the difference in Fe molar ratio is higher than 2.8.
2. The core-shell FeOOH @ NiFe LDH electrocatalytic material as claimed in claim 1, wherein the NiFe LDH shell comprises three-level assembly structures of basic nanosheets, nanosheet nanoclusters and vertically staggered cross-shaped nanoflower shells, the first-level structure is NiFe LDH nanosheets with the thickness of 10-50 nanometers, the second-level structure is NiFe LDH nanosheet nanoclusters formed by parallelly stacking 5-15 layers of nanosheets, and the third-level structure is a cross-shaped nanoflower porous structure formed by vertically staggering multiple groups of nanosheet nanoclusters.
3. A preparation method of the core-shell FeOOH @ NiFe LDH electrocatalytic material is used for preparing the core-shell FeOOH @ NiFe LDH electrocatalytic material as described in any one of claims 1-2, and is characterized by comprising the following steps:
(1) mixing ferric salt, urea and ammonium fluoride according to a molar ratio of 1: 10-30: 2-4, adding a certain amount of deionized water to dissolve the ferric salt, urea and ammonium fluoride, stirring for 1-4 h, transferring the solution into a closed reaction kettle, and performing hydrothermal treatment at 100-120 ℃ for 1-3 h to obtain a microsphere precursor rich in FeOOH;
(2) mixing nickel salt, urea and ammonium fluoride according to a molar ratio of 1: 10-30: 2-4, adding a certain amount of deionized water to dissolve the nickel salt, urea and ammonium fluoride, and uniformly mixing; mixing the product of the step (1) with the product according to a certain proportion, so that the ratio of Fe: the molar ratio of Ni is in the range of 1: 2-1: 3, the mixture is placed in a closed reaction kettle after being uniformly stirred, and hydrothermal treatment is carried out for 10-16 hours at the temperature of 100-120 ℃; naturally cooling to room temperature, centrifugally washing and drying the obtained precipitate to obtain a vertically staggered core-shell FeOOH @ NiFe LDH heterogeneous microsphere electrocatalytic material with a wafer;
the ferric salt in the step (1) is one of ferric nitrate and hydrate thereof or ferric chloride and hydrate thereof;
the nickel salt in the step (2) is one of nickel nitrate and a hydrate thereof or nickel chloride and a hydrate thereof.
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| CN113529120A (en) * | 2021-08-11 | 2021-10-22 | 中国石油大学(北京) | Transition metal sulfide composite electrode, preparation method and application thereof |
| CN114277400A (en) * | 2021-12-06 | 2022-04-05 | 江苏大学 | Self-source etching preparation method and application of nickel-doped iron oxyhydroxide self-supporting electrode material |
| CN118186484A (en) * | 2024-05-16 | 2024-06-14 | 太原理工大学 | Ir-Ni (OH)2FeOOH@NF iridium-based catalyst and preparation method and application thereof |
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