CN114016078A - Nickel-iron alloy/carbon electrocatalytic material, preparation method and application thereof - Google Patents
Nickel-iron alloy/carbon electrocatalytic material, preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a nickel-iron alloy/carbon electro-catalysis material, a preparation method and application thereof, belonging to the technical field of synthesis and electrochemistry of new energy nano materials. The electrocatalytic material is a two-dimensional nanosheet structure of hexagonal nickel-iron alloy particles or cubic nickel-iron alloy particles loaded on carbon. The preparation method utilizes low-temperature plasma to treat Ni3And (3) synthesizing hexagonal phase ferronickel/carbon nanosheets or cubic phase ferronickel/carbon nanosheets by Fe-LDH. Compared with the prior art, the preparation method disclosed by the invention is simple in process, and the obtained catalytic material is high in activity and good in stability, can be used in the field of electrocatalytic full-hydrolysis, and has a good application prospect.
Description
Technical Field
The invention discloses a nickel-iron alloy/carbon electro-catalysis material, a preparation method and application thereof, and belongs to the technical field of synthesis and electrochemistry of new energy nano materials.
Background
The imminent exhaustion of fossil fuels and the numerous environmental problems that arise from them force mankind to develop clean and sustainable energy sources. Hydrogen gas with high energy density plays a key role in achieving carbon neutralization and environmental friendliness, and is considered as an ideal renewable energy source. Compared with the traditional hydrogen production route by reforming coal and natural gas, the electrochemical hydrogen production by water splitting is a clean and feasible technology. However, electrocatalytic analysisThe practical application of the hydrogen reaction (HER) remains challenging, mainly due to the large overpotential of the overall thermodynamic process resulting from the slow kinetics of the four electron Oxygen Evolution Reaction (OER). Therefore, the development of a high-performance water-decomposition electrocatalyst is imperative. In general, the noble metal materials Pt and IrO2/RuO2Are the benchmark catalysts for HER and OER, respectively, but their practical feasibility is limited by the high cost and extreme scarcity. Researchers have focused on exploring earth's abundant and efficient electrocatalysts, of which transition metal-based catalysts (e.g., Fe, Co, Ni, and Mo) have proven promising. Although great progress has been made in non-noble metal-based catalysts, their catalytic performance is far from adequate in terms of activity and stability.
NiFe alloys are among the most effective catalysts for improving HER and OER performance due to their low cost and inherent catalytic activity. Heretofore, various strategies such as morphology and electronic structure modulation have been used to improve the catalytic performance. In addition, the atomic arrangement and the electronic structure are adjusted through the regulation and control of the crystal phase, and the method is an effective means for regulating the catalytic activity of the catalyst. For example, Wang and coworkers demonstrated that hcp Ni (NiFe) decorated carbon shells exhibited higher OER performance than the fcc counterpart, resulting from high temperature pyrolysis of the corresponding MOFs (metal-organic frameworks). Therefore, the realization of the crystal structure control of the NiFe alloy is hopeful to obtain a high-efficiency catalyst. However, due to the synthetic challenges, it is not easy to control the crystalline phase of NiFe alloy nanocatalysts under mild conditions.
Therefore, the research of preparing novel materials with higher catalytic activity and good cycling stability as electrochemical catalytic total hydrolysis materials is a challenging new subject in the field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a nickel-iron alloy/carbon electrocatalytic material. The material can solve the problems of high overpotential, low catalytic activity and the like of the existing electrocatalytic total hydrolysis.
The invention further aims to provide a preparation method of the iron alloy/carbon electro-catalytic material.
A further technical task of the present invention is to provide the use of the above-mentioned ferroalloy/carbon electrocatalytic material.
The nickel-iron alloy/carbon electro-catalysis material is a two-dimensional nanosheet structure with hexagonal nickel-iron alloy particles or cubic nickel-iron alloy particles loaded on carbon.
The preparation method of the nickel-iron alloy/carbon electro-catalysis material is characterized by comprising the following steps:
low temperature plasma treatment of Ni3Synthesizing hexagonal-phase ferronickel alloy/carbon nanosheets from Fe-LDH through in-situ topological reductors;
or: low temperature plasma treatment of Ni3And synthesizing cubic-phase nickel-iron alloy/carbon nanosheets by Fe-LDH.
Preferably, the plasma is methane, ethane, acetylene or ethylene.
Preferably, the Ni is3The preparation of Fe-LDH comprises: ni (NO)3)2·6H2O、Fe(NO3)2·9H2Dissolving O and urea in deionized water, heating in an oven at 100-200 deg.C (preferably 100-150 deg.C) for 10-15h (preferably 11-13h), cooling to room temperature, separating, and purifying to obtain Ni3Fe-LDH。
Preferably, Ni (NO)3)2·6H2O、Fe(NO3)2·9H2The molar ratio of O to urea is (0.1-1): (1-5), particularly preferably (0.5-0.7): (0.1-0.3): (1-3).
Preferably, Ni is treated with plasma3The conditions for preparing the hexagonal-phase nickel-iron alloy/carbon nanosheet by Fe-LDH are as follows: the power is 100-500W (400-500W is particularly preferred), the treatment time is 0-15min (10-15 min is particularly preferred), and the pressure is 10-50Pa (20-30 Pa is particularly preferred). Under this condition, Ni3Fe-LDH nano-sheets can be converted into hexagonal-phase ferronickel/carbon porous nano-sheets, and the obtained product is marked as hcp-Ni3Fe/C。
Preferably, Ni is treated with plasma3The conditions for preparing the cubic phase ferronickel alloy/carbon nanosheet by Fe-LDH are as follows: the power is 100-500W (especially 400-500W), and the processing time is 15-30min (especiallyPreferably 25 to 30min) and a pressure of 10 to 50Pa (particularly preferably 20 to 30 Pa). Under this condition, Ni3Fe-LDH nano-sheets are converted into cubic phase ferronickel alloy/carbon porous nano-sheets. The resulting product was noted as fcc-Ni3Fe/C。
The two-dimensional nanosheet structure material with the hexagonal nickel-iron alloy particles or the cubic nickel-iron alloy particles loaded on carbon can be applied to the field of electrochemical catalysis and full-hydrolysis.
Compared with the prior art, the nickel-iron alloy/carbon electrocatalytic material, the preparation method and the application thereof have the following outstanding beneficial effects:
first, the invention prepares Ni by hydrothermal method3Fe-LDH nanosheets, then Ni-mediated by a simple plasma-assisted strategy3Synthesizing hexagonal nickel-iron alloy/carbon porous nanosheets by in-situ topological reduction of Fe-LDH nanosheets; in addition, by adjusting the plasma treatment time, hexagonal nickel-iron alloy/carbon (hcp-Ni) can be achieved3Fe/C) to cubic ferronickel/carbon (fcc-Ni)3Fe/C) provides a new way for preparing non-noble metal-based catalysts with different crystal phases.
The preparation method adopts methane, ethane, acetylene or ethylene plasma, and high-energy species (free electrons, H, CH) in a plasma system3、CH2Excited atoms, ionized atoms/molecules, and free radicals) into the atmosphere of Ni3OH radicals of Fe-LDH lead to the reconstruction of its surface structure. The arrangement of Ni and Fe atoms is kept unchanged by the mild reaction condition of the low-temperature plasma, thereby realizing the metastable hcp-Ni3And (4) synthesizing Fe/C. Thus, hexagonal phase Ni3Fe-LDH passes through CH in a short time (15min)4Plasma in-situ topological reduction to form hcp-Ni3Fe/C. Metastable hcp-Ni with increasing plasma processing time3Conversion of Fe/C to thermodynamically stable fcc-Ni3Fe/C。
(III) the hcp-Ni obtained3Fe/C and fcc-Ni3The Fe/C can be used in the field of electrocatalytic full-hydrolysis, and has high activity and good stability. And fcc-Ni3Fe/C ratio, hcp-Ni prepared3The Fe/C catalyst showed significantly enhanced activity at 10mA cm-2The overpotential for the Hydrogen Evolution Reaction (HER) was 70mV and the transition point for the Oxygen Evolution Reaction (OER) was 201mV at the current density of (1). Furthermore, hcp-Ni3When Fe/C is respectively used as a cathode and an anode to assemble a full cell for full water decomposition, the catalyst is 10mAcm-2The overpotential at current density is only 1.54V. Theoretical calculations further indicate that hcp-Ni3Fe is energetically favorable for H2Adsorption and dissociation of O molecules.
Drawings
FIG. 1 shows hcp-Ni prepared in examples 2 and 33Fe/C and fcc-Ni3Fe/C synthesis schematic and TEM and HRTEM images;
FIG. 2 shows hcp-Ni prepared in examples 2 and 33Fe/C and fcc-Ni3XRD spectrum and XPS spectrum of Fe/C;
FIG. 3 is Ni prepared in examples 1, 2 and 33Fe-LDH、hcp-Ni3Fe/C and fcc-Ni3The electrocatalytic oxygen evolution performance of Fe/C is compared with that of the Fe/C;
FIG. 4 is Ni prepared in examples 1, 2 and 33Fe-LDH、hcp-Ni3Fe/C and fcc-Ni3The electro-catalytic hydrogen evolution performance of Fe/C is compared with that of the Fe/C;
FIG. 5 shows hcp-Ni prepared in example 33Fe/C electrocatalytic hydrolysis schematic diagram;
FIG. 6 is hcp-Ni prepared in example 33An electrocatalytic full-hydrolysis performance diagram of Fe/C.
Detailed Description
The invention is further described with reference to the drawings and the following detailed description, but is not intended to be limited thereto.
Unless otherwise specified, the contents of the respective components used below are mass% contents.
The first embodiment is as follows:
Ni3preparation of Fe-LDH: weighing 0.6 mmoleNi (NO)3)2·6H2O、0.2mmol Fe(NO3)2·9H2O and 2mmol urea were dissolved in 30mL deionized water. Transferring the uniform solution into a high-pressure autoclave, heating in a 120 ℃ oven for 12h,after cooling to room temperature, the samples were collected by centrifugation and washed several times with deionized water and ethanol. Preparation of Ni3Fe-LDH。
Example two
Preparing hexagonal phase ferronickel alloy/carbon: ni produced by methane plasma treatment3Fe-LDH: the power was 450W, the treatment time 15min and the pressure 25 Pa. Mixing Ni prepared in the above step3And converting the Fe-LDH nano sheets into hexagonal phase ferronickel alloy/carbon porous nano sheets. The resulting product was designated hcp-Ni3Fe/C。
EXAMPLE III
Preparing cubic phase ferronickel alloy/carbon: ni produced by methane plasma treatment3Fe-LDH: the power was 450W, the treatment time was 30min and the pressure was 25 Pa. Ni to be prepared3Fe-LDH nano-sheets are converted into cubic phase ferronickel alloy/carbon porous nano-sheets. The resulting product was noted as fcc-Ni3Fe/C。
FIG. 1(a) is hcp-Ni synthesized in examples 2 and 33Fe/C and fcc-Ni3Schematic diagram of Fe/C synthesis, (b, C) hcp-Ni3TEM and HRTEM images of Fe/C, (d, e) fcc-Ni3TEM and HRTEM images of Fe/C. TEM picture display hcp-Ni3Fe/C nanoplatelets consist of a large number of small nanoparticles separated by ultra-thin carbon layers. Abundant active sites are exposed from abundant pores, so that the nano-catalyst is convenient to directly contact with electrolyte, and the charge transfer and mass diffusion can be accelerated, thereby improving the electrocatalysis performance.
FIG. 2 shows hcp-Ni synthesized in examples 2 and 3, respectively3Fe/C and fcc-Ni3XRD spectrum of Fe/C shows that the hcp-Ni is successfully prepared by methane plasma treatment3Fe/C and fcc-Ni3Fe/C. Examples 2 and 3 Synthesis of hcp-Ni3Fe/C and fcc-Ni3XPS spectra of Fe/C (b) high resolution Ni 2p, (C) Fe 2p, (d) C1 s. The XPS spectra show that both Ni and Fe are in the metallic state in both samples.
FIG. 3(a) hcp-Ni prepared in examples 1, 2 and 33Fe/C、fcc-Ni3Fe/C、Ni3Fe-LDH, commercial IrO2And carbon paper at 10mV s-1LSV curve at scan rateThe results show that3Fe/C、Ni3Fe-LDH, carbon paper and IrO2In contrast, hcp-Ni3The Fe/C electrode has the lowest initial potential and the highest current density. (b) hcp-Ni prepared in examples 1, 2 and 33Fe/C、fcc-Ni3Fe/C、Ni3Fe-LDH and IrO2Tafel curve of (1), hcp-Ni3Tafel slope of Fe/C electrode is minimal (55mV dec)-1) Less than fcc-Ni3Fe/C(72mV dec-1)、Ni3Fe-LDH(82mV dec-1) And IrO2(70mV dec-1) Indicating hcp-Ni3The best OER kinetic activity of Fe/C electrode. (c) hcp-Ni prepared in examples 1, 2 and 33Fe/C、fcc-Ni3Fe/C and Ni3Curve of current density versus scan rate for Fe-LDH, hcp-Ni3C of Fe/C electrodedlIs 14.4mF cm-2Significantly greater than fcc-Ni3Fe/C(5.5mF cm-2) And Ni3Fe-LDH(6.4mF cm-2). The results show that hcp-Ni3Fe/C has the largest electrochemically active area and exposes more active sites, thereby greatly promoting good OER performance. (d) hcp-Ni prepared in examples 1, 2 and 33Fe/C、fcc-Ni3Fe/C、Ni3EIS impedance Curve of Fe-LDH, hcp-Ni3The Rct of Fe/C was the smallest and 15.9. omega. The results show that hcp-Ni3The rate of electron transfer between the Fe/C catalyst and the electrolyte interface is fastest. (e) hcp-Ni prepared in example 23The results of in-situ Raman spectra of the Fe/C catalyst at different OER potentials show that hcp-Ni is subjected to the OER condition in an alkaline medium3The Fe surface is oxidized to γ -NiOOH. (f) A comparison of the OER properties of the related electrocatalysts recently reported shows hcp-Ni3The activity of Fe/C is also superior to most of the reported electrocatalysts of the same type.
Figure 4 is the HER performance of the catalyst. (a) hcp-Ni prepared in examples 1, 2 and 33Fe/C、fcc-Ni3Fe/C、Ni3Fe-LDH, Pt/C and carbon paper at 10 mV.s-1Lower LSV curve, hcp-Ni3Fe/C up to 10mA cm-2Has an overpotential of 70mV, which is comparable to Pt/C, lower than fcc-Ni3Fe/C(114mV) and Ni3Fe-LDH (272mV), showed better HER activity. (b) hcp-Ni prepared in examples 1, 2 and 33Fe/C、fcc-Ni3Fe/C、Ni3Tafel curves for Fe-LDH and Pt/C, hcp-Ni3Tafel slope of the Fe/C sample was 78mV dec-1Less than fcc-Ni3Fe/C(85mV dec-1)、Ni3Fe-LDH(102mV dec-1) And commercial Pt/C (82mV dec)-1) Showing its optimal electron transfer and HER kinetic capability. (c) hcp-Ni prepared in examples 1, 2 and 33Fe/C、fcc-Ni3Fe/C and Ni3Current Density vs. Scan Rate Curve, fcc-Ni, for Fe-LDH3Fe/C and Ni3C of Fe-LDHdlThe values were 3.6mF cm respectively-2And 2.4mF cm-2，hcp-Ni3C of Fe/C catalystdlThe value was 6.3mF cm-2The catalyst studied is the highest performance. (d) hcp-Ni prepared in examples 2 and 33Fe/C and fcc-Ni3The relative energy map of Fe/C and the calculation result show that the Fe/C and fcc-Ni are similar to those of fcc-Ni3Fe vs. hcp-Ni3Fe has faster kinetics of water dissociation and better HER activity.
FIG. 6 hcp-Ni synthesized as in example 23And the Fe/C is an anode and a cathode to assemble an alkaline electrolytic cell, and the electrolysis of water is catalyzed in a 1M KOH electrolyte. (a) hcp-Ni in two-electrode system3Fe/C||hcp-Ni3Fe/C electrode and Pt/C IrO2LSV curve of electrode at 1M KOH; as shown in FIG. 6a, hcp-Ni3Fe/C can reach 10mA cm only by 1.54V-2This is much lower than Pt/C IrO2(1.66V). (b) hcp-Ni3I-t curves at 10mA cm for Fe/C catalysts-2Under the condition of (2), the electrolytic cell can keep stable water decomposition for as long as 36 h.
The foregoing is directed to preferred embodiments of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow. However, any simple modification, equivalent change and modification of the above embodiments according to the technical essence of the present invention are within the protection scope of the technical solution of the present invention.
Claims (7)
1. A nickel-iron alloy/carbon electrocatalytic material is characterized in that: the material is a two-dimensional nanosheet structure of hexagonal nickel-iron alloy particles or cubic nickel-iron alloy particles loaded on carbon.
2. A preparation method of a nickel-iron alloy/carbon electrocatalytic material is characterized by comprising the following steps:
low temperature plasma treatment of Ni3Synthesizing hexagonal-phase ferronickel alloy/carbon nanosheets from Fe-LDH through in-situ topological reductors;
or:
low temperature plasma treatment of Ni3And synthesizing cubic-phase nickel-iron alloy/carbon nanosheets by Fe-LDH.
3. The method for preparing a ferro-nickel alloy/carbon electrocatalytic material as set forth in claim 2, wherein: the plasma is methane, ethane, acetylene or ethylene.
4. The method of preparing a ferro-nickel/carbon electrocatalytic material as set forth in claim 2, wherein Ni is selected from the group consisting of Ni, fe, Ni, si, Ni, si, Ni, or Ni, si, Ni, or a si, Ni3The preparation of Fe-LDH comprises: ni (NO)3)2·6H2O、Fe(NO3)2·9H2Dissolving O and urea in deionized water, heating in 100-200 deg.C oven for 10-15 hr, cooling to room temperature, separating, and purifying to obtain Ni3Fe-LDH。
5. The method for preparing a ferro-nickel alloy/carbon electrocatalytic material as set forth in claim 2, wherein: treatment of Ni with plasma3The conditions for preparing the hexagonal-phase nickel-iron alloy/carbon nanosheet by Fe-LDH are as follows: the power is 100-500W, the processing time is 0-15min, and the pressure is 10-50 Pa.
6. The method of making a nickel-iron alloy/carbon electrocatalytic material as set forth in claim 2Method characterized by treating Ni with plasma3The conditions for preparing the cubic phase ferronickel alloy/carbon nanosheet by Fe-LDH are as follows: the power is 100-500W, the processing time is 15-30min, and the pressure is 10-50 Pa.
7. Use of the ferronickel/carbon electrocatalytic material of claim 1 in total hydrolysis.
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| CN106381506A (en) * | 2016-10-18 | 2017-02-08 | 西安交通大学 | Preparation method of layered ferronickel hydroxide electrode |
| CN109772336A (en) * | 2019-03-05 | 2019-05-21 | 浙江工业大学 | A kind of porous double-metal hydroxide catalyst and its preparation method and application for the oxidation of electro-catalysis alcohols selectivity |
| CN112090426A (en) * | 2020-09-04 | 2020-12-18 | 天津理工大学 | Metal metastable phase electrolyzed water oxygen evolution catalyst and preparation method and application thereof |
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|---|---|---|---|---|
| CN106381506A (en) * | 2016-10-18 | 2017-02-08 | 西安交通大学 | Preparation method of layered ferronickel hydroxide electrode |
| CN109772336A (en) * | 2019-03-05 | 2019-05-21 | 浙江工业大学 | A kind of porous double-metal hydroxide catalyst and its preparation method and application for the oxidation of electro-catalysis alcohols selectivity |
| CN112090426A (en) * | 2020-09-04 | 2020-12-18 | 天津理工大学 | Metal metastable phase electrolyzed water oxygen evolution catalyst and preparation method and application thereof |
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