CN116219468A - Preparation method of metal organic framework derivative material and application of electrolyzed water - Google Patents

Preparation method of metal organic framework derivative material and application of electrolyzed water Download PDF

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CN116219468A
CN116219468A CN202310214614.9A CN202310214614A CN116219468A CN 116219468 A CN116219468 A CN 116219468A CN 202310214614 A CN202310214614 A CN 202310214614A CN 116219468 A CN116219468 A CN 116219468A
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mofs
foam nickel
organic framework
nifum
water
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刘进轩
张瑞佳
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Dalian University of Technology
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Abstract

A preparation method of a metal organic framework derivative material and application of electrolyzed water belong to the technical field of electrochemical catalytic energy storage materials. The method adopts that nickel chloride hexahydrate and fumaric acid are respectively dissolved in anhydrous methanol and NaOH aqueous solution; uniformly mixing the obtained metal salt solution and the organic ligand solution, and transferring the mixture into a high-pressure reaction kettle; vertically placing the treated foam nickel into a reaction kettle, heating for reaction, and naturally cooling; taking out the foam nickel, usingWashing with ethanol and water, and vacuum drying; the obtained sample was subjected to N 2 And carrying out heat treatment in atmosphere to obtain the MOFs derivative material. In a three-electrode system, a metal organic framework derivative material electrocatalyst is directly used as a working electrode to be placed in electrolyte for electrocatalytic water decomposition oxygen precipitation reaction. The prepared electrocatalyst has excellent electrocatalytic oxygen evolution activity and stability.

Description

Preparation method of metal organic framework derivative material and application of electrolyzed water
Technical Field
The invention discloses a method for converting a metal organic framework material NiFum MOF into a metal organic framework material containing alpha-Ni (OH) 2 Phase-derived material electrocatalysisThe preparation method of the catalyst and the application of the catalyst in the alkaline electrocatalytic water decomposition direction are researched, and the catalyst belongs to the technical field of electrochemical catalytic energy storage materials.
Background
The continuous growth of energy demand and the use of non-renewable fossil fuels have led to increasing problems with energy reserves, climate change, environmental pollution and greenhouse effect. Finding clean renewable energy is a necessary trend for global energy conversion. Hydrogen (H) 2 ) As a clean energy source and an energy carrier, the energy source is rich, the energy density is high, the combustion product is water, the preparation of the energy source can be coupled with a renewable energy system, the energy source has a very wide application prospect, and the energy source is one of important technical paths for realizing the 'double carbon' target in China. The hydrogen is prepared by electrolyzing water, which is a zero-carbon hydrogen production mode, can realize green and clean whole process and has important significance for the establishment of a future decarburization energy system. However, the reliance on noble metal catalysts (such as Ir and Ru based catalysts) and low energy conversion efficiency limit the large scale applications of electrocatalytic water splitting hydrogen production. Therefore, development of low-cost, high-stability and high-efficiency electrocatalysis has become one of the research hotspots in recent years.
Among the various emerging candidate materials, metal organic framework Materials (MOFs) show tremendous promise. MOFs are a series of porous coordination polymers built up from organic ligands and metal centers through coordination bonds. Because of their predesigned open porous structure, readily exposed catalytically active sites, and structural functional adjustability, great interest has been seen in the last two decades, and has been used in a wide variety of fields including sensing, gas separation, energy storage and conversion. However, most MOFs have disadvantages of low conductivity and poor stability, which results in hindered charge transfer, thereby reducing their electrochemical performance and limiting their large-scale application.
Disclosure of Invention
The object of the present invention is to provide a method for converting MOFs into a-Ni (OH) containing MOFs by heat treatment 2 A preparation method of MOFs derivative material electrocatalyst of phase. The method uses MOFs as a template or a precursor and adopts heat treatment and chemical treatmentConversion to MOFs-derived metal compounds by such means; the dominant properties of MOFs are fused: the high specific surface area and porosity and abundant metal active sites provide great opportunities for MOFs as electrode catalysts for energy conversion.
NiFum MOF was grown on a foam nickel substrate (NF) by solvothermal method, after which it was placed in N 2 Heat-treating in atmosphere to obtain MOFs derivative containing alpha-Ni (OH) 2 Phase electrocatalyst and application to electrocatalytic water Oxidation (OER) reactions.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
the preparation method of the metal organic framework derivative material specifically comprises the following steps:
(1) Cleaning the foam nickel substrate, and storing the foam nickel substrate in ethanol for use;
(2) Dissolving nickel chloride hexahydrate in absolute ethyl alcohol to obtain a metal salt solution with the concentration of 0.05-0.1 mol/L; dissolving fumaric acid in an aqueous solution of NaOH, wherein the molar ratio of the fumaric acid to the NaOH is 1:2, and obtaining a ligand solution with the fumaric acid concentration of 0.05-0.1 mol/L;
(3) Transferring the metal salt solution and the ligand solution into a Teflon-lined stainless steel autoclave, uniformly mixing, vertically placing a dried foam nickel substrate into the autoclave, and keeping the temperature at 60-100 ℃ for 10-14 hours;
(4) After the reaction kettle is naturally cooled to room temperature, taking out foam nickel, alternately flushing with ethanol and water, and placing a sample for vacuum drying overnight after flushing is finished;
(5) The NiFum MOF material obtained was placed in a tube furnace at N 2 Performing heat treatment in atmosphere at 200-400deg.C for 40-80min, and cooling to room temperature to obtain the product containing alpha-Ni (OH) 2 MOFs derived material of the phases.
The MOFs derivative material is directly used for electrocatalytic water decomposition reaction as an electrolytic water catalyst. Further, drying the pretreated foam Nickel (NF);
0.5mmol of NiCl 2 ·6H 2 O is dissolved in methanol solution and is subjected to ultrasonic treatment for 30s to obtainA metal salt solution; dissolving 0.5mmol of fumaric acid in NaOH aqueous solution, and performing ultrasonic treatment for 1min to obtain colorless and transparent ligand solution;
uniformly mixing a metal salt solution and a ligand solution, transferring the mixture into a Teflon-lined 15mL stainless steel autoclave, vertically placing the treated NF foam nickel substrate, and keeping the temperature at 80 ℃ for 12 hours;
after the autoclave was naturally cooled to room temperature, NF was rinsed with ethanol and water and the obtained sample was dried in a vacuum oven at 60 ℃ to obtain NiFum MOF.
The NiFum MOF material obtained was placed in a tube furnace at N 2 Performing heat treatment in atmosphere at 200-400 deg.c for 60min to cool to room temperature to obtain the product containing alpha-Ni (OH) 2 MOFs derived material of the phases.
Further, the size of the foamed nickel substrate was 2X 2.5cm -2 . Sequentially and respectively ultrasonically cleaning with 1M HCl, acetone, ethanol and deionized water for 15-30 min.
Further, niCl 2 ·6H 2 O was dissolved in 6mL of anhydrous methanol solution, fumaric acid was dissolved in 6mL of aqueous LNaOH (0.167M), and the dissolution was promoted by ultrasound.
Further, the temperature is slowly raised under solvothermal conditions, and the mixture is kept for 12 hours at 80 ℃.
Further, the autoclave was naturally cooled to below 40 ℃ in an oven, a foam nickel sample was clamped out with forceps, and was alternately rinsed three times with ethanol and water to remove unreacted metal salts and ligands, impurities, and the like.
Further, the cleaned NiFum MOF samples were dried overnight in a vacuum oven at 60 ℃.
Further, the obtained NiFum MOF material was placed in a tube furnace at N 2 Performing heat treatment in atmosphere, heating to 200-400 ℃ at a heating rate of 2 ℃/min at a gas flow rate of 15mL/h, maintaining for 60min, and naturally cooling to room temperature after the reaction is finished to obtain the catalyst containing alpha-Ni (OH) 2 MOFs derived material of the phases.
Further, the above materials are directly used for the electrocatalytic moisture desorption oxygen reaction (OER). A standard three-electrode system (Hg/HgO is used as a reference electrode, a platinum wire is used as a counter electrode and a working electrode) is adopted, and the electrolyte is 1M KOH solution.
Compared with the prior art, the invention has the technical advantages that:
1) NiFum MOFs are grown in situ on a foam nickel substrate with good conductivity by a one-step solvothermal method, can be directly used for electrolytic reaction, is beneficial to effective mass transfer and charge transfer, and avoids the defects that the powdery MOFs need a polymer binder to cause partial coverage of active sites and mass transfer at a catalyst-electrolyte interface is blocked.
2) MOFs as precursors were subjected to a simple heat treatment to obtain a catalyst having alpha-Ni (OH) 2 MOFs derived material of the phases. And the heat treatment temperature is increased to remove interlayer water, thereby obtaining alpha-Ni (OH) with lattice contraction phenomenon 2 Phase MOFs derived materials.
3) The electrochemical performance test shows that the derivative material obtained by heat treatment at 300 ℃ has the smallest overpotential, the fastest reaction dynamics, the smallest charge transfer resistance, the largest electrochemical active surface area and long-time electrochemical stability under the same current density and has excellent OER performance compared with other comparison samples.
In summary, the invention obtains the foam nickel substrate with alpha-Ni (OH) by simple heat treatment after in-situ growth of NiFum MOF 2 Phase MOFs derived materials. The preparation method has simple process and easy implementation. The resulting catalyst has a small overpotential and excellent durability in OER process applications.
Drawings
In order to more clearly illustrate the technical solution of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below.
FIG. 1 is an X-ray diffraction pattern of a metal organic framework material NiFum MOF prepared by solvothermal method.
FIG. 2 is an X-ray diffraction pattern of the MOFs-derived material NiFum MOF-T-1 obtained after heat treatment.
FIG. 3 is a scanning electron microscope image of the MOFs-derived material NiFum MOF-300-1 obtained after heat treatment.
FIG. 4 is an EDS spectrum of the MOFs-derived material NiFum MOF-300-1 obtained after heat treatment.
FIG. 5 (a) is an LSV curve of the MOFs-derived material NiFumMOF-300-1 and its comparative sample obtained after heat treatment; (b) Is the Tafil slope of the MOFs derivative material NiFumMOF-300-1 and the comparison sample thereof obtained after the heat treatment; (c) Impedance diagram of MOFs derivative material NiFumMOF-300-1 and comparison sample obtained after heat treatment; (d) The active surface area of the MOFs-derived material NiFumMOF-300-1 and its control obtained after heat treatment.
FIG. 6 is an i-t test of the MOFs-derived material NiFum MOF-300-1 obtained after heat treatment.
FIG. 7 is a LSV curve of NiFum MOF-300-1 before and after i-t testing.
FIG. 8 is a graph of the X-ray diffraction patterns of NiFum MOF-300-1 before and after i-t testing.
FIG. 9 is an in situ electrochemical infrared spectroscopy test spectrum of NiFum MOF-300-1.
Detailed Description
The present invention will be further described with reference to the following examples for the purpose of making the objects, technical solutions and advantages of the present invention more apparent, but the present invention is not limited to the following examples.
Example 1 preparation of MOFs-derived electrocatalytic Material
The foamed nickel substrate was cut to a size of 2X 2.5cm -2 Sequentially and respectively ultrasonically cleaning with 1M HCl, acetone, ethanol and deionized water for 15-30 min, and storing in absolute ethanol for use after cleaning;
placing the pretreated foam Nickel (NF) in a vacuum drying oven, and keeping at 60 ℃ for 30min for drying treatment;
0.5mmol of NiCl 2 ·6H 2 O is dissolved in 6mL of anhydrous methanol solution, and ultrasonic treatment is carried out for 30s, so as to prepare a metal salt solution; dissolving 0.5mmol fumaric acid in 6mL NaOH aqueous solution (0.167M), and performing ultrasonic treatment for 1min to obtain colorless transparent ligand solution;
uniformly mixing the metal salt solution and the ligand solution, transferring the mixture into a Teflon-lined 15mL stainless steel autoclave, vertically placing the treated NF foam nickel substrate, slowly heating the NF foam nickel substrate to 80 ℃ at a heating rate of 2 ℃/min, and keeping the NF foam nickel substrate at the temperature of 80 ℃ for 12 hours;
after the reaction kettle is naturally cooled to room temperature, a foam nickel sample is clamped by forceps, and is alternately washed by ethanol and water for three times to remove unreacted metal salt, ligand, impurities and the like;
placing the cleaned NiFum MOF sample into a vacuum drying oven for overnight drying;
the NiFum MOF material obtained was placed in a tube furnace at N 2 Performing heat treatment in atmosphere at gas flow rate of 15mL/h, heating to 200deg.C, 300deg.C, 400deg.C at heating rate of 2deg.C/min, maintaining for 60min, and naturally cooling to room temperature after the reaction to obtain alpha-Ni (OH) containing material 2 MOFs derived material of phases NiFum MOF-200-1, niFum MOF-300-1 and NiFum MOF-400-1.
Example 2 use of MOFs-derived electrocatalytic Material in OER Process
The prepared NiFum MOF-300-1 was cut into 1X 2cm pieces 2 Directly used for working electrode, the area immersed in electrolyte solution is 1X 1cm 2 . The electrochemical performance of the catalyst was evaluated using a standard three electrode system (Hg/HgO as reference electrode, platinum wire as counter electrode, working electrode) with 1M KOH solution as electrolyte. The model of the electrochemical workstation is Shanghai Chenhua CHI 760.
Example 3
(1) Physical characterization of catalytic materials
The XRD results in figure 1 show that the experimentally synthesized NiFum MOF can be well matched with the simulation results, indicating successful preparation of NiFum MOF. XRD results of heat treatments at 200, 300 and 400℃respectively are shown in FIG. 2, and it can be seen that the original MOFs are converted into α -Ni (OH) after heat treatments at 200 and 300 ℃ 2 And basic nickel carbonate. After heat treatment at 300 ℃, alpha-Ni (OH) 2 The (0 00 6) crystal face of (c) is highly angularly offset, presumably because the heat treatment temperature is increased to cause a decrease in intercalation water, thereby causing occurrence of a lattice contraction phenomenon. The result of the NiFum MOF-300-1 scanning electron microscope is shown in FIG. 3It can be seen that the nickel foam base is covered by irregular massive particles. The EDS results of FIG. 4 show that C, O, ni elements are uniformly distributed in NiFum-300-1.
(2) OER electrochemical performance evaluation of catalyst
The LSV results in FIG. 5 (a) show that NiFum-300-1 has the smallest overpotential at 10mA cm at the same current density -2 And 100mA cm -2 Is 205 and 370mV, respectively. Also in FIG. 5 (b), niFum-300-1 has a minimum Tafil slope of 67.15 mV.dec -1 Indicating that it has the fastest reaction kinetics. In the impedance test results of FIG. 5 (c), niFum MOF-300-1 exhibited the smallest arc with the smallest charge transfer resistance. FIG. 5 (d) shows that NiFum MOF-300-1, which has the greatest slope, has the greatest electrochemically active surface area and can provide a rich active site for the reaction, as assessed by the double layer capacitance. FIG. 6 stability i-t test results show that NiFum MOF-300-1 material can be used at 10mA cm -2 The current density was stable for 118h. FIG. 7 shows that the NiFum MOF-300-1 overpotential was increased by only 25mV before and after the stability test, indicating that the material has excellent stability. The electrochemical performance test result shows that the MOFs material after heat treatment shows excellent OER performance and has potential application value.
(3) Characterization after NiFum MOF-300-1 stability test
FIG. 8NiFum MOF-300-1 shows complete disappearance of the crystal structure after 118h stability test, presumably to amorphous hydroxide or oxyhydroxide.
(4) NiFum MOF-300-1 in situ electrochemical test
In order to investigate the active species of NiFum MOF-300-1 in the OER process, in situ electrochemical infrared spectroscopy tests were performed at different potentials. In FIG. 9, when a voltage is applied to 1.4V, at 1043cm -1 Distinct infrared characteristic peaks appear there and increase with increasing applied voltage, which can be attributed to the generation of critical OOH species.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and not for limiting the same; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some or all of the technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit of the invention.

Claims (2)

1. A method for preparing a metal organic framework derivative material is characterized in that the metal organic framework material is used as a precursor, and alpha-Ni (OH) is prepared by a heat treatment means 2 MOFs derived materials of the phases act as water electrolysis catalysts;
the method specifically comprises the following steps:
(1) Cleaning the foam nickel substrate, and storing the foam nickel substrate in ethanol for use;
(2) Dissolving nickel chloride hexahydrate in absolute methanol to obtain a metal salt solution with the concentration of 0.05-0.1 mol/L; dissolving fumaric acid in NaOH aqueous solution, wherein the molar ratio of fumaric acid to NaOH is 1:2, and obtaining ligand solution with concentration of 0.05-0.1 mol/L;
(3) Transferring the metal salt solution and the ligand solution into a Teflon-lined stainless steel autoclave, uniformly mixing, vertically placing a dried foam nickel substrate into the autoclave, and keeping the temperature at 60-100 ℃ for 10-14 hours;
(4) After the reaction kettle is naturally cooled to room temperature, taking out foam nickel, alternately flushing with ethanol and water, and placing a sample for vacuum drying overnight after flushing is finished;
(5) The NiFum MOF material obtained was placed in a tube furnace at N 2 Performing heat treatment in atmosphere at temperature t, t is 200-400deg.C, and maintaining for 40-80min, and cooling to room temperature to obtain the product containing alpha-Ni (OH) 2 MOFs derived material of the phases.
2. The use of MOFs derived materials made by the method of claim 1, wherein: the MOFs derivative material is directly used for electrocatalytic water decomposition reaction as an electrolytic water catalyst.
CN202310214614.9A 2023-03-08 2023-03-08 Preparation method of metal organic framework derivative material and application of electrolyzed water Pending CN116219468A (en)

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