CN108439549B - Preparation of array structure transition metal selenide electrode and application thereof in electrolytic water - Google Patents
Preparation of array structure transition metal selenide electrode and application thereof in electrolytic water Download PDFInfo
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Abstract
A preparation method of a transition metal selenide electrode with an array structure and an application thereof in electrolytic water belong to the technical field of electrodes. The method comprises the steps of firstly optimizing a nickel sheet (NF) substrate through simple pretreatment, secondly uniformly growing a metal organic framework material (Mn/Fe/Co/Ni/Cu-MOF) nano array on the surface of the NF substrate in situ to obtain an NF-MOFs material, thirdly selenizing the surface of the MOFs nano array in situ to finally obtain the NF-MxSeyA nanoarray electrode material. NF-MxSeyThe water electrolysis electrode has a low initial point position, a large current density, excellent electrocatalytic water decomposition performance and high stability, and can be applied to new energy storage and conversion devices such as electrolyzed water and the like.
Description
Technical Field
The invention belongs to the technical field of electrocatalysis development for converting new energy stored in the conversion field. The technology relates to the construction of metal organic framework Materials (MOFs) and the preparation of transition metal selenides (NF-M) with array structures by selenizing and deriving the templatesxSey) And an electrode.
Background
With the rapid development of industrial production and the increasing population, fossil fuels, mainly represented by coal, oil, and natural gas, have been largely consumed in recent decades, causing inevitable environmental pollution and energy shortage. Therefore, the search for a clean renewable energy source is increasingly demanded in the development of the current times. Among a plurality of materials, hydrogen is used as a clean energy source which is green, environment-friendly, efficient and rich in energy, and is a potential substitute for fossil energy in the future. The reproducible characteristics can be well solvedThe two problems of energy crisis and environmental crisis are solved. Besides being used as clean energy, the hydrogen also has important application in industries such as petroleum, chemical engineering and the like, such as hydrogen used as raw material industry, ammonia formation and the like. At present, a plurality of hydrogen preparation methods are developed, and compared with numerous methods, the electrolyzed water has the advantages of low cost, high yield, high purity, no pollution and the like; meanwhile, oxygen generated by the anode can be used as a good resource to be applied to the fields of medicine and the like, and has huge energy benefits and economic benefits, so that the water electrolysis hydrogen production method is likely to become a core method of the future hydrogen production industry. The electrolysis of water involves two half-cell reactions, respectively cathodic hydrogen evolution (H)ydrogen Evolution Reaction, HER) and anodic oxygen Evolution Reaction (O)xygen Evolution Reaction, OER). Because the reaction kinetics of OER is delayed, the catalyst is often introduced into the half-cell reaction in order to accelerate the reaction, and in the reaction process, the energy consumption and the hydrogen production efficiency are closely related to the catalyst material, so that the research and development of a novel efficient water electrolysis catalyst are significant for the process of converting electrolyzed water into new energy.
Metal-organic frameworks (MOFs) are porous network inorganic-organic hybrid functional materials formed by Metal ions and organic ligands through coordination bonds. Compared with the traditional materials, the MOFs have the advantages of high porosity, large specific surface area, controllable pore structure, easiness in synthesis and the like. In recent years, MOFs have received wide application and attention in many fields such as gas adsorption, molecular recognition, catalysis, separation, and the like. Among them, the porous MOFs and the derivatives thereof show better performance in the field of electrocatalysis, are widely researched particularly in the electrocatalysis water decomposition reaction, and have potential application value. The main reason is that compared with traditional materials, MOFs have various structures and strong adjustability in the synthesis process, can realize targeted synthesis, and the synthesis process is simpler. Nevertheless, MOFs still have some problems in synthesis, such as easy agglomeration of powder, insufficient exposure of active sites, etc., which are unfavorable for mass transfer and electron transfer, inhibiting their development and application. Therefore, a new method is researched and developed, and MOFs and derivatives thereof with various structural compositions, looseness, porosity, large specific surface area, rich active sites, high adjustability and excellent functional groups are prepared for electrochemically decomposing water, so that the electrochemical current density and the electrochemical water decomposition efficiency can be effectively improved.
Disclosure of Invention
The invention aims to provide a preparation method of a transition metal selenide electrode with an array structure.
An array structure transition metal selenide electrode material is characterized in that transition metal selenide grows on a nickel sheet (NF) substrate in an array structure, and the transition metal of the transition metal selenide is preferably: one or more of manganese, iron, cobalt, nickel, copper and the like. The transition metal selenide is of a nano rod-shaped structure; it is preferable to grow the material vertically,
the invention relates to a preparation method of an array structure transition metal selenide electrode material, which mainly comprises the following three steps: firstly, simply pretreating a nickel sheet (NF) substrate; secondly, uniformly growing a transition metal organic framework material array on the surface of the nickel sheet substrate in situ to obtain the NF-MOFs material; and step three, selenizing the surface of the MOFs nano-rod or/and sheet in situ to finally prepare the transition metal selenide electrode material with the array structure.
The synthesis method of the transition metal selenide array electrode materials comprises the following steps:
firstly, respectively carrying out ultrasonic pretreatment on a nickel sheet (NF) substrate by using hydrochloric acid, acetone, ethanol and water in sequence; putting the nickel sheet into hydrochloric acid, wherein the concentration of the hydrochloric acid is 4-8M, and stopping ultrasonic treatment after 10-15 minutes; acetone, ethanol and water are respectively treated by the same ultrasonic treatment mode;
secondly, growing MOFs nano-rods/sheets on the NF substrate by a hydrothermal method; immersing the NF pretreated in the first step into a mother solution B for hydrothermal reaction, wherein the mother solution B is a mixed solution of 2, 5-dihydroxy terephthalic acid, transition metal salt, N-dimethylformamide and water, and adding a proper amount of ethanol or isopropanol; wherein, every 0.1-0.5g of 2, 5-dihydroxyterephthalic acid corresponds to 0.5-1.0g of transition metal salt (the transition metal salt is preferably one or more of manganese chloride tetrahydrate, ferrous chloride tetrahydrate, cobalt nitrate hexahydrate, nickel nitrate hexahydrate and copper nitrate trihydrate) corresponds to 20-45ml of mixed solution of N, N-dimethylformamide and water, and the volume ratio of the N, N-dimethylformamide, the water, the ethanol or the isopropanol is (1-15) to 1: 1; and transferring the mixture into a polytetrafluoroethylene reaction kettle for reaction for 9 to 24 hours, and keeping the temperature at 85 to 135 ℃; after the reaction, washing NF with in-situ grown transition metal MOFs for multiple times by using ethanol and N, N-dimethylformamide respectively to obtain the NF-MOF composite material finally;
and thirdly, placing the selenium powder and the NF-MOF synthesized in the last step into a magnetic boat at the same time, placing the magnetic boat into a tube furnace, and adopting nitrogen protection, wherein the heating temperature is 400 ℃ for 300-.
Further preferably, 0.5 to 1.0g of the transition metal salt in the second step corresponds to 0.1 to 0.3g of the selenium powder in the third step.
The obtained NF-MxSeyThe application of the nano array material as an electrode to decompose water.
Nano array electrode material NF-MxSeyThe selenide nanometer array electrode material has the advantages of being higher in stability, containing various transition metals, various in structural composition, loose and porous, rich in active sites, large in specific surface area, high in adjustability and strong in plasticity.
The invention prepares the ordered nano array electrode material NF-M with regular shapexSeyAs an electrolytic water electrode, the method has the advantages of simple synthesis method, adjustable synthesis process, capability of synthesizing various selenides, universality, various compositions and the like, more importantly, the structure has very large specific surface area and abundant active sites, and further has lower initial point position, larger current density, excellent electrocatalytic decomposition water performance and higher stability in OER, and can be applied to new energy storage and conversion devices such as electrolytic water and the like. The preparation method has simple process, easy implementation and high yield, and is beneficial to batch preparation of high-performance electrode materials. NF-MxSeyHas lower initial point position and larger current as an electrolytic water electrodeThe density, excellent electrocatalytic water decomposition performance and high stability can be applied to new energy storage and conversion devices such as electrolyzed water and the like.
Drawings
FIG. 1 is a schematic scanning electron micrograph of NF-Co-MOF of example 1.
FIG. 2 is NF-CoSe of example 12Scanning electron microscopy of the composite.
FIG. 3 is a schematic scanning electron micrograph of NF-Ni-MOF of example 2.
FIG. 4 shows NF-NiSe in example 22Scanning electron microscopy of the composite.
FIG. 5 multiple NF-MxSeyThe performance of the composite material for electrocatalytic decomposition of water is shown schematically.
Detailed Description
The present invention will be further illustrated with reference to the following examples, but the present invention is not limited to the following examples.
Example 1
The first step is a specific method for treating a nickel sheet (NF) by using hydrochloric acid, acetone, ethanol and water for 10 minutes by ultrasonic treatment: preparing 4-8M hydrochloric acid aqueous solution, placing the NF with the cut shape in the hydrochloric acid aqueous solution, performing ultrasonic cleaning for 10-15 minutes, and performing ultrasonic cleaning by using acetone, ethanol and water sequentially by the same method. And drying the cleaned NF for the next step.
In the second step, NF is immersed in mother liquor B for hydrothermal reaction, wherein the mother liquor B is a mixed solution of 0.15g of 2, 5-dihydroxyterephthalic acid and 0.7g of cobalt nitrate hexahydrate dissolved in 20ml of N, N-dimethylformamide, water and ethanol. Wherein the volume ratio of the N, N-dimethylformamide to the water and the ethanol is 1:1:1, and the N, N-dimethylformamide and the water are transferred into a 100ml reaction kettle to carry out hydrothermal reaction for 15 hours at the temperature of 100 ℃. After the reaction, the NF-Co-MOF composite material is obtained by washing the material for many times by using ethanol and N, N-dimethylformamide.
Thirdly, simultaneously placing 0.1-0.3g of selenium powder and the NF-Co-MOF composite material synthesized in the last step into a magnetic boat, placing the magnetic boat into a tube furnace, adopting nitrogen protection, reacting at 350 ℃ for 1.5 hours, and finally obtaining NF-CoSe2A nanoarray electrode material.
Example 2
The first step is a specific method for pretreating a nickel sheet (NF) by ultrasonic treatment with hydrochloric acid, acetone, ethanol and water for 10 minutes respectively: preparing 4-8M hydrochloric acid aqueous solution, placing the NF with the cut shape in the hydrochloric acid aqueous solution, performing ultrasonic cleaning for 10-15 minutes, and performing ultrasonic cleaning by using acetone, ethanol and water sequentially by the same method. And drying the cleaned NF for the next step.
In the second step, NF is immersed in mother liquor B for hydrothermal reaction, wherein the mother liquor B is a mixed solution of 0.15g of 2, 5-dihydroxyterephthalic acid and 0.7g of nickel nitrate hexahydrate dissolved in 20ml of N, N-dimethylformamide, water and ethanol. Wherein the volume ratio of the N, N-dimethylformamide to the water and the ethanol is 1:1:1, and the N, N-dimethylformamide and the water are transferred into a 100ml reaction kettle to carry out hydrothermal reaction for 15 hours at the temperature of 100 ℃. After the reaction, the NF-Ni-MOF composite material is obtained by washing the material for many times by using ethanol and N, N-dimethylformamide.
Thirdly, simultaneously placing 0.1-0.3g of selenium powder and the NF-Ni-MOF composite material synthesized in the last step into a magnetic boat, placing the magnetic boat into a tube furnace, adopting nitrogen protection, reacting at 350 ℃ for 1.5 hours, and finally obtaining NF-NiSe2A nanoarray electrode material.
The test results of the materials obtained in the above examples are specifically as follows:
(1) and (3) characterizing the material morphology:
respectively taking the NF-Co-MOF and the NF-CoSe2NF-Ni-MOF and NF-NiSe2And a small piece of electrode material is characterized by using a Zeiss SIGMA 500/VP model field emission scanning electron microscope. The structural topography is shown in figure 1, figure 2, figure 3 and figure 4.
(2) And (3) characterization of electrochemical properties of the material:
the electrochemical test apparatus used for this test was a german ZAHNER electrochemical workstation. FIG. 5 shows NF-MxSeyThe current-voltage curve of the composite electrode was tested in 1.0M potassium hydroxide solution (scan speed 5 mv/s).
Claims (5)
1. The transition metal selenide electrode material with the array structure is characterized in that transition metal selenide grows on a nickel sheet NF substrate in the form of the array structure;
transition metals of the transition metal selenides are: one or more of manganese, iron, cobalt, nickel and copper;
the preparation method comprises the following steps: the method mainly comprises the following three steps: firstly, simply pretreating a nickel sheet NF substrate; secondly, uniformly growing a transition metal organic framework material array on the surface of the nickel sheet substrate in situ to obtain the NF-MOFs material; step three, selenizing in situ on the surface of the MOFs nano-rod or/and sheet to finally prepare the transition metal selenide electrode material with the array structure;
the method specifically comprises the following steps:
firstly, respectively carrying out ultrasonic pretreatment on a nickel sheet NF substrate by using hydrochloric acid, acetone, ethanol and water in sequence; putting the nickel sheet into hydrochloric acid, wherein the concentration of the hydrochloric acid is 4-8M, and stopping ultrasonic treatment after 10-15 minutes; acetone, ethanol and water are respectively treated by the same ultrasonic treatment mode;
secondly, growing MOFs nano-rods/sheets on a nickel sheet NF substrate by a hydrothermal method; immersing the nickel sheet NF pretreated in the first step into a mother solution B for hydrothermal reaction, wherein the mother solution B is a mixed solution of 2, 5-dihydroxy terephthalic acid, transition metal salt, N-dimethylformamide and water, and adding a proper amount of ethanol or isopropanol; wherein, every 0.1-0.5g of 2, 5-dihydroxy terephthalic acid corresponds to 0.5-1.0g of transition metal salt corresponds to 20-45ml of mixed solution of N, N-dimethylformamide and water, and the volume ratio of the N, N-dimethylformamide to the water to the ethanol or the isopropanol is (1-15) to 1: 1; and transferring the mixture into a polytetrafluoroethylene reaction kettle for reaction for 9 to 24 hours, and keeping the temperature at 85 to 135 ℃; after the reaction, washing the nickel piece NF with the transition metal MOFs in situ for multiple times by using ethanol and N, N-dimethylformamide respectively to obtain the NF-MOFs composite material finally;
thirdly, the selenium powder and the NF-MOFs synthesized in the last step are simultaneously placed in a magnetic boat, the magnetic boat is placed in a tube furnace, nitrogen protection is adopted, the heating temperature is 300-400 ℃, and the time is 0.5-3 hours.
2. The transition metal selenide electrode material with an array structure according to claim 1, wherein the transition metal selenide is of a nanorod or/and sheet structure; vertical nickel plate NF growth.
3. The transition metal selenide electrode material with an array structure according to claim 1, wherein the transition metal salt is one or more of manganese chloride tetrahydrate, ferrous chloride tetrahydrate, cobalt nitrate hexahydrate, nickel nitrate hexahydrate and copper nitrate trihydrate.
4. The transition metal selenide electrode material of an array structure according to claim 1, wherein 0.5 to 1.0g of the transition metal salt in the second step corresponds to 0.1 to 0.3g of the selenium powder in the third step.
5. The transition metal selenide electrode material of an array structure according to claim 1, wherein the temperature of the third step is 350 ℃ and the time is 1.5 hours.
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