CN115976556A - Self-assembled CoSe 2 /NiSe 2 Composite nano heterostructure electrocatalyst material and preparation method and application thereof - Google Patents

Self-assembled CoSe 2 /NiSe 2 Composite nano heterostructure electrocatalyst material and preparation method and application thereof Download PDF

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CN115976556A
CN115976556A CN202310131018.4A CN202310131018A CN115976556A CN 115976556 A CN115976556 A CN 115976556A CN 202310131018 A CN202310131018 A CN 202310131018A CN 115976556 A CN115976556 A CN 115976556A
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cose
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佴建威
周晓东
陶新永
郭晓虎
姜帆
岳苛
王垚
刘育京
罗剑敏
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Zhejiang University of Technology ZJUT
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    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
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    • Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis

Abstract

The invention belongs to the field of oxygen evolution electrocatalytic materials, and particularly relates to self-assembled CoSe 2 /NiSe 2 Composite nano heterostructure electrocatalyst material and its preparation method and application. Dissolving cobalt acetate, trisodium citrate and a surfactant in a mixed solvent of water and DMSO to obtain a mixed solution, and dissolving K in the mixed solution 2 [Ni(CN) 4 ]Adding the aqueous solution of (1) into the mixed solution, stirring, and thenAging for 4h, extracting the precipitate with water and absolute ethanol, centrifuging, and air drying to obtain two-dimensional orthogonal self-assembled precursor CoNi (CN) 4 A nanosheet; the CoSe is obtained after the selenizing heat treatment of the nano sheet 2 /NiSe 2 A composite nano heterostructure material. The invention synthesizes the nanosheet precursor with the orthogonal self-assembly morphology in one step by a liquid phase method, the nanosheet precursor has the advantages of regular morphology, small size, high specific surface area, rapid electron transmission path and certain structural stability, and CoSe is obtained after selenization heat treatment 2 /NiSe 2 The nano heterostructure material is compounded, the orthogonal self-assembly morphology is reserved, and the method has wide application prospect in the aspects of electrolytic water oxygen evolution reaction and material morphology design.

Description

Self-assembled CoSe 2 /NiSe 2 Composite nano heterostructure electrocatalyst material and preparation method and application thereof
Technical Field
The invention belongs to the field of oxygen evolution electrocatalysis materials, and particularly relates to a preparation method and application of a cobalt diselenide/nickel diselenide nano heterostructure material which is high in stability and high in electrocatalysis oxygen evolution reaction activity and is formed by two-dimensional orthogonal self-assembly.
Background
With the continuous development of economy, environmental problems and energy problems become more serious. In order to solve the urgent need of clean and sustainable energy, the hydrogen production by electrolyzing water is a new method which has high quality and is friendly to the environment. However, since the water electrolysis oxygen evolution reaction is a slow electrochemical process involving four electron transfer, the water electrolysis oxygen production hydrogen production is often energy-consuming and inefficient. Therefore, the search for an efficient and stable oxygen evolution electrocatalyst is a key requirement for reducing activation failure and accelerating reaction, thereby improving energy conversion efficiency and lifetime.
According to research reports, general noble metal-based materials such as RuO 2 、IrO 2 And the like have good electrocatalytic performance, but are often limited by resource reserves and cost price and cannot be widely applied. Therefore, it is necessary to design an electrocatalyst with high activity and low cost from the viewpoints of structure-activity relationship and heterostructure. It is reported that, due to the greater conductivity of Se atoms, a large number of metal selenides are available as electrocatalytic materials for oxygen evolution reactions, such as CoSe 2 、NiSe 2 Etc. have excellent electrocatalytic activity. The invention relies on the layered structure of Hoffman type material, can prepare precursors with different appearances by a novel method of interlayer solvent extraction, and can prepare the metal selenide electrocatalyst which basically keeps the appearances of the precursors by selenizing heat treatment. The invention provides a new idea for reasonably designing and deriving the transition metal matrix composite nano heterostructure electrocatalyst subsequently.
Disclosure of Invention
The invention aims to solve the problems in the prior art and provides a novel efficient and cheap CoSe formed by two-dimensional orthogonal self-assembly 2 /NiSe 2 An oxygen evolution electrocatalyst with a composite nano heterostructure and a preparation method and application thereof are introduced, and a novel method for regulating and controlling the self-assembly morphology of a material is introduced.
The technical scheme adopted by the invention for solving the technical problems is as follows:
the invention provides a preparation method of cobalt diselenide/nickel diselenide composite nano heterostructure electrocatalyst formed by orthogonal self-assembly, which comprises the following steps:
(1) Dissolving cobalt acetate, trisodium citrate and a surfactant in a solvent, wherein the solvent is a mixed solvent of water and DMSO (dimethyl sulfoxide), so as to obtain a mixed solution; will K 2 [Ni(CN) 4 ]Dissolving in water to obtain K 2 [Ni(CN) 4 ]A solution; will K 2 [Ni(CN) 4 ]Adding the solution into the mixed solution, stirring, aging at room temperature for 4h, allowing the growth time of the nano material to influence the appearance, and allowing the nano material to thicken and enlarge if the growth time is too long, or allowing some nano materials to dissolve in the hollow space, washing and extracting the aged precipitate with pure water and absolute ethyl alcohol, centrifuging, and naturally air drying to obtain the two-dimensional orthogonal self-assemblyPacked precursor CoNi (CN) 4 Nanosheets;
the surfactant is preferably polyvinylpyrrolidone (PVP);
in the mixed solution, the volume ratio of water to DMSO is preferably 2:1;
in the mixed solution, the concentration of cobalt acetate is preferably 0.01-0.05 mmol/mL, the concentration of trisodium citrate is preferably 0.03-0.07 mmol/mL, the concentration of surfactant is preferably 0.01-0.04 g/mL, and water is preferably deionized water;
said K 2 [Ni(CN) 4 ]The concentration of the solution is preferably 0.05-0.1 mmol/mL, and the solvent water is preferably deionized water;
said K 2 [Ni(CN) 4 ]The volume ratio of the solution to the mixed solution is preferably 20;
in the invention, the solvent is a mixed solvent of water and DMSO, so that the appearance is changed to a square sheet, the orthogonal self-assembly appearance can be generated by using pure water to perform interlayer extraction, and the absolute ethyl alcohol is used for further washing off redundant moisture, thereby being convenient for drying;
the room temperature is preferably 15-40 ℃;
(2) Selenium powder and precursor CoNi (CN) 4 The nano sheet material is respectively arranged at an upper vent and a lower vent of an atmosphere tube furnace, the temperature is raised to 350-500 ℃ at the speed of 1-10 ℃/min under the protective atmosphere, and the heat preservation and calcination treatment is carried out for 2-5 h to obtain the CoSe 2 /NiSe 2 A composite nano-heterostructure material;
the protective atmosphere during calcination is preferably one or a combination of two of nitrogen and argon in any proportion;
the selenium powder and a precursor CoNi (CN) 4 The mass ratio of the materials is preferably 1 to 8:1.
the preparation method provided by the invention can prepare two-dimensional orthogonal self-assembled CoSe 2 /NiSe 2 The composite nano heterostructure electrocatalyst material provides a novel morphology design method which can be realized in certain Hofmann type materials, and further widens the research thought and direction in the field.
The invention also provides two-dimensional orthogonal self-assembled CoSe prepared by any one of the preparation methods 2 /NiSe 2 Composite nano-heterostructure electrocatalyst materials.
The two-dimensional orthogonal self-assembled cobalt diselenide/nickel diselenide composite nano heterostructure electrocatalyst material prepared by the preparation method can be used for electrolytic water oxygen evolution reaction.
CoSe with two-dimensional orthogonal self-assembly morphology prepared by the invention 2 /NiSe 2 Compared with the prior art, the material has the advantages that:
(1) The invention can synthesize the nanosheet precursor with the orthogonal self-assembly morphology in one step by a simple liquid phase method, the orthogonally-assembled two-dimensional material has regular morphology and smaller size, is a square sheet (shown in the attached drawing 1 in detail) with the length of about 5um and formed by self-assembling small hexagonal sheets with the length of about 900nm and the width of about 300nm, has higher specific surface area, rapid electron transmission path and certain structural stability, is a good precursor template, and can obtain CoSe after subsequent selenization heat treatment 2 /NiSe 2 The nanometer heterostructure material is compounded, the orthogonal self-assembly morphology of the precursor is reserved through heat treatment under proper conditions, in the OER process, the high specific surface area and the heterostructure provide more effective active sites, the ion diffusion and electron conduction speed is increased, and therefore the reaction kinetics of electrocatalytic oxygen evolution is accelerated.
(2) The material belongs to a non-noble metal electrocatalyst, has higher catalytic activity and stability of oxygen evolution reaction while reducing cost, and also provides a method for designing a special appearance, and has wide application prospects in the aspects of electrolytic water oxygen evolution reaction and material appearance design.
Drawings
FIG. 1 is CoNi (CN) obtained in example 1 4 Nanoplatelets a) SEM, b) XRD, c) EDS pattern.
FIG. 2 is CoSe obtained in example 1 2 /NiSe 2 Composite nano-heterostructure material a) SEM, b) XRD, c) EDS plot.
FIG. 3 is a scheme showing a scheme of preparation in example 1The obtained CoSe 2 /NiSe 2 HRTEM images of composite nano-heterostructure materials.
FIG. 4 is CoSe obtained in examples 1-4 at different heat treatment temperatures 2 /NiSe 2 XRD pattern of composite nano-heterostructure material; a) 350 ℃, b) 400 ℃, c) 450 ℃, d) 500 ℃.
FIG. 5 is the precursors of examples 1-4 and CoSe produced at different thermal treatment temperatures 2 /NiSe 2 An LSV map of the composite nano-heterostructure material; a) CoNi (CN) 4 Precursor, b) 500 ℃, c) 400 ℃, d) 350 ℃, e) 450 ℃.
FIG. 6 shows CoNi (CN), which is a precursor material obtained in examples 5-7 by different cleaning and extraction methods 4 SEM picture of (g); a) example 5 precursor, b) example 6 washing the extracted precursor with pure water and ethanol to remove residual water, c) example 7 extracting the precursor with pure water first and then with DMSO.
FIG. 7 shows CoNi (CN), which is a precursor material obtained in examples 5-7 by different cleaning and extraction methods 4 An XRD pattern of (a); a) example 5 precursor, b) example 6 washing the extracted precursor with pure water and ethanol to remove residual moisture, c) example 7 extraction of the precursor with pure water followed by DMSO.
FIG. 8 shows CoNi (CN), a precursor material obtained in examples 5-7 by different cleaning and extraction methods 4 FTIR plot of (a); a) DMSO solvent, b) precursor of example 5, c) precursor of example 6, which is washed with pure water and residual water is washed away with absolute ethanol, d) precursor of example 7, which is extracted with pure water first, followed by DMSO.
Detailed Description
The technical solution of the present invention is further specifically described below by using specific embodiments and with reference to the drawings, but the scope of the present invention is not limited thereto.
Example 1
Dissolving 1.5mmol of cobalt acetate, 2.3mmol of trisodium citrate and 1.0g of PVP (molecular weight of 40000) in a mixed solvent of 30ml of water and 15ml of DMSO, and magnetically stirring to form a transparent solution A; will K 2 [Ni(CN) 4 ]Dissolving in 20ml of deionized water to obtain a solution B; then theSlowly pouring the solution B into the solution A within 5s, continuously stirring for 3 minutes, aging the mixed solution at room temperature for 4 hours, washing and extracting the obtained precipitate for 2 times by using pure water, finally washing away residual water by using absolute ethyl alcohol, centrifuging, and air-drying at room temperature to obtain a square sheet which is formed by orthogonal self-assembly of small hexagonal sheets with the length of about 900nm and the width of about 300nm and has the length of about 5um, namely a precursor CoNi (CN) 4 Powder; weighing 20mg CoNi (CN) 4 Placing the powder in a ceramic boat, placing in a lower vent of a small-sized atmosphere tube furnace (HF-Keying OTF-1200X-S, the same below), placing 120mg selenium powder in an upper vent of another ceramic boat in the atmosphere tube furnace, heating to 450 ℃ at a rate of 2 ℃/min under argon atmosphere, and carrying out heat preservation treatment for 4h to obtain a target product CoSe with the size and appearance basically consistent with that of a precursor 2 /NiSe 2 。
Example 2
Dissolving 1.5mmol of cobalt acetate, 2.3mmol of trisodium citrate and 1.0g of PVP (molecular weight of 40000) in a mixed solvent of 30ml of water and 15ml of DMSO, and magnetically stirring to form a transparent solution A; will K 2 [Ni(CN) 4 ]Dissolving in 20ml of deionized water to obtain a solution B; slowly pouring the solution B into the solution A within 5s, continuously stirring for 3 minutes, aging the mixed solution at room temperature for 4 hours, washing and extracting the obtained precipitate for 2 times by using pure water, finally washing away residual water by using absolute ethyl alcohol, centrifuging, and air-drying at room temperature to obtain a two-dimensional orthogonal self-assembled precursor CoNi (CN) 4 Powder; weighing 20mg CoNi (CN) 4 Placing the powder in a ceramic boat, placing in a lower vent of a small-sized atmosphere tube furnace (HF-Keying OTF-1200X-S, the same below), placing 120mg selenium powder in an upper vent of another ceramic boat in the atmosphere tube furnace, heating to 350 ℃ at a rate of 2 ℃/min under argon atmosphere, and carrying out heat preservation treatment for 4h to obtain a target product CoSe 2 /NiSe 2 。
Example 3
Dissolving 1.5mmol of cobalt acetate, 2.3mmol of trisodium citrate and 1.0g of PVP (molecular weight of 40000) in a mixed solvent of 30ml of water and 15ml of DMSO, and magnetically stirring to form a transparent solution A; will K 2 [Ni(CN) 4 ]Dissolving in 20ml of deionized water to obtain a solution B; then slowly pouring the solution B into the solution A within 5s, continuously stirring for 3 minutes, aging the mixed solution for 4 hours at room temperature,washing the obtained precipitate with pure water for 2 times, washing with anhydrous ethanol to remove residual water, centrifuging, and air drying at room temperature to obtain two-dimensional orthogonal self-assembled precursor CoNi (CN) 4 Powder; weighing 20mg CoNi (CN) 4 Placing the powder in a ceramic boat, placing in a lower vent of a small-sized atmosphere tube furnace (HF-Keying OTF-1200X-S, the same below), placing 120mg selenium powder in an upper vent of another ceramic boat in the atmosphere tube furnace, heating to 400 ℃ at a rate of 2 ℃/min under argon atmosphere, and carrying out heat preservation treatment for 4h to obtain a target product CoSe 2 /NiSe 2 。
Example 4
Dissolving 1.5mmol of cobalt acetate, 2.3mmol of trisodium citrate and 1.0g of PVP (molecular weight of 40000) in a mixed solvent of 30ml of water and 15ml of DMSO, and magnetically stirring to form a transparent solution A; will K 2 [Ni(CN) 4 ]Dissolving in 20ml of deionized water to obtain a solution B; slowly pouring the solution B into the solution A within 5s, continuously stirring for 3 minutes, aging the mixed solution at room temperature for 4 hours, washing and extracting the obtained precipitate for 2 times by using pure water, finally washing away residual water by using absolute ethyl alcohol, centrifuging, and air-drying at room temperature to obtain a two-dimensional orthogonal self-assembled precursor CoNi (CN) 4 Powder; weighing 20mg CoNi (CN) 4 Placing the powder in a ceramic boat, placing in a lower vent of a small-sized atmosphere tube furnace (HF-Keying OTF-1200X-S, the same below), placing 120mg selenium powder in an upper vent of another ceramic boat in the atmosphere tube furnace, heating to 500 deg.C at a rate of 2 deg.C/min under argon atmosphere, and holding for 4h to obtain the target product CoSe 2 /NiSe 2 。
Example 5
Dissolving 1.5mmol of cobalt acetate, 2.3mmol of trisodium citrate and 1.0g of PVP (molecular weight of 40000) in a mixed solvent of 30ml of water and 15ml of DMSO, and magnetically stirring to form a transparent solution A; will K 2 [Ni(CN) 4 ]Dissolving in 20ml of deionized water to obtain a solution B; slowly pouring the solution B into the solution A within 5s, continuously stirring for 3 minutes, aging the mixed solution at room temperature for 4 hours to obtain a precipitate, directly centrifuging without cleaning, and air-drying at room temperature to obtain a two-dimensional orthogonal self-assembled precursor CoNi (CN) 4 And (3) powder.
Example 6
Dissolving 1.5mmol of cobalt acetate, 2.3mmol of trisodium citrate and 1.0g of PVP (molecular weight of 40000) in a mixed solvent of 30ml of water and 15ml of DMSO, and magnetically stirring to form a transparent solution A; will K 2 [Ni(CN) 4 ]Dissolving in 20ml of deionized water to obtain a solution B; slowly pouring the solution B into the solution A within 5s, continuously stirring for 3 minutes, aging the mixed solution at room temperature for 4 hours, washing and extracting the obtained precipitate for 2 times by using pure water, finally washing away residual water by using absolute ethyl alcohol, centrifuging, and air-drying at room temperature to obtain a two-dimensional orthogonal self-assembled precursor CoNi (CN) 4 And (3) powder.
Example 7
Dissolving 1.5mmol of cobalt acetate, 2.3mmol of trisodium citrate and 1.0g of PVP (molecular weight of 40000) in a mixed solvent of 30ml of water and 15ml of DMSO, and magnetically stirring to form a transparent solution A; will K 2 [Ni(CN) 4 ]Dissolving in 20ml of deionized water to obtain a solution B; slowly pouring the solution B into the solution A within 5s, continuously stirring for 3 minutes, aging the mixed solution at room temperature for 4 hours, washing and extracting the obtained precipitate for 2 times by using pure water, then washing and extracting for 2 times by using DMSO, centrifuging, and air-drying at room temperature to obtain a two-dimensional orthogonal self-assembled precursor CoNi (CN) 4 And (3) powder.
Experimental example 1 morphology control of precursor
As can be seen from the SEM image in attached figure 6, the purpose of morphology regulation can be achieved by carrying out different solvent extractions on interlayer molecules of the Hofmann type two-dimensional material, which is specifically represented by a) the precursor is not cleaned and extracted, and when the precursor is directly centrifuged, the precursor is a square sheet with a smooth surface. b) Cleaning and extracting the precursor by using pure water, washing off the residual water on the surface of the precursor by using absolute ethyl alcohol to obtain a precursor square sheet serving as a template, and a square sheet with a small hexagonal sheet orthogonal self-loading surface, c) cleaning and extracting the precursor by using pure water, and extracting by using DMSO (dimethyl sulfoxide) to obtain the precursor square sheet with the precursor square sheet serving as the template and the small square sheet self-loading surface. From the XRD pattern of fig. 7, it can be seen that during the process of extracting the precursor, the material undergoes obvious phase transition, and in combination with the FTIR pattern of fig. 8, it can be seen that during the process of extracting the precursor, the molecules between the material layers undergo mutual exchange. To sum up, canDescription of H 2 The O molecules and the DSMO molecules can be mutually extracted in an interlayer structure of the Hoffman-type material, so that guest molecule exchange is realized, and phase transition is further initiated, thereby influencing the morphology of the material. Therefore, the method can regulate and control the generation of a new phase by controlling the entrance and exit of molecules between layers, and can perform fine design on the morphology of the material, which has great significance on the fine morphology design and the structure design of the future nano material.
Test example 2 Performance test
The precursor product CoNi (CN) of example 1 above was reacted with 4 And the subsequent product CoSe of examples 1-4 heat-treated at different temperatures 2 /NiSe 2 The test method is characterized in that the test method is respectively used as a working electrode, a Pt wire is used as a counter electrode, an Hg/HgO electrode is used as a reference electrode, a three-electrode system test is carried out through a rotating disk electrode, an electrolyte is 1mol/L potassium hydroxide (KOH) solution, the rotating speed is 1600rpm, and relevant performance tests such as LSV, CV, EIS, stability and the like are respectively carried out.
The performance test results are as follows:
precursor product CoNi (CN) in example 1 4 And the subsequent product CoSe of examples 1-4 heat-treated at different temperatures 2 /NiSe 2 The resulting electrodes were subjected to LSV testing at a sweep rate of 5mV s-1 at 10mA cm -2 The corresponding overpotentials at current densities of (2) are 395mV,409mV,429mV,450mV.
The material belongs to a transition metal-based electrocatalyst, has higher electrocatalytic oxygen evolution reaction activity while reducing cost, can realize shape regulation and design of the series of materials by a novel method of interlayer solvent extraction, and has simple preparation process, so the material has wide application prospect in the fields of electrocatalysis and micro-nano shape regulation.
The above-described embodiments are merely preferred embodiments of the present invention, which is not intended to be limiting in any way, and other variations and modifications are possible without departing from the scope of the invention as set forth in the appended claims.

Claims (10)

1. Self-assembled CoSe 2 /NiSe 2 The preparation method of the composite nano heterostructure electrocatalyst material is characterized by comprising the following steps:
(1) Dissolving cobalt acetate, trisodium citrate and a surfactant in a solvent, wherein the solvent is a mixed solvent of water and DMSO (dimethyl sulfoxide), so as to obtain a mixed solution; will K 2 [Ni(CN) 4 ]Dissolving in water to obtain K 2 [Ni(CN) 4 ]A solution; will K 2 [Ni(CN) 4 ]Adding the solution into the mixed solution, stirring, aging at room temperature for 4h, washing the obtained precipitate with pure water and absolute ethanol, extracting, centrifuging, and air drying to obtain two-dimensional orthogonal self-assembled precursor CoNi (CN) 4 Nanosheets;
(2) Selenium powder and precursor CoNi (CN) 4 The nano sheet material is respectively arranged at an upper vent and a lower vent of an atmosphere tube furnace, the temperature is raised to 350-500 ℃ at the speed of 1-10 ℃/min under the protective atmosphere, and the heat preservation and calcination treatment is carried out for 2-5 h to obtain the CoSe 2 /NiSe 2 Composite nano-heterostructure electrocatalyst materials.
2. The self-assembled CoSe of claim 1 2 /NiSe 2 The preparation method of the composite nano heterostructure electrocatalyst material is characterized in that the surfactant is preferably polyvinylpyrrolidone.
3. The self-assembled CoSe of claim 1 2 /NiSe 2 The preparation method of the composite nano heterostructure electrocatalyst material is characterized in that the volume ratio of water to DMSO in the mixed solution is 2:1.
4. The self-assembled CoSe of claim 1 2 /NiSe 2 The preparation method of the composite nano heterostructure electrocatalyst material is characterized in that the concentration of cobalt acetate is 0.01-0.05 mmol/mL, the concentration of trisodium citrate is 0.03-0.07 mmol/mL, and the concentration of a surfactant is 0.01-0.04 g/mL in the mixed solution.
5. The self-assembled CoSe of claim 1 2 /NiSe 2 A preparation method of the composite nano heterostructure electrocatalyst material is characterized in that K is 2 [Ni(CN) 4 ]The concentration of the solution is 0.05-0.1 mmol/mL.
6. The self-assembled CoSe of claim 1 2 /NiSe 2 A preparation method of the composite nano heterostructure electrocatalyst material is characterized in that K is 2 [Ni(CN) 4 ]The volume ratio of the solution to the mixed solution is preferably 20.
7. The self-assembled CoSe of claim 1 2 /NiSe 2 The preparation method of the composite nano heterostructure electrocatalyst material is characterized in that the selenium powder and a precursor CoNi (CN) 4 The mass ratio of the materials is 1-8: 1.
8. the self-assembled CoSe of claim 1 2 /NiSe 2 The preparation method of the composite nano heterostructure electrocatalyst material is characterized in that the protective atmosphere is one or the combination of two of nitrogen and argon in any proportion.
9. Self-assembled CoSe prepared by the method of any one of claims 1 to 8 2 /NiSe 2 Composite nano-heterostructure electrocatalyst materials.
10. The self-assembled CoSe of claim 9 2 /NiSe 2 The application of the composite nano heterostructure electrocatalyst material in the electrolytic water oxygen evolution reaction.
CN202310131018.4A 2023-02-17 2023-02-17 Self-assembled CoSe 2 /NiSe 2 Composite nano heterostructure electrocatalyst material and preparation method and application thereof Pending CN115976556A (en)

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