CN108821245B - CoxNi0.85-xPreparation method and application of Se fixed ratio compound - Google Patents
CoxNi0.85-xPreparation method and application of Se fixed ratio compound Download PDFInfo
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Abstract
The invention relates to CoxNi0.85‑xA preparation method and application of Se proportional compound, belonging to the technical field of inorganic functional material preparation. Compound Co of the inventionxNi0.85‑xIn Se, x is more than or equal to 0.05 and less than or equal to 0.4, and the preparation method comprises the following steps: (1) dissolving nickel chloride hexahydrate and cobalt nitrate hexahydrate in deionized water uniformly, adding sodium selenite, slowly adding an ethanolamine solvent and hydrazine hydrate into the solution in sequence, and continuously stirring to form a uniform mixed solution; (2) and transferring the mixed solution into a reaction kettle, sealing, placing in an electric heating air blowing drying oven, heating to 140 ℃, reacting at constant temperature for 24 hours, washing, centrifuging and drying the obtained product to obtain the product. The invention adopts a one-step hydrothermal method to realize the controllable synthesis of CoxNi0.85-xSe compounds with different cobalt doping amounts, and the product prepared by the invention has excellent electrochemical performance and can be used as an electro-catalytic hydrogen evolution catalyst.
Description
Technical Field
The invention belongs to the technical field of inorganic functional material preparation, particularly relates to preparation and application of an electro-catalytic hydrogen evolution catalyst, and more particularly relates to CoxNi0.85-xA preparation method and application of a Se fixed ratio compound.
Background
Electro-catalytic Hydrogen Evolution (HER) is a green Hydrogen production technology which is recognized to have a great application prospect at present. The hydrogen production technology can greatly reduce the overpotential of hydrogen evolution under the action of the catalyst, and has the advantages of low energy consumption, high efficiency, environmental friendliness and the like. The electrocatalytic hydrogen evolution catalyst can greatly reduce the activation energy of the electrolyzed water, thereby reducing the overpotential of the electrolyzed water. Therefore, the quality of the electrocatalytic hydrogen evolution catalyst determines the total voltage required to electrolyze water and the efficiency of conversion of electrical energy into hydrogen energy.
In the prior art, the catalyst based on noble metals (including Pt, Pd and the like) not only has low overpotential close to zero volt and small Tafel slope, but also has excellent catalytic activity and chemical stability, and is the catalyst with the best hydrogen evolution performance at present, but the raw materials of the noble metal catalyst are too expensive and the application cost is high. Therefore, the non-noble metal hydrogen evolution catalyst is prepared simply, quickly, controllably and at low cost, and has important significance for the property research and the application development of the hydrogen evolution catalyst. At present, a lot of reports are reported on preparation methods of electrocatalytic hydrogen evolution catalysts of Fe, Co and Ni, and a plurality of catalysts with excellent performance are prepared in the prior art, and the catalysts mainly comprise alloys, phosphide, sulfide and the like of Fe, Co and Ni, but the hydrogen evolution catalytic performance of the non-noble metal catalysts is generally lower than that of noble metal catalysts, so that the defects of high production cost, low hydrogen evolution activity and low chemical stability still exist, and the electrocatalytic hydrogen evolution performance of the catalysts is seriously reduced.
Many reports have been made on the synthesis of various inorganic functional materials by hydrothermal method. The hydrothermal method has the advantages of low cost, mild conditions, easiness in operation, high purity of a target product, good dispersibility, controllable morphology and size, excellent performance and the like, and has great advantages in the industrial production of related materials. The present application was made based on this.
Disclosure of Invention
The present invention is directed to the problems identified in the background and deficiencies of the prior art by providing a Co alloyxNi0.85-xA preparation method and application of a Se fixed ratio compound.
In order to achieve the first object of the present invention, the inventors have developed a Co through a large number of experimental studiesxNi0.85-xA method for preparing a Se fixed ratio compound of the formula CoxNi0.85-xIn Se, x is more than or equal to 0.05 and less than or equal to 0.4, and the preparation method comprises the following steps:
(1) nickel chloride hexahydrate (NiCl)2·6H2O), cobalt nitrate hexahydrate (Co (NO)3)2·6H2O) is added into a small amount of deionized water in sequence, after being stirred and dissolved evenly, sodium selenite (Na) is added2SeO3) And an ethanolamine solvent and hydrazine hydrate (N)2H4·H2O) is added into the solution slowly in sequence, and the solution is stirred continuously to form a uniform mixed solution;
(2) transferring the mixed solution obtained in the step (1) into a polytetrafluoroethylene reaction kettle, sealing the reaction kettle, placing the reaction kettle into an electric heating air blowing drying oven, heating the reaction kettle to 140 ℃, reacting for 24 hours at a constant temperature, washing and centrifuging the obtained product for multiple times by using water and ethanol, and finally drying to obtain the Co-based catalyst of the inventionxNi0.85-xSe fixed ratio compound; wherein: the preparation method of the invention controls the mixing amount of cobalt to control the final CoxNi0.85-xThe doping amount of cobalt in Se is adjustable from 0.05 to 0.4.
Further, the molar ratio of cobalt nitrate hexahydrate, nickel chloride hexahydrate and sodium selenite in the technical scheme is (0.06-0.9): 1: 5.
preferably, the molar ratio of cobalt nitrate hexahydrate, nickel chloride hexahydrate and sodium selenite in the technical scheme is 0.1: 1: 5.
further, the ratio of nickel chloride hexahydrate to deionized water in the technical scheme is 0.238 g: 6 mL.
Further, the ratio of nickel chloride hexahydrate to ethanolamine in the technical scheme is 0.238 g: 24 mL.
Further, the ratio of nickel chloride hexahydrate to hydrazine hydrate in the above technical scheme is 0.238 g: 8.5 mL.
Further, the washing and centrifuging mode in the above technical scheme is specifically as follows: and washing the obtained product with water and ethanol alternately and centrifugally for 3-6 times.
Further, the drying manner in the step (2) of the above technical solution is preferably freeze-drying in a freeze-dryer.
Preferably, the volume of the reaction kettle in the step (2) of the technical scheme is 100 mL.
Another object of the present invention is to provide Co prepared by the above methodxNi0.85-xThe Se fixed ratio compound can be used for electrocatalytic hydrogen evolution catalyst.
Compared with the prior art, the Co of the inventionxNi0.85-xThe preparation method and the application of the Se fixed ratio compound have the following beneficial effects:
(1) the invention adopts a simple hydrothermal method, and realizes Co doping amounts of different Co in one step by adjusting the composition ratio of reactants and a solventxNi0.85-xThe Se compound can be controllably synthesized, and the reagent used in the method is common and cheap and has low cost; the synthesis steps are simple, and the industrial production is easy to realize; the product prepared by the method has high purity and good crystallinity, and the synthesized Co with different cobalt doping amountsxNi0.85-xSe compounds can be used for electrocatalytic hydrogen evolution catalysts;
(2) the invention adopts a three-electrode system of 0.5M H2SO4The prepared proportional compound is respectively subjected to electrochemical linear scanning voltammetry test, cyclic voltammetry test, electrochemical impedance test and timed amperometric stability test, and test results show that the proportional compound of the invention has good electrocatalytic hydrogen evolution performance, particularly the compound Co0.1Ni0.75The electrocatalytic hydrogen evolution performance of Se is the most excellent: when the current density reaches 10mA/cm2The overpotential η of hydrogen evolution is 153mV, and the gradient b of Tafel is 47 mV/dec.
Drawings
In FIG. 1, (a) to (e) are X-ray diffraction patterns of the products prepared in examples 1 to 5 of the present invention, respectively;
FIG. 2 (a) and (b) are SEM photographs of the product prepared in example 1 of the present invention; (c) and (d) is an SEM photograph of the product prepared in example 2; (e) and (f) is an SEM photograph of the product prepared in example 3 of the invention; (g) and (h) is an SEM photograph of the product prepared in example 4 of the invention; (i) and (j) is an SEM photograph of the product prepared in example 5 of the invention;
in FIG. 3, (A), (B), (C), (D) are the LSV curve contrast diagram, Tafel slope contrast diagram, ESI (electrochemical impedance spectroscopy) contrast diagram inserted into the equivalent circuit of the product prepared in examples 1-5 of the present invention, respectively; cdlA drawing; (E) the LSV curve comparison plot is tested for stability of the product of example 2 after 5000 cycles of CV and without cycling.
Detailed Description
The following is a detailed description of embodiments of the invention. The embodiment is implemented on the premise of the technical scheme of the invention, and a detailed implementation mode and a specific operation process are given, but the protection scope of the invention is not limited to the following embodiment.
Various modifications to the precise description of the invention will be readily apparent to those skilled in the art from the information contained herein without departing from the spirit and scope of the appended claims. It is to be understood that the scope of the invention is not limited to the procedures, properties, or components defined, as these embodiments, as well as others described, are intended to be merely illustrative of particular aspects of the invention. Indeed, various modifications of the embodiments of the invention which are obvious to those skilled in the art or related fields are intended to be covered by the scope of the appended claims.
For a better understanding of the invention, and not as a limitation on the scope thereof, all numbers expressing quantities, percentages, and other numerical values used in this application are to be understood as being modified in all instances by the term "about". Accordingly, unless expressly indicated otherwise, the numerical parameters set forth in the specification and attached claims are approximations that may vary depending upon the desired properties sought to be obtained. At the very least, each numerical parameter should at least be construed in light of the number of reported significant digits and by applying ordinary rounding techniques.
Example 1 (Co)0.05Ni0.8Preparation of Se Compound
0.238g (1mmol) of nickel chloride hexahydrate (NiCl)2·6H2O) and 0.018g (0.06mmol) of cobalt nitrate hexahydrate (Co (NO)3)2·6H2O) is added into 6mL deionized water in turn, after the mixture is stirred by magnetic force until the mixture is dissolved evenly, 0.845g (5mmol) of sodium selenite (Na) is added2SeO3) And 24mL ethanolamine and 8.5mL hydrazine hydrate (N)2H4·H2O) are added slowly in sequence, and stirring is continued to form a uniform solution. The solution was then poured into a 100mL Teflon lined reactor and allowed to react for 24h at 140 ℃ in an electrically heated forced air drying oven. Washing the obtained product with water and ethanol for multiple times, centrifuging, and freeze-drying in a freeze dryer to obtain Co product0.05Ni0.8Se。
Example 2 (Co)0.1Ni0.75Preparation of Se Compound
0.238g (1mmol) of nickel chloride hexahydrate (NiCl)2·6H2O) and 0.039g (0.1mmol) of cobalt nitrate hexahydrate (Co (NO)3)2·6H2O) is added into 6mL deionized water in turn, after the mixture is stirred by magnetic force until the mixture is dissolved evenly, 0.845g (5mmol) of sodium selenite (Na) is added2SeO3) And 24mL ethanolamine and 8.5mL hydrazine hydrate (N)2H4·H2O) are added slowly in sequence, and stirring is continued to form a uniform solution. The solution was then poured into a 100mL Teflon lined reactor and allowed to react for 24h at 140 ℃ in an electrically heated forced air drying oven. Washing the obtained product with water and ethanol for multiple times, centrifuging, and freeze-drying in a freeze dryer to obtain Co product0.1Ni0.75Se。
Example 3 (Co)0.2Ni0.65Preparation of Se Compound
0.238g (1mmol) of nickel chloride hexahydrate (NiCl)2·6H2O) and 0.09g (0.3mmol) of cobalt nitrate hexahydrate (Co (NO)3)2·6H2O) is added into 6mL deionized water in turn, after the mixture is stirred by magnetic force until the mixture is dissolved evenly, 0.845g (5mmol) of sodium selenite (Na) is added2SeO3) And 24mL ethanolamine and 8.5mL hydrazine hydrate (N)2H4·H2O) successively slowSlowly adding the mixture, and continuously stirring to form a uniform solution. The solution was then poured into a 100mL Teflon lined reactor and allowed to react for 24h at 140 ℃ in an electrically heated forced air drying oven. Washing the obtained product with water and ethanol for multiple times, centrifuging, and freeze-drying in a freeze dryer to obtain Co product0.2Ni0.65Se。
Example 4 (Co)0.3Ni0.55Preparation of Se Compound
0.238g (1mmol) of nickel chloride hexahydrate (NiCl)2·6H2O) and 0.159g (0.5mmol) of cobalt nitrate hexahydrate (Co (NO)3)2·6H2O) is added into 6mL deionized water in turn, after the mixture is stirred by magnetic force until the mixture is dissolved evenly, 0.845g (5mmol) of sodium selenite (Na) is added2SeO3) And 24mL ethanolamine and 8.5mL hydrazine hydrate (N)2H4·H2O) are added slowly in sequence, and stirring is continued to form a uniform solution. The solution was then poured into a 100mL Teflon lined reactor and allowed to react for 24h at 140 ℃ in an electrically heated forced air drying oven. Washing the obtained product with water and ethanol for multiple times, centrifuging, and freeze-drying in a freeze dryer to obtain Co product0.3Ni0.55Se。
Example 5 (Co)0.4Ni0.45Preparation of Se Compound
0.238g (1mmol) of nickel chloride hexahydrate (NiCl)2·6H2O) and 0.259g (0.9mmol) of cobalt nitrate hexahydrate (Co (NO)3)2·6H2O) is added into 6mL deionized water in turn, after the mixture is stirred by magnetic force until the mixture is dissolved evenly, 0.845g (5mmol) of sodium selenite (Na) is added2SeO3) And 24mL ethanolamine and 8.5mL hydrazine hydrate (N)2H4·H2O) are added slowly in sequence, and stirring is continued to form a uniform solution. The solution was then poured into a 100mL Teflon lined reactor and allowed to react for 24h at 140 ℃ in an electrically heated forced air drying oven. Washing the obtained product with water and ethanol for multiple times, centrifuging, and freeze-drying in a freeze dryer to obtain Co product0.4Ni0.45Se。
The physical properties of the products prepared in examples 1-5 were characterized by X-ray diffraction, scanning electron microscope, etc., respectively, wherein:
in FIG. 1, (a) to (e) are X-ray diffraction patterns of the products prepared in examples 1 to 5 of the present invention, respectively.
As can be seen from FIG. 1, the compound Co0.05Ni0.8Se、Co0.1Ni0.75Se、Co0.2Ni0.65Se、Co0.3Ni0.55Se and Co0.4Ni0.45The peak positions of Se are 33.2 DEG, 44.9 DEG, 50.5 DEG, 60.2 DEG, 61.8 DEG, 69.7 DEG, and Ni corresponds to the crystal planes (101), (102), (110), (103), (201), and (202), respectively0.85Cubic Se phase.
FIG. 2 (a) and (b) are SEM photographs of the product prepared in example 1 of the present invention; (c) and (d) is an SEM photograph of the product prepared in example 2; (e) and (f) is an SEM photograph of the product prepared in example 3 of the invention; (g) and (h) is an SEM photograph of the product prepared in example 4 of the invention; (i) and (j) is an SEM photograph of the product prepared in example 5 of the invention.
As can be seen from the SEM photograph of FIG. 2, the product Co obtained in example 10.05Ni0.8The Se morphology is aggregated particles; example 2 product Co0.1Ni0.75The Se morphology is a thin sheet layer; co product from example 30.2Ni0.65Se is more aggregated particles; co product from example 40.3Ni0.55Se is granular; co product from example 50.4Ni0.45Se is also in particulate form.
In addition, the product obtained in example 2 was analyzed by an energy dispersive X-ray spectrometer (EDX) according to the present invention, and the analysis results are shown in table 1 below:
table 1 table of EDX test results for the product obtained in example 2
The results in table 1 further demonstrate the presence of Co, Ni, Se elements in the products produced in the examples.
Application example 1
Adopts a three-electrode system of 0.5M H2SO4In the above-mentioned steps, the products obtained in the above-mentioned examples 1 to 5 were subjected to an electrochemical linear sweep voltammetry test, a cyclic voltammetry test, an electrochemical impedance test, and a chronoamperometric stability test, and the test results of each test method according to a conventional test method known to those skilled in the art are shown in fig. 3.
In FIG. 3, (A), (B), (C), (D) are the LSV curve contrast diagram, Tafel slope contrast diagram, ESI (electrochemical impedance spectroscopy) contrast diagram inserted into the equivalent circuit of the product prepared in examples 1-5 of the present invention, respectively; cdlA drawing; (E) the LSV curve comparison plot is tested for stability of the product of example 2 after 5000 cycles of CV and without cycling.
As can be seen from the electrochemical test results of fig. 3:
(A) in the figure, when the current density jA＝10mA/cm2When (i) is Co, a compound of0.05Ni0.8Se，Co0.1Ni0.75Se， Co0.2Ni0.65Se，Co0.3Ni0.55Se，Co0.4Ni0.45Se hydrogen evolution overpotential is 183mV,153mV,168mV,175 mV,178mV respectively, wherein Co0.1Ni0.75The overpotential of Se is minimum, and the hydrogen evolution performance is best.
In FIG. B, the compound Co0.05Ni0.8Se，Co0.1Ni0.75Se，Co0.2Ni0.65Se，Co0.3Ni0.55Se，Co0.4Ni0.45The Se hydrogen evolution Tafel slopes are 63mV/dec,47mV/dec,50mV/dec,61mV/dec and 55mV/dec respectively, wherein Co is0.1Ni0.75The Se Tafel slope is the lowest, and the hydrogen evolution activity is the highest.
In FIG. C, the compound Co0.05Ni0.8Se，Co0.1Ni0.75Se，Co0.2Ni0.65Se，Co0.3Ni0.55Se,Co0.4Ni0.45Se impedance values are 46.16 omega, 30.23 omega, 34.58 omega and 3 respectively9.79 Ω,42.37 Ω, wherein Co0.1Ni0.75The Se impedance value is lowest, the electrochemical conductivity is best, and the electron transfer rate is fastest.
In FIG. D, the compound Co0.05Ni0.8Se，Co0.1Ni0.75Se，Co0.2Ni0.65Se，Co0.3Ni0.55Se,Co0.4Ni0.45C of SedlThe values are respectively 0.8mF/cm2,1.3mF/cm2,1.19mF/cm2,1.13mF/cm2,0.85mF/cm2In which Co0.1Ni0.75C of SedlThe largest value indicates the largest electrochemically active area and the best catalytic activity.
In FIG. E, the two LSV lines substantially coincide, illustrating Co0.1Ni0.75Se has good stability.
The above test results show that Co prepared in example 2 of the present invention0.1Ni0.75The Se compound shows the most excellent electrocatalytic hydrogen evolution performance. When the current density reaches 10mA/cm2When the catalyst is used, the catalyst has lower hydrogen evolution overpotential eta of 153mV and smaller Tafel slope b of 47mV/dec than other samples.
Claims (5)
1. CoxNi0.85-xA method for preparing a Se fixed ratio compound of the formula CoxNi0.85-xIn Se, x is more than or equal to 0.05 and less than or equal to 0.4, and the method is characterized in that: the preparation method comprises the following steps:
(1) sequentially adding nickel chloride hexahydrate and cobalt nitrate hexahydrate into a small amount of deionized water, stirring and dissolving uniformly, then adding sodium selenite, sequentially and slowly adding an ethanolamine solvent and hydrazine hydrate, and continuously stirring to form a uniform mixed solution; the molar ratio of the cobalt nitrate hexahydrate, the nickel chloride hexahydrate and the sodium selenite is (0.06-0.9): 1: 5; the proportion of the nickel chloride hexahydrate and the deionized water is 0.238 g: 6 mL; the proportion of the nickel chloride hexahydrate to the ethanolamine is 0.238 g: 24 mL; the proportion of the nickel chloride hexahydrate and the hydrazine hydrate is 0.238 g: 8.5 mL;
(2) mixing the mixture obtained in the step (1)Transferring the mixed solution into a polytetrafluoroethylene reaction kettle, sealing, placing the reaction kettle in an electric heating blast drying oven, heating to 140 ℃, reacting for 24 hours at constant temperature, washing and centrifuging the obtained product with water and ethanol for multiple times, and finally drying to obtain the CoxNi0.85-xSe fixed ratio compound; controlling the amount of Co mixed to control the final CoxNi0.85-xThe doping amount of cobalt in Se is adjustable from 0.05 to 0.4.
2. Co according to claim 1xNi0.85-xThe preparation method of the Se fixed ratio compound is characterized in that: the molar ratio of the cobalt nitrate hexahydrate, the nickel chloride hexahydrate and the sodium selenite is 0.1: 1: 5.
3. co according to claim 1xNi0.85-xThe preparation method of the Se fixed ratio compound is characterized in that: the washing and centrifuging mode is as follows: and washing the obtained product with water and ethanol alternately and centrifugally for 3-6 times.
4. Co according to claim 1xNi0.85-xThe preparation method of the Se fixed ratio compound is characterized in that: the drying mode in the step (2) is freeze-drying in a freeze-drying machine.
5. Co produced by the method of any one of claims 1 to 4xNi0.85-xThe application of the Se fixed ratio compound is characterized in that: the compound is used for an electrocatalytic hydrogen evolution catalyst.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466566A (en) * | 2013-08-30 | 2013-12-25 | 天津大学 | Method for synthesizing cobalt diselenide nanocrystal in polyalcohol-base solution |
| CN106492846A (en) * | 2016-10-12 | 2017-03-15 | 吉林大学 | One kind efficiently cracks low overpotential elctro-catalyst of Aquatic product hydrogen and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103466566A (en) * | 2013-08-30 | 2013-12-25 | 天津大学 | Method for synthesizing cobalt diselenide nanocrystal in polyalcohol-base solution |
| CN106492846A (en) * | 2016-10-12 | 2017-03-15 | 吉林大学 | One kind efficiently cracks low overpotential elctro-catalyst of Aquatic product hydrogen and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| Ni-Co-Se nanoparticles modified reduced graphene oxide nanoflakes,an advance electrocatalyst for highly efficient hydrogen evolution reaction;Behzad Rezaei et al.;《Electrochimica Acta》;20160725;第213卷;第423-431页 * |
| Shape-controllable syntheses of ternary Ni-Co-Se alloy hollow microspheres as highly efficient catalytic materials for dye-sensitized solar cells;Li Shao et al.;《Chemical Engineering Journal》;20170117;第315卷;第563页右栏第2段 * |
| Three-dimensional-networked Ni-Co-Se nanosheet/nanowire arrays on carbon cloth: A flexible electrode for efficient hydrogen evolution;Zhen Zhang et al.;《Electrochimica Acta》;20160401;第200卷;第142-151页 * |
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