CN112391646A - beta-Ni (OH) prepared by solvothermal method2Electrode and method and use - Google Patents
beta-Ni (OH) prepared by solvothermal method2Electrode and method and use Download PDFInfo
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- CN112391646A CN112391646A CN202011160487.1A CN202011160487A CN112391646A CN 112391646 A CN112391646 A CN 112391646A CN 202011160487 A CN202011160487 A CN 202011160487A CN 112391646 A CN112391646 A CN 112391646A
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Abstract
The invention discloses a beta-Ni (OH) prepared by a solvothermal method2The method adopts a solvent method, takes a foam nickel sheet as a substrate, takes an ethanol solution of vanadium chloride and urea as a vanadium source, takes cetyl trimethyl ammonium bromide as a morphology regulator, and leads Ni (OH) to be mixed with the electrolyte2Vertically arranged on a foam nickel sheet base, exposes catalytic site activity with high density and large surface area, accelerates electron transfer rate, is favorable for improving electrocatalytic performance, and the foam nickel sheet base is not only favorable for electron transmission, nickel comes from the original position, and generated Ni (OH)2beta-Ni (OH) which is tightly connected with foamed nickel and has more stable structure and is prepared2The electrode has advantagesThe product has different electrocatalysis performance, is applied to the electrolytic water catalytic reaction under the alkaline condition, and improves the electrocatalysis hydrogen production and oxygen production performance of the electrolytic water.
Description
Technical Field
The invention belongs to the field of new energy material preparation, and particularly relates to beta-Ni (OH) prepared by a solvothermal method2An electrode and a method and application.
Background
At present, the demand of modern industry development for energy in various countries in the world is rapidly increased, but since the end of the twentieth century, people face huge energy crisis and increasingly serious environmental pollution problems, so that the conservation of limited energy and the pollution treatment are urgent. The research of electrocatalytic science just meets the requirement. Recent researches show that transition metals and oxides, hydroxides, nitrides, phosphates and selenides thereof not only show excellent HER and OER electrochemical performances in alkaline electrolyte solutions, but also have the advantages of low price, abundant earth resources and the like.
From the current research situation, a plurality of technologists mainly research on the novel foam nickel electrode by filling active substances Ni (OH) by a direct loading method (a slurry scraping method)2This is believed to simplify the process and reduce the cost. This practice is not necessarily the best, despite the literature over the last decade. First, the direct loading technique is used, and the key is how to prepare highly active Ni (OH)2And the adjustment of various parameters, such as material distribution, filling density, pulp scraping pressure and the like. Secondly, whether the activity of the nickel electrode can be improved or not, it is also required to see the highly active Ni (OH)2The process has not changed after the direct loading method. The novel foam nickel electrode manufactured by the direct loading method has high conductivity and the basic structure is close to that of the bonded nickel electrode. In addition, the use of cobalt oxyhydroxides as additives also has a great effect on improving the properties of nickel electrodes, but has its own disadvantages, and thus, Ni (OH)2The acquisition of the method is a prerequisite basis for the bulk density, the surface appearance and the structure of the material, and a method for preparing high-quality Ni (OH) is found2The method of (2) is of great importance.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides a solvent thermal method for preparationβ-Ni(OH)2The electrode, the method and the application have the advantages of simple preparation process, low preparation cost, short preparation period, easy control of the process, and beta-Ni (OH) prepared2The electrode exposes out the catalytic site activity with high density and large surface area, accelerates the electron transfer rate and is beneficial to improving the electrocatalytic performance.
In order to achieve the above purpose, the invention provides a solvothermal method for preparing beta-Ni (OH)2A method of manufacturing an electrode, comprising the steps of:
1) cleaning and drying the foamed nickel for later use;
2) weighing 38.753-39.567 g of vanadium chloride and 73-77 mg of urea, dissolving the vanadium chloride and 73-77 mg of urea in 20-25 mL of ethanol solution, and uniformly stirring to obtain a mixed solution;
3) putting 210-220 mg of the foamed nickel obtained in the step 1) into the mixed solution, adding 0.345-0.465 g of hexadecyl trimethyl ammonium bromide into the mixed solution, uniformly stirring, and reacting at the temperature of 145-155 ℃;
4) after the reaction is finished and the temperature is naturally cooled to the room temperature, taking out the foamed nickel, cleaning and drying to obtain the beta-Ni (OH)2And an electrode.
Further, in the step 1), the foamed nickel is firstly ultrasonically cleaned in an acetone solution, then is alternately cleaned for a plurality of times by deionized water and absolute ethyl alcohol, and is dried in a vacuum box at room temperature after being cleaned.
Further, the foamed nickel is cut into 1.5 multiplied by 4.0cm in the step 1)2A rectangular plate.
Further, in the step 2), the molar ratio is (2-3): 1, weighing deionized water and absolute ethyl alcohol to prepare an ethanol solution.
Further, the stirring in the step 2) and the step 3) is carried out at room temperature for 30-35 min.
Further, the reaction time in the step 3) is 21-25 h.
Further, in the step 4), the cleaning is repeatedly performed with deionized water and absolute ethyl alcohol.
Further, the drying in the step 4) is carried out for 7-8 hours at room temperature by adopting a vacuum drying oven.
The invention also provides a beta-Ni (OH)2The electrode is prepared by the method.
The invention also provides the beta-Ni (OH)2And the electrode is applied to electrolytic water catalytic reaction under alkaline conditions.
Compared with the prior art, the invention has the following advantages:
1) compared with the preparation method, in the existing method, the chemical precipitation method has higher requirement on the control precision of the pH value; the conversion rate of nickel powder in the powder metal method is limited to a certain extent and the equipment is complex; the electrolytic process requires strict control of the composition of the electrolytic solution and the operation procedure of the electrolytic process, and the current efficiency is low. The solvent method adopted by the invention has the characteristics of simple process, short preparation period and easy control of reaction conditions, the reaction process and the morphology size are controlled by adjusting the temperature, various special structural morphologies can be obtained, and different morphological characteristics have great influence on the performance of the material. It overcomes the defects of difficult occurrence and control, low yield, complex process and the like of the traditional preparation process.
2) The foam nickel sheet base is not only beneficial to the transmission of electrons, and the nickel comes from the original position and is generated with Ni (OH)2The structure is more stable because the foam nickel is tightly connected with the foam nickel.
3) The hexadecyl trimethyl ammonium bromide can control the crystal growth power, thereby obtaining a specific shape and selectively exposing a specific crystal face.
4) Vertically arranged on foam nickel base Ni (OH)2The catalytic site activity with high density and large surface area is exposed, the electron transfer rate is accelerated, and the electrocatalytic performance is favorably improved.
Drawings
FIG. 1 is a beta-Ni (OH) prepared in example 1 of the present invention2XRD pattern of the electrode;
FIG. 2 is a beta-Ni (OH) prepared in example 2 of the present invention2SEM images of the electrodes;
FIG. 3 is a beta-Ni (OH) prepared in example 3 of the present invention2A linear sweep voltammetry performance diagram of electrode hydrogen production;
FIG. 4 is a beta-Ni (OH) prepared in example 3 of the present invention2Linear sweep voltammogram performance plots of electrode oxygen production.
Detailed Description
The present invention will be further explained with reference to the drawings and specific examples in the specification, and it should be understood that the examples described are only a part of the examples of the present application, and not all examples. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present application.
The invention provides a solvothermal method for preparing beta-Ni (OH)2A method of manufacturing an electrode, comprising the steps of:
1) cleaning and drying the foamed nickel for later use; preferably, the nickel foam is cut into 1.5X 4.0cm2The foam nickel is firstly cleaned by ultrasonic in acetone solution, then cleaned by deionized water and absolute ethyl alcohol alternately for a plurality of times, and dried in a vacuum box at room temperature, wherein the room temperature is defined as 25 ℃.
2) Weighing 38.753-39.567 g of vanadium chloride and 73-77 mg of urea, dissolving the vanadium chloride and 73-77 mg of urea in 20-25 mL of ethanol solution, and uniformly stirring to obtain a mixed solution; preferably, the molar ratio is (2-3): 1, weighing deionized water and absolute ethyl alcohol to prepare an ethanol solution. Stirring is carried out at room temperature for 30-35 min.
3) Putting 210-220 mg of the foamed nickel obtained in the step 1) into the mixed solution, adding 0.345-0.465 g of hexadecyl trimethyl ammonium bromide into the mixed solution, uniformly stirring, and reacting at the temperature of 145-155 ℃; preferably, the reaction time is 21-25 h. Stirring is carried out at room temperature for 30-35 min.
4) After the reaction is finished and the temperature is naturally cooled to the room temperature, taking out the foamed nickel, cleaning and drying to obtain the beta-Ni (OH)2And an electrode. Preferably, the cleaning is repeatedly washed by deionized water and absolute ethyl alcohol for many times, and the drying is carried out for 7-8 hours at room temperature by using a vacuum drying oven.
The invention also provides beta-Ni (OH) prepared by the method2Electrode, produced Ni (OH)2Closely connected with the foam nickel, stable structure, cetyl trimethyl ammonium bromide to control the crystal growth power, thereby obtaining a specific shape, selectively exposing a specific crystal face, and vertically arranging Ni (OH) on the foam nickel substrate2Exposing high density, large surface area catalytic site activity, accelerating electron transfer rate, facilitating improvement of its electrocatalytic properties, beta-Ni (OH)2The electrode is applied to the electrolytic water catalytic reaction under the alkaline condition, and the electro-catalysis hydrogen production and oxygen production performance of the electrolytic water is improved.
The invention is described below with reference to specific examples:
example 1:
1) cutting the foamed nickel into 1.5 × 4.0cm2Cleaning the rectangular sheet, and drying the rectangular sheet in a vacuum box at room temperature;
2) the molar ratio of the components is (2-3): 1, weighing deionized water and absolute ethyl alcohol, preparing 20mL of ethanol solution, weighing 38.753-39.567 g of vanadium chloride and 73-77 mg of urea, dissolving the vanadium chloride and the urea in the solution consisting of the deionized water and the absolute ethyl alcohol, stirring the solution at room temperature for 30min, and then adding 210-220 mg of treated foam nickel to obtain mixed solution;
3) then adding 0.345-0.465 g of cetyl trimethyl ammonium bromide morphology regulating agent into the mixed solution, stirring for 30min at room temperature, and then placing the mixed solution in an oven to react for 21h at 155 ℃;
4) after the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, and repeatedly washing the foamed nickel for five times by using ultrapure water and absolute ethyl alcohol respectively;
5) finally, putting the washed foam nickel into a vacuum drying oven to be dried for 8h at room temperature to obtain Ni (OH)2Free standing electrodes, i.e. beta-Ni (OH)2And an electrode.
For beta-Ni (OH) prepared in example 12The electrode was subjected to X-ray diffraction, and from FIG. 1, it can be observed that beta-Ni (OH) prepared in example 12XRD spectrum of electrode Ni (OH)2The diffraction peak of (A) is consistent with that of PDF #14-011 card, and proves that the Ni (OH) is successfully synthesized on a foam nickel substrate (PDF #87-0712)2。
Example 2:
1) cutting the foamed nickel into 1.5 × 4.0cm2Cleaning the rectangular sheet, and drying the rectangular sheet in a vacuum box at room temperature;
2) the molar ratio of the components is (2-3): 1, weighing deionized water and absolute ethyl alcohol to prepare 20mL of ethanol solution, weighing 38.753-39.567 g of vanadium chloride and 73-77 mg of urea, dissolving the vanadium chloride and the urea in the ethanol solution, stirring the solution at room temperature for 30min, and then adding 210-220 mg of processed foam nickel to obtain mixed solution;
3) then adding 0.345-0.465 g of cetyl trimethyl ammonium bromide morphology regulating agent into the mixed solution, stirring for 30min at room temperature, and then placing the mixed solution in an oven to react for 22h at 153 ℃;
4) after the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, and repeatedly washing the foamed nickel for five times by using ultrapure water and absolute ethyl alcohol respectively;
5) finally, putting the washed foam nickel into a vacuum drying oven to be dried for 8h at room temperature to obtain Ni (OH)2Free standing electrodes, i.e. beta-Ni (OH)2And an electrode.
Ni (OH) prepared in example 22Electron microscopy scanning of the free-standing electrode, see FIG. 2, from which FIG. 2 it can be observed that sample Ni (OH) prepared in example 22The self-supporting electrodes are vertically grown on the foam nickel and vertically arranged on the foam nickel substrate Ni (OH)2Expose high-density large-surface area catalytic site activity, accelerate electron transfer rate, facilitate to improve its electrocatalytic performance, and generate Ni (OH)2The structure is more stable because the foam nickel is tightly connected with the foam nickel.
Example 3:
1) cutting the foamed nickel into 1.5 × 4.0cm2Cleaning the rectangular sheet, and drying the rectangular sheet in a vacuum box at room temperature;
2) the molar ratio of the components is (2-3): 1, weighing deionized water and absolute ethyl alcohol to prepare 20mL of ethanol solution, weighing 38.753-39.567 g of vanadium chloride and 73-77 mg of urea, dissolving the vanadium chloride and the urea in the ethanol solution, stirring the solution at room temperature for 30min, and then adding 210-220 mg of processed foam nickel to obtain mixed solution;
3) then adding 0.345-0.465 g of cetyl trimethyl ammonium bromide morphology regulating agent into the mixed solution, stirring for 30min at room temperature, and then placing the mixed solution in an oven to react for 23h at 150 ℃;
4) after the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, and repeatedly washing the foamed nickel for five times by using ultrapure water and absolute ethyl alcohol respectively;
5) finally, putting the washed foam nickel into a vacuum drying oven to be dried for 8h at room temperature to obtain Ni (OH)2A self-supporting electrode.
For Ni (OH) prepared in example 32The self-supporting electrode was subjected to electrocatalytic hydrogen production and oxygen production test, referring to FIGS. 3 and 4, from which Ni (OH) prepared in example 3 can be seen2Linear sweep voltammogram of a self-supporting electrode at a current density of 100mA/cm2The overpotential of hydrogen production is 245-255 mV, and the current density is 100mA/cm2The oxygen generation overpotential is 410-420 mV, and the electrode has good electrocatalysis performance.
Example 4:
1) cutting the foamed nickel into 1.5 × 4.0cm2Cleaning the rectangular sheet, and drying the rectangular sheet in a vacuum box at room temperature;
2) the molar ratio of the components is (2-3): 1, weighing deionized water and absolute ethyl alcohol to prepare 20mL of ethanol solution, weighing 38.753-39.567 g of vanadium chloride and 73-77 mg of urea, dissolving the vanadium chloride and the urea in the ethanol solution, stirring the solution at room temperature for 30min, and then adding 210-220 mg of processed foamed nickel to obtain mixed solution;
3) then adding 0.345-0.465 g of cetyl trimethyl ammonium bromide morphology regulating agent into the mixed solution, stirring for 30min at room temperature, and then placing the mixed solution in an oven to react for 24h at 147 ℃;
4) after the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, and repeatedly washing the foamed nickel for five times by using ultrapure water and absolute ethyl alcohol respectively;
5) finally, putting the washed foam nickel into a vacuum drying oven to be dried for 8h at room temperature to obtain Ni (OH)2A self-supporting electrode.
Example 5:
1) cutting the foamed nickel into 1.5 × 4.0cm2Cleaning the rectangular sheet, and drying the rectangular sheet in a vacuum box at room temperature;
2) the molar ratio of the components is (2-3): 1, weighing deionized water and absolute ethyl alcohol to prepare 20mL of ethanol solution, weighing 38.753-39.567 g of vanadium chloride and 73-77 mg of urea, dissolving the vanadium chloride and the urea in the ethanol solution, stirring the solution at room temperature for 30min, and then adding 210-220 mg of treated foam nickel to obtain mixed solution;
3) then adding 0.345-0.465 g of cetyl trimethyl ammonium bromide morphology regulating agent into the mixed solution, stirring for 30min at room temperature, and then placing the mixed solution in an oven to react for 25h at 145 ℃;
4) after the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, and repeatedly washing the foamed nickel for five times by using ultrapure water and absolute ethyl alcohol respectively;
5) finally, putting the washed foam nickel into a vacuum drying oven to be dried for 8h at room temperature to obtain Ni (OH)2A self-supporting electrode.
Example 6:
1) cutting the foamed nickel into 1.5 × 4.0cm2Cleaning the rectangular sheet, and drying the rectangular sheet in a vacuum box at room temperature;
2) the molar ratio of the raw materials is 2: 1, weighing deionized water and absolute ethyl alcohol to prepare 21mL of ethanol solution, weighing 38.753g of vanadium chloride and 73mg of urea, dissolving the vanadium chloride and the urea in the ethanol solution, stirring the solution at room temperature for 30min, and then adding 210mg of treated foam nickel to obtain mixed solution;
3) then 0.345g of cetyl trimethyl ammonium bromide morphology regulating agent is added into the mixed solution, the mixture is stirred for 30min at room temperature, and then the mixed solution is placed in an oven to react for 21h at 145 ℃;
4) after the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, and repeatedly washing the foamed nickel for five times by using ultrapure water and absolute ethyl alcohol respectively;
5) finally, the washed foam nickel is put into a vacuum drying oven to be dried for 7h at room temperature to obtain Ni (OH)2A self-supporting electrode.
Example 7:
1) cutting the foamed nickel into 1.5 × 4.0cm2Cleaning the rectangular sheet, and drying the rectangular sheet in a vacuum box at room temperature;
2) the molar ratio of the components is 3: 1, weighing deionized water and absolute ethyl alcohol to prepare 25mL of ethanol solution, weighing 39.567g of vanadium chloride and 73-77 mg of urea, dissolving the vanadium chloride and the urea in the ethanol solution, stirring at room temperature for 35min, and then adding 220mg of treated foam nickel to obtain mixed solution;
3) then 0.465g of cetyl trimethyl ammonium bromide morphology regulating agent is added into the mixed solution, the mixed solution is stirred for 35min at room temperature, and then the mixed solution is placed in an oven to react for 25h at 155 ℃;
4) after the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, and repeatedly washing the foamed nickel for five times by using ultrapure water and absolute ethyl alcohol respectively;
5) finally, putting the washed foam nickel into a vacuum drying oven to be dried for 8h at room temperature to obtain Ni (OH)2A self-supporting electrode.
Example 8:
1) cutting the foamed nickel into 1.5 × 4.0cm2Cleaning the rectangular sheet, and drying the rectangular sheet in a vacuum box at room temperature;
2) the molar ratio of the components is 2.5: 1, weighing deionized water and absolute ethyl alcohol to prepare 23mL of ethanol solution, weighing 39.160g of vanadium chloride and 75mg of urea, dissolving the vanadium chloride and the urea in the ethanol solution, stirring for 33min at room temperature, and then adding 215mg of treated foam nickel to obtain mixed solution;
3) then 0.415g of cetyl trimethyl ammonium bromide morphology control agent is added into the mixed solution, the mixed solution is stirred for 32min at room temperature, and then the mixed solution is placed in an oven to react for 23h at 151 ℃;
4) after the reaction is finished, naturally cooling to room temperature, taking out the foamed nickel, and repeatedly washing the foamed nickel for five times by using ultrapure water and absolute ethyl alcohol respectively;
5) finally, the washed foam nickel is put into a vacuum drying oven to be dried for 7.5h at room temperature to obtain Ni (OH)2A self-supporting electrode. The solvent method adopted by the method takes a foam nickel sheet as a substrate, takes an ethanol solution of vanadium chloride and urea as a vanadium source, takes cetyl trimethyl ammonium bromide as a morphology regulator, and leads Ni (OH)2The catalyst is vertically arranged on the foam nickel sheet base, the activity of the catalytic sites with high density and large surface area is exposed, the electron transfer rate is accelerated, the electrocatalytic performance of the catalyst is improved, the foam nickel sheet base is not only favorable for the transmission of electrons, and the nickel comes from the original position and is generatedResultant Ni (OH)2beta-Ni (OH) which is tightly connected with foamed nickel and has more stable structure and is prepared2The electrode has excellent electro-catalysis performance, is applied to the electrolytic water catalytic reaction under the alkaline condition, and improves the electro-catalysis hydrogen production and oxygen production performance of the electrolytic water.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; although the present 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 solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. Solvothermal method for preparing beta-Ni (OH)2A method of manufacturing an electrode, comprising the steps of:
1) cleaning and drying the foamed nickel for later use;
2) weighing 38.753-39.567 g of vanadium chloride and 73-77 mg of urea, dissolving the vanadium chloride and 73-77 mg of urea in 20-25 mL of ethanol solution, and uniformly stirring to obtain a mixed solution;
3) putting 210-220 mg of the foamed nickel obtained in the step 1) into the mixed solution, adding 0.345-0.465 g of hexadecyl trimethyl ammonium bromide into the mixed solution, uniformly stirring, and reacting at the temperature of 145-155 ℃;
4) after the reaction is finished and the temperature is naturally cooled to the room temperature, taking out the foamed nickel, cleaning and drying to obtain the beta-Ni (OH)2And an electrode.
2. A solvothermal preparation of β -ni (oh) according to claim 12The method for preparing the electrode is characterized in that in the step 1), the foamed nickel is firstly ultrasonically cleaned in an acetone solution, then is alternately cleaned for a plurality of times by deionized water and absolute ethyl alcohol, and is dried in a vacuum box at room temperature after being cleaned.
3. The method of claim 1Solvothermal method for preparing beta-Ni (OH)2The method for preparing the electrode is characterized in that the foamed nickel is cut into 1.5 multiplied by 4.0cm in the step 1)2A rectangular plate.
4. A solvothermal preparation of β -ni (oh) according to claim 12The electrode method is characterized in that in the step 2), the molar ratio is (2-3): 1, weighing deionized water and absolute ethyl alcohol to prepare an ethanol solution.
5. A solvothermal preparation of β -ni (oh) according to claim 12The electrode method is characterized in that stirring in the step 2) and the step 3) is carried out at room temperature for 30-35 min.
6. A solvothermal preparation of β -ni (oh) according to claim 12The electrode method is characterized in that the reaction time in the step 3) is 21-25 h.
7. A solvothermal preparation of β -ni (oh) according to claim 12The method for cleaning the electrode is characterized in that deionized water and absolute ethyl alcohol are repeatedly used for washing in the step 4).
8. A solvothermal preparation of β -Ni (OH) according to claim 72The method for preparing the electrode is characterized in that the drying in the step 4) adopts a vacuum drying oven to dry for 7-8 hours at room temperature.
9. beta-Ni (OH)2Electrode, characterized in that beta-Ni (OH) is prepared by solvothermal method according to any one of claims 1 to 82The electrode is prepared by a method.
10. A beta-ni (oh) according to claim 92And the electrode is applied to electrolytic water catalytic reaction under alkaline conditions.
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CN110760879A (en) * | 2019-11-05 | 2020-02-07 | 陕西科技大学 | NiV-LDH/NF hydrogen production electrode with optimized electronic structure and preparation method and application thereof |
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