CN110306204B - Silver-doped layered nickel hydroxide composite electrode material and preparation method and application thereof - Google Patents
Silver-doped layered nickel hydroxide composite electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a silver-doped layered nickel hydroxide composite electrode material and a preparation method and application thereof. The composite electrode material is characterized in that foam nickel is used as a substrate, and layered nickel hydroxide grows on the surface of the foam nickel; the layered nickel hydroxide is doped with silver. The composite electrode material has strong corrosion resistance under alkaline conditions, good material conductivity and excellent hydrogen evolution performance. The preparation steps of the material comprise: firstly, preparing a precursor salt solution in the first step; then adding a small amount of silver ammonia solution to obtain a precursor solution in the second step; and then putting the pretreated foamed nickel into the reactor, and generating silver-doped layered nickel hydroxide by adopting a hydrothermal method. The invention adopts a one-step hydrothermal method to realize the combination of the surface active substance and the foam nickel substrate, has simple preparation process, time saving and low energy consumption, meets the requirements of energy saving and environmental protection, and can realize industrial production; the obtained product has higher conductivity and hydrogen evolution catalytic activity.
Description
Technical Field
The invention relates to a silver-doped layered nickel hydroxide composite electrode material and a preparation method and application thereof, belonging to the technical field of electrolytic water catalytic hydrogen evolution.
Technical Field
Hydrogen has been widely paid attention as an important chemical raw material, and is widely applied to various fields of petroleum processing, industrial ammonia synthesis, metal smelting and the like, and plays a very important role in national economy. In recent years, as non-renewable fossil energy such as petroleum and coal is gradually exhausted, and the greenhouse effect caused by the emission of a large amount of greenhouse gas such as carbon dioxide, which is a combustion product of the fossil energy, is increasingly intensified, research is focused in all countries of the world to research and develop new energy. Hydrogen energy is a very superior new energy source, and has the main advantages that: high combustion heat value, cleanness, no pollution, rich resources, wide application range and the like. The selection of the hydrogen production method is crucial to the wide use of hydrogen. The hydrogen production method mainly comprises the steps of water electrolysis hydrogen production, water photolysis hydrogen production, mineral fuel hydrogen production, biomass hydrogen production, hydrogen production by other hydrogen-containing substances, recovery of hydrogen produced by various chemical processes and the like. Wherein the electrocatalytic decomposition of water to produce hydrogen is the most important way for producing hydrogen on a large scale. For the electrolytic hydrogen production industry, the development is mainly restricted by higher cost, the bottleneck of the electrolytic hydrogen production development lies in high energy consumption and low energy conversion efficiency, and the cathode hydrogen evolution electrode material with high catalytic activity plays an important role in reducing the energy consumption of the electrolytic hydrogen production and improving the energy conversion efficiency, so that the design and preparation of the novel cathode catalytic hydrogen evolution material have great significance for the industrial application of the electrolytic hydrogen production.
The hydrogen evolution overpotential can be reduced by reasonably designing the hydrogen evolution electrode material, and the energy consumption and the cost of hydrogen production are reduced. The excellent hydrogen evolution electrode has the following characteristics besides the excellent catalytic hydrogen evolution activity of the material: large specific surface area; the corrosion resistance is better in strong alkaline solution, and the working can be stably carried out for a long time; low manufacturing and maintenance costs, etc. Due to the characteristics of the hydrothermal method, the produced particles have high purity, good dispersibility, good and controllable crystal form and low production cost. The nickel-based material shows excellent corrosion resistance in alkaline solution, so that the nickel-based material is reasonably designed, the catalytic activity of the material is improved, and the nickel-based material has positive significance for reducing the production cost and energy consumption of electrolytic hydrogen production.
Disclosure of Invention
Aiming at the defects in the prior art, the invention aims to provide a silver-doped layered nickel hydroxide composite electrode material, a preparation method and application thereof, wherein the composite electrode material has better conductivity and catalytic activity, the preparation method realizes the combination of a surface active substance and a foam nickel substrate by a one-step hydrothermal method, the preparation process is simple, the equipment requirement is low, the energy consumption is low, and the industrial large-scale production can be realized.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
the silver-doped layered nickel hydroxide composite electrode material is characterized in that foamed nickel is used as a substrate, and layered oxyhydrogen is grown on the surface of the foamed nickelNickel is melted; the layered nickel hydroxide is doped with silver. The composite electrode material has the advantage of having its surface active species (Ni (OH))2And Ag2O) is tightly combined with the foamed nickel substrate, the corrosion resistance is strong under the alkaline condition, the conductivity of the material is good, and the hydrogen evolution performance is greatly improved.
The invention also provides a preparation method of the silver-doped layered nickel hydroxide composite electrode material, which comprises the following steps:
1) preparing a first-step precursor salt solution by using urea, ammonium fluoride and deionized water as raw materials;
2) adding a silver ammonia solution into the precursor salt solution of the first step to prepare a precursor salt solution of the second step;
3) and (3) putting the foamed nickel into the precursor salt solution in the second step, carrying out hydrothermal reaction, and after the reaction is finished, washing and drying the product to obtain the silver-doped layered nickel hydroxide composite electrode material.
According to the above scheme, preferably, the molar ratio of urea to ammonium fluoride in step 1) is 4: 1. more preferably, the amount ratio of the ammonium fluoride to the deionized water is 0.01 to 0.05 mol: 1L of the compound.
According to the scheme, preferably, the raw material in the step 1) further comprises a nickel salt, and the molar ratio of the nickel salt to the urea and the ammonium fluoride is 1:4: 1. More preferably, the nickel salt is nickel nitrate, nickel sulfate or nickel chloride. More preferably, the ratio of the nickel salt to the deionized water is 0.01-0.05 mol: 1L of the compound.
According to the scheme, preferably, the pH value of the silver ammonia solution in the step 2) is 7-8, and the silver ammonia solution is prepared from a silver nitrate solution with a concentration of 0.1-0.2 mol/L and ammonia water.
According to the scheme, the molar amount of the silver ammonia solution in the step 2) is 3/10 which is the molar amount of the ammonium fluoride in the step 1).
According to the scheme, preferably, the purity of the foamed nickel in the step 3) is more than 99.8 percent, and the areal density is 300-450g/cm2。
According to the scheme, preferably, the foamed nickel in the step 3) is pretreated for removing surface oil stains and oxide pollution layers, and is removed by an ultrasonic method after being soaked in an organic solvent and an acid solution. More preferably, the organic solvent is one or more of methanol, ethanol, tetrahydrofuran or chloroform, the acid is diluted hydrochloric acid, and the ultrasonic treatment time is 10-50 min.
According to the scheme, the temperature of the hydrothermal reaction in the step 3) is preferably 160 ℃, and the time is 6-8 hours.
The invention also provides application of the layered nickel hydroxide composite electrode material, which is characterized in that the composite electrode material can be used as an electrode or a catalyst for hydrogen production by water electrolysis.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
(1) the composite electrode material is prepared by taking foamed nickel as a substrate and adopting a one-step hydrothermal method, and the prepared composite electrode material is good in corrosion resistance and controllable in shape; and the nickel-based metal has low price and stable catalytic performance under alkaline conditions.
(2) The preparation method of the silver-doped layered nickel hydroxide composite electrode material adopts a one-step hydrothermal method, has simple process, does not need post-treatment, has low energy consumption in the preparation process, and is convenient for realizing industrial production.
(3) The silver-doped layered nickel hydroxide composite electrode material prepared by the invention has better conductivity and higher catalytic activity. Compared with a pure nickel hydroxide material, the composite electrode material provided by the invention has the current density of 10mA/cm2When the catalyst is used, the hydrogen evolution performance is improved by 150 mv.
(4) The active component Ni (OH) in the silver-doped layered nickel hydroxide composite electrode material prepared by the invention2And Ag2O is an amorphous structure, has excellent performance, can be widely used as an alkaline electrolysis water hydrogen evolution electrode material, and has wide application prospect.
Drawings
FIG. 1 shows the layered Ni (OH) prepared in comparative example 1 of the present invention2Scanning the surface topography of the foamed nickel electrode material.
FIG. 2 shows Ag prepared in example 1 of the present invention2O/Ni(OH)2FoamScanning the surface topography of the nickel composite electrode material.
FIG. 3 shows Ag prepared in example 2 of the present invention2O/Ni(OH)2Scanning the surface topography of the foamed nickel composite electrode material.
FIG. 4 is a linear sweep voltammetry curve diagram of pure nickel foam obtained by the test of the present invention, and the composite electrode materials prepared in comparative example 1 and examples 1-2.
Detailed Description
Comparative example 1
Layered Ni (OH)2The preparation method of the foamed nickel composite electrode material comprises the following steps:
a. pretreatment of a foamed nickel substrate:
selecting the cut 1X 3cm2The nickel foam (purity: 99.8%, areal density: 400 g/cm)2) Soaking in absolute ethyl alcohol, carrying out ultrasonic treatment for 15min, then using 2mol/L hydrochloric acid for further ultrasonic treatment for 15min, and removing oil stains and oxide pollution layers on the surface; finally, the foam nickel substrate is washed clean by deionized water.
b. Hydrothermal reaction on pretreated nickel foam to form Ni (OH)2：
1mmol of nickel nitrate, 4mmol of urea and 1mmol of ammonium fluoride are dissolved in 40ml of deionized water to obtain a precursor salt solution. And (b) placing the foamed nickel substrate pretreated in the step (a) into the precursor salt solution, performing hydrothermal reaction for 6 hours in a high-pressure reaction kettle at 160 ℃, and washing and drying a product after the reaction is finished to obtain the foamed nickel material with the layered nickel hydroxide growing on the surface.
FIG. 1 shows the layered Ni (OH) prepared in this comparative example2Scanning electron microscope image of the surface appearance of the/foamed nickel composite nano material.
Example 1
Ag2O/Ni(OH)2The preparation method of the foamed nickel composite electrode material comprises the following steps:
a. pretreatment of a foamed nickel substrate: the procedure is as in step a of comparative example 1.
b. One-step hydrothermal reaction on pretreated foamed nickel to form Ag2O/Ni(OH)2：
1) 4mmol urea and 1mmol ammonium fluoride were dissolved in 40ml deionized water to obtain the first step precursor solution. Ammonia water is dripped into silver nitrate solution with the concentration of 0.15mol/L to prepare silver ammonia solution with the pH value of about 7.6. And adding 2mL of prepared silver ammonia solution into the precursor solution in the first step to obtain a precursor solution in the second step.
2) And b, putting the foamed nickel substrate pretreated in the step a into the precursor solution in the second step, performing hydrothermal reaction for 6 hours in a high-pressure reaction kettle at 160 ℃, washing and drying the product to obtain the layered nickel hydroxide composite electrode material (Ag) with silver growing in the pores of the sheet layer2O/Ni(OH)2/foamed nickel composite electrode material).
FIG. 2 shows Ag obtained in this example2O/Ni(OH)2Scanning electron microscope image of the surface appearance of the/foamed nickel composite electrode material.
Example 2
Ag2O/Ni(OH)2The preparation method of the foamed nickel composite electrode material comprises the following steps:
a. pretreatment of a foamed nickel substrate: the procedure is as in step a of comparative example 1.
b. One-step hydrothermal reaction on pretreated foamed nickel to form Ag2O/Ni(OH)2：
1) 1mmol of nickel nitrate, 4mmol of urea and 1mmol of ammonium fluoride are dissolved in 40ml of deionized water to obtain a precursor salt solution in the first step. Ammonia water is dripped into silver nitrate solution with the concentration of 0.15mol/L to prepare silver ammonia solution with the pH value of about 7.6. And adding 2mL of prepared silver ammonia solution into the precursor solution in the first step to obtain a precursor solution in the second step.
2) And b, putting the foamed nickel substrate pretreated in the step a into the precursor solution in the second step, performing hydrothermal reaction for 6 hours in a high-pressure reaction kettle at 160 ℃, washing and drying the product to obtain the layered nickel hydroxide composite material (Ag) with the surface growing and covered with silver2O/Ni(OH)2/foamed nickel composite electrode material).
FIG. 3 is a scanning electron microscope image of the surface topography of the layered nickel hydroxide composite electrode material with silver coating grown on the surface prepared in this example.
And (4) analyzing results:
as is clear from the scanning electron micrographs of fig. 1 to 3, in comparative example 1, the lamellar nickel hydroxide was uniformly grown on the foamed nickel; in the embodiment 1, the nickel hydroxide in the sheet layer uniformly grows on the foamed nickel, and the silver oxide nano particles are doped among pores of the sheet layer; in example 2, the silver oxide nanoparticles are uniformly coated on the sheet layer, and small silver oxide nanoparticles are doped among pores of the sheet layer, so that the conductivity and the catalytic activity of the material can be greatly enhanced.
And (3) effect testing:
the composite electrode material prepared in the comparative example 1 and the examples 1 to 2 is applied to hydrogen production by water electrolysis catalysis as an electrolytic water electrode, and pure nickel foam is used as a blank control.
The pure nickel foam and the composite electrode materials prepared respectively in the three examples are subjected to a linear sweep voltammetry curve test:
in the testing process, a three-electrode system is adopted, 1mol/L KOH is used as electrolyte, a carbon rod is used as a counter electrode, a saturated calomel electrode is used as a reference electrode, foamed nickel and composite electrode materials prepared in three embodiments are respectively used as working electrodes in sequence for testing, the foamed nickel and the composite electrode materials prepared in the three embodiments are guaranteed to have the same geometric area, and the testing result is shown in figure 4.
As can be seen from FIG. 4, when the current density was 10mA/cm2In comparison with pure nickel foam, the performances of the silver-doped layered nickel hydroxide composite electrode materials prepared in the examples 1 and 2 are greatly improved. As can be seen from the comparison, when the silver-doped layered nickel hydroxide composite electrode materials prepared in examples 1 and 2 of the present invention are used as an electrolytic water catalyst, the silver-doped layered nickel hydroxide composite electrode material has good conductivity and excellent catalytic performance, compared with the pure layered nickel hydroxide foam nickel material prepared in comparative example 1, and is expected to be able to replace a noble metal catalyst in the field of hydrogen production by electrolytic water.
While the foregoing is directed to the preferred embodiment of the present invention, other and further embodiments of the invention may be devised without departing from the basic scope thereof, and the scope thereof is determined by the claims that follow.
Claims (6)
1. Doped Ag2Preparation method of O-doped layered nickel hydroxide composite electrode material, and Ag-doped layered nickel hydroxide composite electrode material2The layered nickel hydroxide composite electrode material of O takes foamed nickel as a substrate, and layered nickel hydroxide grows on the surface of the foamed nickel; the layered nickel hydroxide is doped with Ag2O, characterized in that it comprises the following steps:
1) preparing a first-step precursor salt solution by using urea, ammonium fluoride and deionized water as raw materials; the raw materials also comprise nickel salt, the molar ratio of the nickel salt to the urea to the ammonium fluoride is 1:4:1, and the dosage ratio of the ammonium fluoride to the deionized water is 0.01-0.05 mol: 1L;
2) adding a silver ammonia solution into the precursor salt solution of the first step to prepare a precursor salt solution of the second step; the molar amount of the silver ammonia solution is 3/10 of the molar amount of the ammonium fluoride in the step 1);
3) putting the foamed nickel into the precursor salt solution in the second step, carrying out hydrothermal reaction, washing and drying the product to obtain the Ag-doped alloy2O, layered nickel hydroxide composite electrode material.
2. Doped Ag according to claim 12The preparation method of the O layered nickel hydroxide composite electrode material is characterized in that the nickel salt is nickel nitrate, nickel sulfate or nickel chloride.
3. Doped Ag according to claim 12The preparation method of the O layered nickel hydroxide composite electrode material is characterized in that the dosage ratio of the nickel salt to the deionized water is 0.01-0.05 mol: 1L of the compound.
4. According to any one of claims 1 to 3The doped Ag2The preparation method of the O layered nickel hydroxide composite electrode material is characterized in that the pH = 7-8 of the silver-ammonia solution in the step 2) is prepared from 0.1-0.2 mol/L silver nitrate solution and ammonia water.
5. Doped Ag according to any one of claims 1 to 32The preparation method of the O layered nickel hydroxide composite electrode material is characterized in that the purity of the foamed nickel in the step 3) is more than 99.8 percent, and the surface density is 300-450g/cm2。
6. Doped Ag according to any one of claims 1 to 32The preparation method of the O layered nickel hydroxide composite electrode material is characterized in that the temperature of the hydrothermal reaction in the step 3) is 160 ℃, and the time is 6-8 h.
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