CN111286750A - Nano hierarchical pore Ti-SiO2Preparation method of/Ni-Mo composite hydrogen evolution electrode - Google Patents
Nano hierarchical pore Ti-SiO2Preparation method of/Ni-Mo composite hydrogen evolution electrode Download PDFInfo
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Abstract
The invention discloses a nano hierarchical pore Ti-SiO2A preparation method of a/Ni-Mo composite hydrogen evolution electrode belongs to the field of electrocatalysis hydrogen evolution. Firstly, preparing nano hierarchical pore Ti-SiO with large specific surface by using in-situ synthesis method2Particles; then by a composite electrodeposition method, taking the pretreated brass sheet as a matrix material, and forming the nano multilevel poresTi‑SiO2The particles are uniformly embedded into the Ni-Mo electrode to form the nano hierarchical pore Ti-SiO with large specific surface and high electro-catalytic hydrogen evolution activity2the/Ni-Mo composite hydrogen evolution electrode. The nano hierarchical pore Ti-SiO prepared by the invention2the/Ni-Mo composite hydrogen evolution electrode can realize low energy consumption and high efficiency hydrogen production by water electrolysis.
Description
Technical Field
The invention belongs to the field of electrocatalytic hydrogen evolution, and particularly relates to a nano hierarchical pore Ti-SiO for electrocatalytic hydrogen evolution2A preparation method of a/Ni-Mo composite hydrogen evolution electrode.
Background
With the continuous increase of petrochemical fuel consumption and the reduction of storage capacity year by year and the increasing emphasis of human on environmental protection, the development of green renewable energy sources is gradually increased. Meanwhile, hydrogen energy is used as an efficient, clean and ideal secondary energy source, and is widely concerned by countries in the world. The hydrogen energy is used as a renewable secondary energy source, has the characteristics of wide source, high heat value, cleanness, good combustion stability and the like, can exist in a gaseous state, a liquid state or a solid metal hydride, can meet different requirements of storage and transportation and various application environments, and has important significance for solving the energy problem in human sustainable development.
The hydrogen production by water electrolysis is an important means for realizing the industrial and cheap hydrogen preparation, but the technology has the biggest problem of high electric energy consumption, so that the production cost is higher, and the main reason of high electric energy consumption is the over-high hydrogen evolution overpotential of an electrolysis electrode, so the research on reducing the hydrogen overpotential to reduce the electrolysis energy consumption is particularly important. The selection of the hydrogen evolution electrode material, particularly the selection of the cathode material, is particularly important for influencing the hydrogen evolution performance, and factors influencing the electrocatalytic hydrogen evolution activity of the cathode hydrogen evolution electrode material mainly comprise energy factors and geometric factors. The energy factor is the bonding energy of metal-hydrogen bonds, because metals with moderate hydrogen adsorption characteristics are beneficial to forming metal alloys with higher activity. The geometrical factors are the specific surface and surface structure morphology of the electrode material. The prior electrode material for water electrolysis has the defects of high price, small specific surface, low electrocatalytic activity and the like, so that the hydrogen evolution potential of the electrolysis electrode is too high, the energy consumption is too high, and the development of the hydrogen production technology by the water electrolysis method is seriously restricted.
Disclosure of Invention
The invention aims to provide the high-efficiency nano hierarchical pore Ti-SiO aiming at the technical defects2A preparation method of a/Ni-Mo composite hydrogen evolution electrode. The invention firstly prepares nano hierarchical pore Ti-SiO by in-situ synthesis2Particles; then plating the surface of the pretreated brass sheet by a composite electrodeposition method to prepare the nano hierarchical pore Ti-SiO2The particles are added into the electroplating solution to form the large-specific-surface nano hierarchical pore Ti-SiO with excellent hydrogen evolution capability, low cathode potential and interconnected electron transfer frameworks2the/Ni-Mo composite hydrogen evolution electrode. The preparation method has the main advantages that the composite electrodeposition method is adopted to obtain the hydrogen evolution electrode with large specific surface area, a large number of electrocatalytic active sites are provided for the hydrogen evolution electrode, the hydrogen evolution overpotential and the exchange current density are greatly reduced, the water electrolysis efficiency is improved, and the hydrogen evolution electrode has excellent hydrogen evolution capacity.
Efficient nano hierarchical pore Ti-SiO2The preparation method of the/Ni-Mo composite hydrogen evolution electrode comprises the following specific steps:
step 1: preparing nano hierarchical pore Ti-SiO by in-situ synthesis method2And (3) particle:
0.54 g CPC and 3.0 g 25wt% PAA aqueous solution (average molecular weight 240,000) were dissolved in 25 mL deionized water at room temperature and stirred, after the solution was uniformly mixed, 4.0 g 25% aqueous ammonia was added, after stirring for 20 minutes, 2.08 g of ethyl n-laurate (TEOS) and a certain amount of ethyl titanate (TEOS/ethyl titanate molar ratio 20/1) which had been previously mixed were added, after stirring vigorously for 2 hours, the mixture was transferred to 80ºAnd C, standing in an oven for 2 days. The reaction product is centrifuged, 60ºC drying, 550ºC roasting to remove the template agent to obtain the nano hierarchical pore Ti-SiO2Particles;
step 2: preparing nanometer hierarchical pore Ti-SiO by composite electrodeposition method2/Ni-Mo composite hydrogen evolution electrode
(1) Pretreatment of metal substrates
Taking a brass sheet with the thickness of 0.2mm as a base material, and obtaining a base body to be plated with a bright and smooth surface through four main processing steps of polishing, pickling and activating, degreasing, washing with distilled water and the like;
(2) taking the pretreated brass sheet as a cathode. Then, the nano hierarchical pore Ti-SiO prepared in the step 12Adding the particles with the concentration of 2 g/L into a citric acid system electroplating solution containing 40 g/L nickel sulfate hexahydrate, 40 g/L sodium citrate, 15g/L sodium molybdate dihydrate, 15g/L boric acid, 1g/L sodium dodecyl sulfate, 15g/L citric acid and 3 g/L saccharin sodium, uniformly stirring for 3 min, adjusting the pH value of the electroplating solution to 5, and controlling the temperature of the electroplating solution to be 30ºC, the cathode current density is 8A/dm2Then carrying out composite electrodeposition to obtain the nano hierarchical pore Ti-SiO2the/Ni-Mo composite hydrogen evolution electrode.
After the technical scheme is adopted, the invention mainly has the following advantages:
1. the technical scheme of the invention prepares the nano hierarchical pore Ti-SiO by an in-situ synthesis method2The preparation process of the particles is simple, and the material has ordered mesoporous and macroporous structures, so that the effective specific surface of the composite electrode is greatly improved;
2. the plating layer prepared by the composite electrodeposition method in the technical scheme of the invention has the advantages of smooth surface, uniformity, fineness and excellent brightness, but the surface roughness and the porosity of the microstructure are high, so that the activity and the stability of electrocatalytic hydrogen evolution are enhanced, and the hydrogen production by electrolyzing water with low energy consumption and high efficiency can be realized.
Drawings
FIG. 1 is a nano hierarchical pore Ti-SiO2Transmission Electron Microscopy (TEM) images of the particles.
FIG. 2 is a graph showing the effect of the concentration of nanoparticles on the composite hydrogen evolution performance.
FIG. 3 is a view of nano hierarchical pore Ti-SiO2The surface appearance of the/Ni-Mo composite electrode.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1:
step 1: in-situ synthesis method for preparing nano hierarchical pore Ti-SiO2Granules
0.54 g of CPC and 3.0 g of 25wt% PAA aqueous solution (average molecular weight 240,000) are dissolved in 25 mL of deionized water at room temperature and stirred, after the solutions are uniformly mixed, 4.0 g of 25wt% ammonia water is added, after stirring for 20 minutes, 2.08 g of premixed ethyl orthosilicate (TEOS) and a certain amount of ethyl titanate (TEOS/ethyl titanate molar ratio 20/1) are added, after stirring vigorously for 2 hours, the mixture is transferred to an oven at 80 ℃ and is kept stand for 2 days. Centrifugally separating the reaction product, drying at 60 ℃, baking at 550 ℃ to remove the template agent to obtain white powder, and obtaining the nano hierarchical pore Ti-SiO2Particles, prepared nano hierarchical pore Ti-SiO2The particles were examined by Transmission Electron Microscopy (TEM) to obtain a Transmission Electron Microscopy (TEM) photograph of fig. 1;
step 2: composite electrodeposition preparation of nano hierarchical pore Ti-SiO2/Ni-Mo composite hydrogen evolution electrode
(1) Pretreatment of metal substrates
Taking a brass sheet with the thickness of 0.2mm as a base material, and obtaining a base body to be plated with a bright and smooth surface through four main processing steps of polishing, pickling and activating, degreasing, washing with distilled water and the like;
(2) taking the pretreated brass sheet as a cathode. Then, the nano hierarchical pore Ti-SiO prepared in the step 12Adding the particles with the concentration of 1g/L into a citric acid system electroplating solution containing 40 g/L nickel sulfate hexahydrate, 40 g/L sodium citrate, 15g/L sodium molybdate dihydrate, 15g/L boric acid, 1g/L sodium dodecyl sulfate, 15g/L citric acid and 3 g/L saccharin sodium, uniformly stirring for 3 min, adjusting the pH value of the electroplating solution to be 5, and controlling the temperature of the electroplating solution to be 30ºC, the cathode current density is 8A/dm2Then carrying out composite electrodeposition to obtain the nano hierarchical pore Ti-SiO2the/Ni-Mo composite hydrogen evolution electrode.
Example 2:
step 1 is the same as step 1 in example 1;
step 2: composite electrodeposition preparation of nano hierarchical pore Ti-SiO2/Ni-Mo composite hydrogen evolution electrode
(1) Pretreating a metal substrate;
taking a brass sheet with the thickness of 0.2mm as a base material, and obtaining a base body to be plated with a bright and smooth surface through four main processing steps of polishing, pickling and activating, degreasing, washing with distilled water and the like;
(2) taking the pretreated brass sheet as a cathode. Then, the nano hierarchical pore Ti-SiO prepared in the step 12Adding the particles with the concentration of 2 g/L into a citric acid system electroplating solution containing 40 g/L nickel sulfate hexahydrate, 40 g/L sodium citrate, 15g/L sodium molybdate dihydrate, 15g/L boric acid, 1g/L sodium dodecyl sulfate, 15g/L citric acid and 3 g/L saccharin sodium, uniformly stirring for 3 min, adjusting the pH value of the electroplating solution to be 5, and controlling the temperature of the electroplating solution to be 30ºC, the cathode current density is 8A/dm2Then carrying out composite electrodeposition to obtain the nano hierarchical pore Ti-SiO2the/Ni-Mo composite hydrogen evolution electrode.
Comparative example:
nano hierarchical pore Ti-SiO2The synthesis of the particles was performed as in example 1, step 1
Step 2: composite electrodeposition preparation of nano hierarchical pore Ti-SiO2/Ni-Mo composite hydrogen evolution electrode
(1) Pretreatment of metal substrates
Taking a brass sheet with the thickness of 0.2mm as a base material, and obtaining a base body to be plated with a bright and smooth surface through four main processing steps of polishing, pickling and activating, degreasing, washing with distilled water and the like;
(2) taking the pretreated brass sheet as a cathode. Then, the nano hierarchical pore Ti-SiO prepared in the step 12Adding the particles with the concentration of 2.5 g/L into a citric acid system electroplating solution containing 40 g/L nickel sulfate hexahydrate, 40 g/L sodium citrate, 15g/L sodium molybdate dihydrate, 15g/L boric acid, 1g/L sodium dodecyl sulfate, 15g/L citric acid and 3 g/L saccharin sodium, uniformly stirring for 3 min, adjusting the pH value of the electroplating solution to be 5, and controlling the temperature of the electroplating solution to be 30ºC, the cathode current density is 8A/dm2Then carrying out composite electrodeposition to obtain the nano hierarchical pore Ti-SiO2the/Ni-Mo composite hydrogen evolution electrode.
The experimental results of the invention are as follows:
1. it can be seen from the scanning electron micrograph (FIG. 1) that the Ti-SiO prepared by the invention2The surface of the particle is of a hierarchical pore structure, the left picture of a foam pore is arranged in the sphere, in an enlarged picture (right picture), except for a foam secondary nanometer pore, ordered mesopores can be observed, and the mesopores in the whole particle keep the same mesoscopic orientation, so that the whole sphere is a mesoscopic structure single crystal, and meanwhile, the nano hierarchical pore particle has larger specific surface area, so that the effective specific surface of the composite electrode can be greatly improved;
2. as can be seen from the influence curve (figure 2) of the concentration of the nano particles on the composite hydrogen evolution performance, the nano hierarchical pore Ti-SiO prepared by the invention2a/Ni-Mo composite hydrogen evolution electrode, which is along with Ti-SiO in the plating solution2The concentration of the nano particles is increased, the hydrogen evolution potential of the composite electrode is gradually shifted positively, the electrocatalytic hydrogen evolution activity of the electrode is gradually increased, but when Ti-SiO is in the plating solution2When the concentration of the nano particles exceeds, the hydrogen evolution potential of the composite electrode is inversely shifted, and the electrocatalytic hydrogen evolution activity of the composite electrode is inversely reduced due to the increase of Ti-SiO in the solution2Nanoparticle concentration to make more Ti-SiO2The nano particles are embedded on the surface of the electrode, the effective surface area of the coating is increased, and Ti-SiO2The nano-particles have better catalytic hydrogen evolution effect, which leads to the enhancement of the electrocatalytic hydrogen evolution activity of the composite electrode, but if Ti-SiO exists in the plating solution2The concentration of the nano particles is too high, so that Ti-SiO is generated2The nano particles are agglomerated on the surface of the electrode, so that the effective surface area of the composite electrode is reduced, and the electrocatalytic hydrogen evolution activity of the composite electrode is reduced, therefore, the concentration of the nano particles in the plating solution should be moderate, and the increase of the electrocatalytic hydrogen evolution activity of the composite electrode is not facilitated when the concentration is too large or too small;
3. it can be seen from the scanning electron micrograph (figure 3) that the nano hierarchical pore Ti-SiO prepared by the invention2The surface of the/Ni-Mo composite hydrogen evolution electrode is provided with obvious nano hierarchical pore particles embedded on the surface of the electrode, and most of the particles are uniformly dispersed and are not agglomerated together, so that the effective surface area of the electrode is greatly improved.
Claims (3)
1. Nano hierarchical pore Ti-SiO2The preparation method of the/Ni-Mo composite hydrogen evolution electrode is characterized by comprising the following steps:
step 1: preparation of nano hierarchical pore Ti-SiO2Granules
Dissolving 0.54 g CPC and 3.0 g 25wt% PAA aqueous solution (average molecular weight 240,000) in 25 mL deionized water at room temperature, stirring, adding 4.0 g 25wt% ammonia water after the solution is uniformly mixed, stirring for 20 minutes, adding 2.08 g of premixed Tetraethoxysilane (TEOS) and a certain amount of ethyl titanate (TEOS/ethyl titanate molar ratio 20/1), continuing to stir strongly for 2 hours, transferring the mixture to 80ºStanding in oven C for 2 days, centrifuging reaction product, and 60ºC drying, 550ºC roasting to remove the template agent to obtain the nano hierarchical pore Ti-SiO2Particles;
step 2: preparing nanometer hierarchical pore Ti-SiO by composite electrodeposition method2/Ni-Mo composite hydrogen evolution electrode
(1) Pretreatment of metal substrates
Taking a brass sheet with the thickness of 0.2mm as a base material, and obtaining a base body to be plated with a bright and smooth surface through four main processing steps of polishing, pickling and activating, degreasing, washing with distilled water and the like;
(2) taking the pretreated brass sheet as a cathode, and taking the nano hierarchical pore Ti-SiO prepared in the step 12Adding the particles into Ni-Mo alloy electroplating solution, stirring for 3 min, adjusting pH to 5, and controlling the temperature of the electroplating solution to 30ºC, the cathode current density is 8A/dm2Then carrying out composite electrodeposition to obtain the nano hierarchical pore Ti-SiO2the/Ni-Mo composite hydrogen evolution electrode.
2. The nano-multilevel pore Ti-SiO of claim 12The preparation method of the/Ni-Mo composite hydrogen evolution electrode is characterized by comprising the following steps:
the electroplating solution is a mixed aqueous solution of sodium molybdate dihydrate, nickel sulfate hexahydrate, sodium citrate, boric acid, sodium dodecyl sulfate, citric acid and sodium saccharin;
the nano hierarchical pore Ti-SiO2The concentration of the particle solution is 0.5-2.0 g/L.
3. The nano-multilevel pore Ti-SiO of claim 22The preparation method of the/Ni-Mo composite hydrogen evolution electrode is characterized by comprising the following steps:
the concentration of the sodium molybdate dihydrate aqueous solution is 15 g/L;
the concentration of the nickel sulfate hexahydrate aqueous solution is 40 g/L;
the concentration of the sodium citrate aqueous solution is 40 g/L;
the concentration of the boric acid is 15 g/L;
the concentration of the sodium dodecyl sulfate is 1 g/L;
the concentration of the citric acid is 15 g/L;
the concentration of the saccharin sodium is 3 g/L.
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| CN112522734A (en) * | 2020-11-17 | 2021-03-19 | 广东省科学院新材料研究所 | Porous electrode for electrolytic gas production in liquid environment and preparation method thereof |
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| CN112522734A (en) * | 2020-11-17 | 2021-03-19 | 广东省科学院新材料研究所 | Porous electrode for electrolytic gas production in liquid environment and preparation method thereof |
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