CN111763955A - Super-hydrophobic platinum hydrogen evolution electrode, preparation method thereof and preparation method of hydrogen - Google Patents
Super-hydrophobic platinum hydrogen evolution electrode, preparation method thereof and preparation method of hydrogen Download PDFInfo
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Abstract
The invention provides an ultra-hydrophobic gas-hydrogen separation electrode, a preparation method thereof and a preparation method of hydrogen. The super-hydrophobic gas hydrogen evolution electrode is provided with a mesh-shaped conductive carrier and platinum nano sheets deposited on the mesh-shaped conductive carrier, wherein the platinum nano sheets are distributed on two surfaces of the mesh-shaped conductive carrier. The super-gas-permeable hydrogen evolution electrode disclosed by the invention is simple in preparation process, short in time consumption and low in cost, the surface of the electrode has excellent wettability and gas permeability, and the electrocatalytic activity of the hydrogen evolution electrode can be improved.
Description
Technical Field
The present invention relates generally to the field of inorganic catalytic material preparation.
Background
Hydrogen is a renewable clean fuel, has high energy density and good energy production efficiency, is an ideal carrier for energy storage, can solve the problems of sustainability, environmental emission and energy safety, and is concerned by countries in the world as it may replace fossil fuels in the future.
Electrocatalytic water decomposition is one of the sustainable approaches to hydrogen production. The hydrogen reduction reaction includes reduction of protons at the electrode surface and desorption of product hydrogen gas at the electrode surface. The traditional thin-sheet platinum hydrogen evolution electrode can only contact with electrolyte on the surface, and the effective reaction area of the electrode is small. Moreover, because the adhesion force of hydrogen on the surface of the electrode is large, hydrogen bubbles are adhered on the surface of the electrode, so that the contact between an electrolyte solution and the surface of a catalyst is hindered, the catalytic activity is reduced, and the requirement of high-efficiency hydrogen reduction reaction for preparing hydrogen cannot be met.
The report of preparing a platinum nanoneedle hydrogen evolution electrode on the surface of a titanium sheet by using a cyclic voltammetry deposition method in the prior art is provided. In addition, there are also other methods in which TiO is used2The report of hydrogen evolution electrode prepared by photocatalytic deposition of platinum particles on nanotubes. However, the hydrogen evolution electrode prepared by the methods is formed by platinum nano needles or nano particles on a thin sheet carrier, so that the effective reaction area is small during hydrogen evolution reaction.
Therefore, how to increase the effective reaction area of the hydrogen evolution electrode and reduce the adhesion on the surface of the electrode is a technical problem to be solved urgently in the field of the platinum hydrogen evolution electrode.
Disclosure of Invention
In order to solve the above problems, the present inventors have conducted extensive studies and found that when a platinum electrode having a nanosheet structure is used as a hydrogen evolution electrode, the contact area between the electrode surface and an electrolyte is large, and the catalytic activity of a hydrogen reduction reaction during the hydrogen evolution reaction is greatly improved. In addition, the platinum is in a sharp nano-sheet structure, so that the bubble adhesion force on the surface of the electrode is further reduced, and the hydrogen generated by the hydrogen evolution reaction is favorably desorbed from the surface of the electrode. The two effects act synergistically to greatly enhance the catalytic activity of the electrode. Thus, the present invention has been completed.
The present invention provides the following technical means.
In one aspect of the invention, an ultrahydrophobic platinum hydrogen evolution electrode is provided, which comprises a mesh-shaped conductive carrier and platinum nanosheets deposited on the mesh-shaped conductive carrier, wherein the platinum nanosheets are distributed on two sides of the conductive carrier.
Preferably, the conductive carrier is made of gold, silver, nickel, titanium or carbon.
Preferably, the mesh conductive carrier is 100 to 1500 mesh.
Preferably, the size of the platinum nanosheet is 10 to 400 nanometers, and the thickness is 1 to 30 nm. More preferably, the size of the platinum nano-sheet is 30-300 nm, and the thickness is 5-20 nm. The size of the platinum nanosheet is the lateral size thereof. For example, a platinum nanosheet having a size of 10nm means that it has a 10 nm-square platelet structure.
In another aspect of the present invention, there is provided a method for preparing an ultraporophobic platinum hydrogen evolution electrode of the present invention, which comprises:
in the presence of H as an electrolyte2PtCl6And KCl in an aqueous solution in which H is formed on the conductive mesh support by electrodeposition2PtCl6Has a concentration of 1 × 10-3mol/L～50×10-3mol/L, concentration of KCl 10 × 10-3mol/L～500×10-3mol/L。
Preferably, the voltage of the electrodeposition is-0.2 to-0.4V, and the deposition time is 10 to 50 min.
In another aspect of the present invention, a method for producing hydrogen is provided, which uses the super-hydrophobic platinum hydrogen evolution electrode of the present invention.
The super-hydrophobic platinum hydrogen evolution electrode uses a mesh conductive carrier, and a platinum catalyst in a sharp nanosheet shape is formed on the surface of the mesh conductive carrier. The grid structure of the conductive carrier is beneficial to the good infiltration of electrolyte on the surface of the electrode, and the sharp nano-sheet structure of the platinum catalyst also increases the contact surface area of the electrode and the electrolyte, thereby greatly improving the catalytic activity of hydrogen reduction reaction during hydrogen evolution reaction. In addition, the sharp nano-sheet structure of the platinum catalyst further reduces the bubble adhesion on the surface of the electrode, thereby being beneficial to the desorption of hydrogen generated by hydrogen evolution reaction from the surface of the electrode. The rapid exit of the gas from the electrode surface also allows for more complete contact of the catalyst with the electrolyte, increasing the effective active area of the electrode. The two effects act synergistically to greatly enhance the catalytic activity of the electrode.
In the preparation method of the super-hydrophobic platinum hydrogen evolution electrode, the mesh-shaped conductive carrier is used as the carrier, and platinum generated by electrodeposition grows along the skeleton of the mesh due to a large number of mesh-shaped holes in the carrier. Compared with the electrode obtained by electro-deposition by using a conductive carrier without a net, the electrolyte containing the platinum precursor is easier to infiltrate the framework of the grid, and the grown platinum catalyst is in a sharp nano-sheet structure vertical to the surface of the framework of the carrier, so that the contact surface area of the platinum catalyst and the electrolyte is large, and the catalytic activity of hydrogen reduction reaction during hydrogen evolution reaction is greatly improved. In addition, the platinum catalyst with a sharp nano-sheet structure further reduces the bubble adhesion force on the surface of the electrode, thereby being beneficial to the desorption of hydrogen generated by hydrogen evolution reaction from the surface of the electrode. The two effects act synergistically to greatly enhance the catalytic activity of the electrode.
Drawings
Fig. 1 is an environmental scanning electron microscope image of an ultraporophobic platinum hydrogen evolution electrode prepared in an example of the present invention.
FIG. 2 is a high magnification environmental scanning electron microscope image of the ultraphobic platinum hydrogen evolution electrode used in FIG. 1.
FIG. 3 is a further magnified environmental scanning electron micrograph of the ultraporophobic platinum hydrogen evolution electrode used in FIG. 1.
Figure 4 is a linear sweep voltammogram of an ultraporophobic platinum hydrogen evolution electrode prepared in examples of the invention (examples 2 and 5) with a bare gold mesh in 0.5M sulfuric acid.
Fig. 5 is a linear scanning voltammogram of the ultraporophobic platinum hydrogen evolution electrodes prepared in example 2 of the present invention and comparative example 1.
Fig. 6 is a photograph of the underwater bubble contact angle of the ultralyophobic platinum hydrogen evolution electrode prepared in example 2 of the present invention.
Fig. 7 is a photograph of the electrode surface when electrochemical hydrogen evolution is performed using the ultraphobic platinum hydrogen evolution electrode prepared in example 2 of the present invention.
Detailed Description
[ platinum Hydrogen evolution electrode with super-hydrophobic gas ]
The super-hydrophobic platinum hydrogen evolution electrode comprises a reticular conductive carrier and platinum nano sheets deposited on the conductive carrier, wherein the platinum nano sheets are distributed on two surfaces of the conductive carrier.
The size of the mesh-shaped conductive carrier is not particularly limited, and may be, for example, 100 to 1500 mesh, preferably 200 to 1000 mesh, and more preferably 400 to 600 mesh.
The platinum nanosheet is in a nano-sized sheet shape, the size of the platinum nanosheet is in a transverse size, the sheet shape is 10-400 nm square, more preferably 30-300 nm square, and the thickness of the platinum nanosheet is preferably 1-30 nm.
The aforementioned ultraphobia is the wettability of the electrode surface with gas under water, and is generally characterized by measuring the contact angle of the electrode with gas bubbles under water. "ultraphobic" means that the contact angle of the electrode to bubbles under water is 140 degrees or more, preferably 150 degrees or more.
Examples of the material of the mesh-like conductive carrier include gold, silver, nickel, titanium, and carbon.
[ preparation method of platinum Hydrogen evolution electrode with super-hydrophobic gas ]
The preparation method of the super-hydrophobic platinum hydrogen evolution electrode comprises the steps of using the hydrogen-containing electrolyte containing H2PtCl6And KCl in an aqueous solution in which H is formed on the conductive mesh support by electrodeposition2PtCl6Has a concentration of 1 × 10-3mol/L～50×10-3mol/L, concentration of KCl 10 × 10-3mol/L～500×10-3mol/L。
Foregoing H2PtCl6More preferably 1 × 10-3mol/L～20×10-3mol/L, more preferably 1 × 10-3mol/L～10×10-3mol/L。
The concentration of KCl is more preferably 10 × 10-3mol/L～300×10-3mol/L, more preferably 10 × 10-3mol/L～200×10-3mol/L。
The voltage range used in the electrodeposition method is-0.2 to-0.4V. For example, -0.2V, -0.3V, or-0.4V. The deposition time in the electrodeposition method is 5 to 80min, more preferably 10 to 50min, and still more preferably 20 to 40 min.
The preparation method of the super-hydrophobic platinum hydrogen evolution electrode can also comprise the following steps: after electrodeposition, the platinum nanosheets deposited on the surface of the electrode are washed with deionized water to remove inorganic salts such as KCl and the like remaining on the surface of the electrode.
[ method for producing Hydrogen gas ]
In the method for producing hydrogen of the present invention, the above-described super-hydrophobic platinum hydrogen evolution electrode of the present invention is used. In addition, other conditions in the method for producing hydrogen according to the present invention may be selected as needed by those skilled in the art with reference to the conditions generally used in the art. For example, the following production method can be employed.
The super-hydrophobic platinum hydrogen evolution electrode is used as a working electrode, a carbon rod is used as a counter electrode, the reference electrode is an Ag/AgCl electrode, and 1M sulfuric acid is used as an electrolyte.
In the preparation method of the hydrogen, the super-hydrophobic platinum hydrogen evolution electrode is large in contact surface area with the electrolyte, so that the catalytic activity of hydrogen reduction reaction in the hydrogen evolution reaction is greatly improved. In addition, the bubble adhesion on the electrode surface is low, thereby facilitating the desorption of the hydrogen generated by the hydrogen evolution reaction from the electrode surface. The two effects act synergistically to greatly enhance the catalytic activity of the electrode.
Examples
The characterization and performance test of the super-hydrophobic gas hydrogen evolution electrode comprises the following steps:
(1) and (3) morphology characterization: the microscopic morphology of the sample was observed using a scanning electron microscope environment Quanta FEG 250, FEI USA. Specifically, the hydrogen evolution electrode with super-hydrophobic properties prepared in the example was topographically characterized using an environmental scanning electron microscope.
(2) Hydrogen reduction test: the electro-catalytic activity of the prepared super-hydrophobic platinum hydrogen evolution electrode in 0.5M sulfuric acid is tested by adopting a three-electrode system of CHI 660D electrochemical workstation of Shanghai Chen Hua electric appliance Co.
(3) Bubble contact angle test: the wettability of the prepared ultraporophobic platinum hydrogen evolution electrode was tested using the last morning JC2000D1 contact angle system.
(4) And (3) bubble desorption measurement: and a camera is adopted to carry out on-site imaging on the evolution process of the hydrogen bubbles on the surface of the prepared super-hydrophobic platinum hydrogen evolution electrode.
Example 1
A three-electrode system is utilized, a gold mesh with the diameter of about 3mm and the mesh number of 600 is used as a working electrode, a platinum sheet is used as an auxiliary electrode, an Ag/AgCl electrode is used as a reference electrode, and the three-electrode system is placed in a position of 3 × 10-3mol/L H2PtCl6、100×10-3Setting the electro-deposition voltage to be-0.3V in a mixed solution of mol/L KCl, carrying out electro-deposition for 10min, washing the surface of the electrode by deionized water after the reaction is finished, and airing to obtain the super-gas-permeable platinum hydrogen evolution electrode 1 with metal platinum deposited on the front and back surfaces of a gold mesh.
Example 2
A three-electrode system is utilized, a gold mesh with the diameter of about 3mm and the mesh number of 600 is used as a working electrode, a platinum sheet is used as an auxiliary electrode, an Ag/AgCl electrode is used as a reference electrode, and the three-electrode system is placed in a position of 3 × 10-3mol/L H2PtCl6、100×10-3Setting the electro-deposition voltage to be-0.3V in the mixed solution of mol/L KCl, electro-depositing for 30min, washing the surface of the electrode by deionized water after the reaction is finished, and airing to obtain the super-gas-permeable platinum hydrogen evolution electrode 2 with metal platinum deposited on the front and back surfaces of the gold mesh.
Example 3
A three-electrode system is utilized, a gold mesh with the diameter of about 3mm and the mesh number of 600 is used as a working electrode, a platinum sheet is used as an auxiliary electrode, an Ag/AgCl electrode is used as a reference electrode, and the three-electrode system is placed in a position of 3 × 10-3mol/L H2PtCl6、100×10-3Setting the electro-deposition voltage to be-0.3V in the mixed solution of mol/L KCl, electro-deposition for 50min, washing the surface of the electrode by deionized water after the reaction is finished, and airing to obtain the super-gas-permeable platinum hydrogen evolution electrode 3 with metal platinum deposited on the front and back surfaces of the gold mesh.
Example 4
A three-electrode system is utilized, a gold mesh with the diameter of about 3mm and the mesh number of 600 is used as a working electrode, a platinum sheet is used as an auxiliary electrode, an Ag/AgCl electrode is used as a reference electrode, and the three-electrode system is placed in a position of 3 × 10-3mol/L H2PtCl6、100×10-3Mixed solution of mol/L KClIn the solution, setting the electro-deposition voltage to be-0.2V, electro-deposition for 30min, washing the surface of the metal platinum by deionized water after the reaction is finished, and airing to obtain the super-hydrophobic platinum hydrogen evolution electrode 4 with metal platinum deposited on the front and back surfaces of the gold mesh.
Example 5
A three-electrode system is utilized, a gold mesh with the diameter of about 3mm and the mesh number of 600 is used as a working electrode, a platinum sheet is used as an auxiliary electrode, an Ag/AgCl electrode is used as a reference electrode, and the three-electrode system is placed in a position of 3 × 10-3mol/L H2PtCl6、100×10-3Setting the electro-deposition voltage to be-0.4V in the mixed solution of mol/L KCl, electro-depositing for 30min, washing the surface of the electrode by deionized water after the reaction is finished, and airing to obtain the super-gas-permeable platinum hydrogen evolution electrode 5 with metal platinum deposited on the front and back surfaces of the gold mesh.
Example 6
A three-electrode system is utilized, a gold mesh with the diameter of about 3mm and the mesh number of 1500 meshes is used as a working electrode, a platinum sheet is used as an auxiliary electrode, an Ag/AgCl electrode is used as a reference electrode, and the three-electrode system is placed at 3 × 10-3mol/L H2PtCl6、100×10-3Setting the electro-deposition voltage to be-0.3V in the mixed solution of mol/L KCl, electro-depositing for 30min, washing the surface of the electrode by deionized water after the reaction is finished, and airing to obtain the super-gas-permeable platinum hydrogen evolution electrode 6 with metal platinum deposited on the front and back surfaces of the gold mesh.
Comparative example 1
Depositing platinum nanosheets on the surface of the gold foil to prepare the platinum hydrogen evolution electrode:
using a three-electrode system, a gold foil having a diameter of about 3mm as a working electrode, a platinum sheet as an auxiliary electrode, and an Ag/AgCl electrode as a reference electrode were placed in a 3 × 10 cell-3mol/L H2PtCl6、100×10-3And (3) setting the electro-deposition voltage to be-0.3V in the mixed solution of mol/L KCl, carrying out electro-deposition for 50min, washing the surface of the platinum-plated hydrogen-evolution electrode by deionized water after the reaction is finished, and airing to obtain the platinum hydrogen-evolution electrode 7 with platinum deposited on the front and back surfaces of the gold mesh.
The super-hydrophobic platinum hydrogen evolution electrodes obtained in the above examples and comparative examples were subjected to morphology characterization, a bubble contact angle test, and a hydrogen reduction test. As can be seen from the appearance characterization, the super-hydrophobic platinum hydrogen evolution electrode prepared in the embodiments 1-6 has a macroscopic porous structure, and the surface of the electrode is provided with sharp platinum nano-sheets which are densely and uniformly distributed. The result of the bubble contact angle test shows that the super-hydrophobic platinum hydrogen evolution electrode obtained in the embodiment 1-6 has super-hydrophobic property under water, and is beneficial to desorption of product gas; the hydrogen reduction activity test result shows that the super-hydrophobic platinum hydrogen evolution electrode shows larger current density under lower overpotential.
(1) Topography characterization
The super-hydrophobic platinum hydrogen evolution electrode 2 prepared in example 2 was observed in morphology by using an environmental scanning electron microscope. As shown in fig. 1 to 3, it can be clearly observed that the surface of the super-hydrophobic platinum hydrogen evolution electrode 2 is deposited with sharp platinum nano-sheets, and is dense and uniform.
(2) Hydrogen reduction Activity test
At room temperature, at 0.5mol/L of H2SO4In the electrolyte, a hydrogen reduction activity test is performed on the super-hydrophobic gas hydrogen evolution platinum electrode 2 prepared in example 2 and the super-hydrophobic gas hydrogen evolution platinum electrode 5 prepared in example 5 by using a CHI660E electrochemical workstation, an air-platinum net is used as a reference, a three-electrode working system is adopted, a saturated Ag/AgCl electrode is used as a reference electrode, a carbon rod is used as an auxiliary electrode, and the prepared super-hydrophobic gas platinum hydrogen evolution electrode 2 or 5 is used as a working electrode to perform a linear scanning voltammetry test. The Reversible Hydrogen Electrode (RHE) was mapped to the standard electrode according to the equation:
the potential (vs. Ag/AgCl) ranged from-0.4V to-0.1V, with the scan rate set at 5 mV/s. As can be seen from fig. 4, the ultraphobic gas evolution hydrogen evolution platinum electrode 2 prepared in example 2 and the ultraphobic gas evolution hydrogen evolution platinum electrode 5 prepared in example 5 of the present invention exhibit excellent hydrogen reduction catalytic activity. Further, the platinum hydrogen evolution electrode 7 obtained in comparative example 1 was also subjected to the above-described hydrogen reduction activity test, and the results are shown in fig. 5 together with example 2. As can be seen from fig. 5, the ultraphobic gas evolution hydrogen platinum electrode 1 prepared in example 2 of the present invention also exhibited excellent hydrogen reduction catalytic activity as compared to comparative example 1.
(3) Measurement of bubble contact Angle
The super-hydrophobic aerohydrogen evolution platinum electrode 2 prepared in example 2 was tested for bubble contact angle under water (CAs) using a (Dataphysics, germany) 0CA20 contact angle system. The super-hydrophobic gas evolution hydrogen platinum electrode 2 is suspended and fixed and placed in a quartz water tank with a certain size, the immersion position is adjusted until the super-hydrophobic gas evolution hydrogen platinum electrode 2 is clearly seen on a screen to be a straight line, the focal length is adjusted to enable imaging to be clear, then a bubble is gently beaten out underwater to enable the bubble to be completely attached to the surface of a gold screen, and finally the bubble contact angle is tested. As shown in fig. 6, the super-hydrophobic gas hydrogen evolution platinum electrode 2 prepared in example 2 has a large bubble contact angle of 148 ° under water, and shows super-hydrophobic property, and bubbles are easily desorbed from the surface of the electrode, thereby greatly improving the electrocatalytic activity.
(4) Bubble desorption test
The evolution process of the hydrogen bubbles in the releasing process is imaged on site by adopting a camera. The super-hydrophobic gas hydrogen evolution platinum electrode 2 prepared in the example 2 is used as a working electrode, and the geometric area is 0.071cm-2The carbon rod is a counter electrode, the 3.5M Ag/AgCl electrode is a reference electrode, and the carbon rod is placed in 0.5MH2SO4 electrolyte, as shown in figure 7, the super-hydrophobic gas evolution hydrogen platinum electrode 2 has a larger bubble contact angle underwater in the hydrogen reduction process, namely, underwater super-hydrophobic gas. The hydrogen bubbles have small size and can leave the surface of the electrode in time without being adhered to the surface of the electrode, so that the full contact between the electrolyte solution and the catalyst is ensured, and the electrocatalytic activity is greatly improved.
It will be apparent to those skilled in the art that various modifications and variations can be made in the specific embodiments of the present disclosure without departing from the scope or spirit of the disclosure. Other embodiments will be apparent to those skilled in the art from consideration of the specification. The specification and examples are exemplary only.
Claims (6)
1. An ultraporophobic platinum hydrogen evolution electrode comprises a reticular conductive carrier and platinum nano sheets deposited on the reticular conductive carrier, wherein the platinum nano sheets are distributed on two sides of the reticular conductive carrier.
2. The platinum hydrogen evolution electrode of claim 1, wherein the conductive carrier is made of gold, silver, nickel, titanium or carbon.
3. The super-hydrophobic platinum hydrogen evolution electrode as claimed in claim 1 or 2, wherein the mesh-shaped conductive carrier is 100-1500 meshes, the platinum nano-sheet is a sharp sheet with a size of 10-400 nm, and the thickness is 1-30 nm.
4. The method for preparing an ultraporophobic platinum hydrogen evolution electrode as set forth in any one of claims 1 to 3, which comprises,
in the presence of H as an electrolyte2PtCl6And KCl in an aqueous solution, electrodepositing the platinum nanosheets on a reticulated conductive support, wherein H is2PtCl6Has a concentration of 1 × 10-3mol/L～50×10-3mol/L, concentration of KCl 10 × 10- 3mol/L～500×10-3mol/L。
5. The preparation method of the super-hydrophobic platinum hydrogen evolution electrode according to claim 4, wherein the voltage of the electrodeposition is-0.2 to-0.4V, and the deposition time is 10 to 50 min.
6. An electrochemical method for producing hydrogen gas, which uses the ultraphobic platinum hydrogen evolution electrode according to any one of claims 1 to 3.
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| CN115125572A (en) * | 2022-06-22 | 2022-09-30 | 北京航空航天大学 | Preparation method and application of mushroom-shaped array electrode |
| CN115125572B (en) * | 2022-06-22 | 2023-12-19 | 北京航空航天大学 | Preparation method and application of mushroom-shaped array electrode |
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