CN114717585A - Double-transition metal electrode material, preparation method thereof and application thereof in hydrogen production by photovoltaic electrolysis of water - Google Patents
Double-transition metal electrode material, preparation method thereof and application thereof in hydrogen production by photovoltaic electrolysis of water Download PDFInfo
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Abstract
The invention belongs to the technical field of photovoltaic-electrolyzed water, and particularly discloses a double-transition metal electrode material which is prepared by the following method: and immersing the cleaned foam metal into an aqueous solution containing cobalt nitrate to perform one-step hydrothermal reaction, and connecting the electrode material obtained after cleaning and drying with a commercial Si-based photovoltaic cell panel in series to obtain the simple photovoltaic electrolyzed water hydrogen production equipment. The composite electrode prepared by the invention can be used as an anode and a cathode for efficient, stable and independent water decomposition, and provides a typical demonstration and valuable guideline for large-scale solar hydrogen production by using cheap materials.
Description
Technical Field
The invention belongs to the technical field of photovoltaic-electrolyzed water, and particularly relates to a double-transition metal electrode material (CoNi LDH/CoFe)2O4With CoFe2O4) A preparation method thereof and application thereof in hydrogen production by photovoltaic electrolysis of water.
Background
Since the advent of semiconductor electrodes, the unique response of light to the electrode has been noted, making it significantly different from conventional metal electrodes. With the development of photovoltaic power generation technology, solar energy conversion technology based on solar cells is continuously and stably developed, the Power Conversion Efficiency (PCE) of a typical monocrystalline silicon solar cell is continuously increased from less than 15% to more than 26%, and the rapidly developed solar cells provide conditions for a substitute method of solar hydrogen production, namely photovoltaic electrolyzed water.
There are three undesirable factors in current laboratory development of photovoltaic-electrolyzed water: (1) complex and costly to manufacture multijunction photovoltaic cells, (2) concentrator solar cells, (3) expensive metal-based electrodes, which can lead to complex and uneconomical photovoltaic-water electrolysis systems.
In recent years, a transition metal-based electrocatalyst is used as an electrode for electrocatalytic decomposition of water with great development prospect, wherein cobalt ferrite or nickel ferrite is a bimetallic spinel oxide, has excellent mixed-valence redox performance, has appropriate adsorption/desorption capacity on an OER intermediate product, and is considered to be an effective way for further reducing overpotential, promoting kinetics and catalytic activity by constructing a heterogeneous structure with other excellent OER active electrocatalysts.
Disclosure of Invention
The invention changes the complex preparation process with high manufacturing cost, provides a simple and feasible liquid phase hydrothermal synthesis process, and controllably synthesizes cobalt-nickel double metal hydroxide, cobalt ferrite and a composite electrode of the cobalt-nickel double metal hydroxide and the cobalt ferrite by respectively taking foamed nickel, foamed iron and foamed nickel-iron as supporting substances. And the solar cell panel is combined with a commercial Si-based photovoltaic cell panel to be assembled and prepared into an economical, efficient and stable photovoltaic-electrolytic water system, so that a certain potential is brought to large-scale application of hydrogen production by photovoltaic electrolytic water.
In order to achieve the purpose, the invention is realized by the following technical scheme:
a preparation method of a double-transition metal electrode material comprises the following steps:
(1) shearing foam metal into a size of 5-10 square centimeters, and sequentially immersing the foam metal in acetone, 0.01-1 mol/L hydrochloric acid and absolute ethyl alcohol for ultrasonic cleaning, wherein the ultrasonic time is 5-10 minutes each time (an oxide layer on the surface can be removed after ultrasonic cleaning);
(2) placing the cobalt nitrate aqueous solution with the concentration of 10-20 mmol/L and the treated foam metal in a high-pressure reaction kettle, setting the environmental temperature and the duration, naturally cooling after the reaction, washing with deionized water and ethanol for multiple times (removing residual reactants), and drying (50-70 ℃) to obtain the catalyst.
Preferably, the foam metal in step (1) is foam nickel, foam iron or foam iron-nickel alloy, wherein the mass ratio of nickel to iron is as follows: 9.99: 0.01, 0.02: 9.98, 0.93: 9.07.
preferably, the temperature in step (2) is set to 100-200 ℃ for 0.5-10 hours.
A high-efficiency photovoltaic water electrolysis hydrogen production device is designed, and comprises an electrode and a Si-based photovoltaic cell panel, wherein the Si-based photovoltaic cell panel is connected in series between a cathode and an anode, and the electrode is made of the double-transition metal electrode material.
Preferably, the starting material foam metal of the double-transition metal electrode material of the anode electrode is foam iron-nickel alloy, and the starting material foam metal of the double-transition metal electrode material of the cathode electrode is foam iron.
The prepared double-transition metal electrode material is connected with a commercial Si-based photovoltaic cell panel in series, so that the solar hydrogen production efficiency of 12.7 percent under the irradiation of natural light can be realized, and the standard requirement of large-scale and commercial photocatalytic hydrogen production is met.
The invention has the following beneficial effects:
the invention aims to construct and improve the catalytic activity of a non-noble metal electrocatalyst electrode, utilizes the excellent mixed valence oxidation-reduction performance of transition metal cobalt ferrite, and constructs a multi-phase structure by combining with cobalt-nickel double metal hydroxide to reduce the OER overpotential and improve the catalytic activity.
The invention adopts a simple and feasible liquid phase hydrothermal synthesis process, controllably synthesizes the cobalt-nickel double metal hydroxide, the cobalt ferrite and the composite electrode of the cobalt-nickel double metal hydroxide and the cobalt ferrite, and reduces the use of noble metal-based electrodes.
The invention combines the electrode material with the Si-based solar cell, can assemble an economical, efficient and stable photovoltaic-electrolytic water system, has the solar hydrogen production efficiency (STH) of 12.7 percent under the irradiation of natural light, and brings certain potential for the large-scale application of the photovoltaic-electrolytic water hydrogen production market.
Drawings
In order to more clearly illustrate the technical solution of the embodiments of the present invention, the following briefly introduces the drawings that need to be used:
FIG. 1 is an X-ray diffraction pattern of the electrode materials obtained in examples 1, 2 and 3 of the present invention, and relevant crystal planes and diffraction peaks can be observed.
FIG. 2 is a scanning electron micrograph of the electrode material obtained in example 1 of the present invention, from which the topography of the surface of example 1 can be clearly seen.
FIG. 3 is a scanning electron micrograph of the electrode material obtained in example 2 of the present invention, from which the topography of the surface of example 2 can be clearly seen.
FIG. 4 is a scanning electron micrograph of the electrode material obtained in example 3 of the present invention, from which the topography of the surface of example 3 can be clearly seen.
FIG. 5 is a graph of the hydrogen evolution reaction for examples 1, 2 and 3 of the present invention.
FIG. 6 is a graph of the oxygen evolution reaction for examples 1, 2 and 3 of the present invention.
FIG. 7 is a schematic structural diagram of the high-efficiency photovoltaic water electrolysis hydrogen production device.
Fig. 8 is a graph showing the hydrogen and oxygen amounts generated by decomposing water and the solar hydrogen production efficiency in the case of a simple photovoltaic-electrolytic water device prepared by connecting a commercial Si photovoltaic cell panel in series with the electrode material obtained in example 3 as an anode and the electrode material obtained in example 2 as a cathode under irradiation of natural light.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, embodiments of the present invention will be described in detail with reference to the accompanying drawings.
Example 1
(1) Pretreatment of foamed nickel: cutting foamed nickel into 2.5 × 3 square centimeters, sequentially putting the foamed nickel into acetone, 0.1mol/L hydrochloric acid and absolute ethyl alcohol for ultrasonic cleaning, and removing oil stains and oxides on the surface.
(2) The nickel foam was immersed in a solution containing 30mL of 14.5mmol/L cobalt nitrate. And transferring the solution and the foamed nickel into a 50mL reaction kettle, and carrying out hydrothermal reaction under the high-temperature and high-pressure environment, wherein the reaction temperature is 150 ℃, and the reaction time is one hour. After the reaction is finished, the reaction product is naturally cooled to room temperature, the material is taken out, and the material is thoroughly washed by deionized water and ethanol for multiple times to remove residues. And (3) putting the cleaned material into an oven, and drying at 60 ℃ to finally obtain the cobalt-nickel double-metal hydroxide nanosheet.
Example 2
(1) Pretreatment of the foamed iron: cutting the foam iron into 2.5 multiplied by 3 square centimeters, sequentially putting the foam iron into acetone, 0.1mol/L hydrochloric acid and absolute ethyl alcohol for ultrasonic cleaning, and removing oil stains and oxides on the surface.
(2) The foam iron was immersed in a solution containing 30mL of 14.5mmol/L cobalt nitrate. And transferring the solution and the foam iron into a 50mL reaction kettle, and carrying out hydrothermal reaction under the high-temperature and high-pressure environment, wherein the reaction temperature is 150 ℃, and the reaction time is one hour. After the reaction is finished, the reaction product is naturally cooled to room temperature, the material is taken out, and the material is thoroughly washed by deionized water and ethanol for multiple times to remove residues. And (3) putting the cleaned material into an oven, and drying at 60 ℃ to finally obtain the cobalt ferrite nano-particles.
Example 3
(1) Pretreating foamed iron and nickel: cutting foamed iron nickel into 2.5 × 3 square centimeters, sequentially putting the foamed iron nickel into acetone, 0.1mol/L hydrochloric acid and absolute ethyl alcohol for ultrasonic cleaning, and removing oil stains and oxides on the surface.
(2) The foamed nickel iron was immersed in a solution containing 30mL of 14.5mmol/L cobalt nitrate. And transferring the solution and the foamed iron-nickel into a 50mL reaction kettle, and carrying out hydrothermal reaction under the high-temperature and high-pressure environment, wherein the reaction temperature is 150 ℃, and the reaction time is one hour. After the reaction is finished, the reaction product is naturally cooled to room temperature, the material is taken out, and the material is thoroughly washed by deionized water and ethanol for multiple times to remove residues. And (3) putting the cleaned material into an oven, and drying at 60 ℃ to finally obtain the composite material of the cobalt-nickel double metal hydroxide and the cobalt ferrite.
The materials obtained in the above examples were subjected to performance analysis:
1. the crystalline phases and compositions of examples 1, 2 and 3 were analyzed by X-ray diffraction. As shown in fig. 1, in example 1 and example 3, there are three strong diffraction peaks at 44.3 °, 51.5 ° and 76.1 ° belonging to the (111), (200) and (220) crystal planes of metallic nickel, respectively. In example 2 and example 3, diffraction peaks at 44.6 ° and 65.0 ° belong to the (110) and (200) crystal planes of iron. And the diffraction peaks at 18.28 °, 30.08 °, 35.43 °, 43.05 °, 56.97 °, 62.58 ° and 65.75 ° correspond to the (111), (220), (311), (400), (511), (440) and (531) crystal planes of cobalt ferrite. Examples 1 and 3 have three diffraction peaks marked at 13.94 °, 24.76 °, 35.24 °, indicating that spinel cobalt ferrite and cobalt nickel bimetallic layered hydroxide have been successfully synthesized.
2. The compositions and morphologies of the prepared metal foams and the synthesized samples of examples 1, 2 and 3 were investigated using Scanning Electron Microscopy (SEM). As shown in fig. 2 and 3: the nickel foam and the iron foam of the embodiment 1 and the embodiment 2 are respectively covered with a layer of nano-sheet and nano-particle, while the morphology of the embodiment 3 is shown in fig. 4, besides the ultra-thin cobalt-nickel bimetal hydroxide nano-sheet is vertically grown on the nickel foam substrate, the nano-particle of cobalt ferrite is also uniformly attached on the nano-sheet, the transverse dimension of the nano-sheet is 2 μm, and the diameter of the nano-particle is 200 nm.
3. The electrochemical test is carried out in an electrochemical workstation, and a three-electrode system is adopted in the experiment, the temperature is 25 ℃, and the electrolyte is 1mol/L potassium hydroxide solution. Wherein 1X 1 square centimeter of the material prepared in examples 1-3 was used as a working electrode, Ag/AgCl was used as a reference electrode, and a platinum sheet was used as a counter electrode. In 1mol/L potassium hydroxide solution at 2 mv s-1Linear Sweep Voltammetry (LSV) polarization curves were measured at the sweep rate of (a). As shown in fig. 5, the catalytic activity of the hydrogen evolution reaction of the materials prepared in examples 1, 2 and 3 was evaluated by comparing the linear sweep voltammetric polarization curves of the hydrogen evolution reaction. The material prepared in example 2 shows excellent hydrogen evolution reaction performance, and reaches 10 mA cm under 100 mV overpotential－2Whereas the materials prepared in example 3 and example 1 reach the same current density at overpotentials of 179 mV and 200 mV, respectively. As shown in FIG. 6, examples 1, 2 and 3 were compared at 20 mA cm-2OER performance under current density, it can be seen that example 3 has excellent OER performance, and the overpotential of 254 mv (vs. standard hydrogen electrode) is only needed to reach 20 mA cm-2The current density, overpotential for examples 1 and 2 was 270 mv and 346 mv, respectively.
4. Photovoltaic-electrolyzed water test: the sample obtained in example 3, which has the best oxygen evolution capacity, was used as the anode, and example 2, which has the best hydrogen evolution capacity, was used as the cathode. Examples 2, 3 and commercially available Si-based photovoltaic cell panels were connected in series to assemble a simple photovoltaic-electrolyzed water apparatus as shown in fig. 7, where fig. 7A is a preparation work of the photovoltaic-electrolyzed water apparatus before irradiation with sunlight. Fig. 7B shows that after the Si-based photovoltaic cell panel is irradiated by sunlight, a stable voltage is applied to the cathode and the anode, so that the cathode and the anode respectively generate hydrogen and oxygen, which enter the burette through the conduit, and the gas volume is obtained through a drainage and integration method. Fig. 8B is a pictorial view of the apparatus. Under the irradiation of the simulated sunlight AM 1.5, the open-circuit voltage of the Si-based photovoltaic cell panel is 2.4V, the short-circuit current is 200 mA, and in this case, the maximum power conversion efficiency of the Si-based photovoltaic cell panel is 14.75%. The solar cell under natural sunlight can provide 1.9V voltage relatively stably, obvious bubbles appear on the cathode and the anode as shown in the right graph of fig. 8B, and generated gas is collected and converted into volumes of hydrogen and oxygen, wherein the molar ratio of the hydrogen to the oxygen is 2:1 as shown in fig. 8C. The solar hydrogen production efficiency per thirty minutes was further calculated according to the following equation.
In the formula rH2The photovoltaic electrolysis level of the product is equal to the hydrogen yield within thirty minutes0Represents one mole of H2Varying Gibbs energy, PtotalIs the natural solar energy which is input averagely and fluctuates around 50-60 at noon. Area is the effective Area of a Si-based photovoltaic panel, about 25.92 cm2. As shown in fig. 8D, the maximum solar hydrogen production efficiency under natural sunlight irradiation is 12.74%. This value is comparable or better than some previously reported photovoltaic electrolytic water systems, including multijunction high cost photovoltaic cells and noble metal electrodes.
Figure 8E shows a possible catalytic mechanism and corresponding charge transfer/separation model. In the photovoltaic water electrolysis process, hydrogen evolution reaction occurs on the surface of cobalt ferrite nano particles, oxygen evolution reaction occurs on the surface of cobalt-nickel double metal hydroxide and cobalt ferrite heterostructure arrays, and electrons flow from an anode to a cathode under an additional bias provided by a commercial Si-based photovoltaic cell panel.
In the photovoltaic-electrolytic water process, hydrogen evolution reactions occur at the surface of the cathode, oxygen evolution reactions occur at the surface of the anode, and electrons flow from the anode to the cathode under the additional bias provided by the Si-based photovoltaic panel. The above can show that the solar-assisted water splitting test assembled by the present invention provides typical demonstration and great hope for large-scale hydrogen production using inexpensive photovoltaic electrolyzed water technology.
The preferred embodiments of the present invention should not be construed as limiting the present invention, that is, the appended claims should be construed to include the preferred embodiments and all such variations and modifications as fall within the scope of the invention.
Claims (10)
1. A preparation method of a double-transition metal electrode material is characterized by comprising the following steps:
(1) immersing the foam metal in acetone, 0.01-1 mol/L hydrochloric acid and absolute ethyl alcohol in sequence for ultrasonic cleaning;
(2) and (3) placing the cobalt nitrate aqueous solution and the treated foam metal in a high-pressure reaction kettle, setting the environmental temperature and the duration, naturally cooling after reaction, washing with deionized water and ethanol for multiple times, and drying to obtain the catalyst.
2. The method of claim 1, wherein: in the step (1), the foam metal is firstly cut into a size of 5-10 square centimeters.
3. The method of claim 1, wherein: the foam metal in the step (1) is foam nickel, foam iron or foam iron-nickel alloy.
4. The method of claim 1, wherein: the concentration of the cobalt nitrate aqueous solution is 10-20 mmol/L.
5. The production method according to claim 3, characterized in that: the mass ratio of nickel to iron in the foamed nickel, the foamed iron and the foamed iron-nickel alloy is respectively 9.99: 0.01, 0.02: 9.98 and 0.93: 9.07.
6. the method of claim 1, wherein: the temperature in the step (2) is set to be 100-200 ℃, and the time is 0.5-10 hours.
7. A double-transition metal electrode material obtained by the production method according to any one of claims 1 to 6.
8. Use of the double-transition metal electrode material of claim 7 in the production of hydrogen by photovoltaic electrolysis of water.
9. The utility model provides a high-efficient photovoltaic electrolysis water hydrogen plant which characterized in that: comprising an electrode and a Si-based photovoltaic cell panel connected in series between a cathode and an anode, said electrode being made of a double-transition metal electrode material according to claim 7.
10. The high-efficiency photovoltaic electrolyzed water hydrogen production apparatus as defined in claim 9, characterized in that: the starting material foam metal of the double-transition metal electrode material of the anode is foam iron-nickel alloy, and the starting material foam metal of the double-transition metal electrode material of the cathode is foam iron.
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| CN108588742A (en) * | 2018-05-21 | 2018-09-28 | 吕逍 | A method of preparing electrolysis water base metal bifunctional catalyst |
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| CN111097423A (en) * | 2020-01-13 | 2020-05-05 | 哈尔滨工业大学 | Nickel-based layered double-metal hydroxide nanosheet and room-temperature rapid green preparation method and application thereof |
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