CN114457348A - Ordered porous titanium-based iron oxide film photoelectrocatalysis material and preparation method and application thereof - Google Patents
Ordered porous titanium-based iron oxide film photoelectrocatalysis material and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an ordered porous titanium-based iron oxide film photoelectrocatalysis material, a preparation method and application thereof. A series of characterization and photoelectrocatalysis performance tests are carried out on the prepared titanium-based iron oxide photoanode material, the titanium-based iron oxide photoanode material is found to have excellent photoelectrocatalysis water decomposition hydrogen production performance, visible light wavelength absorption is enhanced under additional bias voltage, the sunlight utilization rate is improved, the synthesis method is simple and nontoxic, reaction conditions are easy to control, chemical properties are stable, a brand new thought is provided for research of photoelectrocatalysis hydrolysis hydrogen production of the iron oxide material, and the titanium-based iron oxide photoanode material has a good application prospect.
Description
Technical Field
The invention relates to an ordered porous titanium-based iron oxide film photoelectrocatalysis material, a preparation method and application thereof.
Background
With the rapid development of economic society, the population base is huge, the demand of human society for energy resources is continuously increased, although traditional energy resources such as petroleum, coal, natural gas and the like are still the main body of energy consumption, the problems of energy shortage, resource development difficulty, sharp rise of cost and the like are caused by over-development, low energy utilization rate and the like of the traditional energy resources, global greenhouse effect and environmental pollution are aggravated by greenhouse gases and harmful gases generated in the combustion and utilization process, and therefore, the optimization of energy structure and the exploration of sustainable and clean energy are of great importance. Hydrogen is widely used in industry and daily life due to its high calorific value, cleanliness, and easy storage, but currently large-scale hydrogen production still relies on steam reforming of fossil fuels, such as methane, which may cause a series of energy and environmental problems. Therefore, a photoelectrochemical cell (PEC) that uses solar energy to decompose water to generate hydrogen is considered one of the most promising approaches to solve the environmental and energy problems of the world in the 21 st century.
First discovery of TiO in 19722The electrode can decompose water under ultraviolet light, and the research of photocatalysis/photoelectrocatalysis technology is continuously developed. Semiconductor photoanodes, as a key component of PEC cells, play a crucial role in the separation and transfer of photogenerated carriers. Wherein iron oxide (Fe)2O3) Is a promising semiconductor material, and has the advantages of abundant storage on the earth, no toxicity, good stability and the like due to the visible light absorption capacity. Because the conduction band position (CB) of the iron oxide is about 0.4V, and the valence band position (VB) is about 2.4V, the water oxidation process of the hematite can not be carried out spontaneously, and a bias voltage needs to be applied to stimulate the water oxidation reaction, so that the iron oxide is more suitable for preparing a photoanode to carry out the photoelectrocatalysis process to decompose water. The band gap of the iron oxide is about 2.0-2.2 eV, so that the iron oxide can absorb visible light wavelength (lambda)>420nm) with theoretical photocurrent up to 12mA/cm2The theoretical apparent quantum efficiency can reach 15%, but the hole diffusion length is only 2-4nm due to the low conductivity of the ferric oxide and the large particle size of the current carrier, the excited state life is very short (less than 10ps), high current carrier recombination is caused, and the light conversion efficiency is far lower than the theoretical value. Therefore, most of the research on iron oxide focuses on the control of the shape of the iron oxide photoanode, and the iron oxide material is usually made into a rod, a wire, a rod,The nano particles and other one-dimensional and two-dimensional structures are used for controlling the thickness of the ferric oxide film, accelerating the transmission rate of current carriers and improving the light conversion efficiency.
On the other hand, the two-dimensional ordered porous material (2 DOM) has a porous structure and Photonic Band Gap (PBG) characteristics, can regulate and control the absorption of visible light wavelengths, and is widely applied to photonic devices, sensors, batteries, supercapacitors, fuel cells, catalysis, adsorption and other potential applications. The 2DOM has higher porosity, larger surface area and shorter diffusion distance can be controlled, and the characteristics ensure that the ion diffusion coefficient and the current density are increased, and the ion diffusion rate is high, so that the 2DOM can show excellent performance in the photoelectrocatalysis process. Meanwhile, the photo-generated carrier recombination rate of a single semiconductor photocatalytic material is too high, and the situation of low light conversion efficiency exists, so that in the process of constructing the iron oxide film photo-anode, a titanium substrate material with excellent conductivity is selected to be in synergistic action with iron oxide to prepare the titanium-based iron oxide composite photo-anode, and the overall performance of the material is improved by utilizing the photocatalytic characteristics and the surface ordered porous structure of titanium oxide and iron oxide on the surface of titanium substrate.
The invention prepares a novel porous ordered titanium-based Fe by a template method2O3The thin-film photoelectric anode structure shows good visible light absorption performance in a PEC electrolytic cell, improves the light conversion efficiency, realizes high-efficiency hydrogen production by decomposing water through photoelectrocatalysis, provides a new idea for optimizing the photoelectrochemical performance of the iron oxide photoelectric anode, and has good application prospect.
Disclosure of Invention
The purpose of the invention is: aiming at the problems of low catalytic performance and complex preparation of the existing iron oxide material serving as a photoelectric catalyst for decomposing water to prepare hydrogen, the invention takes a single-layer polystyrene film as a template, and iron oxide is loaded on a titanium substrate to prepare the ordered porous titanium-based iron oxide photoanode material.
In order to realize the purpose, the technical scheme of the invention for obtaining the ordered porous titanium-based iron oxide film photo-anode is as follows:
1) before the glass sheetThe processing steps are as follows: ultrasonic cleaning glass sheet (preferably 2.5cm × 7.5 cm) with soap water, acetone, and ethanol for 30min, respectively, and treating with N2After blowing dry, clean glass pieces were placed in piranha solution (H)2SO4With 25wt% of H2O2The volume ratio is preferably 7: 2), soaking for 30s, washing with deionized water, and then adding N2Blowing and drying, repeating for 3 times, and obtaining the glass sheet with clean and hydrophilic surface.
2) Self-assembly of Polystyrene (PS) film: taking 100uL of monodisperse PS microsphere mixed solution (2% volume fraction, average particle size of 1 um) and 100uL of ethanol for ultrasonic treatment for 30min, using 1.5mL of deionized water to fully distribute the clean glass sheet, slowly injecting the PS-ethanol mixed solution from one end of the glass sheet at the speed of 10 s/drop, and enabling the PS microspheres to be self-assembled into a single-layer film at an air-water interface at the other end of the glass sheet; after the PS film is stabilized on the water surface for 30min to strengthen the acting force between the microspheres, absorbing the moisture under the single-layer PS film by using dust-free paper at the injection end, and drying for 10min to obtain a single-layer PS template;
3) the preparation method of the iron oxide photo-anode comprises the following steps: the single-layer PS template is slowly placed into 100mL0.1M Fe (NO) by 30 DEG inclination3)3Maintaining in the precursor solution for 5min, and using 1 × 1cm2Putting a pure titanium sheet (99.99 percent) into the precursor solution, slowly pulling the PS template at 45 degrees, horizontally placing the template for drying, putting the template into an oven for drying at 60 ℃ for 30min, then annealing the template in air at 500 ℃ for 2h, and raising the temperature at the rate of 3 ℃/min. Obtaining the ordered porous titanium-based ferric oxide film photoelectrocatalysis material marked as Fe2O3-PS-Ti. Meanwhile, marking the blank titanium sheet Annealed under the same condition as Annealed Ti; the iron oxide sample taking conductive glass as a substrate is marked as Fe2O3-PS-FTO; mixing 10uL0.1M Fe (NO)3)3The precursor is dripped on a blank titanium sheet, and a disordered sample prepared after drying and annealing is marked as Fe2O3-D-Ti。
The ordered porous titanium-based iron oxide film prepared by the invention is applied to the solar energy conversion process, such as being used as a photo-anode and other control samples to test the electrochemical parameters.
Compared with the prior art, the implementation mode has the following characteristics:
the invention prepares the ordered porous titanium-based iron oxide film photo-anode Fe by adopting a single-layer PS template method, adopting pure titanium as a substrate of the photo-anode and uniformly and orderly loading a trace amount of iron oxide on the titanium substrate2O3PS-Ti, the photocatalytic property is pure ordered ferric oxide photoanode Fe2O3-PS-FTO, disordered titanium-based iron oxide photo-anode Fe2O3427 times, 4.6 times and 12 times of the-D-Ti and pure titanium photoanode Annealed Ti, and shows good visible light absorption performance. The method is simple and easy to prepare, can be used for large-scale preparation, has excellent photoelectrocatalysis performance, and provides a new method for preparing the ferric oxide film photoelectrode.
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The following description of the main parameter features of the present invention is illustrated by the figures
FIG. 1 is a flow chart of the preparation of the ordered porous titanium-based iron oxide film photoelectrocatalysis material, in particular to the flow chart from steps a) to b), c), d), e) to f).
FIG. 2 is a FEI-SEM field emission scanning electron microscope image of a titanium-based iron oxide photoanode; in the figure, a) is Fe2O3FEI-SEM field emission scanning electron microscopy of PS-Ti. The right b) diagram is Fe2O3FEI-SEM field emission scanning Electron microscopy of D-Ti. The result shows that the prepared ordered porous titanium-based iron oxide photo-anode has an ordered porous structure, and the structure is beneficial to the absorption of light in the photoelectrocatalysis process.
FIG. 3 shows Ti-based iron oxide photo-anode Fe2O3-PS-Ti、Fe2O3XRD patterns of D-Ti and analized Ti. The result shows that the ordered porous titanium-based iron oxide photo-anode prepared by the template method has little iron oxide load, and anatase TiO is formed on the surface of the titanium substrate after annealing2And titanium TiO suboxide.
FIG. 4 is X Photoelectron Spectrum (XPS), and the result shows that Fe is Fe on Ti substrate3+When the iron oxide is loaded on the titanium substrate, the metal oxygen peak O1s is obviously shifted, which indicates that a heterostructure exists between the iron oxide and the titanium substrate.
FIG. 5 shows a titanium-based iron oxide photo-anode Fe2O3-PS-Ti、Fe2O3-D-Ti and Anaaled Ti photoelectrocatalytic materials in the presence of 1M KOH and ethanol 1: 1, the total amount of hydrogen produced by photolysis is converted into one sun AM1.5G (100 mw/cm) under different biases2) Hydrogen production rate diagram. The result shows that the ordered porous titanium-based iron oxide photo-anode has excellent hydrogen production performance under certain bias voltage and can absorb visible light.
FIG. 6 is a graph comparing photoanode Fe at different potentials2O3-PS-Ti、Fe2O3The photocurrent densities of D-Ti and Annealed Ti were measured using a three-electrode system with Pt as the counter electrode, Ag/AgCl as the reference electrode and 1M KOH solution as the electrolyte. RHE, Fe at 1.45V vs2O3-PS-Ti、Fe2O3Photocurrent densities of-D-Ti and Anaaled Ti at full spectrum were 1280, 280, 107uA/cm, respectively2This shows the excellent photocatalytic performance of the ordered porous titanium-based iron oxide film material.
FIG. 7 is a comparative photoanode Fe at a constant potential of 1.28V vs. RHE2O3-PS-Ti、Fe2O3Photocurrent densities of D-Ti and Anaaled Ti. The results show that the photocurrent density Fe2O3-PS-Ti》Fe2O3-D-Ti>Annealed Ti and has better stability.
FIG. 8 shows the constant potential wavelength scanning photocurrent density and photoelectric conversion efficiency, the left graph shows the wavelength scanning photocurrent density, the scanning potential is 1.28V vs. RHE, and the right graph shows the corresponding photoelectric conversion efficiency, and the results show that the ordered porous Fe is under bias voltage2O3the-PS-Ti photoanode can generate photocurrent in a visible light range compared with the rest photoanodes, the light absorption edge extends to 600nm, and the light conversion efficiency reaches 5.4% at 420 nm.
FIG. 9 shows the band gap calculation results according to the photoelectric conversion efficiency (IPCE), and the results show that the ordered porous titanium-based iron oxide photoanode Fe is subjected to bias voltage application2O3The band gap of the PS-Ti is 2.33eV, and the absorption of visible light is enhanced.
FIG. 10 shows Mott-SchottkyThe curve test shows that Mott-Schottky result shows that the ordered porous titanium-based iron oxide photo-anode Fe2O3The flat band potential of PS-Ti is about 0.00236V (vs. RHE PH = 6.5), possessing a flat band position more favorable for photoelectron transport.
FIG. 11 is an impedance image (EIS), and the result shows that the ordered porous titanium-based iron oxide photoanode Fe2O3The impedance of the PS-Ti is smaller than that of the rest photo anode, and under the bias voltage, the impedance is further reduced, so that the transmission of photo-generated carriers is facilitated.
Detailed Description
In the invention, by a single-layer PS template method, iron oxide is loaded on a titanium substrate by utilizing the characteristic of the iron oxide material on visible light absorption, and the ordered porous titanium-based iron oxide photoanode for visible light absorption is prepared.
Example 1
Preparation of single-layer polystyrene template (PS): ultrasonic cleaning glass sheet (2.5 cm × 7.5 cm) with soap water, acetone, and ethanol for 30min, respectively, and treating with N2Blowing and drying, and adding clean glass pieces into the solution (H)2SO4With 25wt% of H2O2Prepared with a volume ratio of 7: 2) for 30s, washed clean with deionized water, and then N2Blowing and drying, repeating for 3 times, and obtaining the glass sheet with clean and hydrophilic surface. Taking 100uL of monodisperse PS microsphere mixed solution (the PS microsphere mixed solution is composed of PS microspheres with 2% volume fraction and average particle size of 1um and deionized water with 98% volume fraction) and 100uL of absolute ethyl alcohol, carrying out ultrasonic synthesis for 30min to obtain PS microsphere-ethanol mixed solution, covering 1.5mL of deionized water on a clean glass sheet, slowly injecting the PS microsphere-ethanol mixed solution from one end of the glass sheet at the speed of 10 s/drop, and carrying out self-assembly on the PS microspheres at an air-water interface at the other end of the glass sheet to form a single-layer PS film; and after the monolayer PS film is stabilized on the water surface for 30min to strengthen the acting force between the microspheres, absorbing the moisture under the monolayer PS film by using dust-free paper at the injection end, and drying for 10min to obtain the monolayer PS template. The monolayer PS template obtained by the invention is in six-element close packing.
Example 2
Preparing an ordered porous titanium-based iron oxide photo-anode: the single-layer PS template of example 1 was slowly placed at 30 ℃ tilt in 100mL0.1M Fe (NO)3)3Maintaining in the precursor solution for 5min, and using 1 × 1cm2Putting a pure titanium sheet (with the purity of 99.99%) into the precursor solution, slowly pulling the PS template at 45 degrees, horizontally placing the PS template until the PS template is dried, putting the PS template into an oven for drying at 60 ℃ for 30min, then carrying out air annealing at 500 ℃ for 2h, and raising the temperature at the rate of 3 ℃/min. Obtaining the ordered porous titanium-based ferric oxide film photoelectrocatalysis material marked as Fe2O3-PS-Ti. The ordered porous titanium-based iron oxide photo-anode Fe finally obtained by the invention2O3The distribution of the PS-Ti surface iron oxide follows the template rule, and the distribution is uniform and ordered.
Example 3
Preparing a pure titanium photo-anode: mixing 1X 1cm2Pure titanium sheets (with the purity of 99.99%) are placed in a tube furnace for air annealing at 500 ℃ for 2h, the heating rate is 3 ℃/min, the obtained pure titanium photo-anode is marked as Annealed Ti, and the pure titanium photo-anode obtained by the invention is analyzed by XRD (X-ray diffraction), and the anatase type titanium dioxide film formed by surface annealing is determined.
Example 4
Preparing a disordered titanium-based iron oxide photo-anode: mixing 10uL0.1M Fe (NO)3)3Precursor droplets at 1X 1cm2Pure titanium sheet (purity 99.99%), air annealing at 500 ℃ for 2h after drying, heating rate is 3 ℃/min, and the obtained disordered titanium-based iron oxide sample is marked as Fe2O3-D-Ti。
Example 5
Evaluating the solar hydrolysis hydrogen production performance of the ordered porous titanium-based iron oxide photo-anode: a three-electrode system is used for testing, the working electrode is the ordered porous titanium-based iron oxide thin film material prepared in example 2 and is used as a photo-anode, the counter electrode is a Pt sheet, the reference electrode is Ag/AgCl, 30mL of 1M KOH and 30mL of ethanol are used as electrolyte, a CHI760E electrochemical workstation is used for providing bias voltage and detecting photocurrent density, a xenon lamp corrected by Solar spectrum is used as a simulated sunlight light source, the light source intensity is normalized to be one sunlight intensity namely AM1.5G, and a Solar Lab 6A full-glass automatic acquisition system is used as the simulated sunlight light sourceConnecting FL9700 gas chromatograph as hydrogen output detector, counting hydrogen output by photocatalysis every half an hour, and making full-spectrum hydrogen production rate at 1.28V vs. RHE bias for 3 h be 11.3 umol.h-1·cm-2The hydrogen production rate of visible light is 6.20 umol.h-1·cm-2. Disordered titanium-based iron oxide photo-anode Fe under the same condition2O3The full spectrum hydrogen production rate of-D-Ti is 8.88 umol.h-1·cm-2The hydrogen production rate of visible light is 3.15 umol.h-1·cm-2The full-spectrum hydrogen production rate of the pure titanium photoanode Annealed Ti is 8.72 umol.h-1·cm-2The hydrogen production rate of visible light is 0 umol.h-1·cm-2The ordered porous titanium-based iron oxide photo-anode can utilize solar energy more efficiently.
Example 6
For the ordered porous titanium-based iron oxide photo-anode Fe prepared in example 22O3PS-Ti, disordered titanium-based iron oxide photoanode Fe prepared in example 42O3D-Ti and Annealed Ti of pure titanium prepared in example 3 were subjected to potentiostatic photocurrent testing, using a xenon lamp corrected by solar spectrum to simulate sunlight, with a light intensity of 100mw/cm2, using a platinum sheet as a counter electrode, an Ag/AgCl electrode as a reference electrode, a working electrode as the photoanode prepared in examples 2, 3 and 4 above, using a 1M KOH solution as an electrolyte, and a constant bias voltage of 0.6V vs. Ag/AgCl applied to the working electrode by a CHI760E electrochemical workstation, and a photocurrent-time curve was recorded. The result shows that the ordered porous titanium-based iron oxide photo-anode Fe2O3-PS-Ti, disordered titanium-based iron oxide photo-anode Fe2O3The photocurrent densities of-D-Ti and pure titanium photoanode Annealed Ti are 740, 117 and 99uA/cm2 respectively, which shows that the ordered porous titanium-based iron oxide photoanode Fe2O3PS-Ti enables more efficient use of solar energy.
Example 7
For the ordered porous titanium-based iron oxide photo-anode Fe prepared in example 22O3PS-Ti, disordered titanium-based iron oxide photoanode Fe prepared in example 42O3-D-Ti and examples3, performing constant potential wavelength scanning photocurrent test on the prepared pure titanium photoanode Annealed Ti, simulating sunlight by using a xenon lamp, performing test by using a three-electrode system, taking a platinum sheet as a counter electrode, an Ag/AgCl electrode as a reference electrode, taking a 1MKOH solution as an electrolyte, and controlling the electrochemical workstation to detect photocurrent generated under the irradiation of 300-600nm wavelength spectrum under different constant potential conditions by using the electrochemical workstation in Wuhan Seiki, wherein the scanning precision is 1 nm. The result shows that under the additional bias, the ordered porous titanium-based iron oxide photo-anode Fe2O3The response interval of PS-Ti wavelength is 300-600nm, and almost no photocurrent response exists at the visible light wavelength of the rest photoanode, which indicates that the ordered porous titanium-based iron oxide photoanode Fe2O3PS-Ti has visible light absorption capability and higher photogenerated carrier separation efficiency.
Claims (2)
1. A preparation method of ordered porous titanium-based iron oxide film photoelectrocatalysis material is characterized by comprising the following steps:
1) glass sheet pretreatment: ultrasonic cleaning the glass sheet with soap water, acetone and ethanol for no less than 30min, and treating with N2After blowing dry, clean glass pieces were placed in piranha solution (H)2SO4With 25wt% of H2O2The volume ratio is 7: 2), soaking for 30s, washing with deionized water, and then using N2Blowing and drying, repeating for at least 3 times to obtain a glass sheet with a clean and hydrophilic surface;
2) self-assembly of Polystyrene (PS) film: taking 100uL of monodisperse PS microsphere mixed solution (2% volume fraction, average particle size of 1 um) and 100uL of absolute ethyl alcohol, performing ultrasonic synthesis for no less than 30min to obtain PS microsphere-ethyl alcohol mixed solution, using 1.5-2mL of deionized water to fill the glass sheet obtained in the step 1), and slowly injecting the PS microsphere-ethyl alcohol mixed solution from one end of the glass sheet at the speed of 5-10 s/drop to enable the PS microspheres to self-assemble into a single-layer PS film at an air-water interface at the other end of the glass sheet; after the single-layer PS film is stabilized on the water surface for 20-30min to strengthen the acting force between the microspheres, absorbing the moisture under the single-layer PS film at the injection end by using dust-free paper, and drying for 10min to obtain a single-layer PS template;
3) oxygen gasThe preparation method of the iron-melting photo-anode comprises the following steps: slowly adding 100mL0.1M Fe (NO) into the single-layer PS template obtained in the step 2) at an inclination of 20-30 DEG3)3Maintaining in the precursor solution for 5-10min, and using 1 × 1cm2And (3) putting a pure titanium sheet or a titanium plate into the precursor solution, slowly lifting the single-layer PS template at an inclination angle of 30-45 degrees, horizontally placing the template after drying, putting the template into an oven for drying at 60 ℃ for not less than 30min, then annealing the template in air at 500 ℃ for 2h, and raising the temperature at a rate of not higher than 3 ℃/min to obtain the ordered porous titanium-based iron oxide film photoelectrocatalysis material.
2. The use of the ordered porous titanium-based iron oxide thin film photoelectrocatalytic material prepared by the method in the claim 1 in the solar energy conversion process.
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| CN113774418A (en) * | 2021-09-23 | 2021-12-10 | 常州工程职业技术学院 | Preparation of three-dimensional conductive framework and application of three-dimensional conductive framework in iron oxide photo-anode |
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| CN113774418A (en) * | 2021-09-23 | 2021-12-10 | 常州工程职业技术学院 | Preparation of three-dimensional conductive framework and application of three-dimensional conductive framework in iron oxide photo-anode |
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