CN110993355A - Preparation method of optimized α -phase iron oxide photo-anode with two-dimensional titanium carbide substrate layer - Google Patents
Preparation method of optimized α -phase iron oxide photo-anode with two-dimensional titanium carbide substrate layer Download PDFInfo
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Abstract
The invention relates to the technical field of materials, in particular to a preparation method of an optimized α -phase iron oxide photo-anode of a two-dimensional titanium carbide substrate layer3C2MXene material as substrate layer on FTO surface and α -Fe2O3Firstly, α -Fe is promoted2O3Separating the photo-generated electron hole pairs from the FTO conductive substrate interface; second, tetravalent titanium ion (Ti)4+) Diffusing from the substrate layer to the iron oxide during the high temperature calcination process to form iron titanate/iron oxide (Fe)2TiO5/Fe2O3) The heterojunction photoelectrode promotes the separation and transmission of the photo-generated charges in the ferric oxide, thereby effectively improving α -Fe2O3The photoelectrocatalysis performance of the photoanode.
Description
Technical Field
The invention relates to the technical field of materials, in particular to a preparation method of an optimized α -phase iron oxide photo-anode with a two-dimensional titanium carbide substrate layer.
Background
The photoelectrocatalytic water splitting hydrogen production technology (Photoelectrochemical water splitting) is considered as the most promising hydrogen production method for converting solar energy into hydrogen energy, α phase ferric oxide (α -Fe)2O3) The nanometer α -Fe is considered as a potential solar energy photoelectrocatalysis water decomposition material with great potential due to appropriate forbidden band width (excellent visible light absorption capacity), stable photoelectrochemical property and low price in 19762O3Having been found to have the ability to photoelectrocatalytically decompose water, subsequent theoretical studies have also found that, in standard simulated sunlight (AM 1.5, 100 mW/cm)2) Under the irradiation of (2), nano α -Fe2O3The solar energy-hydrogen energy conversion efficiency of the photoelectrode can reach 16.5 percent and can generate 12.6mA/cm2And an initial potential of about 0.4V vs. rhe (reversible hydrogen electrode potential).
In practice, however, the nanometer α -Fe has a short diffusion path (2-4nm) due to the limitation factors such as poor conductivity, slow oxidation reaction speed of water molecules on the surface of the photoelectrode, and short diffusion path of photogenerated holes2O3The photocurrent density and initial potential of the film are far from the theoretical prediction value, α -Fe2O3The nano material can not be applied to practical commercial application in a large scale, and the research on the photoelectrocatalysis water decomposition of the nano material is in the laboratory research stage at present, so that the α -Fe is effectively improved2O3The photoelectrocatalysis activity of the photoelectrode, and various modification and modification methods are designed and adopted successively, such as appearance control, element doping, surface modification, construction of a heterojunction photoelectrode and the like.
Meanwhile, two-dimensional nanomaterials represented by graphene, molybdenum disulfide and graphite-phase carbon nitride have been widely used in recent years for α -Fe due to their excellent conductivity and large specific surface area2O3In the modification and modification of the photoanode. Transition metal carbides and carbonitrides (MXenes), a new discovery of the two-dimensional family of materials, have developed rapidly since their discovery in 2011. Among these, two-dimensional titanium carbide (Ti)3C2MXene) material has the following three advantages: 1. high charge carrier mobility; 2. adjustable band gap; 3. good optical performance, and can be widely applied in the fields of energy storage and conversion and biology. In the field of water decomposition by iron oxide photoelectrocatalysis, Ti3C2MXene has been used and studied less. Therefore, there is a need to develop a synthetic method with simple operation and easily controlled conditions for preparing Ti3C2MXene modified nanometer α phase iron oxide photo-anode to greatly improve photoelectrocatalysis thereofThe ability to decompose water.
Disclosure of Invention
One purpose of the invention is to solve the problem of the existing nanometer α -Fe2O3The photocurrent density and the initial potential of the film are far from the theoretical predicted value.
Another object of the present invention is to provide a Ti3C2The MXene substrate layer optimized α -phase iron oxide photo-anode preparation method has the advantages of simple preparation, easily-controlled conditions, low cost, no toxicity and environmental friendliness, and provides possibility for industrial large-scale production of electrode materials.
In order to realize the purpose of the invention, the following technical scheme is mainly adopted:
ti3C2MXene substrate layer optimization α -Fe2O3A method for preparing a photoanode, the method comprising the steps of:
(1) and cleaning the FTO glass.
(2) Ti dripped on the cleaned FTO glass conductive surface3C2Putting the solution in a muffle furnace, annealing at 200 ℃ for 15min, and calcining at high temperature to obtain Ti with the surface3C2A layer of FTO glass.
(3) Putting the FTO glass into a reaction kettle in a mode that the conductive surface faces upwards, adding a precursor solution for growing α -phase ferric oxide into the reaction kettle, heating the reaction kettle at 100 ℃ for 4 hours, taking out the FTO conductive glass after the reaction kettle is heated and cooled, annealing the FTO conductive glass at 550 ℃ for 2 hours, and annealing at 750 ℃ for 15 minutes to obtain Ti-containing material3C2Nanometer α -Fe of substrate layer2O3And a photoelectrode.
The Ti3C2The volume ratio of the solution to the precursor solution for growing α -phase ferric oxide is 0.1-0.3: 80, preferably 0.2: 80, and the Ti is3C2The solution concentration is 5mg/mL, and the precursor solution for growing α -phase ferric oxide is prepared by weighing ferric trichloride (FeCl)3·6H2O) and glucose(C6H12O6) Dissolving the FeCl into deionized water, magnetically stirring to obtain FeCl solution3And C6H12O6The concentrations of (A) were 0.15M and 1M, respectively.
The preparation method comprises the following steps: in the step (1), the step of cleaning the FTO glass comprises the following steps: firstly, cleaning stains on the surface of the FTO glass by using a hand sanitizer or a liquid detergent, then sequentially putting the FTO glass into deionized water and absolute ethyl alcohol for ultrasonic cleaning for 15 minutes respectively, and finally drying the FTO glass for later use.
The preparation method comprises the following steps: in the step (2), the heating rate of the whole annealing stage is selected and controlled at 10 ℃/min.
The preparation method comprises the following steps: in the step (3), after the hydrothermal reaction is finished and the reaction kettle is naturally cooled to room temperature, taking the FTO conductive glass out of the reaction kettle and washing the FTO conductive glass with deionized water; the heating rate of the whole annealing stage is also selectively controlled at 10 ℃/min.
α -Fe with excellent photoelectric property is prepared by the method2O3And a photo-anode.
The invention has the beneficial effects that:
the invention adopts a method of embedding a substrate layer to prepare Ti3C2MXene material as substrate layer on FTO surface and α -Fe2O3Firstly, α -Fe is promoted2O3Separating the photo-generated electron hole pairs from the FTO conductive substrate interface; second, tetravalent titanium ion (Ti)4+) Diffusing from the substrate layer to the iron oxide during the high temperature calcination process to form iron titanate/iron oxide (Fe)2TiO5/Fe2O3) The heterojunction photoelectrode promotes the separation and transmission of the photo-generated charges in the ferric oxide, thereby effectively improving α -Fe2O3The photoelectrocatalysis performance of the photoanode.
The preparation method of the invention is simple and easy, and only adopts the traditional α -Fe2O3The method has the advantages of being simple in operation by adding one step in the steps of the photoanode experiment, and having the characteristics of mild treatment conditions, simple process, low energy consumption and environmental friendliness.
Drawings
FIG. 1 is a SEM image comparison of FTO glass before and after deposition of MXene substrate layer in example 3.
FIG. 2 is SEM image comparison of α phase iron oxide with MXene substrate layer modification in example 3.
Fig. 3 is an XRD pattern of α phase iron oxide modified by MXene underlayer in example 3.
FIG. 4 is an XPS spectrum of α phase iron oxide with MXene underlayer modification in example 3.
FIG. 5 is a map of α phase iron oxide XAS modified by MXene underlayer in example 3
Fig. 6 is a graph of photocurrent density versus voltage (J-V) for α phase iron oxide with MXene underlayer modification in example 3.
Detailed Description
The experimental procedures used in the following examples are conventional unless otherwise specified.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified.
Preparation of α -Fe2O3Photo-anode: FTO glass is placed into a reaction kettle in a mode that a conductive surface faces upwards, and precursor solution is added into the reaction kettle (4.05 g FeCl is weighed)3·6H2O and 1.35 g C6H12O6Dissolving the mixture in 100ml of deionized water, magnetically stirring for 15 minutes to obtain FeCl in the obtained solution3And C6H12O6Respectively with the concentration of 0.15M and 1M), heating the reaction kettle at 100 ℃ for 4 hours, taking out the FTO conductive glass after the reaction kettle is cooled after heating, annealing the FTO conductive glass at 550 ℃ for 2 hours, and annealing at 750 ℃ for 15 minutes, thereby obtaining the nano α -Fe2O3And a photoelectrode.
The following example embodiments are all between the cleaning of FTO glass and the preparation of α phase iron oxide photoanode.
Example 1: dropping 100 mu L of Ti on the cleaned FTO glass3C2The solution (5mg/mL) was placed in a muffle furnace and then heated at 250 deg.CAnnealing at high temperature for 15min to obtain Ti with Ti surface3C2A layer of FTO glass. Subsequently, the FTO glass was placed in a 100mL reaction kettle (containing 80mL of FeCl)3And C6H12O6Aqueous solution with the concentration of 0.15M and 1M respectively) and carrying out hydrothermal reaction at 95 ℃ for 4 h. After the reaction is finished and cooled, taking out the FTO glass, washing the FTO glass by deionized water, and finally annealing at 550 ℃ for 2h and 750 ℃ for 15min to obtain Ti3C2Nano α -Fe modified by substrate layer2O3And a photoelectrode.
Example 2: dropping 300 mu L of Ti on the cleaned FTO glass3C2Putting the solution (5mg/mL) in a muffle furnace, annealing at 250 ℃ for 15min, and calcining at high temperature to obtain Ti with the surface3C2A layer of FTO glass. Subsequently, the FTO glass was placed in a 100mL reaction kettle (containing 80mL of FeCl)3And C6H12O6Aqueous solution with the concentration of 0.15M and 1M respectively) and carrying out hydrothermal reaction at 95 ℃ for 4 h. After the reaction is finished and cooled, taking out the FTO glass, washing the FTO glass by deionized water, and finally annealing at 550 ℃ for 2h and 750 ℃ for 15min to obtain Ti3C2Nano α -Fe modified by substrate layer2O3And a photoelectrode.
Example 3: dropping 200 mu L of Ti on the cleaned FTO glass3C2Putting the solution (5mg/mL) in a muffle furnace, annealing at 250 ℃ for 15min, and calcining at high temperature to obtain Ti with the surface3C2A layer of FTO glass. Subsequently, the FTO glass was placed in a 100mL reaction kettle (containing 80mL of FeCl)3And C6H12O6Aqueous solution with the concentration of 0.15M and 1M respectively) and carrying out hydrothermal reaction at 95 ℃ for 4 h. After the reaction is finished and cooled, taking out the FTO glass, washing the FTO glass by deionized water, and finally annealing at 550 ℃ for 2h and 750 ℃ for 15min to obtain Ti3C2Nano α -Fe modified by substrate layer2O3And a photoelectrode.
FIG. 1 is a schematic view ofDeposition of Ti in example 33C2SEM appearance comparison graph of FTO glass before and after MXene substrate layer.
FIG. 2 shows the results of example 3 in which Ti was added3C2SEM (scanning electron microscope) morphology comparison graph of α phase iron oxide modified by MXene substrate layer.
FIG. 1 Scanning Electron Microscopy (SEM) of Ti deposition in example 33C2The morphology of FTO glass before and after the MXene substrate layer is observed and analyzed, which clearly shows Ti3C2MXene substrate layers have been successfully deposited on FTO substrates. FIG. 2 shows SEM techniques for the unmodified Ti and Ti treated in example 33C2α -Fe modified by MXene underlayer2O3The feature of (2) is subjected to characterization analysis. As shown in FIG. 2, both samples exhibited worm-like nanoparticle morphology with no significant difference between the two, indicating the introduction of Ti3C2The substrate layer did not alter the microstructure of the hematite nanostructure.
FIG. 3 shows the results of example 3 in which Ti was added3C2XRD pattern of α phase iron oxide modified by MXene underlayer.
The structural testing of the prepared samples was carried out on a ray diffractometer (XRD) model Bruker D8, germany (Cu-K α rays,
in the range of 10-80 deg.) and a scan rate of 7 deg. min-1. As shown in FIG. 3, through Ti3C2α -Fe modified by MXene underlayer2O3XRD pattern for unmodified nano α -Fe2O3(Pristine Fe2O3) For photoelectrode sample, the diffraction peak energy of the photoelectrode sample was found to be α -Fe after being compared with a standard JCPDS (JCPDS 33-0664) card2O3The diffraction peaks of (A) and (B) are identical, and no diffraction peak of other substances appears (SnO)2The diffraction peak is from FTO substrate), which shows that we prepare relatively pure nanometer α -Fe by using a hydrothermal synthesis method in this chapter2O3And a photoelectrode. In addition, comparative Ti3C2Modified sample (Ti-Fe)2O3) XRD pattern ofWe can also find Ti3C2MXene substrate layer does not change nanometer α -Fe2O3Crystal structure of the photoelectrode.
FIG. 4 and FIG. 5 show the results of example 3 with Ti added3C2XPS spectrum of α phase iron oxide modified by MXene lining layer and XPS spectrum of XPE phase iron oxide modified by Ti phase iron oxide3C2An L-edge XAS spectrum of Ti element in α phase iron oxide modified by MXene underlayer.
Research on unmodified nano α -Fe by X-ray photoelectron spectroscopy (XPS) and synchrotron radiation-based X-ray absorption spectroscopy (XAS) techniques2O3And Ti3C2MXene substrate layer optimization α phase iron oxide photo-anode electronic structure and chemical composition characterization results of XPS and XAS strongly confirm Ti during high temperature sintering4+From Ti3C2The MXene substrate layer diffuses into the ferric oxide and reacts with the ferric oxide to form Fe2TiO5/Fe2O3A heterostructure photoelectrode.
FIG. 6 is a graph of the photocurrent density-voltage (J-V) of α phase iron oxide modified by MXene substrate layer in example 3, the test was performed in a quartz cell of a three-electrode system, and as shown, the unmodified nano α -Fe was used2O3The photocurrent density of the photoelectrode sample at 1.23V vs. RHE reaches 0.80mA/cm2Through Ti3C2After MXene substrate layer modification, the photocurrent density of the photoelectrode sample at 1.23V vs. RHE is increased to 1.30mA/cm2Strongly confirm Ti3C2MXene underlayers α -Fe2O3The performance improvement of photoelectrocatalysis water decomposition hydrogen production by the photoelectrode is very effective.
The above disclosure is only a preferred embodiment of the present invention, and the present invention shall be covered by the protection scope of the present invention by the replacement and modification according to the common knowledge and conventional means in the art without departing from the concept of the method of the present invention.
Claims (6)
1. A preparation method of an optimized α -phase iron oxide photo-anode with a two-dimensional titanium carbide substrate layer is characterized by comprising the following specific steps:
(1) cleaning the FTO glass;
(2) ti dripped on the cleaned FTO glass conductive surface3C2Putting the solution in a muffle furnace, annealing at 200 ℃ for 15min, and calcining at high temperature to obtain Ti with the surface3C2A layer of FTO glass;
(3) putting the FTO glass into a reaction kettle in a mode that the conductive surface faces upwards, adding a precursor solution for growing α -phase ferric oxide into the reaction kettle, heating the reaction kettle at 100 ℃ for 4 hours, taking out the FTO conductive glass after the reaction kettle is heated and cooled, annealing the FTO conductive glass at 550 ℃ for 2 hours, and annealing at 750 ℃ for 15 minutes to obtain Ti-containing material3C2Nanometer α -Fe of substrate layer2O3And a photoelectrode.
2. The method for preparing the optimized α -phase iron oxide photoanode with the two-dimensional titanium carbide substrate layer as claimed in claim 1, wherein the Ti is selected from the group consisting of Ti3C2The volume ratio of the solution to the precursor solution for growing α -phase ferric oxide is 0.1-0.3: 80, and the volume ratio of the Ti to the precursor solution is3C2The solution concentration is 5mg/mL, and the preparation step of the precursor solution for growing α -phase ferric oxide comprises weighing ferric trichloride (FeCl)3·6H2O) and glucose (C)6H12O6) Dissolving the FeCl into deionized water, magnetically stirring to obtain FeCl solution3And C6H12O6The concentrations of (A) were 0.15M and 1M, respectively.
3. The method for preparing the optimized α -phase iron oxide photoanode with the two-dimensional titanium carbide substrate layer as claimed in claim 2, wherein the Ti is selected from the group consisting of Ti3C2The volume ratio of the solution to the precursor solution for growing α -phase ferric oxide was 0.2: 80.
4. The method for preparing the α -phase iron oxide photoanode with the optimized two-dimensional titanium carbide substrate layer according to claim 1, wherein in the step (1), the step of cleaning the FTO glass comprises the steps of firstly cleaning stains on the surface of the FTO glass with a hand sanitizer or a liquid detergent, then sequentially placing the cleaned stains into deionized water and absolute ethyl alcohol for ultrasonic cleaning for 15 minutes respectively, and finally drying the cleaned stains or the dried stains for later use.
5. The method for preparing the α -phase optimized iron oxide photoanode with the two-dimensional titanium carbide substrate layer as claimed in claim 1, wherein in step (2), the temperature rise rate of the whole annealing stage is selectively controlled to 10 ℃/min.
6. The method for preparing the α -phase iron oxide photoanode optimized by the two-dimensional titanium carbide substrate layer as claimed in claim 1, wherein in step (3), after the hydrothermal reaction is finished and the reaction kettle is naturally cooled to room temperature, the FTO conductive glass is taken out of the reaction kettle and washed clean with deionized water, and the heating rate in the whole annealing stage is controlled at 10 ℃/min.
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