CN114262911B - Full-space gradient doped photoelectrode for photolysis of water and preparation method - Google Patents
Full-space gradient doped photoelectrode for photolysis of water and preparation method Download PDFInfo
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Abstract
The invention discloses a full-space gradient doped photoelectrode for photolysis of water and a preparation method thereof, belonging to the field of photoelectrochemistry. Oxide thin film (Cu) by multiple growth of single material absorption layer 2 O,α‑Fe 2 O 3 ) And a layered dopant source (Ta) 2 O 5 ,SnO 2 ,TiO 2 ,SiO 2 ,Al 2 O 3 ,Ga 2 O 3 MgO and NiO) are repeatedly grown, and then the diffusion doped photoelectrode is obtained through high-temperature annealing. By changing the thickness, doping source content and valence state (Ta) of the photoelectrode material 5+ ,Sn 4+ ,Al 3+ ,Mg 2+ ) And atomic radius (Sn) 4+ ,Ti 4+ ,Si 4+ ) And constructing photoelectrodes with different gradient doping by equal parameters. The invention carries out full-space gradient doping on the oxide film, constructs a built-in electric field penetrating through the whole photoelectrode, obtains the built-in electric field with controllable direction and space action range, avoids introducing surface/interface defects, and obviously improves the carrier separation efficiency and photoelectrochemical property of the oxide film photoelectrode.
Description
Technical Field
The invention belongs to the field of photoelectrochemistry, relates to a full-space gradient doped photoelectrode and a preparation method thereof, and particularly relates to separation and transfer of a photon-generated carrier and application thereof in the field of photoelectrochemical water splitting (PEC-WS).
Background
The solar energy capturing technology which takes photoelectrochemistry conversion as a core is taken as a novel, high-efficiency and low-cost energy conversion method, and has wide application prospect in the aspects of solving the problems of energy shortage and environmental pollution. PEC-WS is one of the effective means of photoelectrochemical conversion, and the choice of semiconductor photoelectrode is critical to its performance. The oxide thin film photoelectrode has the advantages of adjustable chemical composition, controllable energy band, stable performance and the like, and has remarkable advantages in the field of PEC-WS, but the low carrier separation efficiency prevents the further application of the oxide thin film photoelectrode in the field of PEC-WS.
In order to solve the problem of low carrier separation efficiency, the current research strategies mainly include: (1) Heterogeneous/homogeneous junction, crystal plane engineering and the like are constructed, although the mode is effective, the action range is limited, and table/interface defects are additionally introduced; (2) A new material with spontaneous polarity is developed, but the material has high requirements on a crystal structure and great synthesis difficulty and is difficult to popularize; (3) The doping regulation energy band structure is that element diffusion and precursor solutions with different concentrations are utilized to construct a built-in electric field, but the problems that the space action range of the built-in electric field and defect introduction cannot be considered simultaneously exist. The built-in electric field has been proved to be effective in promoting the separation of carriers, but how to construct a built-in electric field with controllable direction and space action range and avoid introducing additional defects becomes a key and difficult point of research.
Disclosure of Invention
The invention provides a built-in electric field constructed by a full-space gradient doping mode based on the idea of element doping regulation and control of an energy band structure, so as to improve the carrier separation efficiency of an oxide film photoelectrode.
The invention relates to a full-space gradient doped photoelectrode which sequentially comprises the following components from bottom to top: the FTO substrate, the oxide film and the layered doping source form a modified oxide film, and the concentration of the doping source is reduced from bottom to top in sequence.
Further, in the above technical solution, the oxide thin film layer includes: alpha-Fe 2 O 3 ,TiO 2 ,WO 3 ,Cu 2 O,BiVO 4 Any one of them. These oxide thin film semiconductors can be used as photoelectrodes.
Further, in the above technical solution, the doping source includes: ta 2 O 5 ,SnO 2 ,TiO 2 ,SiO 2 ,Al 2 O 3 MgO, niO, or a combination of two or more thereof. The atomic radius, valence state, etc. of the doping source affect the band structure of the oxide thin film semiconductor.
Further, in the above technical solution, the oxide thin film is obtained by a hydrothermal method, an atomic layer deposition method, and a thermal decomposition method; the doped source is obtained by spray pyrolysis, atomic layer deposition and adsorption.
Further, in the above technical solution, the thickness of the full-space gradient doped photoelectrode (except for FTO substrate) is 450-550nm (optimally 500 nm). As the oxide thin film layer is deposited on the transparent conductive FTO substrate, the appearance of the oxide thin film layer is a planar structure, and 450-550nm (optimally 500 nm) is favorable for regulating and controlling gradient doping in the whole space range and can keep good absorption.
Further, in the above technical solution, the thickness of the oxide thin film layer is 65-75nm (preferably 70 nm), 80-90nm (preferably 85 nm), 95-105nm (preferably 100 nm), 110-120nm (preferably 115 nm) and 125-135nm (preferably 130 nm) in sequence from the FTO substrate to the top. Due to the oxide film thickness in this range, the dopant source can sufficiently diffuse the oxide film at high temperatures. The thickness gradient of 10-20nm (preferably 15 nm) is set to be beneficial to the photo-generated carriers to be fully separated and transferred in the photoelectrode with gradient change.
Further, in the above technical solution, the doping source has a uniform thickness of 1.5 to 2.5nm (preferably 2 nm). After high-temperature annealing, the 1.5-2.5nm (preferably 2 nm) thick doping source not only can dope the oxide film, but also can neglect the heterojunction interface contact formed by the oxide film and the doping source, and is beneficial to carrier transportation.
Further, in the above technical solution, the oxide thin film semiconductor is an n-type or p-type semiconductor, and the doping source is an n-type or p-type doping.
Further, in the above technical solution, the full-space gradient doped photoelectrode is as shown in fig. 1.
The invention relates to a preparation method of a full-space gradient doped photoelectrode, which comprises the following steps: using FTO as substrate, and coating oxide film (Cu) 2 O,α-Fe 2 O 3 ) And a layered dopant source (Ta) 2 O 5 ,SnO 2 ,TiO 2 ,SiO 2 ,Al 2 O 3 ,Ga 2 O 3 MgO and NiO) are repeatedly grown, and then the diffusion doped photoelectrode is obtained through high-temperature annealing.
Furthermore, in the above technical scheme, gradient doping is realized by multiple growth of a single material absorption layer and a high-temperature diffusion mode, and a full-space gradient doped photoelectrode with controllable direction and space action range is obtained by regulating and controlling the thickness, the content and the type of an oxide film and the like.
Further, in the above technical solution, the photoelectrode is grown with FTO as a conductive substrate.
The invention further provides application, namely application of the full-space gradient doped photoelectrode in photoelectrochemical water decomposition.
Further, in the above technical solution, the working principle of photoelectrochemical water decomposition is shown in fig. 2.
In the scheme of the invention, a built-in electric field with controllable gradient doping construction direction and space action range is provided, and the structural configuration with optimal carrier separation efficiency is proved by adjusting and controlling parameters such as the thickness of the light electrode film, the content of a doping source, a valence state, the atomic radius and the like. The oxide film photoelectric electrode has the characteristic of adjustable chemical composition, can accurately design and regulate the position of a semiconductor energy band through element doping, and simultaneously enables the position of the energy band to be continuously changed by means of gradient doping to form a built-in electric field. The method prepares the gradient doped oxide thin film photoelectrode by combining the mode of growing the single material absorption layer for multiple times and high-temperature diffusion doping, can construct a built-in electric field with controllable direction and space action range, can reduce defect introduction through diffusion doping, and ensures good crystallinity of the photoelectrode material.
Technical effects
The invention synthesizes Sn doped alpha-Fe by utilizing a multi-growth single material absorption layer and high-temperature diffusion doping 2 O 3 Photoelectrode by fixing a doping source Sn 4+ Content, continuously changing alpha-Fe 2 O 3 The film thickness method forms a gradient doping. Continuously growing five-cycle FeOOH film and interlayer doping source Sn 4+ Synthesizing alpha-Fe with uniform doping and gradient doping (gradient doping increase and gradient doping decrease from FTO substrate to solid-liquid interface) 2 O 3 And (3) a photoelectrode material. SEM showed that the thickness was 500nm and the absorbance was almost unchanged. But gradient doping reduces alpha-Fe 2 O 3 The photoelectrode exhibited a greater photocurrent density (1.61 mA/cm) 2 ) While the graded doped enlarged photoelectrode has minimum photoelectricityFlow Density (0.66 mA/cm) 2 ). By means of H 2 O 2 The hole scavenger method is used for calculating the separation efficiency and the transfer efficiency of the carrier, and the gradient doping reduces the alpha-Fe 2 O 3 The photoelectrode has larger carrier separation efficiency and transfer efficiency, and the increase of the gradient doping causes the carrier separation efficiency and the transfer efficiency to be relatively low. The main reason is that the gradient doping reduces alpha-Fe 2 O 3 The built-in electric field constructed by the photoelectrode has the same direction with the built-in electric field at the solid/liquid junction, and is beneficial to promoting the separation of current carriers. And the built-in electric field constructed by the gradient doping increased photoelectrode is opposite to the built-in electric field at the solid/liquid junction, so that the carrier separation is hindered, and the PEC-WS performance is reduced.
Drawings
FIG. 1: a schematic diagram of a full-space gradient doping reduction photoelectrode structure for photolysis of water; wherein: e i Representing the built-in electric field direction from the FTO substrate toward the surface of the photoelectrode.
FIG. 2: the working principle of photoelectrochemical water decomposition is shown schematically; wherein: e.g. of a cylinder - Represents photo-generated electrons, h + Representing the photo-generated holes.
FIG. 3: the gradient doping reduces the carrier transport of the photoelectrode; wherein: e i Represents the direction of the built-in electric field, E F Represents the Fermi level, e - Represents photo-generated electrons, h + Representing the photo-generated holes.
FIG. 4 is a schematic view of: alpha-Fe with different cycle numbers 2 O 3 Uniformly doping the photoelectrode, reducing gradient doping and increasing a physical map by the gradient doping; wherein: 1 to 5 are homogeneous doping, 1 is 1 cycle, 2 is 2 cycles, 3 is 3 cycles, 4 is 4 cycles, 5 is 5 cycles; 6 is gradient doping increase, 7 is gradient doping decrease;
FIG. 5: gradient doping to reduce alpha-Fe 2 O 3 A photoelectrode scanning electron microscope top view;
FIG. 6: gradient doping to reduce alpha-Fe 2 O 3 A cross-sectional view of a photoelectrode scanning electron microscope;
FIG. 7: gradient doping to reduce alpha-Fe 2 O 3 Photoelectrode transmission electron micrographs;
FIG. 8: gradient doping to reduce alpha-Fe 2 O 3 A content change diagram of elements Fe, O and Sn in the photoelectrode; wherein: position 1 to position 5 FTO substrate to alpha-Fe 2 O 3 The position of the surface of the photoelectrode changes.
FIG. 9: uniform doping, gradient doping increase and gradient doping decrease of alpha-Fe 2 O 3 Photoelectrode light absorption spectra;
FIG. 10: uniform doping, gradient doping increase and gradient doping decrease of alpha-Fe 2 O 3 The change situation of the photocurrent of the photoelectrode under different bias voltages is illustrated; wherein: at 1.23V RHE Reduced photocurrent density, graded doping compared to homogeneously doped alpha-Fe 2 O 3 The photoelectrode is improved by 36.1 percent, and the gradient doping is increased compared with the uniform doping of alpha-Fe 2 O 3 The photoelectrode is reduced by 44.2%.
FIG. 11: uniform doping, gradient doping increase and gradient doping decrease of alpha-Fe 2 O 3 Photoelectrode at 1.23V RHE A graph of transient photocurrent density variation; wherein: uniform doping, gradient doping increase and gradient doping decrease of alpha-Fe 2 O 3 The photoelectrode surface recombination rates were 33.8%,39.2% and 28.3%, respectively.
FIG. 12: uniform doping, gradient doping increase and gradient doping decrease of alpha-Fe 2 O 3 A graph of the change of the absorption and separation efficiency of photo-generated carriers under different bias voltages of the photoelectrode; wherein: at 1.23V RHE Reduced gradient doping compared to homogeneously doped alpha-Fe at photogenerated carrier separation efficiency 2 O 3 The photoelectrode is improved by 13.3 percent, and the gradient doping is increased compared with the uniform doping of alpha-Fe 2 O 3 The photoelectrode is reduced by 19.5%.
FIG. 13: uniform doping, gradient doping increase and gradient doping decrease of alpha-Fe 2 O 3 The change condition of the photo-generated carrier transfer efficiency of the photoelectrode under different bias voltages is shown; wherein: at 1.23V RHE Reduced gradient doping compared to homogeneously doped alpha-Fe for photo-generated carrier transfer efficiency 2 O 3 The photoelectrode is improved by 15.7 percent, and the gradient doping is increased compared with the uniform doping of alpha-Fe 2 O 3 Photovoltaic deviceThe reduction is extremely 25.5%.
Detailed Description
In order to more clearly illustrate the technical solution, the following is further described with reference to the accompanying drawings and embodiments:
a full-space gradient doped photoelectrode for photolyzing water is disclosed, which can reduce alpha-Fe when the selected photoelectrode is full-space gradient doped 2 O 3 The photoelectrode is such that the photogenerated carrier separation and collection directions are as shown in figure 3. alpha-Fe reduction with graded doping 2 O 3 The photoelectrode energy band curves upward, forming a built-in electric field directed from the FTO substrate to the photoelectrode/electrolyte interface. Because the direction of the built-in electric field is consistent with that of the photoelectrode/electrolyte interface electric field, the separation and transfer of photon-generated carriers are facilitated. Therefore, the photoelectrode with gradient doping reduction is more beneficial to transferring photo-generated electrons to the conductive FTO substrate and transferring photo-generated holes to electrolyte, and the separation of photo-generated carriers is improved.
First, the FTO substrate was ultrasonically cleaned with water, acetone and ethanol in sequence for 15 minutes and tilted at a 45 ° angle in a teflon-lined vessel and using a solution containing 1.5mmol of FeCl 3 And 50mL of a mixed aqueous solution of 1.5mmol of urea was used as a reaction solution. And heating the mixed solution to 100 ℃, keeping the temperature for 12 hours, and cooling to synthesize the FeOOH film. It was then immersed in 0.1M SnCl 4 The ethanol solution is dried for 15 minutes at 60 ℃ in an air atmosphere for 30 minutes, and elemental Sn absorption is formed on the surface of the FeOOH film. The three steps (i.e., hydrothermal reaction, soaking and drying) are referred to as a growth cycle. After the growth cycle was repeated five times, it was annealed at 550 ℃ for 2 hours in an air atmosphere and then at 700 ℃ for 15 minutes to obtain alpha-Fe doped with uniform Sn 2 O 3 A film. Doped alpha-Fe for two other gradient increases or gradient decreases 2 O 3 The film has different hydrothermal reaction time in each growth period and different thickness of FeOOH film prepared in different periods. For the case of increasing gradient doping, the hydrothermal reaction times for five consecutive cycles were 16 hours, 14 hours, 12 hours, 10 hours, and 8 hours, respectively. For gradient doping reduction, the hydrothermal reaction time of five continuous cycles is respectively 8 hours, 10 hours, 12 hours and 14 hoursHours and 16 hours. Other preparation processes and the above uniformly doped alpha-Fe 2 O 3 Sample objects were prepared as shown in FIG. 4, as was the photoelectrode.
For the case of increasing gradient doping, the thickness of the FeOOH film in each growth period decreases with the increase of the cycle number, namely 130nm, 115nm, 100nm, 85nm and 70nm respectively. For the graded doping reduction case, the thickness of the FeOOH film shows the opposite trend for each growth cycle, i.e., 70nm, 85nm, 100nm, 115nm, 130nm, respectively. For three alpha-Fe 2 O 3 The photoelectrode, surface topography was not significantly different, as shown in figure 5. Final alpha-Fe 2 O 3 The overall thickness of the film is nearly equal (-500 nm) as shown in fig. 6.
Reducing alpha-Fe for gradient doping 2 O 3 Photoelectrode, shown in FIG. 7, of α -Fe 2 O 3 The film is composed of nanoparticles with a diameter of 50nm, and is in a microcrystalline state. As shown in FIG. 8, the doping source Sn content gradually decreases from the FTO substrate area to the photoelectrode surface area, the Fe content slightly increases, and the O content hardly changes, which indicates that the reduction of alpha-Fe by gradient doping is successfully realized 2 O 3 And (3) preparing a thin film photoelectrode.
The prepared material is uniformly doped by means of an ultraviolet-visible-near infrared spectrophotometer, the gradient doping is increased, and the gradient doping is reduced by alpha-Fe 2 O 3 The photoelectrode was subjected to reflectance, transmittance spectral measurements, and the test sample light absorption efficiency was calculated by subtracting the sum of reflectance and transmittance from 1. As shown in FIG. 9, uniform doping, gradient doping increase and gradient doping decrease α -Fe 2 O 3 The photoelectrode absorption spectra were almost the same, indicating that the absorbances were the same.
As shown in fig. 10, shows uniform doping, gradient doping increase and gradient doping decrease of α -Fe 2 O 3 Photoelectrode J-V curve; and uniformly doping with alpha-Fe 2 O 3 Gradient doping increases alpha-Fe compared to photoelectrode 2 O 3 Photoelectrode J ph@1.23V Reduced by 44.1% (from 1.18 mA/cm) 2 Reduced to 0.66mA/cm 2 ) But reducing alpha-Fe for doping with a gradient 2 O 3 The photoelectrode increased by 36.4% (from 1.18 mA/cm) 2 Increased to 1.61mA/cm 2 ). The turn-on potentials of the three photoelectrodes were almost the same (0.81V) REH ) And the saturated photocurrent was obtained at almost the same potential (-1.1V) REH ). As shown in FIG. 11, the transient photocurrent density has the same trend as the J-V curve, and the gradient doping reduces the alpha-Fe 2 O 3 The photoelectrode had a minimum decay rate (28.3%), with uniform and graded doping increasing the decay rate by 33.8% and 39.2%, respectively. The attenuation ratio is calculated according to the steady-state and transient photocurrent densities, and can reflect the surface carrier recombination of the photoelectrode. Gradient doping to reduce alpha-Fe 2 O 3 The photoelectrode has a minimum surface recombination rate.
Taking into account alpha-Fe 2 O 3 Absorption wavelength range of photoelectrode, uniform doping, gradient doping increase and gradient doping decrease alpha-Fe 2 O 3 Light absorption efficiency (eta) of the photoelectrode abs ) Almost the same, calculate η abs ×η sep Can directly reflect the carrier separation efficiency (eta) sep ) And (4) relative relation. As shown in FIG. 12, and uniformly doping with alpha-Fe 2 O 3 Gradient doping to reduce alpha-Fe compared to photoelectrode 2 O 3 Photoelectrode at 1.23V RHE Eta of treatment sep Increased by 13.3%, while gradient doping increased alpha-Fe 2 O 3 The photoelectrode is reduced by 19.5%. As shown in FIG. 13, gradient doping reduces α -Fe 2 O 3 Photoelectrode at 1.23V RHE Lower carrier transfer efficiency (. Eta.) tran ) 58.2% greater than homogeneous doping (50.3%) and graded doping increase (37.5%) alpha-Fe 2 O 3 And a photoelectrode. Thus, gradient doping reduces α -Fe 2 O 3 The improved PEC-WS performance of the photoelectrode can be attributed to increased separation and transfer efficiency of photogenerated carriers.
The data fully indicate that the scheme is feasible, the gradient doping is realized by growing the single material absorption layer for multiple times and high-temperature diffusion of elements, the built-in electric field with controllable direction and space action range is formed by depending on the gradient change energy band structure, and finally, the separation of the photo-generated carriers in the whole space range is effectively improved by the gradient dopingEfficiency. The gradient Sn doped alpha-Fe is prepared by the scheme 2 O 3 Photoelectrode, gradient doping found to reduce alpha-Fe 2 O 3 The photoelectrode has the maximum photon-generated carrier separation and transfer efficiency. Therefore, the full-space gradient doping has a remarkable enhancement effect on the separation and transfer efficiency of the photon-generated carriers of the photoelectrode, and the PEC-WS performance can be effectively improved.
The foregoing embodiments have described the general principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the present invention, and that various changes and modifications may be made without departing from the scope of the principles of the present invention, and the invention is intended to be covered by the appended claims.
Claims (5)
1. The utility model provides a full space gradient doping photoelectrode, from the bottom up does in proper order: the FTO substrate, the oxide film and the layered doping source form a modified oxide film, the oxide film is multilayer, and the concentration of the doping source is reduced from bottom to top; the oxide film layer is alpha-Fe 2 O 3 (ii) a The doping source is SnO 2 By fixing the doping source Sn 4+ Content, continuously varying alpha-Fe 2 O 3 Forming gradient doping by a film thickness method; the thickness of the full-space gradient doped photoelectrode except the FTO substrate is 450-550nm; the full-space gradient doped photoelectrode continuously grows five cycles of FeOOH thin films and interlayer doping source Sn 4+ Then, annealing at high temperature to obtain a gradient doped photoelectrode; the thickness of the FeOOH film is 65-75nm, 80-90nm, 95-105nm, 110-120nm and 125-135nm from the FTO substrate to the top in sequence; the interlayer doping source Sn 4+ The thickness is 1.5-2.5nm.
2. The full-space gradient doped photoelectrode of claim 1, wherein: the oxide film is obtained by a hydrothermal method, an atomic layer deposition method or a thermal decomposition method; the layered doping source is obtained by a spray pyrolysis method, an atomic layer deposition method or an adsorption method; the photoelectrode grows by taking FTO as a conductive substrate.
3. The full-space gradient doped photoelectrode of claim 1, wherein: the oxide thin film semiconductor is an n-type or p-type semiconductor, and the doping source is n-type or p-type doping.
4. A method of fabricating a full-space gradient doped photoelectrode as claimed in any one of claims 1 to 3 comprising the steps of: using FTO as a substrate, and mixing FeOOH film and interlayer doping source Sn 4+ And repeatedly growing, and annealing at high temperature to obtain the gradient doped photoelectrode.
5. Use of a full-space gradient doped photoelectrode according to any one of claims 1 to 3 in photoelectrolysis water.
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