CN113201766B - Preparation method of hematite photoanode - Google Patents
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Abstract
The invention relates to the technical field of photoelectric water decomposition, in particular to a preparation method of a hematite photoanode. The preparation method provided by the invention comprises the following steps: mixing a trivalent ferric salt and a solvent to obtain a trivalent ferric salt solution, adding a strong base, and stirring to obtain a reaction solution; carrying out solvothermal reaction on the reaction solution to obtain the hematite photoanode; the solvent comprises water and an alcohol organic solvent; no surfactant is used in the preparation process of the hematite photoanode. The invention does not use a surfactant, and synthesizes the uniform hematite with shuttle, pseudo-shuttle, drum and sheet shapes by adjusting the solvent to be water and alcohol organic solvent and adopting a solvothermal method.
Description
Technical Field
The invention relates to the technical field of photoelectric water decomposition, in particular to a preparation method of a hematite photoanode.
Background
Photoelectrochemical (PEC) water splitting technology is a particularly attractive technology that can collect and convert solar energy into clean and renewable energy sources to address the increasing energy consumption of the world, and semiconductors that generate electron-hole pairs by incident photons are an important area of research in recent years for efficient light-absorbing photoelectrodes and the main components of typical PEC devices. However, a key issue with semiconductor + photoelectrode is the high efficiency of solar hydrogen production (STH), and the overall STH efficiency is mainly controlled by three processes: (1) light collection/charge separation (. eta.)light) (ii) a (2) Charge transport/recombination (η) in semiconductorsct) (ii) a (3) Hole collection (η) at the electrode surfacehc). In the semiconductor material, hematite has a proper valence band position for water oxidation due to the band gap of 2.1eV, excellent robustness and abundance, and has improvementAdvantageous properties of STH efficiency and PEC efficiency. However, since the crystal form and the micro-morphology are important influencing factors influencing the performance of photoelectrochemically decomposing water of the hematite, the problem of how to improve the performance of photoelectrochemically decomposing water of the hematite by changing the crystal form and the micro-morphology of the hematite is a constant concern.
Disclosure of Invention
The hematite photoanode prepared by the preparation method has uniform hematite with shuttle, pseudo-shuttle, drum or sheet shape, and high atomic density, so that the surface activity is further enhanced, and the photoelectrochemistry water decomposition performance is finally improved.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a preparation method of a hematite photoanode, which comprises the following steps:
mixing a trivalent ferric salt and a solvent to obtain a trivalent ferric salt solution, adding a strong base, and stirring to obtain a reaction solution;
carrying out solvothermal reaction on the reaction solution to obtain the hematite photoanode;
the solvent comprises water and an alcohol organic solvent;
no surfactant is used in the preparation process of the hematite photoanode.
Preferably, the alcohol organic solvent comprises ethylene glycol and ethanol;
the volume ratio of the ethylene glycol to the ethanol is 6: (2-10);
the volume ratio of the water to the alcohol organic solvent is (4-12): (8-16).
Preferably, the volume ratio of the molar amount of the ferric iron salt to the solvent is (0.5-1) mmol: 20 mL.
Preferably, the ferric salt is ferric nitrate, ferric trichloride, ferric acetate or ferric sulfate;
the strong base is sodium hydroxide and/or potassium hydroxide.
Preferably, the mixing is carried out under the condition of stirring, the rotating speed of the stirring is 100-3000 rpm, and the time is 1-40 min.
Preferably, the rotating speed of the stirring is 100-3000 rpm, and the time is 20-40 min.
Preferably, the molar ratio of the strong base to the ferric salt is (2-3): (0.5 to 1).
Preferably, the temperature of the solvothermal reaction is 180-220 ℃, and the time is 6-10 h.
Preferably, after the solvothermal reaction is completed, the method further comprises sequentially performing centrifugation, washing and drying.
Preferably, the drying temperature is 60 ℃ and the drying time is 12 h.
The invention provides a preparation method of a hematite photoanode, which comprises the following steps: mixing a trivalent ferric salt and a solvent to obtain a trivalent ferric salt solution, adding a strong base, and stirring to obtain a reaction solution; carrying out solvothermal reaction on the reaction solution to obtain the hematite photoanode; the solvent comprises water and an alcohol organic solvent; no surfactant is used in the preparation process of the hematite photoanode.
Compared with the prior art, the invention has the following advantages and effects:
the invention does not use a surfactant, and synthesizes the uniform hematite with shuttle, pseudo-shuttle, drum and sheet shapes by adjusting the solvent to be water and alcohol organic solvent and adopting a solvothermal method. The results of the examples show that the hematite photoanodes prepared by the preparation method of the present invention have a very high atomic density, which enhances their surface activity. Wherein the shuttle morphology of hematite exhibits a photocurrent onset potential of 1.52V vs. RHE and exhibits a potential of 8.67 mA-cm at 1.94V vs. RHE-2The photocurrent of (c). Further XPS analysis confirmed that the shuttle form of Fe2O3The NPs surface exposes a higher content of iron atoms or oxygen vacancies, resulting in a positively charged surface, thereby promoting OH-Chemisorption of molecules and thus enhanced electrocatalytic activity. This work opens up new possibilities not only for designing efficient electrode materials for PEC devices, but also for passing through shapesThe control and enhancement of the electrochemical performance of the material provide a new method.
Drawings
FIG. 1 is an electron micrograph of products prepared in examples 1 to 4;
FIG. 2 is an XRD pattern, UV-Vis absorption spectrum and Raman spectrum of the product prepared in examples 1-4;
FIG. 3 shows J-V characteristics, O1s XPS spectra and O of products prepared in examples 1 to 4LComponents (black) and OVHistogram of component (red);
FIG. 4 shows α -Fe in examples 1 to 42O3XPS spectra and high resolution Fe 2p region.
Detailed Description
The invention provides a preparation method of a hematite photoanode, which comprises the following steps:
mixing a trivalent ferric salt and a solvent to obtain a trivalent ferric salt solution, adding a strong base, and stirring to obtain a reaction solution;
carrying out solvothermal reaction on the reaction solution to obtain the hematite photoanode;
the solvent comprises water and an alcohol organic solvent;
no surfactant is used in the preparation process of the hematite photoanode.
In the present invention, all the starting materials for the preparation are commercially available products known to those skilled in the art unless otherwise specified.
In the invention, trivalent ferric salt and a solvent are mixed to obtain a trivalent ferric salt solution, and then strong base is added and stirred to obtain a reaction solution.
In the present invention, the ferric salt is preferably ferric nitrate, ferric trichloride, ferric acetate or ferric sulfate.
In the present invention, the solvent includes water and an alcohol organic solvent; the alcohol organic solvent comprises glycol and ethanol; the volume ratio of the ethylene glycol to the ethanol is preferably 6: (2-10); the volume ratio of the water to the alcohol organic solvent is preferably (4-12): (8-16); that is, the volume ratio of the ethylene glycol, water and ethanol is preferably 6: (4-12): (2-10), more preferably 6: 12:2 or 6:10:4 or 6:6:8 or 6:4: 10. In the invention, the micro-morphology of the ferrite red photo-anode can be further adjusted by controlling the mixture ratio of each component in the solvent.
In the present invention, the ratio of the molar amount of the ferric salt to the volume of the solvent is preferably (0.5 to 1) mmol: 20mL, more preferably (0.6 to 0.8) mmol: 20 mL.
In the invention, the mixing is preferably carried out under the condition of stirring, and the rotating speed of the stirring is preferably 100-3000 rpm, more preferably 500-1500 rpm; the time is preferably 1 to 40min, and more preferably 20 to 30 min.
In the present invention, the strong base is preferably sodium hydroxide and/or potassium hydroxide; when the strong base is a mixture of sodium hydroxide and potassium hydroxide, the ratio of the sodium hydroxide to the potassium hydroxide is not limited in any way, and the sodium hydroxide and the potassium hydroxide are mixed according to any ratio.
In the invention, the molar ratio of the strong base to the ferric salt is preferably (2-3): (0.5 to 1), more preferably (2 to 2.6): (0.6-0.8), and most preferably 2: 0.6. In the present invention, the strong base is preferably poured rapidly into the solution of the ferric salt.
In the invention, the rotation speed of stirring after adding the potassium hydroxide is preferably 100-3000 rpm, more preferably 500-1500 rpm; the time is preferably 20 to 40min, and more preferably 25 to 35 min.
After the reaction solution is obtained, the invention carries out solvothermal reaction on the reaction solution to obtain the hematite photoanode.
In the invention, the temperature of the solvothermal reaction is preferably 180-220 ℃, more preferably 190-210 ℃, and most preferably 200 ℃; the time is preferably 6 to 10 hours, and more preferably 6 to 8 hours.
In the invention, the process of the solvothermal reaction is to add the reaction solution into a 50mL reaction kettle with a polytetrafluoroethylene stainless steel substrate and transfer the reaction solution into an electrothermal blowing dry box for solvothermal reaction.
After the solvothermal reaction is finished, the invention also preferably comprises the steps of sequentially centrifuging, washing and drying; preferably, the centrifugation further comprises cooling; the cooling process is not particularly limited in the present invention, and may be performed by a process known to those skilled in the art. The centrifugation process is not particularly limited in the present invention, and may be performed by a process known to those skilled in the art. In the present invention, the detergent used for the washing is preferably deionized water. In the present invention, the drying temperature is preferably 60 ℃ and the drying time is preferably 12 hours.
The method for producing hematite according to the present invention will be described in detail with reference to examples, but they should not be construed as limiting the scope of the present invention.
Example 1
Mixing 0.6mmol of ferric nitrate and 20mL of solvent (6mL of ethylene glycol, 12mL of distilled water and 2mL of ethanol) under the condition of stirring, wherein the rotating speed of stirring is 600rpm, the time is 20min, after obtaining ferric nitrate solution, adding 2mmol of potassium hydroxide, and stirring for 20min to obtain reaction liquid;
adding the reaction solution into a 50mL reaction kettle with a polytetrafluoroethylene stainless steel substrate, transferring the reaction solution into an electrothermal blowing drying oven, carrying out solvothermal reaction at 200 ℃ for 6h, cooling to room temperature, centrifuging to obtain a precipitate, washing the precipitate with ethanol and deionized water, and carrying out vacuum drying at 60 ℃ for 12h to obtain the shuttle-shaped alpha-Fe2O3NPs, as Shuttle-like Fe2O3。
Example 2
Mixing 0.6mmol of ferric nitrate and 20mL of solvent (6mL of ethylene glycol, 10mL of distilled water and 4mL of ethanol) under the condition of stirring, wherein the rotating speed of stirring is 600rpm, the time is 20min, after obtaining ferric nitrate solution, adding 2mmol of potassium hydroxide, and stirring for 20min to obtain reaction liquid;
adding the reaction solution into a 50mL reaction kettle with a polytetrafluoroethylene stainless steel substrate, transferring the reaction solution into an electrothermal blowing dry box, carrying out a solvothermal reaction at 200 ℃ for 6 hours, cooling to room temperature, centrifuging to obtain a precipitate, washing with ethanol and deionized water, and then washing at 60 DEG CVacuum drying for 12h to obtain pseudo-shuttle-shaped alpha-Fe2O3NPs, as Pseudo-Shuttlle-like Fe2O3。
Example 3
Mixing 0.6mmol of ferric nitrate and 20mL of solvent (6mL of ethylene glycol, 6mL of distilled water and 8mL of ethanol) under the condition of stirring at the rotating speed of 600rpm for 20min to obtain a ferric nitrate solution, adding 2mmol of potassium hydroxide, and stirring for 20min to obtain a reaction solution;
adding the reaction solution into a 50mL reaction kettle with a polytetrafluoroethylene stainless steel substrate, transferring the reaction solution into an electrothermal blowing drying oven, carrying out solvothermal reaction at 200 ℃ for 6h, cooling to room temperature, centrifuging to obtain a precipitate, washing with ethanol and deionized water, and carrying out vacuum drying at 60 ℃ for 12h to obtain drum-shaped alpha-Fe2O3NPs, as dry-like Fe2O3。
Example 4
Mixing 0.6mmol of ferric nitrate and 20mL of solvent (6mL of ethylene glycol, 4mL of distilled water and 10mL of ethanol) under the condition of stirring, wherein the rotating speed of stirring is 600rpm, the time is 20min, after obtaining ferric nitrate solution, adding 2mmol of potassium hydroxide, and stirring for 20min to obtain reaction liquid;
adding the reaction solution into a 50mL reaction kettle with a polytetrafluoroethylene stainless steel substrate, transferring the reaction solution into an electrothermal blowing drying oven, carrying out solvothermal reaction at 200 ℃ for 6h, cooling to room temperature, centrifuging to obtain a precipitate, washing the precipitate with ethanol and deionized water, and carrying out vacuum drying at 60 ℃ for 12h to obtain flaky alpha-Fe2O3NPs, note tablet-like Fe2O3。
Test example
XRD, XPS, SEM and TEM tests were performed on the products prepared in examples 1-4, respectively, wherein FIG. 1 is an electron micrograph (SEM pictures for a-d, TEM pictures for a 1-d 1 and HRTEM pictures for a 2-d 2) of the products prepared in examples 1-4, and it can be seen from a-d that the products prepared in examples 1-4The microscopic appearances of the product are in a shuttle shape, a pseudo-shuttle shape, a drum shape and a sheet shape in sequence; wherein a1 and a2 show that the volume ratio of ethanol to water is 1: 6 synthesizing shuttle-shaped alpha-Fe2O3And (4) NPs. Shuttle-shaped alpha-Fe2O3The average peak-to-peak length (L) of the NPs is about 190.3nm, the average edge-to-edge distance (D) is about 96.9nm, the lattice spacing is 0.22nm and alpha-Fe2O3The (113) faces of the NPs are matched. b1 and b2 show that when the ethanol/water ratio is increased to 2: at 5, L of the NPs decreased and D increased (forming pseudo-shuttle NPs), with a lattice spacing of 0.22nm and α -Fe2O3The (113) faces of the NPs are matched. c1 and c2 show that when the volume ratio is further increased, drum-like α -Fe is obtained2O3NPs and both ends of the NP are truncated (c1) with a lattice spacing of 0.27nm corresponding to alpha-Fe2O3The (104) plane of the NPs. Finally, FIGS. d1 and d2 show flaky alpha-Fe2O3NPs having an average diameter of about 148.6nm and a thickness of 65.9nm, with a corresponding lattice spacing of 0.229nm indexed to alpha-Fe2O3The (006) plane of the NPs.
FIG. 2 is an XRD pattern, UV-Vis absorption spectrum and Raman spectrum of the product prepared in examples 1-4; wherein a is an XRD pattern; b is UV-Vis absorption spectrum; c is a Raman spectrum; from a, the products prepared in examples 1 to 4 were compared with standard Ka α -Fe2O3(JCPDS No.33-0664) proved successful synthesis of alpha-Fe2O3NP; it can be known from b that the light absorption of the products prepared in examples 1-4 from ultraviolet to near infrared is significantly enhanced, which indicates that the prepared products may have potential application in photocatalysts and photothermal therapy; according to the results of c, the products prepared in examples 1-4 exhibit typical Raman active vibration mode and A1g mode (220 and 495 cm)-1) And Eg mode (286, 403 and 602 cm)-1) Frequency band of (2) and magnon scattering (1305 cm)-1). At larger wavenumbers, overtones of first order scattering or second order scattering processes can be observed.
FIG. 4 shows XPS plots (a) and high-resolution Fe 2P regions (b) of the products prepared in examples 1 to 4, and it can be seen from FIG. 4 that the products prepared in examples 1 to 4 include Fe and O elements, and the Fe exists in +3 valence.
The product prepared in the embodiment 1-4 is prepared into a photo-anode material and an electrode, and the specific preparation process comprises the following steps: dripping 150 mu L of nafion suspension of the photoanode material with the concentration of 1mg/mL on an ITO electrode, and drying in a drying oven at 60 ℃ to obtain an electrode;
the electrode is taken as a working electrode, silver/silver chloride (Ag/AgCl) is taken as a reference electrode, a platinum sheet is taken as an auxiliary electrode, and simulated solar light (100 mW/cm)2150W xenon lamp plus AM 1.5G filter), the test results are shown in FIG. 3, a is the J-V characteristic of the electrode prepared from the product prepared in examples 1-4, b is the shuttle-shaped alpha-Fe2O3O1s XPS spectrum of NPs, c is pseudo-shuttle alpha-Fe2O3O1s XPS spectrum of NPs, d is drum-like alpha-Fe2O3O1s XPS spectrum of NPs, e is flaky alpha-Fe2O3O1s XPS spectrum of NPs, f is OLComponent sum OVHistograms of components); a is understood to be a shuttle-shaped alpha-Fe2O3NPs have optimal photoelectrochemical properties; from b to f, XPS analysis confirmed that the shuttle-like Fe2O3NPs surfaces expose a higher content of iron atoms or oxygen vacancies, resulting in a more positively charged surface; shuttle-shaped alpha-Fe2O3The NPs are surrounded by facets and have a very high atomic density, which enhances their surface activity, and these results indicate that shuttle-like α -Fe2O3NPs tend to absorb ionized oxygen, in other words, their surface is more electrophilic than other samples. It exhibited a photocurrent initiation potential of 1.52Vvs. RHE and showed 8.67 mA-cm at a potential of 1.94V vs. RHE-2Photocurrent (example 1); RHE photocurrent initial potential was 1.55V vs. cm, and 5.21 mA-cm was shown at a potential of 1.94V vs. RHE-2Photocurrent (example 2); RHE photocurrent initial potential was 1.57V vs. cm, and 3.93mA cm was shown at a potential of 1.94V vs. RHE-2Photocurrent (example 3); RHE photocurrent initiation potential of 1.56V vs. cm, and showed 5.76 mA/cm at a potential of 1.94V vs. RHE-2The photocurrent of (c).
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (7)
1. A preparation method of a hematite photoanode is characterized by comprising the following steps:
mixing a trivalent ferric salt and a solvent to obtain a trivalent ferric salt solution, adding a strong base, and stirring to obtain a reaction solution;
carrying out solvothermal reaction on the reaction solution to obtain the hematite photoanode;
the solvent comprises water and an alcohol organic solvent;
no surfactant is used in the preparation process of the hematite photoanode;
the alcohol organic solvent comprises glycol and ethanol;
the volume ratio of the ethylene glycol to the ethanol is 6: (2-10);
the volume ratio of the water to the alcohol organic solvent is (4-12): (8-16);
the volume ratio of the molar weight of the trivalent ferric salt to the solvent is (0.5-1) mmol: 20 mL;
the molar ratio of the strong base to the ferric iron salt is (2-3): (0.5 to 1).
2. The method of claim 1, wherein the ferric salt is ferric nitrate, ferric trichloride, ferric acetate, or ferric sulfate;
the strong base is sodium hydroxide and/or potassium hydroxide.
3. The method according to claim 1, wherein the mixing is performed under stirring at a rotation speed of 100 to 3000rpm for 1 to 40 min.
4. The method according to claim 1, wherein the stirring is performed at a rotation speed of 100 to 3000rpm for 20 to 40 min.
5. The preparation method according to claim 1, wherein the temperature of the solvothermal reaction is 180 to 220 ℃ and the time is 6 to 10 hours.
6. The method according to claim 1 or 5, wherein the solvothermal reaction is completed, and further comprising centrifugation, washing and drying in this order.
7. The method of claim 6, wherein the drying is carried out at a temperature of 60 ℃ for a period of 12 hours.
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