CN114108022B - Heterojunction KNbO 3 /ZnFe 2 O 4 Preparation method and application of photoelectrode film - Google Patents
Heterojunction KNbO 3 /ZnFe 2 O 4 Preparation method and application of photoelectrode film Download PDFInfo
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Abstract
The invention discloses a heterojunction KNbO 3 /ZnFe 2 O 4 A preparation method and application of photoelectrode film. Placing the washed conductive glass (FTO) on KNbO 3 In the acetone solution of (2), KNbO is obtained by adopting an electrophoretic deposition method 3 A film. Then ZnFe is added 2 O 4 Putting into acetone solution, ultrasonic dispersing, and collecting KNbO 3 The film is placed in ZnFe 2 O 4 In the acetone solution of (2) in KNbO by adopting an electrophoretic deposition method 3 A layer of ZnFe is overlapped on the film 2 O 4 A film; annealing the obtained product at high temperature to obtain KNbO 3 /ZnFe 2 O 4 A heterojunction thin film. KNbO prepared by the invention 3 /ZnFe 2 O 4 Photoelectrode thin film for improving KNbO 3 The photogenerated electron transport capability of the photoelectrode,further can effectively improve the photoelectrochemical property and strengthen KNbO 3 Is resistant to photo-etching.
Description
Technical Field
The invention belongs to the technical field of photoelectrochemistry, and in particular relates to a high-performance heterojunction KNbO 3 /ZnFe 2 O 4 A preparation method and application of photoelectrode film.
Background
In environmental pollution control, there is a dramatic interaction between energy crisis and environmental pollution, as pollution control generally requires a significant amount of energy consumption. Energy crisis and environmental pollution have become global problems. To address the energy crisis and environmental pollution, it is necessary to combine the use of clean and sustainable energy, such as solar energy with hydrogen or electrical energy in pollution control. Hydrogen molecules have a high gravimetric energy density compared to other fuels, and water is the only combustion product and is therefore considered a promising alternative to future energy supplies. Currently, H 2 The large scale production of (c) relies primarily on steam methane reforming and coal gasification rather than electrolysis of water. Despite the strategic advantages of electrolysis of water to produce hydrogen, one of the major obstacles to large-scale electrochemical cleavage of water is the lack of efficient and stable Hydrogen Evolution Reaction (HER) catalysts. Platinum (Pt) is the most active and durable HER catalyst, however, its widespread use is greatly hampered by the high cost and scarcity. Therefore, development of a noble metal-free photocatalyst is imperative.
KNbO 3 Is an n-type visible light driven semiconductor, has a band gap of about 3.3eV, and accords with the characteristics of hydrogen generating energy band structure and the like. Currently, with respect to KNbO 3 There are few reports of applications in PEC.
Disclosure of Invention
The invention aims to provide a high-performance heterojunction material KNbO 3 /ZnFe 2 O 4 The preparation method and application of the photoelectrode film have the advantages of simple and convenient preparation method, low cost and mild conditionAnd the experimental conditions are easy to control.
In order to achieve the above purpose, the invention adopts the following technical scheme: heterojunction KNbO 3 /ZnFe 2 O 4 The preparation method of the photoelectrode film comprises the following steps:
1) To KNbO 3 Adding the powder into acetone solution, and adding I 2 Obtaining KNbO through ultrasonic dispersion 3 Depositing the suspension, and preparing KNbO by adopting an electrophoretic deposition method 3 A film;
2) ZnFe (ZnFe) 2 O 4 Adding the powder into acetone solution, and adding I 2 Ultrasonic dispersing to obtain ZnFe 2 O 4 Depositing a suspension, and adding KNbO obtained in the step 1) 3 The film is placed in ZnFe 2 O 4 In the deposition suspension, the electrophoretic deposition method is adopted to deposit on KNbO 3 A layer of ZnFe is overlapped on the film 2 O 4 A film;
3) Calcining the product obtained in the step 2) at high temperature under the condition of inert gas or air to obtain heterojunction KNbO 3 /ZnFe 2 O 4 A photoelectrode thin film.
Further, according to the preparation method, the KNbO 3 The preparation method of the powder comprises the following steps: proper amount of potassium salt and Nb 2 O 5 Mixing the materials in deionized water, and magnetically stirring the materials for 0.5 to 2 hours; transferring the obtained mixed solution into a high-pressure hydrothermal kettle, and carrying out hydrothermal reaction for 8-14h at 140-180 ℃; washing the obtained product with deionized water and ethanol, oven drying at 60-90deg.C, and annealing at 500-700deg.C for 1-3 hr to obtain KNbO 3 And (3) powder.
Further, in the above preparation method, the potassium salt is potassium hydroxide, potassium carbonate, potassium nitrate, or potassium sulfate.
Further, according to the preparation method, the ZnFe 2 O 4 The preparation method of the powder comprises the following steps: adding zinc salt and ferric salt into glycol, mixing, adding citric acid aqueous solution, magnetically stirring, stirring in water bath at 50-70deg.C for 0.5-1 hr, oven drying at 110-150deg.C, and annealing at 400-600deg.C for 1-3 hr to obtain ZnFe 2 O 4 And (3) powder.
Further, in the preparation method, the zinc salt is zinc nitrate, zinc acetate or zinc chloride; the ferric salt is ferric nitrate, ferric sulfate or ferric chloride.
Further, the preparation method, step 1) specifically comprises the following steps: to KNbO 3 Adding the powder into acetone solution, ultrasonic dispersing, adding I 2 Continuing ultrasonic dispersion to obtain KNbO 3 Depositing a suspension; to KNbO 3 Inserting two pieces of cleaned equal-area conductive glass FTO into the deposition suspension, and immersing the conductive surfaces of the two pieces of conductive glass FTO in KNbO in parallel with each other 3 Depositing the suspension under 15-25V DC voltage for 1-7min to obtain KNbO 3 A film.
Further, the preparation method, step 2) specifically comprises the following steps: znFe (ZnFe) 2 O 4 Adding the powder into acetone solution, ultrasonic dispersing, adding I 2 Continuously performing ultrasonic dispersion to obtain ZnFe 2 O 4 Depositing a suspension; to ZnFe 2 O 4 Depositing the suspension, wherein the KNbO is covered by the suspension obtained in the step 1) 3 The conductive glass FTO of the film and a conductive glass FTO with the same area are opposite to each other, and the conductive surfaces of the two conductive glass FTOs are immersed in ZnFe in parallel 2 O 4 Depositing the suspension under 15-25V DC voltage for 1-7min to obtain KNbO 3 A layer of ZnFe is overlapped on the film 2 O 4 A film.
Further, in the above preparation method, 0.012g of I was added to 25mL of acetone solution 2 。
Further, in the above preparation method, in step 3), the high temperature calcination is calcination at 300-500 ℃ for 1-3 hours.
Heterojunction KNbO provided by the invention 3 /ZnFe 2 O 4 The photoelectrode film is used as a photocathode semiconductor material in the hydrogen production by photodecomposition of water.
The beneficial effects of the invention are as follows:
1. KNbO prepared by the invention 3 /ZnFe 2 O 4 The photoelectrode film has a heterojunction structure, so that the photoelectrode is easier to generateThe positive holes are effectively separated, the recombination rate is reduced, and the photoelectrochemical property can be effectively improved.
2. The invention prepares KNbO 3 /ZnFe 2 O 4 The photoelectrode film, as a cathode material, can effectively improve the transmission efficiency of carriers and the collection efficiency of the conductive substrate to electrons, and can obtain high PEC performance.
3. The preparation method provided by the invention has the advantages of low raw material cost, simplicity in operation, great reduction in cost, no pollution to the environment and realization of green chemistry.
Drawings
FIG. 1 is KNbO 3 Powder, znFe 2 O 4 Powder and KNbO 3 /ZnFe 2 O 4 XRD contrast pattern of photoelectrode thin film.
FIG. 2 is KNbO 3 /ZnFe 2 O 4 Photoelectrode thin film and KNbO 3 Photo current contrast plot of the film.
FIG. 3 is KNbO 3 /ZnFe 2 O 4 Photoelectrode thin film and KNbO 3 Comparison of impedance spectra of films.
Detailed Description
Example 1 heterojunction KNbO 3 /ZnFe 2 O 4 Preparation method of photoelectrode film
The preparation method (one) is as follows
1) Preparation of KNbO by hydrothermal method 3 Powder
18.845g KOH and 1.785g Nb 2 O 5 Adding the solution into 10mL of deionized water, magnetically stirring for 0.5h, transferring the solution into a high-pressure hydrothermal kettle, and carrying out hydrothermal reaction for 10h at 160 ℃; the obtained product is respectively washed by centrifugation with deionized water and ethanol for three times, the obtained precipitate is dried for 12 hours at 80 ℃, and the obtained powder is calcined for 2 hours at 600 ℃ in the air to obtain KNbO 3 And (3) powder.
2) ZnFe prepared by sol-gel method 2 O 4 Powder
6.3g of citric acid is dissolved in 13mL of deionized water and magnetically stirred for 10min to obtain an aqueous solution of citric acid. 2.975g Zn (NO) 3 ) 2 And 8.08g Fe (NO) 3 ) 3 Adding 13mL of ethylene glycol, magnetically stirring for 10min, adding citric acid aqueous solution, magnetically stirring in water bath at 60deg.C for 1h, oven drying the obtained product at 130deg.C, and calcining at 400 deg.C for 2h to obtain ZnFe 2 O 4 And (3) powder.
3) Preparation of KNbO 3 Film and method for producing the same
0.06g KNbO 3 Adding the powder into 25mL acetone solution, ultrasonic dispersing for 0.5h, adding 0.012 and 0.012g I 2 Continuing ultrasonic dispersion for 0.5h to obtain KNbO 3 The suspension is deposited. Preparing two pieces of cleaned conductive glass FTO with equal area, and immersing the conductive surfaces of the two pieces of conductive glass FTO in parallel into KNbO 3 Depositing for 5min under the condition of 25V direct current voltage in the deposition suspension to obtain KNbO 3 A film.
4)KNbO 3 /ZnFe 2 O 4 Preparation of films
0.06g of ZnFe 2 O 4 Adding the powder into 25mL acetone solution, ultrasonic dispersing for 0.5h, adding 0.012 and 0.012g I 2 Continuing ultrasonic dispersion for 0.5h to obtain ZnFe 2 O 4 The suspension is deposited. To ZnFe 2 O 4 Depositing the suspension, wherein the KNbO is covered in the step 3) 3 The conductive glass FTO of the film and a conductive glass FTO with the same area are opposite to each other, and the conductive surfaces of the two conductive glass FTOs are immersed in ZnFe in parallel 2 O 4 Depositing the suspension under 25V DC voltage for 7min and KNbO 3 A layer of ZnFe is overlapped on the film 2 O 4 A film.
5) Annealing the product obtained in the step 4) at a high temperature of 400 ℃ for 2 hours to obtain heterojunction KNbO 3 /ZnFe 2 O 4 A photoelectrode thin film.
(II) detection
FIG. 1 is KNbO 3 Powder, znFe 2 O 4 Powder and KNbO 3 /ZnFe 2 O 4 XRD contrast pattern of photoelectrode thin film. As can be seen from FIG. 1, KNbO 3 Eight distinct diffraction peaks at 22.1 °, 31.5 °, 45.1 °, 50.8 °, 56.1 °, 65.8 °, 70.2 °, 74.7 ° were KNbO 3 Characteristic peaks of (4) pure KNbO 3 The diffraction peak of the sample is completely consistent with the peak spectrum of the potassium niobate standard card, which shows that KNbO is prepared 3 A material. ZnFe (ZnFe) 2 O 4 Ten obvious diffraction peaks at 18.1 degrees, 29.9 degrees, 35.2 degrees, 36.8 degrees, 42.8 degrees, 53 degrees, 56.5 degrees, 62.1 degrees, 70.4 degrees and 73.4 degrees are ZnFe 2 O 4 Characteristic peak of (4) pure ZnFe 2 O 4 The diffraction peak of the sample is completely consistent with the peak spectrum of the zinc ferrite standard card, which shows that ZnFe is prepared 2 O 4 A material. As can be seen from FIG. 1, KNbO 3 /ZnFe 2 O 4 With KNbO 3 And ZnFe 2 O 4 The diffraction peaks of (2) are almost identical and correspond to KNbO respectively 3 And ZnFe 2 O 4 Is a diffraction peak of (2). Indicating that KNbO is successfully prepared 3 /ZnFe 2 O 4 A photoelectrode thin film.
Example 2 heterojunction KNbO 3 /ZnFe 2 O 4 Application of photoelectrode film
The pure KNbO of example 1 was used separately 3 Film and KNbO 3 /ZnFe 2 O 4 Photoelectrode thin films are tested for photoelectrochemical properties such as photocurrent and impedance.
All electrochemical experimental testing procedures were performed in the electrochemical workstation (Princeton Applied Research 2273) of the three-electrode system. The sample film is used as a working electrode, the platinum sheet is used as a counter electrode, ag/AgCl is used as a reference electrode, the electrolyte is 1M NaOH, and the light irradiation area of the sample is 1cm 2 。
Photocurrent testing: the light source is a 300W xenon lamp, the bias voltage is 1.23Vvs. VRHE, the measured result is shown in figure 2, and the result shows that the heterojunction KNbO 3 /ZnFe 2 O 4 The photocurrent of the photoelectrode film is about 5 mu A, KNbO 3 The photocurrent of the photoelectrode thin film was about 0.6 μA, and the result showed that heterojunction KNbO 3 /ZnFe 2 O 4 Photocurrent ratio KNbO of photoelectrode thin film 3 The large photoelectrode film indicates that the load is ZnFe 2 O 4 Improved post photoelectrochemical properties and KNbO 3 /ZnFe 2 O 4 The binding efficiency of heterojunction electron-hole pairs increases.
Electrochemical Impedance Spectroscopy (EIS)And (3) testing: the fixed voltage is 0Vvs. Voc, and the frequency range is 0.1-10 5 Hz. The results are shown in fig. 3, which shows that a larger radius of semicircle means a larger composite resistance. Thus, heterojunction KNbO 3 /ZnFe 2 O 4 The minimum radius of the capacitive arc of the photoelectrode film indicates heterojunction KNbO 3 /ZnFe 2 O 4 The charge transfer resistance of the photoelectrode film is smaller than KNbO 3 A film. The impedance is relatively small and the photocurrent is maximal, consistent with fig. 2.
In summary, from fig. 2 and 3, heterojunction KNbO can be observed 3 /ZnFe 2 O 4 Photoelectrochemical property ratio KNbO of film 3 The photoelectrochemical property of the film is more stable.
Claims (10)
1. Heterojunction KNbO 3 /ZnFe 2 O 4 The preparation method of the photoelectrode film is characterized by comprising the following steps:
1) To KNbO 3 Adding the powder into acetone solution, and adding I 2 Obtaining KNbO through ultrasonic dispersion 3 Depositing the suspension, and preparing KNbO by adopting an electrophoretic deposition method 3 A film;
2) ZnFe (ZnFe) 2 O 4 Adding the powder into acetone solution, and adding I 2 Obtaining ZnFe through ultrasonic dispersion 2 O 4 Depositing a suspension, and adding KNbO obtained in the step 1) 3 The film is placed in ZnFe 2 O 4 In the deposition suspension, the electrophoretic deposition method is adopted to deposit on KNbO 3 A layer of ZnFe is overlapped on the film 2 O 4 A film;
3) Calcining the product obtained in the step 2) at high temperature under the condition of inert gas or air to obtain heterojunction KNbO 3 /ZnFe 2 O 4 A photoelectrode thin film.
2. The method of manufacture according to claim 1, wherein the KNbO 3 The preparation method of the powder comprises the following steps: proper amount of potassium salt and Nb 2 O 5 Mixing the materials in deionized water, and magnetically stirring the materials for 0.5 to 2 hours; dissolving the obtained mixtureTransferring the liquid into a high-pressure hydrothermal kettle, and carrying out hydrothermal reaction for 8-14h at 140-180 ℃; washing the obtained product with deionized water and ethanol, oven drying at 60-90deg.C, and annealing at 500-700deg.C for 1-3 hr to obtain KNbO 3 And (3) powder.
3. The method of claim 2, wherein the potassium salt is potassium hydroxide, potassium carbonate, potassium nitrate, or potassium sulfate.
4. The method of claim 1, wherein the ZnFe is 2 O 4 The preparation method of the powder comprises the following steps: adding zinc salt and ferric salt into glycol, mixing, adding citric acid aqueous solution, magnetically stirring, stirring in water bath at 50-70deg.C for 0.5-1 hr, oven drying at 110-150deg.C, and annealing at 400-600deg.C for 1-3 hr to obtain ZnFe 2 O 4 And (3) powder.
5. The method of claim 4, wherein the zinc salt is zinc nitrate, zinc acetate, or zinc chloride; the ferric salt is ferric nitrate, ferric sulfate or ferric chloride.
6. The preparation method according to claim 1, wherein the step 1) specifically comprises: to KNbO 3 Adding the powder into acetone solution, ultrasonic dispersing, adding I 2 Continuing ultrasonic dispersion to obtain KNbO 3 Depositing a suspension; to KNbO 3 Inserting two pieces of clean conductive glass FTO with equal area into the deposition suspension, and immersing the conductive surfaces of the two pieces of conductive glass FTO in KNbO in parallel with each other 3 Depositing the suspension under 15-25V DC voltage for 1-7min to obtain KNbO 3 A film.
7. The method according to claim 6, wherein step 2) comprises: znFe (ZnFe) 2 O 4 Adding the powder into acetone solution, ultrasonic dispersing, adding I 2 Continuously performing ultrasonic dispersion to obtain ZnFe 2 O 4 Deposition suspensionA liquid; to ZnFe 2 O 4 Depositing the suspension, wherein the KNbO is covered by the suspension obtained in the step 1) 3 The conductive glass FTO of the film and a conductive glass FTO with the same area are opposite to each other, and the conductive surfaces of the two conductive glass FTOs are immersed in ZnFe in parallel 2 O 4 Depositing the suspension under 15-25V DC voltage for 1-7min to obtain KNbO 3 A layer of ZnFe is overlapped on the film 2 O 4 A film.
8. The process according to claim 6 or 7, wherein 0.012g of I is added to 25mL of the acetone solution 2 。
9. The method according to claim 1, wherein in step 3), the high-temperature calcination is calcination at a temperature of 300 to 500 ℃ for 1 to 3 hours.
10. Heterojunction KNbO prepared according to the method of any one of claims 1 to 9 3 /ZnFe 2 O 4 The photoelectrode film is used as a photocathode semiconductor material in the hydrogen production by photodecomposition of water.
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