CN116631780A - BiOCl-Bi 2 O 2 S in-situ heterojunction photoelectrode material and preparation method thereof - Google Patents
BiOCl-Bi 2 O 2 S in-situ heterojunction photoelectrode material and preparation method thereof Download PDFInfo
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- 238000011065 in-situ storage Methods 0.000 title claims abstract description 42
- 239000000463 material Substances 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 38
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000758 substrate Substances 0.000 claims abstract description 21
- 239000013078 crystal Substances 0.000 claims abstract description 12
- 238000004729 solvothermal method Methods 0.000 claims abstract description 9
- 239000002243 precursor Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 31
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 20
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 238000001354 calcination Methods 0.000 claims description 13
- 239000011780 sodium chloride Substances 0.000 claims description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims description 10
- 229910052717 sulfur Inorganic materials 0.000 claims description 10
- 239000011593 sulfur Substances 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 7
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 5
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 5
- 239000007864 aqueous solution Substances 0.000 claims description 4
- 238000010335 hydrothermal treatment Methods 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 3
- 238000009210 therapy by ultrasound Methods 0.000 claims description 3
- 239000004809 Teflon Substances 0.000 claims description 2
- 229920006362 Teflon® Polymers 0.000 claims description 2
- 239000003054 catalyst Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000000630 rising effect Effects 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims 2
- 238000005406 washing Methods 0.000 claims 2
- 230000035484 reaction time Effects 0.000 claims 1
- 230000006798 recombination Effects 0.000 abstract description 5
- 238000005215 recombination Methods 0.000 abstract description 5
- 230000005012 migration Effects 0.000 abstract description 4
- 238000013508 migration Methods 0.000 abstract description 4
- 239000002131 composite material Substances 0.000 abstract description 2
- 238000010276 construction Methods 0.000 abstract description 2
- 230000004298 light response Effects 0.000 abstract 1
- 230000004044 response Effects 0.000 description 8
- 230000031700 light absorption Effects 0.000 description 7
- 239000000969 carrier Substances 0.000 description 6
- 238000000926 separation method Methods 0.000 description 5
- 238000012512 characterization method Methods 0.000 description 3
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- 238000010586 diagram Methods 0.000 description 3
- 230000002708 enhancing effect Effects 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 230000009466 transformation Effects 0.000 description 2
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002135 nanosheet Substances 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 150000004763 sulfides Chemical class 0.000 description 1
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G9/00—Electrolytic capacitors, rectifiers, detectors, switching devices, light-sensitive or temperature-sensitive devices; Processes of their manufacture
- H01G9/20—Light-sensitive devices
- H01G9/2027—Light-sensitive devices comprising an oxide semiconductor electrode
- H01G9/2036—Light-sensitive devices comprising an oxide semiconductor electrode comprising mixed oxides, e.g. ZnO covered TiO2 particles
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/30—Hydrogen technology
- Y02E60/36—Hydrogen production from non-carbon containing sources, e.g. by water electrolysis
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Abstract
The invention discloses a BiOCl-Bi 2 O 2 An S in-situ heterojunction photoelectrode material and a preparation method thereof belong to the technical field of photoelectrochemistry. The invention comprises the following contents: first growing BiOCl crystal on FTO substrate based on solvothermal method, then preparing BiOCl-Bi based on in-situ conversion strategy by taking BiOCl grown on FTO substrate as precursor 2 O 2 S in-situ heterojunction photoelectrode material. The invention has the advantages that: construction of visible light response BiOCl-Bi based on in-situ conversion strategy 2 O 2 S heterojunction between BiOCl and Bi 2 O 2 And a heterojunction interface in close contact is formed between S, so that carrier interface migration is promoted, interface recombination is inhibited, and meanwhile, the stability of a composite material is enhanced, and the photoelectric performance is greatly improved.
Description
Technical Field
The invention discloses a BiOCl-Bi 2 O 2 An S in-situ heterojunction photoelectrode material and a preparation method thereof belong to the technical field of photoelectrochemistry.
Background
Photoelectrode materials are the core of photoelectrochemistry technology, and reasonable design and preparation of high-performance photoelectrodes are important to efficiently utilizing solar energy through photoelectrochemistry technology so as to relieve global energy crisis and environmental problems. In order to achieve excellent photoelectric conversion efficiency, researchers have developed a number of high-activity semiconductor photoelectrodes including metal oxides, sulfides, nitrides, and the like. Among them, biOCl is widely focused on due to the advantages of high light stability, low cost, environmental friendliness and the like, and is considered to have good application prospects. However, the problem of high photo-generated electron-hole pair recombination rate and narrow light absorption range of the BiOCl material leads to the fact that the photoelectric conversion efficiency of the BiOCl material still needs to be improved. At present, constructing a heterojunction is the most commonly used method for inhibiting photon-generated carrier recombination, and although certain progress is made, most of traditional heterojunction is based on random stacking of two semiconductor materials, energy barriers for preventing carrier interface migration exist between components, spatial separation of electrons and holes is not facilitated, and further enhancement of photoelectric performance is limited to a certain extent. It is still a challenge to promote the separation of the BiOCl carriers and expand the light absorption range of the BiOCl carriers, so as to greatly improve the photoelectric conversion efficiency of the BiOCl carriers.
Bi 2 O 2 S is a fine photosensitive material with narrow band gap (1.5 eV) and high carrier mobility. Meanwhile, similar to BiOCl, bi 2 O 2 S crystal is also composed of [ Bi ] 2 O 2 ] 2+ The layers and the halogen layers are alternately stacked, and the two crystals have similar layered structures. In view of this, the present invention assembles energy level matched Bi on BiOCl by in situ transformation strategy 2 O 2 S crystal promotes the separation and transmission of carriers with high efficiency, and simultaneously expands the light absorption range. Due to Bi 2 O 2 S crystal is formed by in-situ conversion by taking BiOCl as precursor, and BiOCl-Bi 2 O 2 And a heterojunction interface in close contact is formed between S, so that carrier interface migration is promoted, and material stability is enhanced. Thanks to such intimate interface contact, the BiOCl-Bi is driven by the staggered energy level structure 2 O 2 S in-situ heterojunction can realize efficient spatial separation of photogenerated carriers. In addition, due to Bi 2 O 2 S band gap is narrower, bi is assembled in situ 2 O 2 S can effectively expand the BiOCl light absorption rangeTo the visible region, thereby greatly enhancing its photoelectric properties.
Disclosure of Invention
In order to solve the technical problems existing at present, the invention provides a BiOCl-Bi 2 O 2 S in-situ heterojunction photoelectrode material and a preparation method thereof.
The above object of the present invention is achieved by the following means:
one of the technical proposal is as follows: biOCl-Bi 2 O 2 The preparation method of the S in-situ heterojunction photoelectrode material is characterized in that BiOCl crystals are firstly grown on an FTO substrate based on a solvothermal method, and then BiOCl-Bi is prepared based on an in-situ conversion strategy by taking BiOCl grown on the FTO substrate as a precursor 2 O 2 S in-situ heterojunction photoelectrode material. The scheme specifically comprises the following steps:
(1) Preparing BiOCl by a solvothermal method: and sequentially ultrasonically cleaning the FTO substrate by using acetone, absolute ethyl alcohol and deionized water. After drying, placing the FTO substrate conductive surface downward in a reaction kettle and adding a catalyst containing Bi (NO 3 ) 3 ·5H 2 O and NaCl, followed by solvothermal reaction to grow BiOCl crystals on the FTO substrate. After sample removal, the samples were rinsed three times with deionized water and dried in a vacuum oven at 60℃for 4-6. 6 h.
(2) Preparation of BiOCl-Bi by in situ conversion 2 O 2 S: placing the sample obtained in the step (1) in a reaction kettle, adding an aqueous solution with a sulfur source dissolved therein, and then performing hydrothermal treatment. After the reaction, the sample was rinsed three times with deionized water and dried in a vacuum oven at 60℃for 4-6. 6 h. Then, calcining the sample by utilizing a muffle furnace to obtain BiOCl-Bi 2 O 2 S in-situ heterojunction photoelectrode material.
The Bi (NO) -containing material of step (1) 3 ) 3 ·5H 2 The preparation method of the growth solution of O and NaCl comprises the following steps: weighing 0.4-2 g Bi (NO) 3 ) 3 ·5H 2 O is dissolved in 20-50 mL organic solvent to obtain solution A, wherein the organic solvent is selected from one of glycol and N, N-dimethylformamide. And weighing 0.05-0.8 g of NaCl and dissolving in 20-50 mL methanol to obtain solution B.Solution a and solution B were then mixed at room temperature and sonicated 1-2 h to give a growth solution.
The reaction kettle in the step (1) is provided with a Teflon lining, and the solvothermal reaction condition is that the reaction is carried out at 150-190 ℃ for 6-10 h.
The sulfur source in the step (2) is selected from one of sodium sulfide and thiourea; the preparation method of the aqueous solution with the dissolved sulfur source comprises the following steps: weighing 50-300-mg sulfur source, adding into 30-50-mL deionized water, and performing ultrasonic treatment until the sulfur source is completely dissolved.
The hydrothermal treatment condition in the step (2) is that the reaction is carried out for 0.5 to 1.5 hours at 180 to 200 ℃.
The calcination treatment conditions in the step (2) are as follows: the temperature is 300-450 ℃, the heat preservation time is 70-180 min, the temperature rising rate of the muffle furnace is 2-10 ℃/min, and the calcined sample is naturally cooled along with the furnace.
The second technical scheme is as follows: biOCl-Bi 2 O 2 S in-situ heterojunction photoelectrode material is characterized in that the material is obtained by any one of the preparation methods,
the invention has the beneficial effects that:
(1) Construction of BiOCl-Bi based on in situ transformation strategy 2 O 2 S heterojunction between BiOCl and Bi 2 O 2 And a heterojunction interface in close contact is formed between S, so that carrier interface migration is promoted, interface recombination is inhibited, and meanwhile, the stability of the composite material is enhanced.
(2) Bi with narrow band gap and high carrier mobility 2 O 2 S modifies BiOCl, can widen its light absorption range by a wide margin, strengthen the photocurrent response of visible light district, simultaneously, the energy level structure that both are crisscross can promote the space separation of photogenerated carrier by high efficiency to promote photoelectric performance by a wide margin.
(3) Constructed BiOCl-Bi 2 O 2 The S in-situ heterojunction photoelectrode is of a nano-sheet array structure (shown in figure 1), has abundant photoelectrochemical reaction active sites, and is beneficial to promoting carrier transmission and enhancing photoelectrode light absorption efficiency.
Drawings
FIG. 1 shows BiOCl-Bi obtained in example 1 2 O 2 SEM image of S in situ heterojunction.
Fig. 2 is an XRD pattern of the photoelectrode material obtained in example 1.
Fig. 3 is a photocurrent response diagram of the photoelectrode material obtained in example 1.
Fig. 4 is a photocurrent response diagram of the photoelectrode material obtained in example 2.
Fig. 5 is a photocurrent response diagram of the photoelectrode material obtained in example 3.
Detailed Description
For a better understanding of the present invention, the following examples are set forth to illustrate the present invention further, but are not to be construed as limiting the present invention.
Example 1
(1) Weighing 0.48 g Bi (NO) 3 ) 3 ·5H 2 O was dissolved in 20 mL glycol to give solution A. Another 0.056 g NaCl was weighed out and dissolved in 20 mL methanol to give solution B. Solution a and solution B were then mixed at room temperature and sonicated 1 h to give a growth solution. And then sequentially ultrasonically cleaning the FTO substrate by using acetone, absolute ethyl alcohol and deionized water. After drying, placing the FTO substrate conductive surface downwards in a reaction kettle and adding prepared Bi (NO) 3 ) 3 ·5H 2 O with NaCl followed by reaction at 180 ℃ 6 h to grow BiOCl crystals on FTO substrates. After sample removal, the samples were rinsed three times with deionized water and dried in a vacuum oven at 60 ℃ for 4 h.
(2) 60 mg sodium sulfide is weighed and added into 40 mL deionized water, and ultrasonic treatment is performed until the sodium sulfide is completely dissolved. The sample obtained in step (1) was placed in a reaction vessel and the above solution was added, followed by reaction 1 h at 200 ℃. After the reaction was completed, the samples were rinsed three times with deionized water and dried in a vacuum oven at 60 ℃ for 4 h. And then calcining the sample by using a muffle furnace, wherein the calcining temperature is 400 ℃, the calcining time is 2 h, and the heating rate of the muffle furnace is 5 ℃/min. Naturally cooling the calcined sample along with a furnace to obtain BiOCl-Bi 2 O 2 S in-situ heterojunction photoelectrode material.
(3) Taking a xenon lamp as a light source, carrying out photoelectric performance characterization on the obtained sample by means of an electrochemical workstation, and testing the sample to be set as follows: the lamp 20 was turned on s, the lamp 20 was turned off s, and the sample photocurrent response was recorded 3 cycles.
As shown in FIG. 3, biOCl-Bi is compared with pure BiOCl 2 O 2 S in situ heterojunction exhibits a stronger photocurrent response due to in situ assembly of Bi 2 O 2 S can effectively inhibit the recombination of carriers and expand the light absorption range, thereby greatly enhancing the photoelectrode performance of the photoelectrode.
Example 2
(1) 1.2 g Bi (NO) was weighed out 3 ) 3 ·5H 2 O was dissolved in 40 mL of N, N-dimethylformamide to give solution A. Another 0.15 g NaCl was weighed out and dissolved in 40 mL methanol to give solution B. Solution a and solution B were then mixed at room temperature and sonicated 1.5. 1.5 h to give a growth solution. And then sequentially ultrasonically cleaning the FTO substrate by using acetone, absolute ethyl alcohol and deionized water. After drying, placing the FTO substrate conductive surface downwards in a reaction kettle and adding prepared Bi (NO) 3 ) 3 ·5H 2 O with NaCl followed by reaction 8 h at 170 ℃ to grow BiOCl crystals on FTO substrates. After sample removal, the samples were rinsed three times with deionized water and dried in a vacuum oven at 60 ℃ for 4 h.
(2) 150 mg thiourea was weighed and added to 50 mL deionized water and sonicated until completely dissolved. The sample obtained in step (1) was placed in a reaction vessel and the above solution was added, followed by reaction at 190℃for 1.5. 1.5 h. After the reaction was completed, the samples were rinsed three times with deionized water and dried in a vacuum oven at 60 ℃ for 4 h. And then calcining the sample by using a muffle furnace, wherein the calcining temperature is 350 ℃, the calcining time is 2.5-h, and the heating rate of the muffle furnace is 5 ℃/min. Naturally cooling the calcined sample along with a furnace to obtain BiOCl-Bi 2 O 2 S in-situ heterojunction photoelectrode material.
(3) Taking a xenon lamp as a light source, carrying out photoelectric performance characterization on the obtained sample by means of an electrochemical workstation, and testing the sample to be set as follows: the lamp 20 was turned on s, the lamp 20 was turned off s, and the sample photocurrent response was recorded 3 cycles.
As shown in FIG. 4, bi is assembled in situ 2 O 2 After S, sample photocurrentThe density is obviously enhanced, indicating that BiOCl-Bi 2 O 2 The formation of S in-situ heterojunction can greatly improve photoelectric performance.
Example 3
(1) Weighing 0.5 g Bi (NO) 3 ) 3 ·5H 2 O was dissolved in 25 mL glycol to give solution A. Another 0.06 g NaCl was weighed out and dissolved in 25 mL methanol to give solution B. Solution a and solution B were then mixed at room temperature and sonicated 1.5. 1.5 h to give a growth solution. And then sequentially ultrasonically cleaning the FTO substrate by using acetone, absolute ethyl alcohol and deionized water. After drying, placing the FTO substrate conductive surface downwards in a reaction kettle and adding prepared Bi (NO) 3 ) 3 ·5H 2 O with NaCl followed by reaction at 190 ℃ 6 h to grow BiOCl crystals on FTO substrates. After sample removal, the samples were rinsed three times with deionized water and dried in a vacuum oven at 60 ℃ for 4 h.
(2) 100 mg sodium sulfide was weighed and added to 50 mL deionized water and sonicated until completely dissolved. The sample obtained in step (1) was placed in a reaction vessel and the above solution was added, followed by reaction at 200℃for 1.5. 1.5 h. After the reaction was completed, the samples were rinsed three times with deionized water and dried in a vacuum oven at 60 ℃ for 4 h. And then calcining the sample by using a muffle furnace, wherein the calcining temperature is 450 ℃, the calcining time is 1.5-h, and the heating rate of the muffle furnace is 5 ℃/min. Naturally cooling the calcined sample along with a furnace to obtain BiOCl-Bi 2 O 2 S in-situ heterojunction photoelectrode material.
(3) Taking a xenon lamp as a light source, carrying out photoelectric performance characterization on the obtained sample by means of an electrochemical workstation, and testing the sample to be set as follows: the lamp 20 was turned on s, the lamp 20 was turned off s, and the sample photocurrent response was recorded 3 cycles.
As shown in FIG. 5, bi is assembled in situ 2 O 2 After S, the photocurrent density of the sample is obviously enhanced, which shows that BiOCl-Bi 2 O 2 The formation of S in-situ heterojunction can greatly improve photoelectric performance.
Claims (8)
1. BiOCl-Bi 2 O 2 A preparation method of an S in-situ heterojunction photoelectrode material is characterized in that,first growing BiOCl crystal on FTO substrate based on solvothermal method, then preparing BiOCl-Bi based on in-situ conversion strategy by taking BiOCl grown on FTO substrate as precursor 2 O 2 S in-situ heterojunction photoelectrode material.
2. BiOCl-Bi according to claim 1 2 O 2 The preparation method of the S in-situ heterojunction photoelectrode material is characterized by comprising the following steps of:
(1) Preparing BiOCl by a solvothermal method: sequentially ultrasonically cleaning the FTO substrate by using acetone, absolute ethyl alcohol and deionized water; after drying, placing the FTO substrate conductive surface downward in a reaction kettle and adding a catalyst containing Bi (NO 3 ) 3 ·5H 2 O and NaCl growth solution, and then carrying out solvothermal reaction to grow BiOCl crystals on the FTO substrate; after the sample is taken out, washing three times by deionized water, and drying in a vacuum drying oven at 60 ℃ for 4-6 h;
(2) Preparation of BiOCl-Bi by in situ conversion 2 O 2 S: placing the sample obtained in the step (1) into a reaction kettle, adding an aqueous solution with a sulfur source dissolved therein, and then performing hydrothermal treatment; after the reaction is finished, washing the sample with deionized water for three times, and placing the sample in a vacuum drying oven at 60 ℃ for drying 4-6 h; then, calcining the sample by utilizing a muffle furnace to obtain BiOCl-Bi 2 O 2 S in-situ heterojunction photoelectrode material.
3. BiOCl-Bi according to claim 2 2 O 2 The preparation method of the S in-situ heterojunction photoelectrode material is characterized in that the Bi (NO) is contained in the step (1) 3 ) 3 ·5H 2 The preparation method of the growth solution of O and NaCl comprises the following steps: weighing 0.4-2 g Bi (NO) 3 ) 3 ·5H 2 O is dissolved in 20-50 mL organic solvent to obtain solution A, wherein the organic solvent is selected from one of glycol and N, N-dimethylformamide; weighing 0.05-0.8 g NaCl and dissolving in 20-50 mL methanol to obtain solution B; solution a and solution B were then mixed at room temperature and sonicated 1-2 h to give a growth solution.
4. BiOCl-Bi according to claim 2 2 O 2 S, preparing an in-situ heterojunction photoelectrode material, which is characterized in that the reaction kettle in the step (1) is provided with a Teflon lining; the solvothermal reaction condition is that the reaction is carried out at the temperature of 150-190 ℃ and the reaction time is 6-10 h.
5. BiOCl-Bi according to claim 2 2 O 2 S in-situ heterojunction photoelectrode material preparation method is characterized in that the sulfur source in the step (2) is selected from one of sodium sulfide and thiourea; the preparation method of the aqueous solution with the dissolved sulfur source comprises the following steps: weighing 50-300-mg sulfur source, adding into 30-50-mL deionized water, and performing ultrasonic treatment until the sulfur source is completely dissolved.
6. BiOCl-Bi according to claim 2 2 O 2 The preparation method of the S in-situ heterojunction photoelectrode material is characterized in that the hydrothermal treatment condition in the step (2) is that the reaction is carried out for 0.5 to 1.5 hours at 180 to 200 ℃.
7. BiOCl-Bi according to claim 2 2 O 2 The preparation method of the S in-situ heterojunction photoelectrode material is characterized in that the calcining treatment conditions in the step (2) are as follows: the temperature is 300-450 ℃, the heat preservation time is 70-180 min, the temperature rising rate of the muffle furnace is 2-10 ℃/min, and the calcined sample is naturally cooled along with the furnace.
8. BiOCl-Bi 2 O 2 An S in situ heterojunction photoelectrode material characterized in that it is obtained by the preparation method of any of the preceding claims 1 to 7.
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| CN116984001A (en) * | 2023-09-20 | 2023-11-03 | 中国市政工程西北设计研究院有限公司 | Full-spectrum-driven ranitidine degrading photocatalysis nano material and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN116984001A (en) * | 2023-09-20 | 2023-11-03 | 中国市政工程西北设计研究院有限公司 | Full-spectrum-driven ranitidine degrading photocatalysis nano material and preparation method thereof |
| CN116984001B (en) * | 2023-09-20 | 2024-02-09 | 中国市政工程西北设计研究院有限公司 | Full-spectrum-driven ranitidine degrading photocatalysis nano material and preparation method thereof |
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