CN116273133A - Double Z type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, and preparation and application thereof - Google Patents
Double Z type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, and preparation and application thereof Download PDFInfo
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Abstract
The invention relates to a double Z type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, preparation and application thereof, bi 3 O 4 Cl and Cd 0.5 Zn 0.5 S is added to g-C 3 N 4 And ultrasonic for 2 hours, then stirring the obtained mixed suspension for 12 hours, washing with deionized water, drying and grinding. The invention synthesizes and obtains the double Z-type heterojunction g-C through a simple method 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S photocatalyst, CO 2 Photocatalytic reduction to CO and CH 4 By g-C 3 N 4 The nano-sheet is supported to form a stable double-Z-shaped heterostructure, so that separation and transfer of photo-generated electron hole pairs are promoted. The photocatalyst has the characteristics of high specific surface area, wide visible light response range and effective separation of photo-generated electron hole pairs, thereby improving the catalytic activity of the photocatalyst.
Description
Technical Field
The invention relates to the field of photocatalysts, in particular to a double Z-type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, and preparation and application thereof.
Background
High-volume combustion of fossil fuels and excess CO 2 Emissions pose a serious threat to the environment. Furthermore, since fossil fuels are not renewable, renewable energy sources are needed to meet the needs of human life and production. The environmental problems and energy crisis can be relieved simultaneously by converting carbon dioxide into hydrocarbon fuel through a green photocatalysis technology. Therefore, photocatalytic reduction of carbon dioxide is receiving great attention for its effectiveness, economy and environmental friendliness. Photocatalysts, such as metal oxides, metal sulfides and metal phosphides, have been studied and developed for photocatalytic reduction of carbon dioxide as one of the most critical problems in photocatalysis. However, most of them have limited application in photocatalysis due to low solar energy utilization efficiency and rapid recombination of photo-generated charges.
In the photocatalysts studied, g-C 3 N 4 As a nonmetallic material, attention is paid to its narrow band gap, excellent stability and low toxicity. However, pure g-C 3 N 4 The low solar efficiency and the rapid recombination of photo-induced charges limit the practical application of the solar energy in the field of photo-catalytic reduction of carbon dioxide. Thus, various methods have been explored to promote pure g-C 3 N 4 The photocatalytic activity of the catalyst comprises element doping, metal nanoparticle decoration, morphology control, heterostructure construction and the like. Notably, it is noted thatIs obtained by mixing g-C 3 N 4 And the Z-shaped heterojunction is constructed by coupling with an auxiliary semiconductor, and the photo-generated electron-hole pairs can be effectively separated and transferred, so that the photocatalysis performance of g-C3N4 is promoted.
Recently, g-C 3 N 4 Base double Z-type heterojunction for high-efficiency CO 2 The report of the photocatalytic conversion is very few, and the catalytic effect is not satisfactory. Thus, a double Z-type g-C was constructed 3 N 4 The base heterojunction is a lifting CO 2 Potential strategies for reducing activity.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a double Z-type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, and preparation and application thereof. The double Z-type g-C is synthesized by a simple method 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, CO 2 Photocatalytic reduction to CO and CH 4 By g-C 3 N 4 The nano-sheet is supported to form a stable double-Z-shaped heterostructure, so that separation and transfer of photo-generated electron hole pairs are promoted. The photocatalyst has the characteristics of high specific surface area, wide visible light response range and effective separation of photo-generated electron hole pairs, thereby improving the catalytic activity of the photocatalyst and reducing g-C 3 N 4 Recombination and exposure of photogenerated electron-hole pairs of catalyst g-C 3 N 4 The catalyst has more active sites.
The aim of the invention can be achieved by the following technical scheme:
double Z type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, composed of g-C 3 N 4 、Bi 3 O 4 Cl and Cd 0.5 Zn 0.5 S composition, wherein g-C 3 N 4 Is taken as a matrix and g-C is calculated according to the mass ratio 3 N 4 ：Bi 3 O 4 Cl：Cd 0.5 Zn 0.5 S＝1：0.005～0.015：0.01～0.03，
The g-C 3 N 4 Is of a layered structure, the Bi 3 O 4 Cl is of a sheet structure, and Bi is in a sheet shape 3 O 4 Cl intercalated layered g-C 3 N 4 In the matrix, the Cd 0.5 Zn 0.5 S is nanocrystalline, cd 0.5 Zn 0.5 S is attached to lamellar g-C 3 N 4 Is provided.
Further, the g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, g-C according to mass ratio 3 N 4 ：Bi 3 O 4 Cl：Cd 0.5 Zn 0.5 S＝1：0.01：0.02。
The invention also provides a double Z-type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst comprises the following specific steps:
s1, preparation of g-C 3 N 4 A base;
s2, preparing Bi 3 O 4 Cl: bi (NO) 3 ) 3 ·5H 2 O is dissolved in glycol and NH is added 4 Cl, obtaining Bi after hydrothermal reaction 3 O 4 Cl；
S3, preparing Cd 0. 5Zn 0.5 S: cd (OAc) 2 ·2H 2 O and Zn (OAc) 2 ·2H 2 O is mixed and dissolved in deionized water, and Na is added 2 S·9H 2 After O solution, cd is obtained 0.5 Zn 0.5 S；
S4, preparation of g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S: the g-C obtained in the step S1 3 N 4 Dissolving the matrix in deionized water to obtain g-C 3 N 4 Suspending liquid, bi obtained in step S2 is mixed with 3 O 4 Cl and Cd obtained in step S3 0.5 Zn 0.5 S is added to g-C 3 N 4 In suspension, a double Z-type g-C is obtained 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst.
Further, in step S1, urea is calcined to obtain g-C 3 N 4 。
The calcination temperature is 500-600deg.C, preferably 550deg.C, the calcination time is 3-6 h, preferably 4h, and the temperature rising rate is 4deg.C/min.
Further, in step S2, bi (NO 3 ) 3 ·5H 2 O: ethylene glycol=0.03 to 0.06g:1ml.
Further on, bi (NO 3 ) 3 ·5H 2 O: ethylene glycol = 0.0458g:1ml.
Further, in step S2, the hydrothermal reaction temperature is 140-180 ℃, preferably 160 ℃, and the hydrothermal reaction time is 10-14 hours, preferably 12 hours.
Further, in step S2, bi (NO 3 ) 3 ·5H 2 O is dissolved in glycol, mixed solution A is obtained after ultrasonic treatment, NH is obtained 4 Cl is dissolved in deionized water, mixed solution B is obtained after stirring,
mixing the mixed solution A and the mixed solution B, transferring into a polytetrafluoroethylene stainless steel autoclave, performing hydrothermal reaction, cooling to room temperature, centrifugally collecting the obtained powder, washing, and drying to obtain Bi 3 O 4 Cl。
Above, further, NH 4 Cl: deionized water = 0.005-0.01 g:1ml.
Above, further, NH 4 Cl: deionized water = 0.0072g:1ml.
The above further, the ultrasonic time is 5 to 20 minutes, preferably 10 minutes.
The stirring time is 5 to 20 minutes, preferably 10 minutes.
The washing mode is that deionized water is used for washing 3 times.
The drying is vacuum drying, the drying temperature is 60 ℃, and the drying time is 12-24 hours.
Further, in step S3, cd (OAc) 2 ·2H 2 O：Zn(OAc) 2 ·2H 2 O：Na 2 S·9H 2 O solution: deionized water = 0.01-0.02 g: 0.008-0.018 g: 0.4-0.8 ml:1ml.
Further on, cd (OAc) 2 ·2H 2 O：Zn(OAc) 2 ·2H 2 O：Na 2 S·9H 2 O solution: deionized water = 0.01599g:0.01317g:0.6ml:1ml.
Further, in step S3, the Na 2 S·9H 2 The concentration of the O solution is 0.1-0.5 mol/L.
Above, further, the Na 2 S·9H 2 The concentration of the O solution is 0.3mol/L.
Further, in step S3, cd (OAc) 2 ·2H 2 O and Zn (OAc) 2 ·2H 2 O is mixed and dissolved in deionized water, and Na is added after magnetic stirring 2 S·9H 2 O solution, magnetic stirring, centrifuging, washing and drying to obtain Cd 0.5 Zn 0.5 S。
Further, the time of the two magnetic stirring is 12-24 hours, preferably 24 hours.
The washing mode is that deionized water is used for washing 3 times.
The drying is vacuum drying, the drying temperature is 60 ℃, and the drying time is 12-24 hours.
Further, in step S4, the g-C obtained in step S1 is subjected to 3 N 4 Dissolving the matrix in deionized water to obtain g-C 3 N 4 Suspending liquid, bi obtained in step S2 is mixed with 3 O 4 Cl and Cd obtained in step S3 0.5 Zn 0.5 S is added to g-C 3 N 4 In the suspension, after ultrasonic treatment and stirring, washing and drying, the double Z-type g-C3N4/Bi is obtained 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst.
Further, the stirring time is 12-24 hours, preferably 12 hours.
The washing mode is that deionized water is used for washing 3 times.
The drying is vacuum drying, the drying temperature is 60 ℃, and the drying time is 12-24 hours.
In addition, the invention also provides a double Z-shaped g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 Application of S heterojunction photocatalyst, g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The application of the S heterojunction photocatalyst in preparing carbon monoxide and methane by reducing carbon dioxide through photocatalysis.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention prepares and controls the synthesis of double Z-type g-C by a simple method 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, CO 2 Photocatalytic reduction to CO and CH 4 By g-C 3 N 4 The nanosheets are supported to form a stable double Z-shaped heterostructure, so that separation and transfer of photo-generated electron hole pairs are promoted;
2.g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 the S heterojunction photocatalyst has the characteristics of high specific surface area, wide visible light response range and effective separation of photo-generated electron hole pairs, thereby improving the catalytic activity of the photocatalyst and reducing g-C 3 N 4 Recombination and exposure of photogenerated electron-hole pairs of catalyst g-C 3 N 4 More active sites of the catalyst;
3. double Z-type heterojunction can provide shorter carrier transmission path and Cd 0.5 Zn 0.5 The S nano particles can provide more active sites, the synergistic effect among the three components can effectively promote the light absorption of the composite material in the near infrared region, and the double Z type g-C can be used for preparing the composite material 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst integrates g-C 3 N 4 、Bi 3 O 4 Cl、Cd 0.5 Zn 0.5 S has the advantages of effective light utilization rate, higher separation rate of photo-generated electron hole pairs, greatly inhibits the recombination of the photo-generated electron hole pairs, and can be effectiveCO reduction of (c) 2 ；
4. Double Z type g-C prepared by the application 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst is composed of water and CO only 2 And CO can be efficiently processed under the condition of visible light 2 Reduction to CO and CH 4 ；
5. Double Z type g-C prepared by the application 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The CO and formation rate of the S heterojunction photocatalyst is about 21.92 mu mol g -1 And 152.01 mu mol g -1 The yield of the product is greatly improved compared with the traditional heterojunction.
Drawings
FIG. 1 is an SEM image of a catalyst prepared according to example 1 of the present application;
FIG. 2 is a HRTEM chart of the catalyst prepared in example 1 of the present application;
FIG. 3 is an XRD pattern of the catalysts prepared in examples 1-3 and of the catalysts of comparative examples 1-5 herein;
FIG. 4 is a photoluminescence spectrum of the catalysts prepared in examples 1-3 and the catalysts of comparative examples 1-5 of the present application;
FIG. 5 is a graph of transient photocurrent response spectra of the catalysts prepared in examples 1-3 of the present application and the catalysts of comparative examples 1-5;
FIG. 6 is a graph of CO and CH for the catalysts prepared in examples 1-4 and comparative examples 3-5 of the present application 4 Yield versus time.
FIG. 7 is a CO of the catalyst prepared in example 1 of the present application 2 Reduction cycle test;
FIG. 8 is a double Z-type g-C prepared in example 1 of the present application 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 And (3) an energy band structure, an electron transfer model and a mechanism schematic diagram of the S heterojunction photocatalyst.
Detailed Description
In order to make the above objects, features and advantages of the present application more comprehensible, embodiments accompanied with figures are described in detail below.
In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present application, but the present application may be practiced in other ways other than those described herein, and persons skilled in the art will readily appreciate that the present application is not limited to the specific embodiments disclosed below.
Next, the present application will be described in detail with reference to the schematic drawings, wherein the cross-sectional views of the device structure are not to scale for the sake of illustration, and the schematic drawings are merely examples, which should not limit the scope of protection of the present application. In addition, the three-dimensional dimensions of length, width and depth should be included in actual fabrication.
Further still, reference herein to "one embodiment" or "an embodiment" means that a particular feature, structure, or characteristic may be included in at least one implementation of the present application. The appearances of the phrase "in one embodiment" in various places in the specification are not necessarily all referring to the same embodiment, nor are separate or alternative embodiments mutually exclusive of other embodiments.
Example 1
Double Z type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst comprises the following specific steps:
s1, calcining a certain amount of urea for 4 hours at 550 ℃, wherein the heating rate is 4 ℃/min, and obtaining g-C 3 N 4 。
S2.0.458g of Bi (NO 3 ) 3 ·5H 2 O was added to 10ml of ethylene glycol and sonicated for 10min to give solution A, after which 0.018g of NH was added 4 Dissolving Cl in 25ml deionized water, stirring for 10min to obtain solution B, mixing the solution A and the solution B, transferring into a polytetrafluoroethylene lining autoclave, reacting at 160 ℃ for 12h, centrifuging, washing with deionized water for 3 times, and vacuum drying the washed product at 60 ℃ for 12-24h to obtain Bi 3 O 4 Cl。
S3.0.7995g Cd (OAc) 2 ·2H 2 O and 0.6585g of Zn (OAc) 2 ·2H 2 O was mixed and dissolved in 50ml of deionized water, magnetically stirred for 3 hours, then 30ml of Na was added 2 S·9H 2 Dripping O (0.3 mol/L) solution into the mixed solution, magnetically stirring for 24h, centrifuging, washing with deionized water for 3 times, and vacuum drying the washed product at 60deg.C for 12-24h to obtain Cd 0. 5Zn 0.5 S。
S4, obtaining 1g of g-C in the step S1 3 N 4 Dissolving the matrix in deionized water to obtain g-C 3 N 4 Suspension, 0.01g of Bi 3 O 4 Cl and 0.02g Cd 0.5 Zn 0.5 S is added to g-C 3 N 4 And ultrasonic treating in suspension for 2 hr, stirring the mixed suspension for 12 hr, centrifuging, washing with deionized water for 3 times, and vacuum drying at 60deg.C for 12-24 hr to obtain g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S。
Example 2
Double Z type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst comprises the following specific steps:
s1, calcining a certain amount of urea for 4 hours at 550 ℃, wherein the heating rate is 4 ℃/min, and obtaining g-C 3 N 4 。
S2.0.458g of Bi (NO 3 ) 3 ·5H 2 O was added to 10ml of ethylene glycol and sonicated for 10min to give solution A, after which 0.018g of NH was added 4 Dissolving Cl in 25ml deionized water, stirring for 10min to obtain solution B, mixing the solution A and the solution B, transferring into a polytetrafluoroethylene lining autoclave, reacting at 160 ℃ for 12h, centrifuging, washing with deionized water for 3 times, and vacuum drying the washed product at 60 ℃ for 12-24h to obtain Bi 3 O 4 Cl。
S3.0.7995g Cd (OAc) 2 ·2H 2 O and 0.6585g of Zn (OAc) 2 ·2H 2 O was mixed and dissolved in 50ml of deionized water, magnetically stirred for 3 hours, then 30ml of Na was added 2 S·9H 2 Dripping O (0.3 mol/L) solution into the mixed solution, magnetically stirring for 24 hr, centrifuging, and removingWashing with son water for 3 times, and vacuum drying the washed product at 60 ℃ for 12-24h to obtain Cd 0. 5Zn 0.5 S。
S4, obtaining 1g of g-C in the step S1 3 N 4 Dissolving the matrix in deionized water to obtain g-C 3 N 4 Suspension, 0.01g of Bi 3 O 4 Cl and 0.01g Cd 0.5 Zn 0.5 S is added to g-C 3 N 4 And ultrasonic treating in suspension for 2 hr, stirring the mixed suspension for 12 hr, centrifuging, washing with deionized water for 3 times, and vacuum drying at 60deg.C for 12-24 hr to obtain g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S。
Example 3
Double Z type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst comprises the following specific steps:
s1, calcining a certain amount of urea for 4 hours at 550 ℃, wherein the heating rate is 4 ℃/min, and obtaining g-C 3 N 4 。
S2.0.458g of Bi (NO 3 ) 3 ·5H 2 O was added to 10ml of ethylene glycol and sonicated for 10min to give solution A, after which 0.018g of NH was added 4 Dissolving Cl in 25ml deionized water, stirring for 10min to obtain solution B, mixing the solution A and the solution B, transferring into a polytetrafluoroethylene lining autoclave, reacting at 160 ℃ for 12h, centrifuging, washing with deionized water for 3 times, and vacuum drying the washed product at 60 ℃ for 12-24h to obtain Bi 3 O 4 Cl。
S3.0.7995g Cd (OAc) 2 ·2H 2 O and 0.6585g of Zn (OAc) 2 ·2H 2 O was mixed and dissolved in 50ml of deionized water, magnetically stirred for 3 hours, then 30ml of Na was added 2 S·9H 2 Dripping O (0.3 mol/L) solution into the mixed solution, magnetically stirring for 24h, centrifuging, washing with deionized water for 3 times, and vacuum drying the washed product at 60deg.C for 12-24h to obtain Cd 0. 5Zn 0.5 S。
S4, obtaining 1g of g-C in the step S1 3 N 4 Matrix bodyDissolving in deionized water to obtain g-C 3 N 4 Suspension, 0.01g of Bi 3 O 4 Cl and 0.03g Cd 0.5 Zn 0.5 S is added to g-C 3 N 4 And ultrasonic treating in suspension for 2 hr, stirring the mixed suspension for 12 hr, centrifuging, washing with deionized water for 3 times, and vacuum drying at 60deg.C for 12-24 hr to obtain g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S。
Comparative example 1
Cd (cadmium sulfide) 0.5 Zn 0.5 The preparation method of the S catalyst comprises the following specific steps:
0.7995g Cd(OAc) 2 ·2H 2 o and 0.6585g Zn (OAc) 2 ·2H 2 The O mixture was dissolved in 50ml deionized water and magnetically stirred for 3h. Then 30ml of Na 2 S.9H2O (0.3 mol/L) solution is dripped into the mixed solution, and the magnetic stirring is carried out for 24 hours. After centrifugation, washing 3 times with deionized water, and vacuum drying the obtained precipitate at 60 ℃ for 12-24 hours to obtain Cd 0.5 Zn 0.5 S。
Comparative example 2
Bi (Bi) 3 O 4 The preparation method of the Cl catalyst comprises the following specific steps:
0.458g Bi(NO 3 ) 3 5H2O was added to 10ml of ethylene glycol and sonicated for 10min to give solution A. Thereafter 0.018g NH 4 Cl was dissolved in 25ml deionized water and stirred for 10min to give solution B. Solutions a and B were then mixed, transferred to a teflon lined autoclave and reacted at 160 ℃ for 12h. After centrifugation, the mixture was washed 3 times with deionized water. Drying the washed product at 60 ℃ for 12-24 hours to obtain Bi 3 O 4 Cl。
Comparative example 3
g-C 3 N 4 The preparation method of the catalyst comprises the following specific steps:
adding urea into a crucible with a cover, and calcining in a muffle furnace at 550 ℃ for 4h to obtain g-C 3 N 4 。
Comparative example 4
g-C 3 N 4 /Cd 0.5 Zn0 .5 The preparation method of the S catalyst comprises the following specific steps:
0.02g of Cd 0.5 Zn 0.5 S is added to 1g of g-C 3 N 4 And ultrasonic treating for 2 hr, stirring the obtained mixed suspension for 12 hr, centrifuging, washing with deionized water for 3 times, and vacuum drying the obtained precipitate at 60deg.C for 12-24 hr to obtain g-C 3 N 4 /Cd 0.5 Zn 0. 5S。
Comparative example 5
g-C 3 N 4 /Bi 3 O 4 The preparation method of the Cl catalyst comprises the following specific steps:
0.01g of Bi 3 O 4 Cl was added to 1g of g-C 3 N 4 And ultrasonic treating for 2 hr, stirring the obtained mixed suspension for 12 hr, centrifuging, washing with deionized water for 3 times, and vacuum drying the obtained precipitate at 60deg.C for 12-24 hr to obtain g-C 3 N 4 /Bi 3 O 4 Cl。
Conclusion analysis
Referring to FIGS. 1 and 2, it is apparent that when g-C 3 N 4 、Bi 3 O 4 Cl and Cd 0.5 Zn 0.5 When S forms a composite catalyst, the original structure of the three components is still unchanged, bi is obtained 3 O 4 Cl and Cd 0.5 Zn 0.5 S is uniformly dispersed in g-C 3 N 4 The surface of the layered structure indicates successful recombination of the ternary components. And g-C 3 N 4 、Bi 3 O 4 Cl and Cd 0.5 Zn 0.5 The S edge has a clear boundary line, which indicates that g-C is successfully synthesized 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction.
Referring to FIG. 3, g-C can be seen 3 N 4 、Bi 3 O 4 Cl and Cd 0.5 Zn 0.5 All diffraction peaks of S are clearly visible, g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S has g-C at the same time 3 N 4 、Bi 3 O 4 Cl and Cd 0.5 Zn 0.5 The characteristic X-ray diffraction peak of S indicates successful synthesis of the heterojunction.
Referring to FIG. 4, lower g-C because electron-hole binding causes energy to dissipate in the form of fluorescence, heat 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S photoluminescence peak intensity indicates that it is equal to g-C 3 N 4 Compared with a single-component catalyst, the electron-hole pair recombination is obviously inhibited, which indicates that the formation of heterojunction inhibits the electron-hole pair recombination.
Referring to fig. 5, the larger photocurrent response illustrates that the heterojunction has better transport kinetics, facilitating the separation and transport of electron-hole pairs. Larger g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The S photocurrent intensity showed a significant enhancement in electron-hole pair separation and transport compared to the single component catalyst.
Referring to FIGS. 6 and 7, it can be seen that g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 After S forms heterojunction, CO 2 Reduction to CO and CH 4 The activity and selectivity of the heterojunction are greatly improved, the yield is obviously improved compared with other Z-type heterojunctions, and the tertiary cycle test proves that the heterojunctions have better stability, and FIG. 7 shows the double Z-type g-C prepared in example 1 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The CO and formation rate of the S heterojunction photocatalyst is about 21.92 mu mol g -1 And 152.01 mu mol g -1 The yield of the product is greatly improved compared with the traditional heterojunction.
Referring to FIG. 8, bi is generated due to a faster electron transfer rate in the double Z-mode 3 O 4 Cl and Cd 0.5 Zn 0.5 The photo-generated electrons in the conduction band of S pass through Cd respectively 0.5 Zn 0.5 S→g-C 3 N 4 And Bi (Bi) 3 O 4 Cl→g-C 3 N 4 Interface migration and g-C 3 N 4 The photogenerated holes on the valence band of (2) combine. Finally, the photo-generated electrons are at g-C 3 N 4 Is concentrated in the conduction band of (c). At the same time, light induces holes in Bi 3 O 4 Cl and Cd 0.5 Zn 0.5 And accumulated in the valence band of S. Therefore, bi 3 O 4 Cl and Cd 0.5 Zn 0.5 Holes and g-C in the valence band of S 3 N 4 Electrons in the conduction band of (2) can be effectively separated, and the photo-catalytic reduction of CO 2 Providing advantageous conditions.
This is due to g-C 3 N 4 Forming a layered nano-sheet structure, thereby being Bi 3 O 4 Cl and Cd 0.5 Zn 0.5 S-loaded to provide a large specific surface area to make it compatible with Bi 3 O 4 Cl and Cd 0.5 Zn 0.5 S is successfully compounded to form a double Z-shaped heterojunction catalyst, and the catalyst has the characteristics of high specific surface area, wide visible light response range and effective separation of photo-generated electron hole pairs.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. Double Z type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst characterized by comprising g-C 3 N 4 、Bi 3 O 4 Cl and Cd 0.5 Zn 0.5 S composition, wherein g-C 3 N 4 Is taken as a matrix and g-C is calculated according to the mass ratio 3 N 4 ：Bi 3 O 4 Cl：Cd 0.5 Zn 0.5 S＝1：0.005～0.015：0.01～0.03，
The g-C 3 N 4 Is of a layered structure, the Bi 3 O 4 Cl is of a sheet structure, and Bi is in a sheet shape 3 O 4 Cl insertionLamellar g-C 3 N 4 In the matrix, the Cd 0.5 Zn 0.5 S is nanocrystalline, cd 0.5 Zn 0.5 S is attached to lamellar g-C 3 N 4 A surface.
2. A double Z-type g-C according to claim 1 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, characterized in that the g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst, g-C according to mass ratio 3 N 4 ：Bi 3 O 4 Cl：Cd 0.5 Zn 0.5 S＝1：0.01：0.02。
3. A double Z-type g-C as claimed in claim 1 or claim 2 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst is characterized by comprising the following specific steps:
s1, preparation of g-C 3 N 4 A base;
s2, preparing Bi 3 O 4 Cl: bi (NO) 3 ) 3 ·5H 2 O is dissolved in glycol and NH is added 4 Cl, obtaining Bi after hydrothermal reaction 3 O 4 Cl；
S3, preparing Cd 0. 5Zn 0.5 S: cd (OAc) 2 ·2H 2 O and Zn (OAc) 2 ·2H 2 O is mixed and dissolved in deionized water, and Na is added 2 S·9H 2 After O solution, cd is obtained 0.5 Zn 0.5 S；
S4, preparation of g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S: the g-C obtained in the step S1 3 N 4 Dissolving the matrix in deionized water to obtain g-C 3 N 4 Suspending liquid, bi obtained in step S2 is mixed with 3 O 4 Cl and Cd obtained in step S3 0.5 Zn 0.5 S is added to g-C 3 N 4 In the suspension, a double Z-type is obtainedg-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst.
4. A double Z-type g-C according to claim 3 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst is characterized in that in the step S1, urea is calcined to obtain g-C 3 N 4 ；
The calcination temperature is 500-600 ℃, the calcination time is 3-6 h, and the heating rate is 4 ℃/min.
5. A double Z-type g-C according to claim 3 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst is characterized in that in the step S2, bi (NO 3 ) 3 ·5H 2 O: ethylene glycol=0.03 to 0.06g:1ml;
the hydrothermal reaction temperature is 140-180 ℃, and the hydrothermal reaction time is 10-14 h;
bi (NO) 3 ) 3 ·5H 2 O is dissolved in glycol, mixed solution A is obtained after ultrasonic treatment, NH is obtained 4 Cl is dissolved in deionized water, mixed solution B is obtained after stirring,
mixing the mixed solution A and the mixed solution B, transferring into a polytetrafluoroethylene stainless steel autoclave, performing hydrothermal reaction, cooling to room temperature, centrifugally collecting the obtained powder, washing, and drying to obtain Bi 3 O 4 Cl。
6. A double Z-type g-C according to claim 5 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst is characterized by comprising the following steps of 4 Cl: deionized water = 0.005-0.01 g:1ml of the gel was used for the preparation of a gel,
the ultrasonic time is 5-20 min, the stirring time is 5-20 min, the washing mode is washing with deionized water for 3 times, the drying is vacuum drying, the drying temperature is 60 ℃, and the drying time is 12-24h.
7. A double Z-type g-C according to claim 3 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst is characterized in that in the step S3, cd (OAc) 2 ·2H 2 O：Zn(OAc) 2 ·2H 2 O：Na 2 S·9H 2 O solution: deionized water = 0.01-0.02 g: 0.008-0.018 g: 0.4-0.8 ml:1ml;
the Na is 2 S·9H 2 The concentration of the O solution is 0.1-0.5 mol/L;
in step S3, cd (OAc) 2 ·2H 2 O and Zn (OAc) 2 ·2H 2 O is mixed and dissolved in deionized water, and Na is added after magnetic stirring 2 S·9H 2 O solution, magnetic stirring, centrifuging, washing and drying to obtain Cd 0.5 Zn 0.5 S。
8. A double Z-type g-C according to claim 7 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst is characterized in that the magnetic stirring time is 12-24 hours for two times, the washing mode is that deionized water is washed for 3 times, the drying is vacuum drying, the drying temperature is 60 ℃, and the drying time is 12-24 hours.
9. A double Z-type g-C according to claim 3 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The preparation method of the S heterojunction photocatalyst is characterized in that in the step S4, g-C obtained in the step S1 is prepared 3 N 4 Dissolving the matrix in deionized water to obtain g-C 3 N 4 Suspending liquid, bi obtained in step S2 is mixed with 3 O 4 Cl and Cd obtained in step S3 0.5 Zn 0.5 S is added to g-C 3 N 4 In the suspension, after ultrasonic treatment and stirring, washing and drying, the double Z-type g-C3N4/Bi is obtained 3 O 4 Cl/Cd 0.5 Zn 0.5 S heterojunction photocatalyst;
the stirring time is 12-24h, the washing mode is deionized water washing for 3 times, the drying is vacuum drying, the drying temperature is 60 ℃, and the drying time is 12-24h.
10. Double Z type g-C 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 Use of a S heterojunction photocatalyst according to claim 1 or claim 2, characterized in that 3 N 4 /Bi 3 O 4 Cl/Cd 0.5 Zn 0.5 The application of the S heterojunction photocatalyst in preparing carbon monoxide and methane by reducing carbon dioxide through photocatalysis.
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