CN110665525A - Perovskite of composite carbon nitride photocatalytic material and preparation method and application thereof - Google Patents
Perovskite of composite carbon nitride photocatalytic material and preparation method and application thereof Download PDFInfo
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- CN110665525A CN110665525A CN201910759853.6A CN201910759853A CN110665525A CN 110665525 A CN110665525 A CN 110665525A CN 201910759853 A CN201910759853 A CN 201910759853A CN 110665525 A CN110665525 A CN 110665525A
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- 239000000463 material Substances 0.000 title claims abstract description 47
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 45
- 239000002131 composite material Substances 0.000 title claims abstract description 28
- JMANVNJQNLATNU-UHFFFAOYSA-N oxalonitrile Chemical compound N#CC#N JMANVNJQNLATNU-UHFFFAOYSA-N 0.000 title claims abstract description 15
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 39
- 238000006243 chemical reaction Methods 0.000 claims abstract description 18
- 239000002243 precursor Substances 0.000 claims abstract description 15
- 238000000034 method Methods 0.000 claims abstract description 13
- 239000002904 solvent Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 15
- 238000001035 drying Methods 0.000 claims description 8
- 239000012296 anti-solvent Substances 0.000 abstract description 4
- 238000005215 recombination Methods 0.000 abstract description 4
- 230000006798 recombination Effects 0.000 abstract description 4
- 150000001875 compounds Chemical class 0.000 abstract description 3
- 239000000969 carrier Substances 0.000 abstract description 2
- 238000013508 migration Methods 0.000 abstract description 2
- 230000005012 migration Effects 0.000 abstract description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 abstract 1
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 abstract 1
- 229910052794 bromium Inorganic materials 0.000 abstract 1
- WVDDGKGOMKODPV-UHFFFAOYSA-N Benzyl alcohol Chemical compound OCC1=CC=CC=C1 WVDDGKGOMKODPV-UHFFFAOYSA-N 0.000 description 24
- HUMNYLRZRPPJDN-UHFFFAOYSA-N benzaldehyde Chemical compound O=CC1=CC=CC=C1 HUMNYLRZRPPJDN-UHFFFAOYSA-N 0.000 description 20
- QNGNSVIICDLXHT-UHFFFAOYSA-N para-ethylbenzaldehyde Natural products CCC1=CC=C(C=O)C=C1 QNGNSVIICDLXHT-UHFFFAOYSA-N 0.000 description 10
- 235000019445 benzyl alcohol Nutrition 0.000 description 8
- 239000011941 photocatalyst Substances 0.000 description 6
- 239000000843 powder Substances 0.000 description 5
- 238000004817 gas chromatography Methods 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000005286 illumination Methods 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 238000003915 air pollution Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007772 electrode material Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000003900 soil pollution Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C45/00—Preparation of compounds having >C = O groups bound only to carbon or hydrogen atoms; Preparation of chelates of such compounds
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- H10K—ORGANIC ELECTRIC SOLID-STATE DEVICES
- H10K30/00—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation
- H10K30/10—Organic devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation comprising heterojunctions between organic semiconductors and inorganic semiconductors
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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Abstract
The invention belongs to the technical field of perovskite material preparation, and discloses a perovskite of a composite carbon nitride photocatalytic material, and a preparation method and application thereof. The method comprises the steps of preparing perovskite reaction precursor liquid by taking DMF as a solvent, FApB as an FA source and PbBr as a bromine source; then C is added3N4Adding the photocatalytic material into toluene, and then dropwise adding the perovskite precursor solution. The method adopts an anti-solvent method to prepare the perovskite composite photocatalytic material. The perovskite material can be applied to the field of solar cells. The invention prepares the compound C3N4Perovskite of the photocatalytic material forms a Z-scheme heterojunction structure, shortens the migration path of current carriers, and reduces the costAnd the hole and electron recombination is reduced, so that the number of electrons and holes participating in the reaction is increased, and the reaction rate is improved.
Description
Technical Field
The invention belongs to the technical field of perovskite material preparation, and particularly relates to a perovskite of a composite carbon nitride photocatalytic material, and a preparation method and application thereof.
Background
In recent years, with the progress of society and the rapid increase of economy, the problems of energy shortage and environmental pollution are becoming more serious, and the search for sustainable and pollution-free clean energy is urgent. Solar energy is increasingly favored by the energy industry as a representative of green clean energy.
The semiconductor photocatalysis technology is a new technology for directly utilizing solar energy, has the advantages of economy, environmental protection and the like, and becomes one of the hottest solar energy utilization methods. The photocatalysis technology isThe photocatalyst can only solve the problem of water pollution, can also be used for solving the problems of air pollution, soil pollution, organic matter degradation, sterilization and the like, has wide market application space and value, and can also be used for photolyzing water to generate hydrogen to solve the energy problem. Recently developed g-C3N4As a two-dimensional nano semiconductor material, the photocatalyst is called as a hotspot of research in recent years and is widely applied to the aspects of photocatalysts and the like due to the advantages of higher photocatalytic activity, good stability, special optical performance, no toxicity, easy preparation and the like, particularly the outstanding advantage of no metal.
The perovskite is a functional material with excellent optical and electrical properties, and has wide application prospect in the fields of solar cells, light emitting diodes, micro lasers and the like. And FAPBBr3The perovskite material is an organic-inorganic perovskite material which is very popular at present, and has a wide application prospect in various fields such as gas sensors, electrode materials, solar cells and the like due to good light absorption capacity. However, with the human pairing to FAPBBr3Further research shows that the photocatalyst is also a good photocatalyst, and more people apply the photocatalyst to the field of photocatalysis. Therefore, to better exploit FAPBR3The role in the field of photocatalysis has to be solved by a problem: reducing the recombination rate of the photo-generated electron-hole pairs.
Disclosure of Invention
In order to overcome the disadvantages and shortcomings of the prior art, the invention provides a composite carbon nitride (C)3N4) A preparation method of perovskite of the photocatalytic material; the method adopts an anti-solvent method to prepare the compound C3N4The perovskite of the photocatalytic material has simple preparation process and low cost.
Still another object of the present invention is to provide a composite carbon nitride (C) prepared by the above preparation method3N4) Perovskite of photocatalytic material.
It is still another object of the present invention to provide the above composite carbon nitride (C)3N4) Use of a perovskite of photocatalytic material.
The purpose of the invention is realized by the following technical scheme:
composite carbon nitride (C)3N4) The preparation method of the perovskite of the photocatalytic material comprises the following operation steps: adding FAPb and PbBr into a solvent to prepare a reaction precursor solution of 0.5 mol/L-3 mol/L; 50mg to 300mg of C3N4Adding the photocatalytic material into 5-15 ml of toluene, magnetically stirring, dropwise adding 10-150 mul of reaction precursor liquid into the stirred toluene, continuously stirring for 10-20 h, and drying to obtain the perovskite of the composite carbon nitride photocatalytic material.
The solvent is DMF.
The stirring speed is 800-1500 r/min.
The drying time is 1-3 h, and the temperature is 30-60 ℃.
The perovskite of the composite carbon nitride photocatalytic material prepared by the preparation method.
The perovskite of the composite carbon nitride photocatalytic material is applied to the field of solar cells.
The principle of the invention is as follows: the invention prepares the compound C3N4The perovskite of the photocatalytic material forms a Z-scheme heterojunction structure, shortens the migration path of a current carrier, and reduces the recombination of holes and electrons, thereby increasing the quantity of the electrons and the holes participating in the reaction and improving the reaction rate.
Compared with the prior art, the invention has the following advantages and effects:
(1) the method adopts an anti-solvent method, takes DMF as a solvent, and adds FAPb and PbBr to prepare a reaction precursor solution; reuse of antisolvent in process C3N4Synthesizing perovskite particles on the surface.
(2) Composite C synthesized by the invention3N4The perovskite of the photocatalytic material forms a Z-scheme heterojunction structure, so that the recombination rate of holes and electrons can be effectively reduced, the service life of carriers is prolonged, and the performance of the material is improved.
(3) The invention has simple required equipment and preparation process and low cost, and can be directly produced in large batch.
Drawings
FIG. 1 shows C used in example 13N4SEM photographs of the perovskite of the photocatalytic material.
FIG. 2 shows composite C of a Z-scheme heterojunction structure prepared in example 13N4SEM photographs of the perovskite surface of the photocatalytic material.
FIG. 3 shows composites C prepared in examples 1-43N4The perovskite powder of the photocatalytic material converts benzaldehyde into a ratio graph of benzaldehyde.
Detailed Description
The following examples are presented to further illustrate the present invention and should not be construed as limiting the invention. Unless otherwise specified, the technical means used in the examples are conventional means well known to those skilled in the art. Reagents, methods and apparatus used in the present invention are conventional in the art unless otherwise indicated.
Example 1
Adding FAPb and PbBr into DMF solvent to prepare 0.5mol/L reaction precursor solution; 300mgC3N4Adding the photocatalytic material into 15ml of toluene, magnetically stirring at the rotating speed of 1500r/min, dropwise adding 10ul of reaction precursor liquid into the stirred toluene, and continuously stirring at the rotating speed of 1500r/min for 20 hours; putting the stirred sample into a vacuum drying oven for drying at 50 ℃ to obtain a composite C3N4Perovskite powder of photocatalytic material.
FIG. 1 shows a graph C used in this example3N4SEM photograph of the photocatalytic material, as shown in FIG. 1, C observed under a scanning electron microscope of 10000 times3N4Morphology of the photocatalytic material before compositing with the perovskite. FIG. 2 shows composite C prepared in this example3N4SEM photograph of the surface of the perovskite after photocatalytic material. As can be seen from FIG. 2, the load observed under the scanning electron microscope of 7000 times is C3N4The perovskite particles of (a). Composite C prepared in this example3N4Photocatalytic materialThe ratio of benzyl alcohol to benzaldehyde of the following perovskite was measured by gas chromatography and the relative ratio of benzyl alcohol to benzaldehyde after light irradiation was as shown in FIG. 3.
Example 2
Adding FAPb and PbBr into DMF solvent to prepare 3mol/L reaction precursor solution; 300mgC3N4Adding the photocatalytic material into 15ml of toluene, magnetically stirring at the rotating speed of 1500r/min, dropwise adding 10ul of reaction precursor liquid into the stirred toluene, and continuously stirring at the rotating speed of 1500r/min for 20 hours; putting the stirred sample into a vacuum drying oven for drying at 50 ℃ to obtain a composite C3N4Perovskite powder of photocatalytic material. Composite C prepared in this example3N4The perovskite behind the photocatalytic material converts benzyl alcohol to benzaldehyde, and the relative ratio of benzyl alcohol to benzaldehyde after illumination is obtained through a gas chromatography test and is shown in fig. 3.
Example 3
Adding FAPb and PbBr into DMF solvent to prepare 0.5mol/L reaction precursor solution; will 100mgC3N4Adding the photocatalytic material into 5ml of toluene, and magnetically stirring at the rotating speed of 1500 r/min; then dripping 10ul of the reaction precursor liquid into the toluene in stirring, and continuously stirring for 20 hours at the rotating speed of 1500 r/min; putting the stirred sample into a vacuum drying oven for drying at 50 ℃ to obtain a composite C3N4Perovskite powder of photocatalytic material. Composite C prepared in this example3N4The perovskite behind the photocatalytic material converts benzyl alcohol to benzaldehyde, and the relative ratio of benzyl alcohol to benzaldehyde after illumination is obtained through a gas chromatography test and is shown in fig. 3.
Example 4
Adding FAPb and PbBr into DMF solvent to prepare 3mol/L reaction precursor solution; 50mgC3N4Adding the photocatalytic material into 15ml of toluene, magnetically stirring at the rotating speed of 1500r/min, dropwise adding 50ul of reaction precursor liquid into the stirred toluene, and stirring at the rotating speed of 1500r/min for 20 hours; putting the stirred sample into a vacuum drying oven for drying at 30 ℃ to obtain a composite C3N4Perovskite of photocatalytic materialAnd (4) mineral powder. Composite C prepared in this example3N4The perovskite behind the photocatalytic material converts benzyl alcohol to benzaldehyde, and the relative ratio of benzyl alcohol to benzaldehyde after illumination is obtained through a gas chromatography test and is shown in fig. 3.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (6)
1. A preparation method of perovskite of composite carbon nitride photocatalytic material is characterized by comprising the following operation steps: adding FAPb and PbBr into a solvent to prepare a reaction precursor solution of 0.5 mol/L-3 mol/L; 50mg to 300mg of C3N4Adding the photocatalytic material into 5-15 ml of toluene, magnetically stirring, dropwise adding 10-150 mul of reaction precursor liquid into the stirred toluene, continuously stirring for 10-20 h, and drying to obtain the perovskite of the composite carbon nitride photocatalytic material.
2. The method of claim 1, wherein: the solvent is DMF.
3. The method of claim 1, wherein: the stirring speed is 800-1500 r/min.
4. The method of claim 1, wherein: the drying time is 1-3 h, and the temperature is 30-60 ℃.
5. A perovskite of a composite carbon nitride photocatalytic material prepared by the preparation method according to any one of claims 1 to 4.
6. Use of the perovskite of the composite carbon nitride photocatalytic material according to claim 5 in the field of solar cells.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112892573A (en) * | 2021-01-20 | 2021-06-04 | 陕西师范大学 | Perovskite composite material coated by CN as well as preparation method and application thereof |
| CN115569659A (en) * | 2022-08-18 | 2023-01-06 | 电子科技大学长三角研究院(湖州) | In-situ generated perovskite heterojunction photocatalyst, preparation method and application |
| CN115805092A (en) * | 2022-11-18 | 2023-03-17 | 南开大学 | g-C 3 N 4 Preparation method of/Ag/AgCl/ZnO composite photocatalyst and product |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112892573A (en) * | 2021-01-20 | 2021-06-04 | 陕西师范大学 | Perovskite composite material coated by CN as well as preparation method and application thereof |
| CN112892573B (en) * | 2021-01-20 | 2023-07-18 | 陕西师范大学 | CN-coated perovskite composite material and preparation method and application thereof |
| CN115569659A (en) * | 2022-08-18 | 2023-01-06 | 电子科技大学长三角研究院(湖州) | In-situ generated perovskite heterojunction photocatalyst, preparation method and application |
| CN115569659B (en) * | 2022-08-18 | 2023-11-10 | 电子科技大学长三角研究院(湖州) | In-situ generation perovskite heterojunction photocatalyst, preparation method and application |
| CN115805092A (en) * | 2022-11-18 | 2023-03-17 | 南开大学 | g-C 3 N 4 Preparation method of/Ag/AgCl/ZnO composite photocatalyst and product |
| CN115805092B (en) * | 2022-11-18 | 2024-05-03 | 南开大学 | G-C3N4Preparation method of Ag/AgCl/ZnO composite photocatalyst and product |
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Application publication date: 20200110 |