CN113813970B - Bismuth vanadate/lead cesium bromide photocatalytic material with 2D/2D structure and application thereof - Google Patents
Bismuth vanadate/lead cesium bromide photocatalytic material with 2D/2D structure and application thereof Download PDFInfo
- Publication number
- CN113813970B CN113813970B CN202111176776.5A CN202111176776A CN113813970B CN 113813970 B CN113813970 B CN 113813970B CN 202111176776 A CN202111176776 A CN 202111176776A CN 113813970 B CN113813970 B CN 113813970B
- Authority
- CN
- China
- Prior art keywords
- bismuth vanadate
- lead
- cesium
- bromide
- dimensional
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 229910052797 bismuth Inorganic materials 0.000 title claims abstract description 63
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 title claims abstract description 63
- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 title claims abstract description 63
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 58
- 239000000463 material Substances 0.000 title claims abstract description 53
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 title claims abstract description 18
- 239000002135 nanosheet Substances 0.000 claims abstract description 33
- NAJCQJKJQOIHSH-UHFFFAOYSA-L [Pb](Br)Br.[Cs] Chemical compound [Pb](Br)Br.[Cs] NAJCQJKJQOIHSH-UHFFFAOYSA-L 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 30
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 30
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 30
- 239000005642 Oleic acid Substances 0.000 claims description 30
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 30
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 30
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 30
- 239000000243 solution Substances 0.000 claims description 26
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims description 21
- 239000011259 mixed solution Substances 0.000 claims description 21
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 claims description 19
- 229910000024 caesium carbonate Inorganic materials 0.000 claims description 19
- QGLWBTPVKHMVHM-KTKRTIGZSA-N (z)-octadec-9-en-1-amine Chemical compound CCCCCCCC\C=C/CCCCCCCCN QGLWBTPVKHMVHM-KTKRTIGZSA-N 0.000 claims description 15
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 15
- UNTBPXHCXVWYOI-UHFFFAOYSA-O azanium;oxido(dioxo)vanadium Chemical compound [NH4+].[O-][V](=O)=O UNTBPXHCXVWYOI-UHFFFAOYSA-O 0.000 claims description 15
- 229910017604 nitric acid Inorganic materials 0.000 claims description 15
- 229910052792 caesium Inorganic materials 0.000 claims description 14
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 12
- 239000012046 mixed solvent Substances 0.000 claims description 11
- CCCMONHAUSKTEQ-UHFFFAOYSA-N octadecene Natural products CCCCCCCCCCCCCCCCC=C CCCMONHAUSKTEQ-UHFFFAOYSA-N 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 230000035484 reaction time Effects 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000007146 photocatalysis Methods 0.000 claims description 6
- 238000002360 preparation method Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 3
- 238000011065 in-situ storage Methods 0.000 claims description 3
- 239000002904 solvent Substances 0.000 claims description 3
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 abstract description 24
- 229910002092 carbon dioxide Inorganic materials 0.000 abstract description 15
- 239000001569 carbon dioxide Substances 0.000 abstract description 12
- 239000002114 nanocomposite Substances 0.000 abstract description 2
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 description 9
- 230000005540 biological transmission Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 3
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910052794 bromium Inorganic materials 0.000 description 2
- 239000002131 composite material Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 235000019253 formic acid Nutrition 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000002064 nanoplatelet Substances 0.000 description 2
- 230000006798 recombination Effects 0.000 description 2
- 238000005215 recombination Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- 229910002915 BiVO4 Inorganic materials 0.000 description 1
- 241000510672 Cuminum Species 0.000 description 1
- 235000007129 Cuminum cyminum Nutrition 0.000 description 1
- NCFBWCVNPJEZMG-UHFFFAOYSA-N [Br].[Pb].[Cs] Chemical compound [Br].[Pb].[Cs] NCFBWCVNPJEZMG-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000012071 phase Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000005556 structure-activity relationship Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
-
- 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
- B01J27/06—Halogens; Compounds thereof
- B01J27/135—Halogens; Compounds thereof with titanium, zirconium, hafnium, germanium, tin or lead
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/20—Vanadium, niobium or tantalum
- B01J23/22—Vanadium
-
- 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
- B01J35/20—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state
- B01J35/23—Catalysts, in general, characterised by their form or physical properties characterised by their non-solid state in a colloidal state
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/40—Carbon monoxide
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Catalysts (AREA)
Abstract
Bismuth vanadate with 2D/2D structureA cesium lead bromide photocatalytic material, belonging to the field of nano composite materials. The photocatalytic material is a heterostructure formed by two-dimensional bismuth vanadate nanosheets and two-dimensional lead-cesium bromide nanosheets; the two-dimensional bismuth vanadate nanosheet is square with a sawtooth-shaped structure at four corners, the side length is 600-1000 nm, and the thickness is 50-60 nm; the two-dimensional cesium lead bromide nanosheet is rectangular, has the length of 200-1300 nm, the width of 180-1200 nm and the thickness of 35-45 nm; the mass ratio of the lead-cesium bromide to the bismuth vanadate is (3.2-9.5): 1. when the bismuth vanadate/lead cesium bromide photocatalytic material is applied to photocatalytic carbon dioxide reduction, the CO generation rate is up to 16.9 mu mol g under the irradiation of visible light‑1h‑1The selectivity of the product of CO reduction is over 94%, and the method has potential application prospect in the field of photocatalytic carbon dioxide reduction.
Description
Technical Field
The invention belongs to the field of nano composite materials, and particularly relates to a bismuth vanadate/lead cesium bromide photocatalytic material with a 2D/2D structure and application thereof in photocatalysis of CO2Application in reduction.
Background
Photocatalytic carbon dioxide reduction to obtain methane (CH)4) And carbon monoxide (CO) is a very promising approach to achieve solar-to-fuel conversion. However, the products of carbon dioxide reduction are of great complexity due to the nature of the multi-electron reactions, i.e., there are a variety of gas phase products such as CH4And CO, as well as various liquid phase products such as formic acid (HCOOH), methanol (CH)3OH), etc. Therefore, materials for photocatalytic carbon dioxide are required to have high target product selectivity in addition to high catalytic activity. In recent years, perovskite materials have been developed rapidly, wherein, the all-inorganic lead-bromine perovskite materials have the characteristics of narrow band gap, wide color gamut, high photoluminescence quantum yield, high carrier mobility, high chemical stability and the like, and have wide application in the photoelectric field such as light emitting devicesThe use of (1). Meanwhile, due to the characteristics, the bromine-lead-cesium perovskite material is gradually expanded and applied to the field of photocatalysis. However, the single use of the bromine-lead-cesium-perovskite material as a photocatalytic material still suffers from the high photon-generated electron-hole recombination rate and low selectivity to CO, and therefore, it is very important to construct a heterostructure through a structural design or with a semiconductor having a suitable band gap and band position.
The structure-activity relationship of the materials, namely the relationship between the structure and the performance, is the subject of cumin search of scientific researchers. The structure of the material greatly affects the properties of the material. For example, two-dimensional (2D) nanomaterials have the advantages of having a larger specific surface area, more exposed active sites, and higher light capture efficiency compared to bulk materials. However, only few reports are reported about the two-dimensional nano-sheet structured cesium lead bromide material, and the application of the two-dimensional cesium lead bromide material in the field of photocatalysis still needs to be deeply developed.
Disclosure of Invention
The invention aims to provide a bismuth vanadate/lead cesium bromide photocatalytic material with a 2D/2D structure and application thereof, wherein the photocatalytic material is applied to photocatalysis of CO2In reduction, the catalyst has higher CO selectivity.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a bismuth vanadate/lead cesium bromide photocatalytic material with a 2D/2D structure is characterized in that the photocatalytic material is a heterostructure formed by a two-dimensional bismuth vanadate nanosheet and a two-dimensional lead cesium bromide nanosheet; the two-dimensional bismuth vanadate nanosheet is square with a sawtooth-shaped structure at four corners, the side length is 600-1000 nm, and the thickness is 50-60 nm; the two-dimensional cesium lead bromide nanosheet is rectangular, has the length of 200-1300 nm, the width of 180-1200 nm and the thickness of 35-45 nm; the mass ratio of the lead-cesium bromide to the bismuth vanadate is (3.2-9.5): 1. the 2D/2D structure can form a stable heterogeneous interface, and the size of the heterogeneous interface is diversified due to the size difference of the nanosheets.
A preparation method of a bismuth vanadate/lead cesium bromide photocatalytic material with a 2D/2D structure is characterized by comprising the following steps:
1.1 dispersing pentahydrate bismuth nitrate in a mixed solvent of oleylamine, oleic acid and octadecene, and uniformly stirring to obtain a mixed solution A; wherein, in the mixed solvent, the volume ratio of oleylamine, oleic acid and octadecene is 1:1:10, the mass concentration of the pentahydrate bismuth nitrate in the mixed solution A is 20g/L;
1.2 heating the mixed solution A to be transparent at 150 ℃, then naturally cooling to 100 ℃, dropwise adding a nitric acid solution containing ammonium metavanadate, and stirring for reacting for 40min to obtain two-dimensional bismuth vanadate nanosheets; the nitric acid solution containing ammonium metavanadate is prepared by taking ammonium metavanadate as a solute and taking a mixed solution of concentrated nitric acid and deionized water as a solvent, wherein the mass concentration of ammonium metavanadate in the nitric acid solution containing ammonium metavanadate is 9.7g/L, and the volume ratio of the concentrated nitric acid, the deionized water and the oleylamine in the step 1.1 is 2;
placing cesium carbonate in oleic acid, and stirring to obtain an oleic acid solution of cesium carbonate; then heating the oleic acid solution of cesium carbonate at 100-140 ℃ for 30-60 min to prepare an oleic acid precursor solution of cesium carbonate with the mass concentration of 3.2 g/L;
step 3, adding lead bromide and the two-dimensional bismuth vanadate nanosheets prepared in the step 1 into a mixed solvent of oleylamine, oleic acid and octadecene, and uniformly stirring to obtain a mixed solution B; wherein, in the mixed solvent, the volume ratio of oleylamine, oleic acid and octadecene is 1; the mass concentration of lead bromide in the mixed solution B is 1-1.2 g/L, and the mass concentration of bismuth vanadate is 0.2-0.5 g/L;
step 4, heating the mixed solution B obtained in the step 3 at 120 ℃ for 40-120 min, then heating to 150 ℃, adding the oleic acid precursor solution of cesium carbonate obtained in the step 2 for in-situ growth, wherein the reaction time is 1-5 min; after the reaction is finished, cooling, separating and drying to obtain the bismuth vanadate/lead-cesium bromide photocatalytic material; wherein the volume ratio of the oleic acid precursor solution of cesium carbonate to the oleylamine in step 3 is 2.
The invention also provides bismuth vanadate/bromine with the 2D/2D structureApplication of lead-cesium photocatalytic material in photocatalysis of CO2Application in reduction.
Compared with the prior art, the invention has the following beneficial effects:
1. the bismuth vanadate/lead cesium bromide photocatalytic material with the 2D/2D structure is a heterostructure formed by two-dimensional bismuth vanadate nanosheets and two-dimensional lead cesium bromide nanosheets, and due to the size difference of the nanosheets, the size of the heterostructure formed has diversity, so that the recombination efficiency of a photon-generated carrier is greatly reduced, and the photocatalytic material has excellent photocatalytic performance. When the bismuth vanadate/lead cesium bromide photocatalytic material is applied to photocatalytic carbon dioxide reduction, the CO generation rate is up to 16.9 mu mol g under the irradiation of visible light (300W xenon lamp)-1h-1The selectivity of the product of CO reduction is over 94%, and the method has potential application prospect in the field of photocatalytic carbon dioxide reduction.
2. According to the bismuth vanadate/lead cesium bromide photocatalytic material with the 2D/2D structure, any sacrificial agent or cocatalyst is not required to be added in the carbon dioxide reduction, so that the economic cost is greatly saved, and no environmental pollution is caused.
Drawings
FIG. 1 is an X-ray diffraction (XRD) spectrum of a 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material obtained by a reaction for 2.5 minutes in example 1 of the present invention;
FIG. 2 is a Transmission Electron Microscope (TEM) photograph (scale 200 nm) of the 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material of example 1 of the present invention; wherein a, b, c correspond to the products of example 1 with reaction times of 1 minute, 2.5 minutes and 5 minutes, respectively;
FIG. 3 is a high-power transmission electron microscope (HRTEM) photograph (scale 10 nm) of a 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material obtained by a reaction for 5 minutes in example 1 of the present invention;
FIG. 4 is an Atomic Force Microscope (AFM) photograph (scale 400 nm) of a 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material obtained at a reaction time of 2.5 minutes in example 1 of the present invention, and the inset is a height sectional view of a linear region in the drawing;
FIG. 5 is a graph comparing the generation rates of the carbon dioxide photocatalytic reduction products of the 2D/2D bismuth vanadate/lead cesium bromide photocatalytic material according to example 1 of the present invention; wherein BC1, BC2 and BC3 correspond to the products of example 1 with reaction times of 1 minute, 2.5 minutes and 5 minutes, respectively;
FIG. 6 is a graph showing the selectivity of the product of the photocatalytic reduction of carbon dioxide in the 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material according to example 1 of the present invention; wherein BC1, BC2 and BC3 correspond to the products of example 1 with reaction times of 1 minute, 2.5 minutes and 5 minutes, respectively.
Detailed Description
The technical solutions of the present invention are described in detail below with reference to the accompanying drawings and embodiments, but the scope of protection of the present invention is not limited to these embodiments.
Example 1
A preparation method of a bismuth vanadate/lead cesium bromide photocatalytic material with a 2D/2D structure specifically comprises the following steps:
1.1 dispersing 0.24g of pentahydrate bismuth nitrate into a mixed solvent of 1mL of oleylamine, 1mL of oleic acid and 10mL of octadecene, and uniformly stirring to obtain a mixed solution A;
1.2 heating the mixed solution A to be transparent at 150 ℃, then naturally cooling to 100 ℃, dropwise adding a nitric acid solution containing ammonium metavanadate, and stirring for reacting for 40min to obtain a two-dimensional bismuth vanadate nanosheet; wherein the ammonium metavanadate-containing nitric acid solution is prepared by taking ammonium metavanadate as a solute and taking a mixed solution of concentrated nitric acid and deionized water as a solvent, the mass concentration of ammonium metavanadate in the ammonium metavanadate-containing nitric acid solution is 9.7g/L, and the volume ratio of the concentrated nitric acid, the deionized water and the oleylamine in the step 1.1 is 2;
placing cesium carbonate in oleic acid, and stirring to obtain an oleic acid solution of cesium carbonate; then heating the oleic acid solution of cesium carbonate at 140 ℃ for 30min to prepare an oleic acid precursor solution of cesium carbonate with the mass concentration of 3.2 g/L;
step 3, adding 26mg of lead bromide and 5mg of the two-dimensional bismuth vanadate nanosheet prepared in the step 1 into a mixed solvent of oleylamine, oleic acid and octadecene, and uniformly stirring to obtain a mixed solution B; wherein, in the mixed solvent, the volumes of oleylamine, oleic acid and octadecene are respectively 1mL, 3mL and 20mL;
step 4, placing the mixed solution B obtained in the step 3 in a three-neck flask, heating the mixed solution B at 120 ℃ for 60min, then heating the mixed solution B to 150 ℃, adding 2mL of oleic acid precursor solution of cesium carbonate obtained in the step 2, and carrying out in-situ growth for 1 min, 2.5 min and 5min; and after the reaction is finished, cooling, separating and drying to obtain the bismuth vanadate/lead-cesium bromide photocatalytic material.
FIG. 1 is an X-ray diffraction (XRD) spectrum of a 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material obtained by a reaction for 2.5 minutes in example 1 of the present invention; it can be seen that bismuth vanadate in the composite material corresponds to monoclinic system BiVO4(PDF 14-0688), cesium lead bromide corresponds to the cubic CsPbBr system3(PDF 54-0752)。
FIG. 2 is a Transmission Electron Microscope (TEM) photograph (scale 200 nm) of the 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material of example 1 of the present invention; wherein a, b, c correspond to the products of example 1 with reaction times of 1 minute, 2.5 minutes and 5 minutes, respectively; it can be seen that cesium lead bromide is successfully loaded on the two-dimensional bismuth vanadate nanosheets, the bismuth vanadate nanosheets are square with sawtooth-shaped structures at four corners, the cesium lead bromide nanosheets are rectangular, and the size of the heterointerfaces of the cesium lead bromide nanosheets is diversified.
FIG. 3 is a high-power transmission electron microscope (HRTEM) photograph (scale 10 nm) of a 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material obtained by a reaction for 5 minutes in example 1 of the present invention; it can be seen that the interfaces of bismuth vanadate and cesium lead bromide are clearly seen, wherein the 0.26nm and 0.25nm lattice stripes correspond to the (200) and (002) crystal faces of bismuth vanadate, respectively, and the 0.58nm lattice stripe corresponds to the (001) crystal face of cesium lead bromide, and HRTEM further proves that the bismuth vanadate/cesium lead bromide composite material has a 2D/2D structure.
FIG. 4 is an Atomic Force Microscope (AFM) photograph (scale 400 nm) of a 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material obtained at a reaction time of 2.5 minutes in example 1 of the present invention, and the inset is a height sectional view of a linear region in the drawing; wherein the nanoplatelets of 40nm thickness correspond to cesium lead bromide and the nanoplatelets of 54nm and 59nm thickness correspond to bismuth vanadate.
FIG. 5 is a graph comparing the generation rates of the products of the 2D/2D bismuth vanadate/cesium lead bromide photocatalytic materials according to example 1 of the present invention by carbon dioxide photocatalytic reduction; it can be seen that the CO generation rates of the obtained photocatalytic materials are all over 13.5 mu mol g-1h-1Up to 16.9. Mu. Mol g-1h-1。
FIG. 6 is a graph showing the selectivity of the product of the photocatalytic reduction of carbon dioxide in the 2D/2D bismuth vanadate/cesium lead bromide photocatalytic material according to example 1 of the present invention; it can be seen that the selectivity of the obtained photocatalytic material for CO products exceeds 94%.
Example 2
Example 2 differs from example 1 in that: in the step 3, the mass of the added two-dimensional bismuth vanadate nanosheet prepared in the step 1 is 12mg, and the mass of the lead bromide is 28mg; in step 4, the reaction time was 2.5 minutes. The rest of the procedure was the same as in example 1.
Example 3
Example 3 is different from example 2 in that: in the step 3, the mass of the added two-dimensional bismuth vanadate nanosheet prepared in the step 1 is 8mg, and the mass of the lead bromide is 24mg; in step 4, the mixture B is placed in a three-necked flask and heated at 120 ℃ for 120min. The remaining steps were the same as in example 2.
Example 4
Example 4 differs from example 2 in that: in the step 3, the mass of the added two-dimensional bismuth vanadate nanosheet prepared in the step 1 is 8mg, and the mass of the lead bromide is 28mg; in step 4, the mixture B was heated in a three-necked flask at 120 ℃ for 40min. The remaining procedure was the same as in example 2.
Claims (4)
1. A bismuth vanadate/lead cesium bromide photocatalytic material with a 2D/2D structure is characterized in that the photocatalytic material is a heterostructure formed by a two-dimensional bismuth vanadate nanosheet and a two-dimensional lead cesium bromide nanosheet; the two-dimensional bismuth vanadate nanosheet is square with a sawtooth-shaped structure at four corners, the side length is 600-1000 nm, and the thickness is 50-60 nm; the two-dimensional cesium lead bromide nanosheet is rectangular, has the length of 200-1300 nm, the width of 180-1200 nm and the thickness of 35-45 nm; the mass ratio of the lead-cesium bromide to the bismuth vanadate is (3.2-9.5): 1.
2. a preparation method of a bismuth vanadate/lead cesium bromide photocatalytic material with a 2D/2D structure is characterized by comprising the following steps:
step 1, preparing a two-dimensional bismuth vanadate nanosheet:
1.1 dispersing pentahydrate bismuth nitrate in a mixed solvent of oleylamine, oleic acid and octadecene, and uniformly stirring to obtain a mixed solution A; wherein, in the mixed solvent, the volume ratio of oleylamine, oleic acid and octadecene is 1:1:10, the mass concentration of the pentahydrate bismuth nitrate in the mixed solution A is 20g/L;
1.2 heating the mixed solution A to be transparent at 150 ℃, then naturally cooling to 100 ℃, dropwise adding a nitric acid solution containing ammonium metavanadate, and stirring for reacting for 40min to obtain a two-dimensional bismuth vanadate nanosheet; wherein the ammonium metavanadate-containing nitric acid solution is prepared by taking ammonium metavanadate as a solute and taking a mixed solution of concentrated nitric acid and deionized water as a solvent, the mass concentration of ammonium metavanadate in the ammonium metavanadate-containing nitric acid solution is 9.7g/L, and the volume ratio of the concentrated nitric acid, the deionized water and the oleylamine in the step 1.1 is 2;
step 2, preparation of an oleic acid precursor solution of cesium carbonate:
placing cesium carbonate in oleic acid, and stirring to obtain an oleic acid solution of cesium carbonate; then heating the oleic acid solution of cesium carbonate at 100-140 ℃ for 30-60 min to prepare an oleic acid precursor solution of cesium carbonate with the mass concentration of 3.2 g/L;
step 3, adding lead bromide and the two-dimensional bismuth vanadate nanosheets prepared in the step 1 into a mixed solvent of oleylamine, oleic acid and octadecene, and uniformly stirring to obtain a mixed solution B; wherein, in the mixed solvent, the volume ratio of oleylamine, oleic acid and octadecene is 1; the mass concentration of lead bromide in the mixed solution B is 1-1.2 g/L, and the mass concentration of bismuth vanadate is 0.2-0.5 g/L;
step 4, heating the mixed solution B obtained in the step 3 at 120 ℃ for 40-120 min, then heating to 150 ℃, adding the oleic acid precursor solution of cesium carbonate obtained in the step 2 for in-situ growth, wherein the reaction time is 1-5 min; and after the reaction is finished, cooling, separating and drying to obtain the bismuth vanadate/lead-cesium bromide photocatalytic material.
3. Use of the bismuth vanadate/cesium lead bromide photocatalytic material as defined in claim 1 in the photocatalysis of CO2Application in reduction.
4. The bismuth vanadate/lead cesium bromide photocatalytic material obtained by the method of claim 2 for photocatalytic CO2Application in reduction.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111176776.5A CN113813970B (en) | 2021-10-09 | 2021-10-09 | Bismuth vanadate/lead cesium bromide photocatalytic material with 2D/2D structure and application thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202111176776.5A CN113813970B (en) | 2021-10-09 | 2021-10-09 | Bismuth vanadate/lead cesium bromide photocatalytic material with 2D/2D structure and application thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113813970A CN113813970A (en) | 2021-12-21 |
| CN113813970B true CN113813970B (en) | 2022-11-01 |
Family
ID=78919860
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202111176776.5A Expired - Fee Related CN113813970B (en) | 2021-10-09 | 2021-10-09 | Bismuth vanadate/lead cesium bromide photocatalytic material with 2D/2D structure and application thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113813970B (en) |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114950500B (en) * | 2022-02-24 | 2024-04-23 | 电子科技大学长三角研究院(湖州) | Preparation method and application of bismuth/bromine lead cesium composite photocatalytic material |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113318761B (en) * | 2021-04-29 | 2022-05-27 | 杭州师范大学 | Preparation method of Bi3O4Br/CsPbBr3 composite material |
-
2021
- 2021-10-09 CN CN202111176776.5A patent/CN113813970B/en not_active Expired - Fee Related
Also Published As
| Publication number | Publication date |
|---|---|
| CN113813970A (en) | 2021-12-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107456991B (en) | g-C3N4Preparation method of quantum dot supported bismuth tungstate nanosheet photocatalyst | |
| CN111115649B (en) | Preparation method of BCN nanosheet, BCN nanosheet prepared by preparation method and application of BCN nanosheet | |
| CN110721698B (en) | Bismuth vanadate/copper vanadate composite photocatalyst and preparation method and application thereof | |
| CN106925304B (en) | Bi24O31Br10/ZnO composite visible light catalyst and preparation method thereof | |
| CN112371189A (en) | Hydroxide-coated ZIF (zinc-oxygen-doped organic framework) MOFs (metal-organic frameworks) heterogeneous catalyst and preparation and application thereof | |
| Gautam et al. | Hot injection-induced synthesis of ZnCdS–rGO/MoS 2 heterostructures for efficient hydrogen production and CO 2 photoreduction | |
| CN110013880B (en) | MIL-101 composite photocatalytic material, preparation method and application | |
| CN110280281B (en) | Preparation method of zinc ferrite/black phosphorus microsphere compound and application of zinc ferrite/black phosphorus microsphere compound in photocatalysis field | |
| CN111203231A (en) | Indium zinc sulfide/bismuth vanadate composite material and preparation method and application thereof | |
| CN114618537B (en) | Red phosphorus/strontium titanate heterojunction photocatalyst, and preparation method and application thereof | |
| CN113813970B (en) | Bismuth vanadate/lead cesium bromide photocatalytic material with 2D/2D structure and application thereof | |
| Tan et al. | Photocatalytic syngas synthesis from CO 2 and H 2 O using ultrafine CeO 2-decorated layered double hydroxide nanosheets under visible-light up to 600 nm | |
| Huang et al. | A highly efficient and stable TiO2@ NH2-MIL-125 material for enhanced photocatalytic conversion of CO2 and CH4 | |
| CN114054068A (en) | Preparation method of h-BN-based catalyst for hydrogen production by photolysis of water | |
| CN112717958B (en) | Oxygen-rich vacancy BiOBr/HNb3O8Preparation method and application of nanosheet photocatalyst | |
| Liu et al. | g-C3N4/MnFe2O4 pn hollow stratified heterojunction to improve the photocatalytic CO2 reduction activity | |
| CN113546687A (en) | Preparation method and application of visible light catalyst of ultrathin titanium-based MOFs nanosheets | |
| Zhang et al. | Preparation of 2D WO3 nanomaterials and their catalytic performance during the synthesis of imines under visible light irradiation | |
| CN110639581B (en) | WP (total weight) 2 /g-C 3 N 4 Preparation method of heterojunction photocatalyst | |
| CN111871445A (en) | CN/BOS van der Waals heterostructure photocatalyst and preparation method thereof | |
| CN112495411A (en) | Carbon nitride nanosheet loaded indium vanadate quantum dot photocatalyst and preparation and application thereof | |
| CN116689006A (en) | Carbon nitride nano-sheet composite material and preparation method and application thereof | |
| CN114308126B (en) | K (K)4Nb6O17Micron flower/Co-TCPP MOF hydrogen evolution catalyst and preparation method and application thereof | |
| CN109289898A (en) | Cuprous quantum dot light catalysis material of graphite phase carbon nitride foam combined oxidation and preparation method thereof | |
| Wang et al. | Recent progress of MXene as a cocatalyst in photocatalytic carbon dioxide reduction |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20221101 |