CN111013613A - Metal-doped composite perovskite nanocrystal and preparation method and application thereof - Google Patents
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- CN111013613A CN111013613A CN201911079601.5A CN201911079601A CN111013613A CN 111013613 A CN111013613 A CN 111013613A CN 201911079601 A CN201911079601 A CN 201911079601A CN 111013613 A CN111013613 A CN 111013613A
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- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000002159 nanocrystal Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 15
- 239000002105 nanoparticle Substances 0.000 claims abstract description 22
- 230000001699 photocatalysis Effects 0.000 claims abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 9
- 239000002082 metal nanoparticle Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims description 39
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 22
- CPELXLSAUQHCOX-UHFFFAOYSA-N Hydrogen bromide Chemical compound Br CPELXLSAUQHCOX-UHFFFAOYSA-N 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 229910019131 CoBr2 Inorganic materials 0.000 claims description 10
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 6
- 230000009467 reduction Effects 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 4
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 4
- 239000001569 carbon dioxide Substances 0.000 claims description 4
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 4
- 229910001509 metal bromide Inorganic materials 0.000 claims description 4
- 239000003495 polar organic solvent Substances 0.000 claims description 4
- 239000007788 liquid Substances 0.000 claims description 3
- 229910021576 Iron(III) bromide Inorganic materials 0.000 claims description 2
- 229910021585 Nickel(II) bromide Inorganic materials 0.000 claims description 2
- 229910017052 cobalt Inorganic materials 0.000 claims description 2
- 239000010941 cobalt Substances 0.000 claims description 2
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- FEONEKOZSGPOFN-UHFFFAOYSA-K tribromoiron Chemical compound Br[Fe](Br)Br FEONEKOZSGPOFN-UHFFFAOYSA-K 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 3
- 238000000034 method Methods 0.000 claims 3
- 238000013032 photocatalytic reaction Methods 0.000 claims 2
- 239000007809 chemical reaction catalyst Substances 0.000 claims 1
- 239000013078 crystal Substances 0.000 abstract description 6
- 238000007146 photocatalysis Methods 0.000 abstract description 4
- 238000000975 co-precipitation Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 description 7
- 239000004065 semiconductor Substances 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000010521 absorption reaction Methods 0.000 description 4
- 230000003197 catalytic effect Effects 0.000 description 4
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 238000003917 TEM image Methods 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 2
- 238000005119 centrifugation Methods 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- JBRZTFJDHDCESZ-UHFFFAOYSA-N AsGa Chemical compound [As]#[Ga] JBRZTFJDHDCESZ-UHFFFAOYSA-N 0.000 description 1
- 229910001218 Gallium arsenide Inorganic materials 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000002211 ultraviolet spectrum Methods 0.000 description 1
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
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Abstract
The invention discloses a metal-doped composite perovskite nanocrystal and a preparation method and application thereof. The metal-doped composite perovskite nanocrystalline of the invention is composed of Cs with cubic crystal system structure4PbBr6Nanoparticles, embedded in Cs4PbBr6CsPbBr in nanoparticles3Nanoparticles and doped Cs4PbBr6The metal nanoparticles on the surfaces of the nanoparticles are composed of three parts, and the metal nanoparticles are prepared through coprecipitation reaction. The metal-doped composite perovskite nanocrystalline disclosed by the invention is strong in photocatalytic activity, high in stability, simple in preparation process and suitable for large-scale application in the field of photocatalysis.
Description
Technical Field
The invention relates to a metal-doped composite perovskite nanocrystal and a preparation method and application thereof.
Background
Nano-semiconductor materials generally refer to nano-materials made of semiconductor materials such as silicon, gallium arsenide, etc., which have many excellent properties, such as: the quantum tunnel effect in the nano semiconductor material makes the electron transport of some semiconductor materials abnormal and the conductivity reduced, and the electric conductivity coefficient of heat is reduced along with the reduction of the grain size, even negative.
The perovskite nanocrystal is a new nano semiconductor material, has the advantages of wide light absorption range, long carrier service life, bipolar charge transmission and the like, and is widely used for preparing high-efficiency solar cells, light emitting diodes, lasers, photoelectric detectors and the like. However, the existing perovskite nanocrystals generally have the defects of poor stability, low catalytic activity, inapplicability to the field of photocatalysis, and the like, and the preparation process is complex, the reaction conditions are harsh, the raw material utilization rate is low, and the actual application requirements are difficult to meet.
Therefore, it is necessary to develop a perovskite nanocrystal with good stability, strong photocatalytic activity and simple preparation process.
Disclosure of Invention
The invention aims to provide a metal-doped composite perovskite nanocrystal and a preparation method and application thereof.
The technical scheme adopted by the invention is as follows:
the metal doped composite perovskite nano crystal is formed from Cs with cubic crystal system structure4PbBr6Nanoparticles, embedded in Cs4PbBr6CsPbBr in nanoparticles3Nanoparticles and doped Cs4PbBr6The metal nanoparticles on the surface of the nanoparticles are composed of three parts.
Preferably, the particle size of the metal-doped composite perovskite nanocrystal is 20-120 nm.
Preferably, the metal nanoparticles are at least one of cobalt nanoparticles, iron nanoparticles and nickel nanoparticles.
The preparation method of the metal-doped composite perovskite nanocrystal comprises the following steps:
1) reacting PbBr2Dispersing in aqueous HBr solution to obtain solution A;
2) dispersing CsBr in an HBr aqueous solution to obtain a solution B;
3) the metal bromide CoBr2、FeBr3、NiBr2Is dispersed in a polar organic solvent to obtain a solution C;
4) keeping the temperature of the solution A at-5-0 ℃, dropwise adding the solution C while stirring, fully stirring after adding, dropwise adding the solution B while stirring, fully reacting after adding, performing solid-liquid separation, drying the solid obtained by separation,
obtaining the metal-doped composite perovskite nanocrystalline.
Preferably, the PbBr is2The molar ratio of CsBr to metal bromide is (0.25-2): 1: (0.008-0.012).
Preferably, the aqueous HBr solution obtained in steps 1) and 2) is 45-55% by mass.
Preferably, the polar organic solvent in step 3) is at least one of N, N-dimethylformamide and dimethyl sulfoxide.
Preferably, the reaction time in the step 4) is 2-4 h.
Preferably, the solid-liquid separation in the step 4) is centrifugation, the rotation speed of the centrifuge is 11000-12000 rpm, and the centrifugation time is 5-10 min.
Preferably, the drying in the step 4) is carried out at 75-85 ℃, and the drying time is 3-7 h.
The invention has the beneficial effects that: the metal-doped composite perovskite nanocrystalline disclosed by the invention is strong in photocatalytic activity, high in stability, simple in preparation process and suitable for large-scale application in the field of photocatalysis.
1) The metal-doped composite perovskite nanocrystalline of the invention is composed of Cs with cubic crystal system structure4PbBr6Nanoparticles, embedded in Cs4PbBr6CsPbBr in nanoparticles3Nanoparticles and doped Cs4PbBr6The metal nano particles on the surfaces of the nano particles are composed of three parts, so that the composite structure can improve the stability of the nano crystal material, the doping of the metal nano particles can obviously improve the photocatalytic activity of the nano crystal material, and the defect that the traditional perovskite nano crystal is not suitable for the field of photocatalysis is overcome.
2) The metal-doped composite perovskite nanocrystalline disclosed by the invention is simple in preparation process, mild in reaction conditions, high in raw material utilization rate and capable of being produced in a large scale.
Drawings
FIG. 1 shows CsPbBr of example 33/Cs4PbBr6XRD pattern of @ Co.
FIG. 2 shows CsPbBr of example 33/Cs4PbBr6@ Co.
FIG. 3 is CsPbBr of example 33/Cs4PbBr6TEM image of @ Co.
FIG. 4 shows CsPbBr of example 33/Cs4PbBr6XPS spectra for @ Co.
FIG. 5 shows CsPbBr of example 33/Cs4PbBr6@ Co is used for preparing a catalytic effect test chart of carbon monoxide by photocatalytic reduction of carbon dioxide.
Detailed Description
The invention will be further explained and illustrated with reference to specific examples.
Example 1:
a metal-doped composite perovskite nanocrystal and a preparation method thereof comprise the following steps:
1) reacting PbBr2Dispersing in HBr aqueous solution with mass fraction of 48 percent to prepare PbBr2Solution A with the concentration of 0.25 mol/L;
2) dispersing CsBr in HBr aqueous solution with mass fraction of 48% to prepare solution B with CsBr concentration of 1 mol/L;
3) adding CoBr2Dispersed in DMF to prepare CoBr2Solution C with the concentration of 0.01 mol/L;
4) keeping the temperature of the solution A at 0 ℃, dropwise adding the solution C with the same volume while stirring, stirring for 2min after adding, dropwise adding the solution B with the same volume while stirring, stirring for reaction for 3h after adding, centrifuging, drying the solid obtained by centrifuging at 80 ℃ for 5h to obtain the metal-doped composite perovskite nanocrystal (namely CsPbBr)3/Cs4PbBr6@Co)。
Example 2:
a metal-doped composite perovskite nanocrystal and a preparation method thereof comprise the following steps:
1) reacting PbBr2Dispersing in HBr aqueous solution with mass fraction of 48 percent to prepare PbBr2Solution A with the concentration of 0.5 mol/L;
2) dispersing CsBr in HBr aqueous solution with mass fraction of 48% to prepare solution B with CsBr concentration of 1 mol/L;
3) adding CoBr2Dispersed in DMF to prepare CoBr2Solution C with the concentration of 0.01 mol/L;
4) keeping the temperature of the solution A at 0 ℃, dropwise adding the solution C with the same volume while stirring, stirring for 2min after adding, dropwise adding the solution B with the same volume while stirring, stirring for reaction for 3h after adding, centrifuging, drying the solid obtained by centrifuging at 80 ℃ for 5h to obtain the metal-doped composite perovskite nanocrystal (namely CsPbBr)3/Cs4PbBr6@Co)。
Example 3:
a metal-doped composite perovskite nanocrystal and a preparation method thereof comprise the following steps:
1) reacting PbBr2Dispersing in HBr aqueous solution with mass fraction of 48 percent to prepare PbBr2Solution A with the concentration of 1 mol/L;
2) dispersing CsBr in HBr aqueous solution with mass fraction of 48% to prepare solution B with CsBr concentration of 1 mol/L;
3) adding CoBr2Dispersed in DMF to prepare CoBr2Solution C with the concentration of 0.01 mol/L;
4) keeping the temperature of the solution A at 0 ℃, dropwise adding the solution C with the same volume while stirring, stirring for 2min after adding, dropwise adding the solution B with the same volume while stirring, stirring for reaction for 3h after adding, centrifuging, drying the solid obtained by centrifuging at 80 ℃ for 5h to obtain the metal-doped composite perovskite nanocrystal (namely CsPbBr)3/Cs4PbBr6@Co)。
Example 4:
a metal-doped composite perovskite nanocrystal and a preparation method thereof comprise the following steps:
1) reacting PbBr2Dispersing in HBr aqueous solution with mass fraction of 48 percent to prepare PbBr2Solution A with the concentration of 2 mol/L;
2) dispersing CsBr in HBr aqueous solution with mass fraction of 48% to prepare solution B with CsBr concentration of 1 mol/L;
3) adding CoBr2Dispersed in DMF to prepare CoBr2Concentration of0.01mol/L of solution C;
4) keeping the temperature of the solution A at 0 ℃, dropwise adding the solution C with the same volume while stirring, stirring for 2min after adding, dropwise adding the solution B with the same volume while stirring, stirring for reaction for 3h after adding, centrifuging, drying the solid obtained by centrifuging at 80 ℃ for 5h to obtain the metal-doped composite perovskite nanocrystal (namely CsPbBr)3/Cs4PbBr6@Co)。
And (3) performance testing:
tested, CsPbBr of examples 1-43/Cs4PbBr6@ Co has similar structure and performance, so only CsPbBr of example 3 is described below3/Cs4PbBr6The structural characterization and application effect test results of @ Co were analyzed in detail.
1) CsPbBr of example 33/Cs4PbBr6The XRD pattern of @ Co is shown in FIG. 1.
As can be seen from fig. 1: CsPbBr3The diffraction peak of (A) is very weak, because CsPbBr3A large amount of Cs is wrapped around4PbBr6Influence on CsPbBr3The test of diffraction peak proves CsPbBr3Is embedded in Cs4PbBr6In cubic crystals.
2) CsPbBr of example 33/Cs4PbBr6The UV spectrum of @ Co is shown in FIG. 2.
As can be seen from fig. 2: absorption at 320nm is Cs4PbBr6Characteristic absorption of (1), absorption at 505nm is CsPbBr3And Cs4PbBr6Characteristic absorption of the interaction of the two crystals.
3) CsPbBr of example 33/Cs4PbBr6TEM images of @ Co are shown in FIG. 3.
As can be seen from fig. 3: CsPbBr3(black dots) embedded in Cs4PbBr6In cubic crystals.
4) CsPbBr of example 33/Cs4PbBr6XPS spectra for @ Co are shown in FIG. 4.
As can be seen from fig. 4: the Co 2p peak of the metal Co can be observed, and the fact that the metal Co is doped on the surface of the composite perovskite nanocrystal is proved.
5) CsPbBr of example 33/Cs4PbBr6The test chart of the catalytic effect of @ Co in preparing carbon monoxide by photocatalytic reduction of carbon dioxide is shown in FIG. 5.
As can be seen from fig. 5: CsPbBr3/Cs4PbBr6@ Co has high catalytic activity for the reaction of preparing carbon monoxide by photocatalytic reduction of carbon dioxide.
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 (10)
1. A metal-doped composite perovskite nanocrystal characterized by: cs of cubic system structure4PbBr6Nanoparticles, embedded in Cs4PbBr6CsPbBr in nanoparticles3Nanoparticles and doped Cs4PbBr6The metal nanoparticles on the surface of the nanoparticles are composed of three parts.
2. The metal-doped composite perovskite nanocrystal of claim 1, wherein: the particle size of the metal-doped composite perovskite nanocrystal is 20-120 nm.
3. The metal-doped composite perovskite nanocrystal according to claim 1 or 2, characterized in that: the metal nanoparticles are at least one of cobalt nanoparticles, iron nanoparticles and nickel nanoparticles.
4. A method for preparing a metal-doped composite perovskite nanocrystal as claimed in any one of claims 1 to 3, characterized in that: the method comprises the following steps:
1) reacting PbBr2Dispersing in aqueous HBr solution to obtain solution A;
2) dispersing CsBr in an HBr aqueous solution to obtain a solution B;
3) the metal bromide CoBr2、FeBr3、NiBr2Is dispersed in a polar organic solvent to obtain a solution C;
4) and keeping the temperature of the solution A at-5-0 ℃, dropwise adding the solution C while stirring, fully stirring after adding, dropwise adding the solution B while stirring, fully reacting after adding, performing solid-liquid separation, and drying the solid obtained by separation to obtain the metal-doped composite perovskite nanocrystal.
5. The method of claim 4, wherein: the PbBr is2The molar ratio of CsBr to metal bromide is (0.25-2): 1: (0.008-0.012).
6. The production method according to claim 4 or 5, characterized in that: the HBr aqueous solution in the steps 1) and 2) is 45-55% of HBr aqueous solution in mass fraction.
7. The production method according to claim 4 or 5, characterized in that: and 3) the polar organic solvent is at least one of N, N-dimethylformamide and dimethyl sulfoxide.
8. The production method according to claim 4 or 5, characterized in that: and 4) the reaction time in the step 4) is 2-4 h.
9. Use of the metal-doped composite perovskite nanocrystal of any one of claims 1 to 3 for preparing a photocatalytic reaction catalyst.
10. Use according to claim 9, characterized in that: the photocatalytic reaction is a reaction for preparing carbon monoxide by photocatalytic reduction of carbon dioxide.
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| CN113636588A (en) * | 2020-04-27 | 2021-11-12 | 南京大学 | Cs4PbBr6Nanocrystalline of analogue thereof and preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109516496A (en) * | 2018-12-18 | 2019-03-26 | 江南大学 | A kind of full-inorganic perovskite CsPbBr of stable dispersion3Nanocrystalline preparation method |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109516496A (en) * | 2018-12-18 | 2019-03-26 | 江南大学 | A kind of full-inorganic perovskite CsPbBr of stable dispersion3Nanocrystalline preparation method |
Non-Patent Citations (1)
| Title |
|---|
| YAN-FEI MU: "Water-Tolerant Lead Halide Perovskite Nanocrystals as Efficient Photocatalysts for Visible-Light-Driven CO2 Reduction in Pure Water", 《CHEMSUSCHEM》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113636588A (en) * | 2020-04-27 | 2021-11-12 | 南京大学 | Cs4PbBr6Nanocrystalline of analogue thereof and preparation method |
| CN113636588B (en) * | 2020-04-27 | 2022-10-14 | 南京大学 | Cs 4 PbBr 6 Nanocrystalline of analogue thereof and preparation method |
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