CN116266998A - Method for preparing stable perovskite on paper base - Google Patents
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- 238000000034 method Methods 0.000 title claims abstract description 23
- 239000002243 precursor Substances 0.000 claims abstract description 36
- 239000002904 solvent Substances 0.000 claims abstract description 17
- FZHAPNGMFPVSLP-UHFFFAOYSA-N silanamine Chemical compound [SiH3]N FZHAPNGMFPVSLP-UHFFFAOYSA-N 0.000 claims abstract description 8
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 15
- WYTZZXDRDKSJID-UHFFFAOYSA-N (3-aminopropyl)triethoxysilane Chemical compound CCO[Si](OCC)(OCC)CCCN WYTZZXDRDKSJID-UHFFFAOYSA-N 0.000 claims description 10
- 239000000758 substrate Substances 0.000 claims description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 8
- 239000002033 PVDF binder Substances 0.000 claims description 7
- 229920002981 polyvinylidene fluoride Polymers 0.000 claims description 7
- WWZKQHOCKIZLMA-UHFFFAOYSA-N octanoic acid Chemical compound CCCCCCCC(O)=O WWZKQHOCKIZLMA-UHFFFAOYSA-N 0.000 claims description 6
- 239000012528 membrane Substances 0.000 claims description 4
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 2
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 2
- ZYAASQNKCWTPKI-UHFFFAOYSA-N 3-[dimethoxy(methyl)silyl]propan-1-amine Chemical compound CO[Si](C)(OC)CCCN ZYAASQNKCWTPKI-UHFFFAOYSA-N 0.000 claims description 2
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 claims description 2
- 239000000020 Nitrocellulose Substances 0.000 claims description 2
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 2
- 239000005642 Oleic acid Substances 0.000 claims description 2
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 2
- 229920001220 nitrocellulos Polymers 0.000 claims description 2
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 6
- 239000002086 nanomaterial Substances 0.000 abstract description 4
- 239000013078 crystal Substances 0.000 description 8
- 150000004820 halides Chemical class 0.000 description 8
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- 239000002159 nanocrystal Substances 0.000 description 5
- 239000002096 quantum dot Substances 0.000 description 5
- 230000007613 environmental effect Effects 0.000 description 4
- 238000002360 preparation method Methods 0.000 description 4
- 238000001878 scanning electron micrograph Methods 0.000 description 4
- QBVXKDJEZKEASM-UHFFFAOYSA-M tetraoctylammonium bromide Chemical compound [Br-].CCCCCCCC[N+](CCCCCCCC)(CCCCCCCC)CCCCCCCC QBVXKDJEZKEASM-UHFFFAOYSA-M 0.000 description 4
- 229910004298 SiO 2 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 229910052792 caesium Inorganic materials 0.000 description 2
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 230000007062 hydrolysis Effects 0.000 description 2
- 238000006460 hydrolysis reaction Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000010791 quenching Methods 0.000 description 2
- 230000000171 quenching effect Effects 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
- 229910002808 Si–O–Si Inorganic materials 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- FJDQFPXHSGXQBY-UHFFFAOYSA-L caesium carbonate Chemical compound [Cs+].[Cs+].[O-]C([O-])=O FJDQFPXHSGXQBY-UHFFFAOYSA-L 0.000 description 1
- 229910000024 caesium carbonate Inorganic materials 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002798 polar solvent Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 229910000077 silane Inorganic materials 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E10/00—Energy generation through renewable energy sources
- Y02E10/50—Photovoltaic [PV] energy
- Y02E10/549—Organic PV cells
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- Chemical & Material Sciences (AREA)
- Nanotechnology (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention relates to a method for preparing perovskite on a paper base, belonging to the field of nano materials. The method comprises the following steps: (1) preparing a solution a of a perovskite precursor I; (2) Preparing a perovskite precursor II, a perovskite precursor II solvent and an aminosilane solution b; (3) Dropping the solution b on the surface of the paper base, then dropping the solution a on the surface of the paper base at the same position, and volatilizing the solvent to obtain perovskite nanocrystalline growing on the paper base; the perovskite precursor I is selected from Cs 2 CO 3 At least one of MABr; the perovskite precursor II is selected from PbBr 2 、PbI 2 At least one of them. The invention provides a novel, simple, quick, efficient and low-cost in-situ methodMethods of growing and protecting perovskite.
Description
Technical Field
The invention relates to the field of nano materials, in particular to a method for preparing stable perovskite on a paper base.
Background
In recent years, perovskite nano materials are attracting attention and research due to their excellent photoelectric properties. The perovskite nano material has the advantages of high fluorescence quantum efficiency (PLQY), wide adjustable range of emission wavelength, excellent photoelectric transmission performance, simple synthesis, low cost and the like, has good application prospect in the fields of photoelectric devices and sensing, and is one of hot spots for research when perovskite is prepared on a paper base.
The paper base is used as a carrier, so that the perovskite can be widely and conveniently applied, for example, the perovskite is used for constructing a paper base sensor, the detection time is greatly shortened, and a user-friendly portable sensor is developed for online monitoring. However, the perovskite quantum dots are greatly affected by the environment, the stability is poor, and because the perovskite belongs to ionic crystals, factors such as air, humidity, temperature, polar solvents and the like can lead to the reduction of the luminous efficiency of the perovskite quantum dots, even complete quenching. Stability has been a major impediment to its commercial use.
To improve the stability of perovskite in the environment, doping, polymer encapsulation, silica (SiO 2 ) Wrapping, etc. have been reported, in which SiO 2 Is a common way to stabilize perovskite in perovskite LED manufacture, and perovskite quantum dots are generally embedded in SiO formed by silane hydrolysis 2 In the matrix, the obtained SiO 2 The coated perovskite quantum dots can maintain long-term stability in air and have high fluorescence quantum yield. However, this way of protecting perovskite is generally performed in solution, and further research is required on how to protect perovskite on paper, and the lack of such research results in that paper-based perovskite sensors suffer from unstable properties and extremely short shelf life, which greatly limits the application of perovskite in the sensing field.
Disclosure of Invention
The invention aims to overcome the defects of the existing method for growing perovskite on a paper base, and provides a method capable of growing perovskite nanocrystals on the paper base in situ and having good environmental stability.
According to one aspect of the present invention there is provided a method of preparing a stable perovskite on a paper substrate comprising the steps of:
(1) Preparing a solution a of a perovskite precursor I;
(2) Preparing a perovskite precursor II, a perovskite precursor II solvent and an aminosilane solution b;
(3) Dropping the solution b on the surface of the paper base, then dropping the solution a on the surface of the paper base at the same position, and volatilizing the solvent to obtain perovskite nanocrystalline;
the perovskite precursor I is selected from Cs 2 CO 3 At least one of MABr;
the perovskite precursor II is selected from PbBr 2 、PbI 2 At least one of them.
Optionally, the volume ratio of the solution a to the solution b is 1:10-10:1.
Optionally, the volume ratio of the solution a to the solution b is selected from 1:1, 1:2, 1:3, 1:5, 1:6, 1:8, 1:9, 2:1, 2:3, 2:5, 2:8, 2:9, 3:1, 3:4, 3:7, 3:10, 5:1, 5:3, 5:7, 5:9, 8:3, 8:5, 8:7, 8:9, 9:1, 9:2, 9:5, 9:8, or any value between any two of the above.
Optionally, the aminosilane is selected from at least one of 3-aminopropyl triethoxysilane (APTES), 3-aminopropyl methyldimethoxysilane;
the volume fraction of the aminosilane in the solution b is 1% -10%.
Optionally, the volume fraction of the aminosilane in solution b is selected from 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, or any value between any two of the above.
Optionally, the perovskite precursor II solvent is selected from at least one of toluene and n-hexane.
Preferably, when the perovskite precursor ii is selected from the group consisting of halides, the perovskite precursor ii solvent has the same halogen as the perovskite precursor ii.
Optionally, in the solution a, the molar concentration of the perovskite precursor I is 0.05-0.2 mmol/L;
in the solution b, the molar concentration of the perovskite precursor II is 0.05-0.2 mmol/L; the molar concentration of the perovskite precursor II solvent is 0.1-0.3 mmol/L.
Optionally, the solvent of the solution a is selected from at least one of n-octanoic acid and oleic acid; the solvent of the solution b is at least one selected from toluene, normal hexane and cyclohexane.
Optionally, the paper base is selected from one of filter paper, nitrocellulose membrane, polyvinylidene fluoride (PVDF) membrane.
According to one aspect of the present invention, there is provided a paper-based sensor employing a paper-based with perovskite grown thereon; the paper base with the perovskite grown thereon is prepared by the method.
The application has at least the following advantages and beneficial effects:
1. compared with the reported preparation method of paper-based perovskite, the preparation method of the invention has the advantages of simple operation and extremely small amount of required organic solvent, and the prepared perovskite can stably exist in the air for 50 days without vacuum or inert gas protection and has certain moisture resistance.
2. APTES can be rapidly hydrolyzed by utilizing the existence of water molecules in the air, and SiO is rapidly generated in a precursor solution of perovskite 2 The network and the perovskite can nucleate and grow in the network, so that the protection is provided for perovskite crystals to the greatest extent, the damage of an induced crystal structure caused by oxygen, humidity and the like in the environment is avoided, meanwhile, the aggregation quenching in the crystal growth process is avoided due to the existence of the network, and the high PLQY of the perovskite on a paper base is stabilized from the other layer.
3. The invention provides a simple, quick, efficient and low-cost method for preparing stable perovskite on a paper base, which provides a basis for the stable existence of perovskite quantum dots on the paper base.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are needed in the description of the embodiments will be briefly described below, it being obvious that the drawings in the following description are only some embodiments of the present invention, and that other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is a graph of UV-visible and fluorescence spectra of paper-based perovskite according to example 1 of the present invention.
Fig. 2 is an XRD pattern of the paper-based perovskite of example 2 of the present invention.
FIG. 3 is an infrared spectrum of a paper-based perovskite according to example 3 of the present invention.
In fig. 4, (a) is an SEM image of a blank paper base, and (b) is an SEM image of a paper base perovskite according to example 3 of the present invention.
In fig. 5, (a) is a humidity test result, and (b) is a stability test result.
Detailed Description
The foregoing objects, features and advantages of the invention will be more readily apparent from the following detailed description of the invention. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, and the present invention will fully be described in such detail in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein, but may be similarly practiced by those skilled in the art without departing from the spirit or scope of the invention. The scope of the invention is not limited to the embodiments mentioned herein.
Example 1
The embodiment provides a method capable of growing perovskite nanocrystals on a paper substrate in situ and having good environmental stability, which comprises the following specific steps:
step (1): cs is processed by 2 CO 3 (cesium carbonate) is dissolved in n-octanoic acid to obtain cesium precursor solution of perovskite, pbBr is prepared 2 Dissolving TOAB and APTES in toluene to obtain a lead halide precursor solution of perovskite;
Cs 2 CO 3 is 0.1mmol/L, pbBr 2 The molar concentration of APTES in the lead halide precursor solution of perovskite was 5%, and the molar concentration of TOAB was 0.1mM/mL, and the molar concentration of TOAB was 0.2 mM/mL;
step (2): sucking 1 mu L of cesium precursor solution of perovskite to drop on the surface of a PVDF film, sucking 2 mu L of lead halide precursor solution of perovskite to drop on the surface of a paper base at the same position, and volatilizing the solvent to obtain the perovskite nanocrystalline grown in situ on the paper base.
The ultraviolet-visible and fluorescence spectra of the paper-based perovskite prepared above are shown in fig. 1, and the results show that the characteristic absorption peak is located at 510nm, the phase transition is not generated, the characteristic emission is located at 518nm, the half-peak width is 21nm, the monochromaticity is good, and the synthesized crystal size is uniform.
Example 2
The present example proposes a method capable of growing perovskite nanocrystals on paper substrates in situ and having good environmental stability, the preparation method being the same as in example 1, with the difference that:
(1) the solvent of the lead halide precursor solution of the perovskite in the step (1) is n-hexane; the volume fraction of APTES in the lead halide precursor solution of the perovskite was 10%;
(2) the volume of the lead halide precursor solution that aspirates the perovskite in step (2) is 1 μl.
XRD of the paper-based perovskite prepared above is shown in FIG. 2, and the result shows that CsPbBr is generated 3 Cubic phase crystals, diffraction peaks of 15.2 °, 21.5 °, 30.8 ° and 34.5 ° respectively corresponding to CsPbBr were observed compared with a blank PVDF film 3 The (100), (110), (200), and (210) planes of the crystal, the network of silica does not cause phase transformation of the perovskite crystal, and good crystallinity and phase stability are maintained.
Example 3
The present example proposes a method capable of growing perovskite nanocrystals on paper substrates in situ and having good environmental stability, the preparation method being the same as in example 1, with the difference that:
(1) PbBr in step 1 2 TOAB concentrations were 0.05mM/mL and 0.1mM/mL, respectively;
(2) the volume fraction of APTES in the lead halide precursor solution of the perovskite was 6%.
The infrared spectrogram of the prepared paper-based perovskite is shown in FIG. 3, and the result shows that the paper-based perovskite is matched with a blank1107cm compared to PVDF film -1 Can be attributed to the Si-O-C stretching vibration, and 1033cm -1 The absorption at this point can be categorized as an antisymmetric stretching vibration of Si-O-Si, which can be indicative of successful hydrolysis of APTES.
In fig. 4, (a) is an SEM image of a blank paper substrate, and (b) is an SEM image of a paper-based perovskite of the present embodiment, it can be seen by comparing (a) with (b) that the composite of perovskite nanocrystals and silica grown on the paper substrate does not change the porous structure of the paper substrate, but maintains the porous structure so that the paper substrate has potential for gas sensing, providing a concept for the subsequent application of the paper-based perovskite.
Fig. 5a shows the results of a paper-based perovskite resistance test to water vapour in the humidity range of 70% to 90%, with half an hour of full contact maintained at each humidity condition, indicating good resistance to humidity. In an air environment, the material shows more stable property, as shown in fig. 5b, the fluorescence intensity is not obviously reduced in the unprotected storage process of 50 days, which indicates that the prepared material has good stability.
Claims (8)
1. A method for preparing perovskite on paper substrate, comprising the steps of:
(1) Preparing a solution a of a perovskite precursor I;
(2) Preparing a perovskite precursor II, a perovskite precursor II solvent and an aminosilane solution b;
(3) Dropping the solution b on the surface of the paper base, then dropping the solution a on the surface of the paper base at the same position, and volatilizing the solvent to obtain perovskite nanocrystalline;
the perovskite precursor I is selected from Cs 2 CO 3 At least one of MABr;
the perovskite precursor II is selected from PbBr 2 、PbI 2 At least one of them.
2. The method according to claim 1, wherein the volume ratio of the solution a to the solution b is 1:10 to 10:1.
3. The method according to claim 1, wherein the aminosilane is selected from at least one of 3-aminopropyl triethoxysilane (APTES), 3-aminopropyl methyldimethoxysilane;
the volume fraction of the aminosilane in the solution b is 1% -10%.
4. The method according to claim 1, wherein the perovskite precursor ii solvent is selected from at least one of toluene, n-hexane.
5. The method according to claim 1, wherein the molar concentration of the perovskite precursor i in the solution a is 0.05-0.2 mmol/L;
in the solution b, the molar concentration of the perovskite precursor II is 0.05-0.2 mmol/L; the molar concentration of the perovskite precursor II solvent is 0.1-0.3 mmol/L.
6. The method according to claim 1, wherein the solvent of the solution a is selected from at least one of n-octanoic acid, oleic acid; the solvent of the solution b is at least one selected from toluene, normal hexane and cyclohexane.
7. The method of claim 1, wherein the paper substrate is selected from one of filter paper, nitrocellulose membrane, polyvinylidene fluoride (PVDF) membrane.
8. A paper-based sensor characterized by using a paper-based with perovskite grown thereon; the paper base with perovskite grown thereon is prepared by the method of any one of claims 1 to 7.
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