CN112029500A - Method for preparing bromine-iodine doped perovskite nanowire through solvent-mediated nanocrystal self-assembly - Google Patents
Method for preparing bromine-iodine doped perovskite nanowire through solvent-mediated nanocrystal self-assembly Download PDFInfo
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Abstract
A method for preparing bromine-iodine doped perovskite nano-wires by solvent-mediated nano-crystal self-assembly comprises the steps of firstly preparing well-dispersed bromine-iodine doped nano-crystals by a thermal injection method, adding a proper amount of toluene solvent after centrifugal separation for purification and separation again, finally dissolving in a certain amount of toluene solvent, standing for 6-10 days at low temperature in a dark place, and standing in the solvent for 6-10 daysThe nano-crystal is self-assembled into a one-dimensional single-crystal nano-wire through the coordination of the interaction between the solvent and the ligand and the interaction between the ligands. CsPbBr prepared by liquid phase method1.2I1.8The diameter of the one-dimensional single crystal nanowire is 30-100nm, the surface is smooth, and the length can reach several micrometers to dozens of micrometers. The method has the excellent characteristics of simple and convenient operation, high repeatability, high crystal quality, controllable appearance, size and height and the like. CsPbBr1.2I1.8The one-dimensional single crystal nanowire has higher polarization anisotropy ratio due to the extremely high aspect ratio, and has good application prospect in the aspects of polarized fluorescent materials and polarization sensitive photoelectric detectors.
Description
Technical Field
The invention relates to preparation of a nano material, in particular to a method for preparing a bromine-iodine doped perovskite nanowire by solvent-mediated nanocrystal self-assembly.
Background
The perovskite material as a star material has many excellent properties, such as low Ulbach energy, small Stokes displacement, high carrier mobility, long exciton diffusion length, large absorption coefficient and the like; thus, it is often used as a gain medium and a photovoltaic material. The quantum dot nanocrystalline morphology of perovskites has also been widely studied due to its quantum confinement effect and quantum size effect. When the concentration of the quantum dots in the solution reaches a certain value, the quantum dots are spontaneously arranged together in order according to a certain rule through van der waals force, electrostatic action and the like to form a long-range ordered nano structure, namely self-assembly.
Self-assembly is ubiquitous in nature and has now become a method of engineering and controlling performance on the nanometer scale. Colloidal nanocrystals self-assemble into ordered nanostructures of one, two, or three dimensions, which brings many exciting application prospects. The ligand on the surface of the nanocrystal plays a key role in the self-assembly process, and the arrangement of the nanocrystal is strongly influenced in a solvent through the delicate balance between the interaction of the ligand and the interaction of the ligand and the solvent. There are also many studies on the self-assembly of nanocrystals: the Self-Assembly of colloidal Pt nanoparticles into two different types of ordered Superlattices, simple cubic and volume-centered tetragonal structures, is described in Solvent-media Self-Assembly of Nanocube superlatices, J.AM.chem.Soc.2014,136, 1352-1359; the Road from Particles to Colloidal Molecules and Crystals, Angew. chem. int. Ed.2011,50, 360-.
The morphological features and unique properties exhibited by one-dimensional nanostructures as compared to bulk materials are advantageous in a number of important applications. For example, elongated shaped nanorods are highly attractive for optoelectronic and photocatalytic applications because it facilitates charge transport and efficiently facilitates charge separation. At the same time, nanowires with high aspect ratios are considered to be a powerful nanomaterial, providing a great number of opportunities for the fabrication of new electronic, optoelectronic and sensing devices. There are also some literature reports on the research and application of one-dimensional nanowires: the Crystagonographical Aligned Perovskite Structures for High-Performance Polarization-Sensitive photonic devices, adv. Mater.2017,29,1605993 article describes a template method for controlling the growth and crystal arrangement of Perovskite single crystals and shows the application of the Perovskite single crystals in High-Performance Photodetectors; and wavelet Sensitivity of Single Nanofire amplification Polarization of doped through a Generalized Treatment of the same Linear Absorption, ACS NANO 2009,3,1979-1987 studied the induced Polarization anisotropy of individual semiconductor nanowires by solution chemistry, as well as similar wires made by chemical vapor deposition, and monitored the band edge emission above 680nm to elucidate the origin of Their strong Polarization response.
Disclosure of Invention
The invention aims to provide nanocrystalline self-assembly bromine-iodine doping with simple operation, convenience, high efficiency and controllable sizeA method of perovskite nanowires. The prepared one-dimensional CsPbBr1.2I1.8The nanowires are relatively uniform in diameter and between a few microns and tens of microns in length. The preparation method has the advantages of simple process, high yield, good repeatability, controllable size and good quality. The one-dimensional ultrafine nanowires are beneficial to charge transmission, have extremely high aspect ratio, and provide a great deal of opportunity for manufacturing novel electronic, photoelectric and sensing equipment. The one-dimensional all-inorganic bromine-iodine doped nanowire prepared by the method has larger fluorescence polarization degree, and has bright prospect of being used as a fluorescence polarization material and used for a polarization sensitive photoelectric detector.
The technical solution of the invention is as follows:
CsPbBr3The preparation method of the perovskite three-dimensional cubic microcavity sample is characterized by comprising the following steps:
(1) weighing 200mg of cesium carbonate powder in a three-neck flask, adding 7.5ml of octadecene and 1ml of oleic acid, uniformly mixing, continuously stirring and heating the mixture to 110-120 ℃, and naturally cooling to room temperature to obtain a cesium oleate precursor;
(2) 27.6mgPbBr was weighed in a molar ratio of 2:32And 51.6mgPbI2Putting the powder into a three-neck flask, adding 5ml of octadecene, 0.05ml of long carbon chain ligand oleic acid and 0.5ml of long carbon chain ligand oleylamine, and fully stirring and uniformly mixing; slowly heating to 160-175 ℃, stopping heating, quickly injecting the cesium oleate precursor, standing for 5-10s, putting the three-neck flask into an ice-water mixture, and quickly cooling to room temperature to obtain the product CsPbBr1.2I1.8A quantum dot colloid;
(3) for the obtained CsPbBr1.2I1.8Performing centrifugal separation and purification on the quantum dot colloid, setting the rotating speed of a centrifuge to 10000rmp-12000rmp, and setting the time to 3 min; sucking out the supernatant liquid after centrifugation by using a liquid transfer gun, adding a toluene solvent, and centrifuging again at a constant rotating speed for 1 min; removing the supernatant, and absorbing the residual trace liquid with cotton swab; finally, the obtained precipitate is dissolved in a certain amount of toluene solvent.
(4) Will obtainCsPbBr of1.2I1.8Putting the quantum dot toluene solution into a reagent bottle with good brown light-tight tightness, standing for 6-10 days in a low-temperature environment, and dropwise adding a proper amount of CsPbBr1.2I1.8And depositing the quantum dot toluene solution on a deposition sheet to obtain the one-dimensional single crystal nanowire structure.
The heating steps in (1) and (2) are carried out under the protection of nitrogen.
In the step (2), the temperature is kept at 100 ℃ for 20min before the temperature is slowly raised to 160-175 ℃.
And (4) the deposition sheet in the step (4) is a sapphire sheet, a monocrystalline silicon sheet or a quartz sheet, and the dropwise addition amount of the solution is 30 uL.
Compared with the prior art, the invention has the following technical effects:
the dosage proportion of oleic acid oleylamine ligand, nitrogen flow rate, heating rate, reaction temperature and standing time in the self-assembly process can influence one-dimensional CsPbBr1.2I1.8Morphology and dimensional quality of all-inorganic perovskite nanowires. Various parameters are adjusted within a certain range to control the appearance and the size of the product, so that the controllable synthesis of the product is realized.
The prepared one-dimensional CsPbBr1.2I1.8The full inorganic perovskite nanowire has smooth surface, uniform diameter and good quality, and the length is between several micrometers and tens of micrometers.
The preparation method has the advantages of simple process, high yield, good repeatability, controllable size and good quality. The one-dimensional ultrafine nanowires are beneficial to charge transmission, have extremely high aspect ratio, and provide a great deal of opportunity for manufacturing novel electronic, photoelectric and sensing equipment. The one-dimensional all-inorganic bromine-iodine doped nanowire prepared by the method has larger fluorescence polarization degree, and has bright prospect of being used as a fluorescence polarization material and used for a polarization sensitive photoelectric detector.
Drawings
FIGS. 1a and b show CsPbBr of the present invention1.2I1.8Scanning Electron Microscope (SEM) picture of perovskite quantum dot nanocrystalline self-assembled one-dimensional nanowire, and figures 1c and d are CsPbBr of the invention1.2I1.8Self-assembly of perovskite quantum dot nanocrystalTransmission Electron Microscope (TEM) images of dimensional nanowires.
FIG. 2 shows CsPbBr in the present invention1.2I1.8Fluorescence (PL) spectra of perovskite quantum dot nanocrystals.
FIG. 3a shows CsPbBr of the present invention1.2I1.8Fluorescence spectrograms of different polarization states of the perovskite one-dimensional nanowire, wherein the solid line is a fluorescence spectrum with the polarization state parallel to the nanowire, and the dotted line is a fluorescence spectrum with the polarization state vertical to the nanowire; FIG. 3b shows CsPbBr of the present invention1.2I1.8Polarization polar coordinate diagram of perovskite one-dimensional nanowire.
Detailed Description
For CsPbBr1.2I1.8The preparation of the perovskite quantum dot nanocrystalline self-assembled one-dimensional nanowire is further explained, and the embodiment is implemented according to the technical scheme of the invention, and a specific implementation mode and a specific flow are given.
Example 1
(1) Weighing 200mg of cesium carbonate powder in a three-neck flask, adding 7.5ml of octadecene and 1ml of oleic acid, uniformly mixing, continuously stirring and heating the mixture to 110-120 ℃, and naturally cooling to room temperature to obtain a cesium oleate precursor;
(2) 27.6mgPbBr was weighed in a molar ratio of 2:32And 51.6mgPbI2Putting the powder into a three-neck flask, adding 5ml of octadecene, 0.05ml of long carbon chain ligand oleic acid and 0.5ml of long carbon chain ligand oleylamine, and fully stirring and uniformly mixing; slowly heating to 160-175 ℃, stopping heating, quickly injecting the cesium oleate precursor, standing for 5-10s, putting the three-neck flask into an ice-water mixture, and quickly cooling to room temperature to obtain the product CsPbBr1.2I1.8A quantum dot colloid;
(3) for the obtained CsPbBr1.2I1.8Performing centrifugal separation and purification on the quantum dot colloid, setting the rotating speed of a centrifuge to 10000rmp, and setting the time to 3 min; sucking out the supernatant liquid after centrifugation by using a liquid transfer gun, adding a toluene solvent, and centrifuging again at a constant rotating speed for 1 min; removing the supernatant, and absorbing the residual trace liquid with cotton swab; finally, the obtained sedimentThe precipitate was dissolved in a certain amount of toluene solvent.
(4) The obtained CsPbBr1.2I1.8Putting the quantum dot toluene solution into a brown opaque reagent bottle with good tightness, standing for 6-10 days in a low-temperature environment, and then dropwise adding 30uLCsPBBr1.2I1.8The quantum dot toluene solution is deposited on a monocrystalline silicon wafer with the thickness of 10mm multiplied by 10mm to obtain a one-dimensional monocrystalline nanowire structure with good appearance.
CsPbBr obtained in this example1.2I1.8The perovskite quantum dot nanocrystalline self-assembly one-dimensional nanowire is subjected to morphology observation through SEM and TEM, and the relevant results are shown in FIG. 1 in detail; FIG. 2 and FIG. 3 are CsPbBr, respectively1.2I1.8Fluorescence (PL) spectrogram of perovskite quantum dot nanocrystal and lattice distortion (phase change) of the perovskite quantum dot nanocrystal in toluene solvent form a fluorescence graph and a polarization polar coordinate graph of one-dimensional nanowire.
Example 2
This example mainly considers CsPbBr1.2I1.8In the preparation process of the perovskite quantum dot nanocrystalline self-assembly one-dimensional nanowire, the influence of the reaction temperature, the ligand oleic acid oleylamine ratio, the heating rate, the carrier gas rate and the standing time on the appearance and the size of the obtained sample. For the specific experimental procedures, refer to example 1, with the following differences: the reaction temperature, the ligand oleic acid oleylamine ratio, the heating rate, the carrier gas rate and the standing time were changed respectively, and the specific experimental parameters are shown in table 1.
TABLE 1 preparation of CsPbBr as described above3Experimental conditions of the perovskite three-dimensional cubic microcavity:
according to the experimental result, the temperature rise time and the carrier gas speed have almost no influence on the shape and the size of the sample. The change of the reaction temperature has great influence on the size uniformity and the appearance of the preliminarily prepared quantum dot nanocrystal; a relative proportion of ligand oleylamine oleate has a minor effect on the size of the resulting nanocrystals; the set standing time has a great influence on the self-assembly of the quantum dot nanocrystals into one dimension of the one-dimensional nanowire, and the length of the prepared nanowire tends to increase along with the increase of the standing time.
Example 3
This example examines CsPbBr obtained in example 11.2I1.8The one-dimensional single crystal nanowire has better fluorescence polarization performance and has the potential of being well applied to polarization fluorescent materials and polarization sensitive photodetectors.
The experimental equipment is an ultrafast transient spectrometer (model HR Evolution)&FLS 980). The specific experimental steps are as follows: firstly, a light path for detecting fluorescence polarization is built, and a broadband polaroid with the wavelength of 400-800nm and an 1/2 wave plate are arranged in front of a receiving light path of a laser, so that the polarization characteristic of the received light is detected; then horizontally placing the substrate containing the sample on a sample stage of a micro fluorescence spectrometer, adjusting the sample stage, and selecting CsPbBr under a microscope1.2I1.8A one-dimensional single crystal nanowire. A325 nm LASER (He-Cd LASER, CW,325nm, MAX,200mW) was turned on and the LASER was directed into the spectrometer. And adjusting a microscope lens, focusing the light spot to the minimum, and performing spectrum detection to obtain the fluorescence spectrum of the sample. Next, the polarization angle of the polarizing plate was continuously rotated to find an angle at which the fluorescence intensity was maximum, and the fluorescence peak at that time was recorded, and the fluorescence peak at that time was rotated to an angle at which the fluorescence intensity was minimum, and was recorded as shown in fig. 3(a), thereby calculating the degree of polarization. The intensity of the fluorescence peak at that time was then recorded every 15 ° rotation, and a polar graph showing the change in fluorescence intensity with the polarization angle was prepared as shown in fig. 3 (b).
Claims (5)
1. A method for preparing bromine-iodine doped perovskite nanowires through solvent-mediated nanocrystal self-assembly is characterized by comprising the following steps:
(1) weighing 200mg of cesium carbonate powder in a three-neck flask, adding 7.5ml of octadecene and 1ml of oleic acid, uniformly mixing, continuously stirring and heating the mixture to 110-120 ℃, and naturally cooling to room temperature to obtain a cesium oleate precursor;
(2) weighing according to the molar ratio of 2:3An amount of 27.6mgPbBr2And 51.6mgPbI2Putting the powder into a three-neck flask, adding 5ml of octadecene, 0.05ml of long carbon chain ligand oleic acid and 0.5ml of long carbon chain ligand oleylamine, and fully stirring and uniformly mixing; slowly heating to 160-175 ℃, stopping heating, quickly injecting the cesium oleate precursor, standing for 5-10s, putting the three-neck flask into an ice-water mixture, and quickly cooling to room temperature to obtain the product CsPbBr1.2I1.8A quantum dot colloid;
(3) for the obtained CsPbBr1.2I1.8Performing centrifugal separation and purification on the quantum dot colloid, sucking out the centrifuged supernatant by using a pipette gun, adding a toluene solvent for performing centrifugal separation again, removing the supernatant, absorbing the residual trace liquid by using a cotton swab, and finally dissolving the obtained precipitate in a certain amount of toluene solvent;
(4) the obtained CsPbBr1.2I1.8Putting the quantum dot toluene solution into a reagent bottle with good brown light-tight tightness, standing for 6-10 days in a low-temperature environment, and dropwise adding a proper amount of CsPbBr1.2I1.8And depositing the quantum dot toluene solution on a deposition sheet to obtain the one-dimensional single crystal nanowire structure.
2. The method for preparing bromine-iodine doped perovskite nanowires through solvent-mediated nanocrystalline self-assembly according to claim 1, wherein the heating steps in the steps (1) and (2) are carried out under the protection of nitrogen.
3. The method for preparing bromine-iodine doped perovskite nanowire through solvent-mediated nanocrystal self-assembly according to claim 1, wherein the temperature is maintained at 100 ℃ for 20min before slowly raising the temperature to 165 ℃ in the step (2).
4. The method for preparing the bromine-iodine doped perovskite nanowire through solvent-mediated nanocrystal self-assembly according to claim 1, wherein the deposition sheet in the step (4) is a sapphire sheet, a monocrystalline silicon sheet or a quartz sheet, and the CsPbBr is added dropwise1.2I1.8The amount of the quantum dot toluene solution was 30 uL.
5. The method for preparing the bromine-iodine doped perovskite nano-wire by the solvent-mediated nanocrystal self-assembly as claimed in claim 1, wherein the rotation speed of a centrifuge for the first separation in the centrifugal separation and purification is set to 10000rmp-12000rmp, and the time is set to 2-5 min; the rotation speed of the centrifuge for the second separation is 10000rmp-12000rmp, and the time is set to be 1-2 min.
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| CN115072768A (en) * | 2022-07-04 | 2022-09-20 | 广州医科大学 | CsPbI 3 Perovskite nanowire and preparation method and application thereof |
| CN115161025A (en) * | 2022-07-05 | 2022-10-11 | 中国科学院上海光学精密机械研究所 | Method for preparing superlattice microcavity by self-assembly of bromine-chlorine doped perovskite quantum dots |
| CN115627162A (en) * | 2022-11-14 | 2023-01-20 | 兰州城市学院 | Preparation method of high-stability overlong one-dimensional perovskite quantum dot array |
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| CN115072768A (en) * | 2022-07-04 | 2022-09-20 | 广州医科大学 | CsPbI 3 Perovskite nanowire and preparation method and application thereof |
| CN115161025A (en) * | 2022-07-05 | 2022-10-11 | 中国科学院上海光学精密机械研究所 | Method for preparing superlattice microcavity by self-assembly of bromine-chlorine doped perovskite quantum dots |
| CN115161025B (en) * | 2022-07-05 | 2024-07-23 | 中国科学院上海光学精密机械研究所 | Method for preparing superlattice microcavity by self-assembled bromine-chlorine doped perovskite quantum dots |
| CN115627162A (en) * | 2022-11-14 | 2023-01-20 | 兰州城市学院 | Preparation method of high-stability overlong one-dimensional perovskite quantum dot array |
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