CN113149066A - CsPbI3 nanocrystal synthesis method - Google Patents
CsPbI3 nanocrystal synthesis method Download PDFInfo
- Publication number
- CN113149066A CN113149066A CN202110424546.XA CN202110424546A CN113149066A CN 113149066 A CN113149066 A CN 113149066A CN 202110424546 A CN202110424546 A CN 202110424546A CN 113149066 A CN113149066 A CN 113149066A
- Authority
- CN
- China
- Prior art keywords
- cspbi3
- nanocrystal
- precursor
- iodide
- csco3
- 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.)
- Pending
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/006—Compounds containing, besides lead, two or more other elements, with the exception of oxygen or hydrogen
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/16—Halides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Nanotechnology (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Manufacturing & Machinery (AREA)
- Composite Materials (AREA)
- Materials Engineering (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention relates to a CsPbI3 nanocrystal synthesis method, which comprises the following steps: ultrasonically dissolving PbI2 and tetrahexyl ammonium iodide in toluene to obtain a Pb precursor; dissolving cesium carbonate CsCO3 in caprylic acid to obtain a CsCO3 precursor; ultrasonically dissolving oleylamine iodide in a toluene solution, injecting a CsCO3 precursor into a lead precursor by using an injector, stirring for reaction, adding the oleylamine iodide toluene solution, and stirring for the second time to obtain a CsPbI3 nanocrystal stock solution; adding ethyl acetate into CsPbI3 nanocrystal stock solution, centrifuging to obtain precipitate, dispersing the precipitate by using normal hexane to obtain CsPbI3 nanocrystal, centrifuging to remove supernatant, dispersing the precipitate CsPbI3 nanocrystal stock solution by using an organic solvent to obtain CsPbI3 nanocrystal.
Description
Technical Field
The invention relates to the technical field of quantum dot materials, in particular to a CsPbI3 nanocrystal synthesis method.
Background
In recent years, nanocrystalline materials are materials composed of crystals having a nanometer size (1 to 10 nm). Since the crystals are extremely fine, the grain boundaries may account for 50% or more of the entire material. Their atomic arrangement differs from ordered crystalline states and from disordered amorphous states (glassy states). Its properties are also different from those of a crystal or amorphous of the same composition.
The preparation process comprises the following steps: the material is thermally evaporated in inert gas (0.1-1 kPa), and then condensed into nano-scale crystals, and the fine powder is scraped down and compacted. Instead of thermal evaporation, a sputtering method, an electron gun or a laser method may be used. The nano-scale crystal can also be prepared by ball milling, gas phase synthesis or gel decomposition and other methods. Is a hot spot of current material science. The nanocrystalline material has incomparable performance compared with the conventional material due to the superfine characteristic. Nanocrystalline metal powders are insulators due to the metal-insulator transition effect caused by size. The nanometer powder can be used for preparing a long and thin conductive tunnel by a thick film technology, and can also be used as a dispersed phase of a high-dispersion material taking ceramic or high polymer materials as a matrix, which is widely applied in the field of high-frequency technology. The porous nano material sintered body has extremely strong activity and is suitable for being used as a catalyst and a high-power capacitor. The compact nano material is obtained by pressing nano powder into a compact at room temperature under very high pressure and then sintering at 100-200 ℃, and residual pores can tend to be zero. Due to its high grain boundary density, the strength can be increased by an order of magnitude.
As the size of the ultrafine grain is reduced, under certain conditions, the change of macroscopic physical, chemical, mechanical and other properties of the material is caused, and the change is generally called small-size effect. In addition, since the size of nanoparticles is small and the surface energy is high, which is called the surface effect of nanoparticles, it means that the ratio of the number of surface atoms to the total number of atoms of nanoparticles is greatly increased as the size of nanoparticles is reduced, and thus the surface energy and surface tension of particles are also increased, thereby causing the property change of nanoparticles. Because of the particularity of the composition and the structure of the nanocrystalline material, the performance of the nanocrystalline material is obviously improved compared with that of the traditional material, and particularly, the nanocrystalline material has the particularity of super hardness, super modulus effect and the like.
Perovskite Nanocrystals (NCs) have received unprecedented attention in recent years due to their wide application in optoelectronic devices. Of all inorganic perovskites, CsPbI3 has the closest ideal solar cell bandgap.
CsPbI 3-based devices developed rapidly, but at the same time also showed the least stable of the three halide perovskites.
Therefore, the stability of the CsPbI3 material is improved, and therefore, the phase stability of the CsPbI3 material is improved, which plays an important role in the commercialization of the material in the photoelectric field.
Disclosure of Invention
Therefore, the invention provides a CsPbI3 nanocrystal synthesis method, which is used for solving the problems mentioned in the background.
The invention provides a CsPbI3 nanocrystal synthesis method, which comprises the following steps:
step 1, ultrasonically dissolving PbI2 and tetrahexyl ammonium iodide in toluene to obtain a Pb precursor;
and 4, adding ethyl acetate into the CsPbI3 nanocrystal stock solution, centrifuging to obtain precipitates, dispersing the precipitates by using n-hexane to obtain CsPbI3 nanocrystals, centrifuging to remove supernate, and dispersing the precipitates of the CsPbI3 nanocrystal stock solution by using an organic solvent to obtain the CsPbI3 nanocrystals.
Further, in the step 1, the content of the toluene solution is 20ml-30ml, the content of PbI2 and tetrahexyl ammonium iodide is 1mmol and 2mmol, and PbI2 and tetrahexyl ammonium iodide need to be fully dissolved in the toluene solution C7H 8.
Further, in the step 2, the content of caprylic acid is 3ml-5ml, and the added content of cesium carbonate is 0.2mmol or 0.3mmol according to the proportion of the content of caprylic acid, and the CsCO3 precursor is obtained by mixing.
Further, the temperature of the reaction in the step 1 is 30-40 ℃.
Further, in the step 3, after dissolving oleylamine iodide in a toluene solution by ultrasound, injecting the CsCO3 precursor into the lead precursor by using an injector, stirring and reacting for 3-4min, adding the oleylamine iodide toluene solution, and stirring and reacting for 4min to obtain the CsPbI3 nanocrystal stock solution.
Further, in the step 4, the content of ethyl acetate is 30ml, and the content of n-hexane is 6 ml.
Further, centrifuging the CsPbI3 nanocrystal stock solution in the step 4 to obtain a precipitate, wherein the centrifugation speed is 5000-; the washing reagent is acetone, toluene or ethyl acetate.
Compared with the prior art, the method can complete the reaction at the temperature of 30-40 ℃ or normal temperature, effectively stabilize the black-phase structure of CsPbI3, realize the stable synthesis of the CsPbI3 nanocrystal with low cost and high quality at the room temperature, and effectively improve the stability of the CsPbI3 nanocrystal material.
Drawings
FIG. 1 is an X-ray diffraction pattern of a material obtained in step 1 of example 1 of the CsPbI3 nanocrystal synthesis method according to the present invention;
FIG. 2 is an X-ray diffraction pattern of a material obtained in step 2 of example 1 of the CsPbI3 nanocrystal synthesis method according to the present invention;
FIG. 3 is an X-ray diffraction pattern of a material obtained in step 3 of embodiment 1 of the CsPbI3 nanocrystal synthesis method according to the present invention;
fig. 4 is an X-ray diffraction pattern of the material obtained in step 4 of embodiment 1 of the CsPbI3 nanocrystal synthesis method according to the present invention.
Detailed Description
In order that the objects and advantages of the invention will be more clearly understood, the invention is further described below with reference to examples; it should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Preferred embodiments of the present invention are described below with reference to the accompanying drawings. It should be understood by those skilled in the art that these embodiments are only for explaining the technical principle of the present invention, and do not limit the scope of the present invention.
It should be noted that in the description of the present invention, the terms of direction or positional relationship indicated by the terms "upper", "lower", "left", "right", "inner", "outer", etc. are based on the directions or positional relationships shown in the drawings, which are only for convenience of description, and do not indicate or imply that the device or element must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the present invention.
Furthermore, it should be noted that, in the description of the present invention, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood by those skilled in the art according to specific situations.
The invention will be further explained and explained with reference to the following examples and the accompanying drawings.
The first embodiment,
Referring to fig. 1-4, the present embodiment relates to a method for synthesizing CsPbI3 nanocrystals, which includes the following steps:
step 1, ultrasonically dissolving 1mmol of PbI2 and 2mmol of tetrahexyl ammonium iodide in 20ml of toluene, and fully dissolving to obtain a Pb precursor;
and 4, adding 30ml of ethyl acetate into the CsPbI3 nanocrystal stock solution, centrifuging for 5-10min to obtain precipitates, dispersing the precipitates by using 6ml of n-hexane to obtain CsPbI3 nanocrystals, centrifuging for 5-10min to remove supernate, and dispersing the precipitates by using an organic solvent to obtain CsPbI3 nanocrystal stock solution to obtain CsPbI3 nanocrystals.
Specifically, in the course of the stirring reaction, the time for stirring may be increased or shortened as appropriate depending on the room temperature, so that the materials are sufficiently fused.
Example II,
The same procedure as in example one was used except that cesium carbonate in step 2 of example one was changed to cesium acetate and the other conditions were kept the same.
Example III,
The same process as in the example is adopted, and the difference is that tetrabutylammonium iodide is replaced by tetraoctylammonium iodide, the prepared precursor becomes turbid, and the synthesized CsPbI3 has large particles, is difficult to disperse and is easy to agglomerate, so that the optical performance of the CsPbI3 is poor.
Example four,
The same process is adopted in the first embodiment, and the difference is that the proportion of each material in the first embodiment is correspondingly improved by 2 times, and the specific implementation steps are as follows:
step 1, ultrasonically dissolving 2mmol of PbI2 and 4mmol of tetrahexyl ammonium iodide in 40ml of toluene, and fully dissolving to obtain a Pb precursor;
and 4, adding 60ml of ethyl acetate into the CsPbI3 nanocrystal stock solution, centrifuging for 5-10min to obtain a precipitate, dispersing the precipitate by using 6ml of n-hexane to obtain CsPbI3 nanocrystals, centrifuging for 5-10min to remove a supernatant, and dispersing the precipitate CsPbI3 nanocrystal stock solution by using an organic solvent to obtain CsPbI3 nanocrystals.
So far, the technical solutions of the present invention have been described in connection with the preferred embodiments shown in the drawings, but it is easily understood by those skilled in the art that the scope of the present invention is obviously not limited to these specific embodiments. Equivalent changes or substitutions of related technical features can be made by those skilled in the art without departing from the principle of the invention, and the technical scheme after the changes or substitutions can fall into the protection scope of the invention.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention; various modifications and alterations to this invention will become apparent to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (7)
1. A CsPbI3 nanocrystal synthesis method is characterized by comprising the following steps:
step 1, ultrasonically dissolving PbI2 and tetrahexyl ammonium iodide in toluene to obtain a Pb precursor;
step 2, dissolving cesium carbonate CsCO3 in caprylic acid to obtain a CsCO3 precursor;
step 3, ultrasonically dissolving oleylamine iodide in a toluene solution, injecting the CsCO3 precursor into the lead precursor by using an injector, adding the oleylamine iodide toluene solution into the mixture through stirring reaction, and stirring the mixture for the second time to obtain CsPbI3 nanocrystal stock solution;
and 4, adding ethyl acetate into the CsPbI3 nanocrystal stock solution, centrifuging to obtain precipitates, dispersing the precipitates by using n-hexane to obtain CsPbI3 nanocrystals, centrifuging to remove supernate, and dispersing the precipitates of the CsPbI3 nanocrystal stock solution by using an organic solvent to obtain the CsPbI3 nanocrystals.
2. The CsPbI3 nanocrystal synthesis method as claimed in claim 1, wherein the content of toluene solution in step 1 is 20ml-30ml, the content of PbI2 and tetrahexyl ammonium iodide are 1mmol and 2mmol, and it is necessary to dissolve PbI2 and tetrahexyl ammonium iodide in toluene solution C7H8 sufficiently.
3. The CsPbI3 nanocrystal synthesis method according to claim 1, wherein in step 2, the octanoic acid content is 3ml-5ml, cesium carbonate is added in an amount of 0.2mmol or 0.3mmol according to the proportion of the octanoic acid content, and the CsCO3 precursor is obtained by mixing.
4. The method for synthesizing CsPbI3 nanocrystals, according to claim 1, wherein the temperature of the reaction of step 1 is 30-40 ℃.
5. The method for synthesizing CsPbI3 nanocrystals according to claim 1, wherein in step 3, after oleylamine iodide is ultrasonically dissolved in toluene solution, CsCO3 precursor is injected into lead precursor by a syringe, the stirring reaction time is 3-4min, oleylamine iodide toluene solution is added, and the stirring reaction time is 4min, so as to obtain CsPbI3 nanocrystal stock solution.
6. The method for synthesizing CsPbI3 nanocrystals, according to claim 1, wherein the ethyl acetate content in step 4 is 30ml and the n-hexane content is 6 ml.
7. The CsPbI3 nanocrystal synthesis method as claimed in claim 1, wherein the CsPbI3 nanocrystal stock solution in step 4 is centrifuged to obtain the precipitate, the centrifugation speed is 5000-10000r/min, and the centrifugation time is 5-10 min; the washing reagent is acetone, toluene or ethyl acetate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110424546.XA CN113149066A (en) | 2021-04-20 | 2021-04-20 | CsPbI3 nanocrystal synthesis method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110424546.XA CN113149066A (en) | 2021-04-20 | 2021-04-20 | CsPbI3 nanocrystal synthesis method |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN113149066A true CN113149066A (en) | 2021-07-23 |
Family
ID=76869052
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110424546.XA Pending CN113149066A (en) | 2021-04-20 | 2021-04-20 | CsPbI3 nanocrystal synthesis method |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113149066A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107128967A (en) * | 2017-05-08 | 2017-09-05 | 厦门大学 | A kind of nanocrystalline synthetic method of full-inorganic CsPbX3 perovskites |
| US20170260218A1 (en) * | 2016-03-10 | 2017-09-14 | Samsung Electronics Co., Ltd. | Nanocrystal and preparation method thereof |
| CN111268724A (en) * | 2020-02-14 | 2020-06-12 | 南京理工大学 | Synthesis of CsPbI by room-temperature nonpolar solvent system3Method for perovskite nanocrystalline |
-
2021
- 2021-04-20 CN CN202110424546.XA patent/CN113149066A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170260218A1 (en) * | 2016-03-10 | 2017-09-14 | Samsung Electronics Co., Ltd. | Nanocrystal and preparation method thereof |
| CN107128967A (en) * | 2017-05-08 | 2017-09-05 | 厦门大学 | A kind of nanocrystalline synthetic method of full-inorganic CsPbX3 perovskites |
| CN111268724A (en) * | 2020-02-14 | 2020-06-12 | 南京理工大学 | Synthesis of CsPbI by room-temperature nonpolar solvent system3Method for perovskite nanocrystalline |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| He et al. | Review on nanoscale Bi-based photocatalysts | |
| Sun et al. | One‐dimensional nanostructured pseudocapacitive materials: design, synthesis and applications in supercapacitors | |
| Peng et al. | Electrospun carbon nanofibers and their hybrid composites as advanced materials for energy conversion and storage | |
| Wang et al. | Synthesis and enhanced intercalation properties of nanostructured vanadium oxides | |
| Muraliganth et al. | Facile synthesis of carbon-decorated single-crystalline Fe3O4 nanowires and their application as high performance anode in lithium ion batteries | |
| Liu et al. | Anisotropic Co 3 O 4 porous nanocapsules toward high-capacity Li-ion batteries | |
| Yang et al. | Size-tailored synthesis and luminescent properties of one-dimensional Gd2O3: Eu3+ nanorods and microrods | |
| Bairi et al. | Mesoporous fullerene C 70 cubes with highly crystalline frameworks and unusually enhanced photoluminescence properties | |
| CN104704577A (en) | Radiation shielding composite material including radiation absorbing material and method for preparing the same | |
| CN100355649C (en) | Method of in-situ filling symbiotic iron nanometer wire on thin wall nanometer pipe | |
| Zhu et al. | Recent progress on nanostructured transition metal oxides as anode materials for lithium-ion batteries | |
| Wei et al. | Recent progress in synthesis, growth mechanisms, and electromagnetic wave absorption properties of silicon carbide nanowires | |
| Nadaraia et al. | Preparation of Tungstate nanopowders by Sol-Gel method | |
| CN110885473A (en) | Nano-particles, composite film, and preparation method and application thereof | |
| CN113149066A (en) | CsPbI3 nanocrystal synthesis method | |
| KR20060013510A (en) | Nano-fiber or nano-tube comprising v group transition metal dichalcogenide crystals, and method for preparation thereof | |
| Yu et al. | Design and preparation of continuous titanium carbide fibers via simple precursor route | |
| CN104190921A (en) | Nano particle of Au/Ni12P5 nuclear shell structure and preparation method thereof | |
| Lv et al. | Preparation of ZnS nanotubes via surfactant micelle-template inducing reaction | |
| Geetha et al. | Nanoporous transition metal sulfide (Cd–CuS) active electrode material for electrochemical energy storage device | |
| Fang et al. | Si/Cu/C Nanohybrid Lithium-Ion Battery Anode with in Situ Incorporation of Nonagglomerated Super-Small Copper Nanoparticles Based on Epoxy Resin | |
| Zou et al. | Process, fundamental and application of one-step molten-salt synthezed BaTi2O5 nanorods | |
| KR100672811B1 (en) | Method for preparing indium oxide nano particle and soluble indium oxide nano particle prepared by the same | |
| Mudra et al. | Preparation and characterization of ceramic nanofibers based on lanthanum tantalates | |
| CN101319383B (en) | Preparation method of nanometer barium zirconate |
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 | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20210723 |
|
| RJ01 | Rejection of invention patent application after publication |