CN110156071A - A kind of preparation method of the full-inorganic perovskite nanocluster assembly of high-sequential - Google Patents
A kind of preparation method of the full-inorganic perovskite nanocluster assembly of high-sequential Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of the full-inorganic perovskite nanocluster assembly of high-sequential, the present invention prepares presoma caesium solution using solwution method, secondly lead halide powder is dissolved in nonpolar solvent with organic acid and organic amine ligand obtains lead precursor solution, then suitable oleic acid caesium solution is injected in lead precursor solution at room temperature, stir about obtains cotton-shaped full-inorganic perovskite nanocluster assembly after one minute.The type and content for adjusting ligand, can prepare the cluster assembly of two-dimentional hexagonal closs packing and two-dimensional layered structure.The method of the present invention is simple and novel, and controllability is strong, raw material is easy to get, and cost is relatively low, can be used in photovoltaic device.Secondly cluster assembly template-policy proposed by the present invention is a kind of universal method, is adapted to the preparation of a variety of two-dimensional layer nanocrystals, gained nano crystal material is with a wide range of applications in fields such as opto-electronic device, solar energy.
Description
Technical field
The invention belongs to technical field of inorganic material, and in particular to a kind of full-inorganic perovskite nanocluster of high-sequential
The preparation method of assembly.
Background technique
Nanocluster is be bonded together by physically or chemically active force, metastable microcosmic or submicroscopic atom
Or molecule aggregate.Because of its small size and moldable surface, in self-assembled material, photoelectric device, biomarker, medical treatment and the sun
The fields such as energy battery have become a hot topic of research.Under micro-scale, the pattern of nanocluster is to its electronic structure and optical property
Have a great impact, by adjusting the microstructure of semiconductor nanoclusters, can be designed the material with particular characteristic.It is being situated between
It sees under scale, nanocluster can be used as construction unit, can be prepared by conventional chemical route or other self assembly strategies
The superstructure material of good symmetry and geometry, and the nano material with special construction can be further converted to.
In recent years, the material based on perovskite crystal structure causes extensive pass in photovoltaic and field of photoelectric devices
Note.Especially full-inorganic perovskite CsPbX3(X=Cl, Br, I) nanocrystal shows adjustable in entire visibility region
Fluorescent emission feature, even more bring research boom.Perovskite crystal refers to and calcium titanate compound (CaTiO3) there is phase
The substance of allomeric structure, general molecular formula ABO3, due to perovskite CsPbX3It is photoconductivity, therefore can be used as and partly lead
Body material.It is synthesized at present go out pattern include zero dimension (0D) quantum dot, one-dimensional (1D) nano wire and two-dimentional (2D) nanometer sheet,
In reaction system, the structure of intermediate state has conclusive effect to the control of subsequent pattern, but currently without about calcium titanium
The intermediate state research of mine nanocrystal.
Therefore it provides a kind of method is simple, what raw material was easy to get prepares a kind of full-inorganic perovskite nanoclusters of high-sequential
The preparation method of cluster assembly means a great.
Summary of the invention
The purpose of the present invention is to provide a kind of method is simple, what raw material was easy to get prepares a kind of full-inorganic calcium of high-sequential
The preparation method of titanium ore nanocluster assembly.
In order to achieve the above object, the technical scheme adopted by the invention is as follows:
By using organic acid and organic amine ligand auxiliary dissolution lead halide solid in nonpolar solvent, before available lead
Liquid solution is driven, is then rapidly injected a certain amount of oleic acid caesium solution at room temperature, after continuing stir about one minute, is obtained stable
Shine floccule, which is the full-inorganic perovskite nanocluster assembly of high-sequential.This assembly is structurally ordered, ruler
It is very little regular, it can be used as the soft template of subsequent nanobelt.
Specific step is as follows:
A kind of preparation method of the full-inorganic perovskite nanocluster assembly of high-sequential, the specific steps are as follows:
(1) using lead halide as presoma, using organic acid and organic amine as ligand, in nonpolar reaction solvent at 20 ~ 25 DEG C
Middle stirring and dissolving 10-12 hours;
At (2) 20 ~ 25 DEG C, it is rapidly injected oleic acid caesium solution in step (1) products therefrom, after stirring, obtains floccule, as
The full-inorganic perovskite nanocluster assembly of high-sequential;
Wherein, lead halide described in step (1) is one or more of lead fluoride, lead bromide or lead iodide;
Organic acid described in step (1) is one or more of oleic acid, octanoic acid or stearic acid;
Organic amine described in step (1) can be one or more of oleyl amine, lauryl amine, octylame or octadecylamine;
Nonpolar reaction solvent described in step (1) is one of octadecylene, n-hexane, hexamethylene or carbon tetrachloride or several
Kind.
In the present invention, oleic acid caesium solution preparation step described in step (2) is as follows:
In the biexhaust pipe of standard, deoxygenation and N are removed water2Under atmosphere, by oleic acid and Cs2CO3Mixing, vacuumizes 30 at 20 ~ 25 DEG C
It is warming up to 120 DEG C after min to continue to vacuumize 30min, after being cooled to 20 ~ 25 DEG C, is transferred quickly to N2It is protected in the glove box of atmosphere
It deposits.
Wherein, oleic acid and Cs2CO3Molar ratio be 76:1.
In the present invention, the molar ratio of lead halide and organic amine as described in step (1) are as follows: 1:17.
In the present invention, the volume ratio of oleic acid caesium solution described in step (2) and step (1) products therefrom are as follows: 1:10.
The present invention prepares presoma caesium solution using solwution method, secondly molten in nonpolarity with organic acid and organic amine ligand
Lead halide powder is dissolved in agent obtains lead precursor solution, it is then at room temperature that suitable oleic acid caesium solution injection lead presoma is molten
In liquid, stir about obtains cotton-shaped full-inorganic perovskite nanocluster assembly after one minute.The type and content of ligand are adjusted,
The cluster assembly of two-dimentional hexagonal closs packing and two-dimensional layered structure can be prepared.The method of the present invention is simple and novel, controllability is strong,
Raw material is easy to get, and cost is relatively low, and application value is extensive, and the synthesis of full-inorganic perovskite nanocluster and its self assembly behavior
Research helps to further understand the relationship between molecular precursor and nanocrystal product, while being anisotropic calcium titanium
The synthesis of mine nanocrystal provides new approaches.
The beneficial effects of the present invention are:
The present invention is ligand using the organic molecule of different length carbochain, adjusts the type and content of ligand, can prepare two dimension
The cluster assembly of hexagonal closs packing and two-dimensional layered structure, especially CsPbI3Nanocluster assembly has good light
Characteristic is learned, is expected to be applied to photovoltaic device.The method of the present invention is simple and novel, and controllability is strong, raw material is easy to get, and cost is relatively low, application
Value is extensive.
Detailed description of the invention
Fig. 1 is CsPbI prepared by the embodiment of the present invention 23The UV absorption and fluorescence spectrum of nanocluster assembly;
Fig. 2 is CsPbBr prepared by the embodiment of the present invention 13The ultra-violet absorption spectrum of nanocluster;
Fig. 3 is CsPbI prepared by the embodiment of the present invention 23The electron microscopic picture of nanocluster assembly;
Fig. 4 is CsPbBr prepared by the embodiment of the present invention 13The electron microscopic picture of nanocluster assembly;
Fig. 5 is CsPbI prepared by the embodiment of the present invention 23The X-ray diffraction spectrogram of nanocluster assembly;
Fig. 6 is CsPbBr prepared by the embodiment of the present invention 13The small angle x-ray diffraction (SAXD) phenogram of nanocluster assembly;
Fig. 7 is CsPbI prepared by the embodiment of the present invention 23The thermal gravimetric analysis curve of nanocluster assembly;
Fig. 8 is CsPbBr prepared by the embodiment of the present invention 13The thermal gravimetric analysis curve of nanocluster assembly.
Specific embodiment
Embodiment 1
(1) synthesis of presoma oleic acid caesium (CsOA): all synthesis steps are all in the Schlenk-line of standard and N2Atmosphere
Lower operation.By 60 mL OA(oleic acid) and 1.22 g Cs2CO3(2.5 mmol) is mixed to join in there-necked flask, first at room temperature
It vacuumizes and is warming up to 120 DEG C after 30 min and continues to vacuumize 30min, obtain light yellow clear solution.After being cooled to room temperature,
Oleic acid caesium is promptly transferred to N2It is saved in the glove box of atmosphere.
(2) OA/OAm is the CsPbBr of ligand3The synthesis of nanocluster: 69 mg PbBr2(0.188 mmol), 1 mL
OAm(oleyl amine), 0.5 mL OA(oleic acid) and 5 mL ODE(octadecylenes) mixing be added 20 ml vials in, in glove box
The stirring and dissolving at 25 DEG C of room temperature, obtains the solution of clear, colorless after 12 h, then injects 0.5 mL oleic acid caesium rapidly,
Solution colour rapidly goes to light yellow, the floccule of silver color occurs after stir about 1min, this floccule is CsPbBr3Nanometer
Cluster assembly.
The optical property phenetic analysis of sample:
Fig. 2 is the CsPbBr that oleic acid oleyl amine does ligand3The ultra-violet absorption spectrum of nanocluster.The ultraviolet suction of light yellow clear solution
It receives spectrum and occurs obvious blue shift, and the strong trap exciton characteristic peak that peak type is sharp at 391 nm, show to be possible to generate
Minimum CsPbBr3Nanocluster, the ultraviolet spectra display dispersion of 7 nm of red shift, isolated CsPbBr3Nanocluster self assembly
For aggregation, i.e. assembly.
The morphology and size phenetic analysis of sample:
Fig. 4 is CsPbBr3The electron microscopic picture of nanocluster assembly.TEM characterization display CsPbBr3Nanocluster assembly is presented
The quasi- rectangle pencil aggregation of mesoscopic size.
The structural characterization of sample is analyzed:
Fig. 6 is the CsPbBr of the high-sequential of preparation3The small angle x-ray diffraction (SAXD) (SAXRD) of nanocluster assembly characterizes.It is logical
It crosses and the two-dimentional Hexagonal array structure that assembly is p6mm with space group is calculated.
The Surface Characterization of sample is analyzed:
Fig. 8 is CsPbBr3The thermal gravimetric analysis curve of nanocluster assembly.As seen from the figure, black curve can be calculated and receive
The content of rice cluster assembly surface ligand is about 67%.
Embodiment 2
(1) synthesis of presoma oleic acid caesium (CsOA): with embodiment 1.
(2) stearic acid/OAm(oleyl amine) it is the CsPbI of ligand3The synthesis of nanocluster: by 0.087 g PbI2、0.09 g
Stearic acid, 0.35 ml oleyl amine and 10 ml anhydrous n-hexanes are stirred at room temperature dissolution in the vial of 20 ml, and 12 hours
Afterwards, 0.5 ml oleic acid caesium solution is added in room temperature, continues to stop after stirring 1min, this crocus floccule is CsPbI3Nanoclusters
Cluster assembly.
The optical property phenetic analysis of sample:
Fig. 1 is CsPbI3The UV absorption and fluorescence spectrum of nanocluster assembly.The obvious blue shift of absorption peak, and peak type compares
Sharply, with the characteristic feature of cluster absorption spectrum, illustrate to have synthesized that size is minimum and new structural nanocluster.It is more strong
Strong fluorescence emission peak shows that product has good optical property.
The morphology and size phenetic analysis of sample:
Fig. 3 is CsPbI3The electron microscopic picture of nanocluster assembly.It is shown as the aggregation of large scale, class rectangle on TEM figure, gathers
Single cluster is bound together by collective, the pattern and (ZnSe)13Clusters body is closely similar.
The structural characterization of sample is analyzed:
Fig. 5 is CsPbI3The X-ray diffraction spectrogram of nanocluster assembly.Multiorder diffractive peak shows that assembly has 2-dimensional mesoscopic
Layer structure.
The Surface Characterization of sample is analyzed:
Fig. 7 is CsPbI3Thermogravimetric analysis (TGA) curve of nanocluster assembly.It can estimate roughly from thermogravimetric analysis (TGA) figure
Calculating the amount of ligand contained by cluster is about 68%, thus can indirect proof nanocluster there is minimum size.
Claims (4)
1. a kind of preparation method of the full-inorganic perovskite nanocluster assembly of high-sequential, which is characterized in that specific steps
It is as follows:
(1) using lead halide as presoma, using organic acid and organic amine as ligand, at 20 ~ 25 DEG C, in nonpolar reaction solvent
Middle stirring and dissolving 10-12 hours;
At (2) 20 ~ 25 DEG C, be rapidly injected oleic acid caesium solution in step (1) products therefrom, after stirring, obtain floccule to get
To the full-inorganic perovskite nanocluster assembly of high-sequential;
Wherein, lead halide described in step (1) is one or more of lead fluoride, lead bromide or lead iodide;
Organic acid described in step (1) is one or more of oleic acid, octanoic acid or stearic acid;
Organic amine described in step (1) can be one or more of oleyl amine, lauryl amine, octylame or octadecylamine;
Nonpolar reaction solvent described in step (1) is one of octadecylene, n-hexane, hexamethylene or carbon tetrachloride or several
Kind.
2. a kind of preparation method of the full-inorganic perovskite nanocluster assembly of high-sequential according to claim 1,
It is characterized in that, oleic acid caesium solution preparation step described in step (2) is as follows:
In the biexhaust pipe of standard, deoxygenation and N are removed water2Under atmosphere, by oleic acid and Cs2CO3Mixing, vacuumizes 30 at 20 ~ 25 DEG C
It is warming up to 120 DEG C after min to continue to vacuumize 30min, after being cooled to 20 ~ 25 DEG C, is transferred quickly to N2It is protected in the glove box of atmosphere
It deposits, wherein oleic acid and Cs2CO3Molar ratio be 76:1.
3. a kind of preparation method of the full-inorganic perovskite nanocluster assembly of high-sequential according to claim 1,
It is characterized in that, the molar ratio of lead halide as described in step (1) and organic amine are as follows: 1:17.
4. a kind of preparation method of the full-inorganic perovskite nanocluster assembly of high-sequential according to claim 1,
It is characterized in that, the volume ratio of oleic acid caesium solution described in step (2) and step (1) products therefrom are as follows: 1:10.
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CN113135590A (en) * | 2021-05-27 | 2021-07-20 | 南京邮电大学 | Preparation method of perovskite nanorod |
CN113980670A (en) * | 2021-10-29 | 2022-01-28 | 中国科学院深圳先进技术研究院 | Solid perovskite cluster, preparation method thereof and photoelectric device |
CN114988463A (en) * | 2022-05-27 | 2022-09-02 | 郑州大学 | Halide perovskite patterning assembly method and application thereof |
WO2023070866A1 (en) * | 2021-10-29 | 2023-05-04 | 中国科学院深圳先进技术研究院 | Perovskite cluster solution and preparation method therefor, and optoelectronic device |
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CN113980670A (en) * | 2021-10-29 | 2022-01-28 | 中国科学院深圳先进技术研究院 | Solid perovskite cluster, preparation method thereof and photoelectric device |
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WO2023070866A1 (en) * | 2021-10-29 | 2023-05-04 | 中国科学院深圳先进技术研究院 | Perovskite cluster solution and preparation method therefor, and optoelectronic device |
CN113980670B (en) * | 2021-10-29 | 2023-11-14 | 中国科学院深圳先进技术研究院 | Solid perovskite cluster, preparation method thereof and photoelectric device |
CN114988463A (en) * | 2022-05-27 | 2022-09-02 | 郑州大学 | Halide perovskite patterning assembly method and application thereof |
CN114988463B (en) * | 2022-05-27 | 2023-10-24 | 郑州大学 | Halide perovskite patterning assembly method and application thereof |
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