CN107500344A - A kind of full-inorganic halide perovskite material CsPbI3Nanotube and its preparation method and application - Google Patents

A kind of full-inorganic halide perovskite material CsPbI3Nanotube and its preparation method and application Download PDF

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CN107500344A
CN107500344A CN201710676024.2A CN201710676024A CN107500344A CN 107500344 A CN107500344 A CN 107500344A CN 201710676024 A CN201710676024 A CN 201710676024A CN 107500344 A CN107500344 A CN 107500344A
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CN107500344B (en
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熊维伟
郑芬芬
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Jiangsu University of Science and Technology
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    • C01G21/00—Compounds of lead
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    • B82—NANOTECHNOLOGY
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    • B82Y40/00—Manufacture or treatment of nanostructures
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2002/00—Crystal-structural characteristics
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    • C01P2002/80—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70
    • C01P2002/85—Crystal-structural characteristics defined by measured data other than those specified in group C01P2002/70 by XPS, EDX or EDAX data
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
    • C01P2004/13—Nanotubes
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2004/60—Particles characterised by their size
    • C01P2004/62—Submicrometer sized, i.e. from 0.1-1 micrometer
    • C—CHEMISTRY; METALLURGY
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    • C01P2006/60—Optical properties, e.g. expressed in CIELAB-values

Abstract

The invention discloses a kind of full-inorganic halide perovskite material CsPbI3Nanotube and its preparation method and application, the CsPbI3Nanotube is by CsPbI3Nanocrystal solution is obtained by microwave reaction；The CsPbI3CsPbI in nanotube3Mol ratio be 1:1‑1.1:3‑3.3.The CsPbI that the present invention is prepared by microwave method3Nanotube is a brand-new material, and nanotubes are prepared in perovskite first by this method.Full-inorganic halide perovskite material CsPbI prepared by the present invention3Nanotube, there is fluorescence and photoelectric respone, synthetic yield is high, and pattern is homogeneous, and nanotube stability is high；The preparation method of the present invention is simple and convenient simultaneously, and raw material sources are wide, and cost is low, and microwave method heating is rapid, is heated homogeneous；The CsPbI of the present invention3Nanotube has huge application potential in fields such as photoelectrons because it has unique form, structure and electronic property.

Description

A kind of full-inorganic halide perovskite material CsPbI3Nanotube and preparation method thereof and Using
Technical field
The present invention relates to full-inorganic halide perovskite material, and in particular to a kind of microwave irradiation prepares full-inorganic halogenation Thing perovskite material CsPbI3Nanotube and its preparation method and application.
Background technology
In recent years, full-inorganic halide perovskite material CsPbX3(X=Cl, Br, I) be found to have excellent optics and Electronic Performance, and be proved to can be applied to optoelectronic areas, including solar cell, light emitting diode (LED), nonlinear optical Learn property, laser, photodetector.In full-inorganic halide perovskite material field, Kovalenko etc. is first by " heat is noted Enter-method for quick cooling " it has been successfully prepared CsPbX3Nanocrystal.It is reported that these not optimized cubic nanometers are brilliant with super High quantum fluorescent yield (PLQY) and narrow fluorescence spectrum, and spectral wavelength can be changed by adjusting halogenic ingredient, be covered Cover whole visible region.Meanwhile these CsPbX3Nanocrystal is proven to have the Amplified Spontaneous Emission performance of ultralow threshold value And it is successfully applied to laser.Then, people have synthesized full-inorganic halogen by changing reaction experiment parameter or experimental strategy The nano materials such as perovskite nano wire, nanometer rods, nano-cluster, nanometer sheet, nanometer paper, assemble them into photoelectric device, obtain Excellent performance.However, one-dimensional full-inorganic halide perovskite nanotube is not reported so far.Particularly one dimension semiconductor is received Mitron, because it has unique form, structure and electronic property, full-inorganic CsPbX3Nanotube has in fields such as photoelectrons There is huge application potential.
The content of the invention
Goal of the invention：The problem of existing for prior art, the present invention provide a kind of full-inorganic halide perovskite material CsPbI3Mitron；The CsPbI3Nanotube has fluorescence and photoelectric respone, and synthetic yield is high, and purity is high, and stability is high, and pattern is equal One.
The present invention also provides full-inorganic halide perovskite material CsPbI3The preparation method and application of nanotube.
Technical scheme：To achieve these goals, a kind of full-inorganic halide perovskite material as described in the present invention CsPbI3Nanotube, by CsPbI3Nanocrystal solution is obtained by microwave reaction；The CsPbI3Cs in nanotube:Pb:I moles Than for 1:1-1.1:3-3.3
Preferably, CsPbI3Cs in nanotube:Pb:I mol ratios are 1:1:3.
Further, the CsPbI3Nanotube is monocrystalline, hollow nanotube.
Further, the CsPbI3Nanotube is that length is 5-15 μm, and width 200nm-1000nm, thickness are 100-500nm。
Wherein, the CsPbI3Nanotube has fluorescence property, has fluorescence near 460nm and 550nm wavelength Peak.
Wherein, the CsPbI3Nanotube has photoelectric properties, has photosensitive response to the light of 405nm wavelength.
Full-inorganic halide perovskite material CsPbI of the present invention3The preparation method of nanotube, including following step Suddenly：
(1) by CsCO3, oleic acid, vaccenic acid mixing add high temperature drying, then rising temperature for dissolving CsCO3, obtain Cs- oleic acid Salting liquid；Wherein oleic acid can dissolve CsCO3, mole ratio CsCO3Slightly more, vaccenic acid is as solvent；
(2)PbI2It is added in vaccenic acid and dries, adds oleic acid and oleyl amine dissolving PbI2；Then heat up, add step (1) the Cs- oleate solutions obtained carry out fast reaction, stop reacting with ice bath immediately after, cooling, obtain CsPbI3Nanometer Brilliant solution.
(3) by CsPbI3Nanocrystal solution carries out microwave reaction；Reaction product is obtained by low-speed centrifugal, n-hexane washing CsPbI3Nanotube.CsPbI3Nanotube Cord blood is standby in hexane solution.
Preferably, the time of step (2) described fast reaction is the 10-15 seconds.It is preferred that fast reaction 10 seconds.
Preferably, step (3) the microwave reaction temperature is 90-150 DEG C, the time is 5-120 minutes.
Full-inorganic halide perovskite material CsPbI of the present invention3Application of the nanotube in optoelectronic areas.
Further, the CsPbI3Nanotube is assembled into photodetector in optoelectronic areas, in ultraviolet wavelength Scope has response characteristics to light.
Beneficial effect：Compared with prior art, the invention has the advantages that：
The CsPbI that the present invention is prepared by microwave method3Nanotube is a brand-new material, by this method first in calcium Nanotubes are prepared in titanium ore.Full-inorganic halide perovskite material CsPbI prepared by the present invention3Nanotube, have fluorescence and Photoelectric respone, synthetic yield is high, and pattern is homogeneous, and nanotube stability is high；The preparation method of the present invention is simple and convenient simultaneously, raw material Source is wide, and cost is low, and microwave method heating is rapid, is heated homogeneous；The CsPbI of the present invention3Nanotube is by controlling temperature 90- 150 DEG C, microwave reaction different time obtains different CsPbI3Nanotube, because it has unique form, structure and electro Matter, there is huge application potential in fields such as photoelectrons.
Brief description of the drawings
Fig. 1 is CsPbI prepared by the embodiment of the present invention 13The I- x ray diffration pattern xs of nanotube；
Fig. 2 is CsPbI prepared by the embodiment of the present invention 13The EDS spectrograms of nano-tube material；
Fig. 3 is CsPbI prepared by the embodiment of the present invention 13Nanotube scanning electron microscope (SEM) photograph；
Fig. 4 is CsPbI prepared by the embodiment of the present invention 13The transmission electron microscope picture of nanotube；
Fig. 5 is CsPbI prepared by the embodiment of the present invention 13The high-resolution-ration transmission electric-lens and lattice diffraction pattern of nanotube；
Fig. 6 is CsPbI prepared by the embodiment of the present invention 13The Solid fluorescene spectrum figure of nanotube；
Fig. 7 is CsPbI prepared by the embodiment of the present invention 13Nanotube is assembled into the photosensitive response figure of photodetector；
Fig. 8 is CsPbI prepared by the embodiment of the present invention 13Nanotube entire scan electron microscope；
Fig. 9 is CsPbI prepared by the embodiment of the present invention 23Nanotube scanning electron microscope (SEM) photograph；
Figure 10 is CsPbI prepared by the embodiment of the present invention 33Nanotube scanning electron microscope (SEM) photograph；
Figure 11 is CsPbI prepared by the embodiment of the present invention 43Nanotube scanning electron microscope (SEM) photograph.
Embodiment
Below in conjunction with drawings and examples, the invention will be further described.
Embodiment 1
(1) 0.2g CsCO3,0.6ml oleic acid, 10ml vaccenic acids are mixed and add the drying 1 hour of 120 DEG C of three-neck flask, Then rising temperature for dissolving CsCO3, Cs- oleate solutions are obtained；
(2)0.348g PbI2120 DEG C of dryings in 20mL vaccenic acids are added to, add 2ml oleic acid and 2ml oleyl amines (altogether Same-action) dissolving PbI2；Then 150 DEG C are warming up to, it is quick anti-to add the Cs- oleate solutions 1.6mL progress that step (1) obtains Answer 10 seconds, stop reacting with ice bath immediately after, cooling, obtain CsPbI3Nanocrystal solution；
(3) by CsPbI3Nanocrystal solution, which is transferred in microwave quartz ampoule, carries out microwave reaction, 130 DEG C of reaction temperature, instead Answer 30 minutes；Reaction product obtains CsPbI by low-speed centrifugal, n-hexane washing3Nanotube.
CsPbI manufactured in the present embodiment3Cs in nanotube:Pb:I mol ratio is 1:1:3.
CsPbI manufactured in the present embodiment3The x-ray diffraction pattern of nanotube is as shown in figure 1, wherein numeral is CsPbI3Receive The crystal face of mitron, corresponding standard card JCPDS 18-0376, CsPbI3Nanotube is through X-ray diffraction analysis, the results showed that The crystal face and normal data of the main diffraction peak of the nanotube of preparation are completely corresponding, are pure CsPbI3 nano-tube materials.
CsPbI manufactured in the present embodiment3The EDS spectrograms of nano-tube material are as shown in Fig. 2 Fig. 2 shows the original of three kinds of elements Sub-count ratio about 1：1：3.
CsPbI manufactured in the present embodiment3Nanotube scanning electron microscope (SEM) photograph is as shown in figure 3, CsPbI3Nanotube scanned Electronic Speculum point Analysis, the results showed that the one-dimensional CsPbI of preparation3Nanotube is openning shape nanotube.
CsPbI manufactured in the present embodiment3The transmission electron microscope picture of nanotube is as shown in figure 4, CsPbI3Nanotube is through transmission electron microscope Analysis, the results showed that the one-dimensional CsPbI of preparation3Nanotube is hollow nanotube.
CsPbI manufactured in the present embodiment3The high-resolution-ration transmission electric-lens and lattice diffraction pattern of nanotube as shown in figure 5, CsPbI3Nanotube is analyzed through high-resolution-ration transmission electric-lens, the results showed that the one-dimensional CsPbI of preparation3Nanometer materials in the tube are monocrystalline.
CsPbI manufactured in the present embodiment3The Solid fluorescene spectrum figure of nanotube is as shown in fig. 6, CsPbI3Nanotube is through solid Spectrofluorimetry, the results showed that the CsPbI of preparation3Nanotube has two fluorescence emission peaks, and maximum emission peak is located at respectively 460nm and 550nm or so.
CsPbI manufactured in the present embodiment3Nanotube is assembled into the photosensitive response figure of photodetector as shown in fig. 7, (Fig. 7 a For CsPbI3The rough schematic of nanotube photoelectric detector；Fig. 7 b represent CsPbI3Nanotube detector is in details in a play not acted out on stage, but told through dialogues and 405nm I-V indicatrixes under wavelength；Fig. 7 c represent repeatable ON/OFF experiment of the photo-detector under different illumination intensity；Fig. 7 d tables Show that photo-detector has good stability.CsPbI3Nanotube is assembled into photodetector, and analysis result shows that nanotube exists Ultraviolet wavelength range has quick response characteristics to light.CsPbI is can be seen that from Fig. 7 a, b, c3Nanotube has photo electric Can, CsPbI3Nanotube has photosensitive response to the light of 405nm wavelength.
CsPbI manufactured in the present embodiment3The entire scan electron microscope of nanotube is as shown in figure 8, CsPbI3Nanotube has height Purity, homogeneous structure.Length is 5-15 μm, width 200nm-1000nm, thickness 100-500nm.
Embodiment 2
CsPbI is prepared by the identical raw material and step of embodiment 13Nanotube, difference are microwave reaction temperature It is changed into 110 DEG C, result of implementation scanning electron microscope (SEM) photograph is as shown in figure 9, CsPbI3Nanotube has high purity, homogeneous structure, but Narrowed width.
Embodiment 3
CsPbI is prepared by the identical raw material and step of embodiment 13Nanotube, difference are the microwave reaction time For 15 minutes, result of implementation scanning electron microscope (SEM) photograph was as shown in Figure 10, and nanotube average length is short compared to embodiment 1.
Embodiment 4
CsPbI is prepared by the identical raw material and step of embodiment 13Nanotube, difference are the microwave reaction time It is changed into 60 minutes, result of implementation scanning electron microscope (SEM) photograph is as shown in figure 11, and nanotube length average length will be grown compared to embodiment 1.
Embodiment 5
CsPbI is prepared by the identical raw material and step of embodiment 13Nanotube, difference are that step (2) is quick Reaction 15 seconds, stop reacting with ice bath immediately after, cooling, obtain CsPbI3Nanocrystal solution；Step (3) microwave reaction, instead 90 DEG C of temperature is answered, is reacted 120 minutes；Reaction product obtains CsPbI by low-speed centrifugal, n-hexane washing3Nanotube.This implementation CsPbI prepared by example3Cs in nanotube:Pb:I mol ratio is 1:1.1:3.3.
Embodiment 6
CsPbI is prepared by the identical raw material and step of embodiment 13Nanotube, difference are that step (2) is quick Reaction 12 seconds, stop reacting with ice bath immediately after, cooling cooling, obtain CsPbI3Nanocrystal solution；Step (3) microwave is anti- Should, 150 DEG C of reaction temperature, react 5 minutes；Reaction product obtains CsPbI by low-speed centrifugal, n-hexane washing3Nanotube.This CsPbI prepared by embodiment3Cs in nanotube:Pb:I mol ratio is 1:1.1:3.2.

Claims (10)

  1. A kind of 1. full-inorganic halide perovskite material CsPbI3Nanotube, it is characterised in that by CsPbI3Nanocrystal solution passes through Microwave reaction obtains；The CsPbI3Cs in nanotube:Pb:I mol ratio is 1:1-1.1:3-3.3.
  2. 2. CsPbI according to claim 13Nanotube, it is characterised in that the CsPbI3Nanotube is monocrystalline, hollow Nanotube.
  3. 3. CsPbI according to claim 13Nanotube, it is characterised in that the CsPbI3Nanotube is that length is 5-15 μ M, width 200nm-1000nm, thickness 100-500nm.
  4. 4. CsPbI according to claim 13Nanotube, it is characterised in that the CsPbI3Nanotube has fluorescence property, There is fluorescence emission peak near 460nm and 550nm wavelength.
  5. 5. CsPbI according to claim 13Nanotube, it is characterised in that the CsPbI3Nanotube has photoelectric properties, There is photosensitive response to the light of 405nm wavelength.
  6. A kind of 6. full-inorganic halide perovskite material CsPbI as claimed in claim 13The preparation method of nanotube, its feature It is, comprises the following steps：
    (1) by CsCO3, oleic acid, vaccenic acid mixing add high temperature drying, then rising temperature for dissolving CsCO3, it is molten to obtain Cs- oleates Liquid；
    (2)PbI2It is added in vaccenic acid and dries, add oleic acid and oleyl amine, dissolves PbI2；Then heat up, add step (1) Obtained Cs- oleate solutions carry out fast reaction, stop reacting with ice bath immediately after, cooling, obtain CsPbI3It is nanocrystalline Solution；
    (3) by CsPbI3Nanocrystal solution carries out microwave reaction；Reaction product is obtained by low-speed centrifugal, n-hexane washing CsPbI3Nanotube.
  7. 7. preparation method according to claim 6, it is characterised in that the time of step (2) described fast reaction is the 10-15 seconds.
  8. 8. the preparation method stated according to claim 6, it is characterised in that step (3) the microwave reaction temperature is 90-150 DEG C, Time is 5-120 minutes.
  9. A kind of 9. full-inorganic halide perovskite material CsPbI as claimed in claim 13Nanotube is in optoelectronic areas Using.
  10. 10. application according to claim 1, the CsPbI3Nanotube is assembled into photodetector in optoelectronic areas, There is response characteristics to light in ultraviolet wavelength range.
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CN110255608A (en) * 2019-07-29 2019-09-20 云南师范大学 A kind of microwave synthesis two dimension PbI2The method of nanostructure
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CN116359451A (en) * 2023-06-01 2023-06-30 之江实验室 Gas-sensitive material for detecting nitrogen oxides, preparation method, element and application

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CN108534055A (en) * 2018-03-05 2018-09-14 清华大学 A kind of fluorescence concentrated solar energy lighting system
CN108534055B (en) * 2018-03-05 2020-02-11 清华大学 Fluorescent light-collecting solar lighting system
CN108217718A (en) * 2018-03-13 2018-06-29 南方科技大学 A kind of ABX3Nanocrystalline synthetic method of perovskite and products thereof and purposes
CN108726583A (en) * 2018-07-17 2018-11-02 中山大学 A kind of full-inorganic perovskite A stablizing unleaded low band gaps2PdX6It is nanocrystalline and preparation method thereof
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CN111024672A (en) * 2020-01-06 2020-04-17 云南大学 Method for detecting mercury ions based on fluorescent perovskite liquid-liquid extraction
CN116359451A (en) * 2023-06-01 2023-06-30 之江实验室 Gas-sensitive material for detecting nitrogen oxides, preparation method, element and application
CN116359451B (en) * 2023-06-01 2023-10-31 之江实验室 Gas-sensitive material for detecting nitrogen oxides, preparation method, element and application

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