CN110117024A - A kind of unleaded caesium copper iodine perovskite blue light of zero dimension is nanocrystalline and preparation method thereof - Google Patents
A kind of unleaded caesium copper iodine perovskite blue light of zero dimension is nanocrystalline and preparation method thereof Download PDFInfo
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- CN110117024A CN110117024A CN201910556439.5A CN201910556439A CN110117024A CN 110117024 A CN110117024 A CN 110117024A CN 201910556439 A CN201910556439 A CN 201910556439A CN 110117024 A CN110117024 A CN 110117024A
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- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/006—Compounds containing, besides copper, two or more other elements, with the exception of oxygen or hydrogen
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- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/61—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing fluorine, chlorine, bromine, iodine or unspecified halogen elements
- C09K11/615—Halogenides
- C09K11/616—Halogenides with alkali or alkaline earth metals
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Abstract
It is nanocrystalline and preparation method thereof the present invention relates to a kind of unleaded caesium copper iodine perovskite blue light of zero dimension, belong to photoelectron material preparation technical field.This is nanocrystalline to be prepared as follows: cesium iodide and cuprous iodide are dissolved in N, in dinethylformamide or dimethyl sulfoxide, obtain precursor solution, then the precursor solution is injected in organic solution, centrifuging and taking precipitates, after washing after 3-6min is stirred to react under the speed of 5000-9000rpm.This is nanocrystalline not only with good crystal structure, yield height, fluorescence efficiency height and stable structure, and does not contain heavy metal lead, reduces the harm to human body and environment, has a wide range of applications in terms of photoelectric device.This nanometer of crystal preparation method simply easily realize, and at low cost, can be promoted in the industrial production.
Description
Technical field
The invention belongs to photoelectron material preparation technical fields, and in particular to a kind of unleaded caesium copper iodine perovskite blue light of zero dimension
It is nanocrystalline and preparation method thereof.
Background technique
Full-inorganic lead halogen perovskite nano material is as a kind of novel inorganic functional material, with excellent optically and electrically property
It can be with a wide range of applications in solar battery, the fields such as light emitting diode and micro- laser.Although full-inorganic lead halogen calcium titanium
The preparation of mine nano material has been achieved for biggish development, but it still remains following problems: 1, high-performance blue light is nanocrystalline
Luminescent material lacks, at present type of the adjusting of the nanocrystalline emission wavelength of lead halogen perovskite dependent on halogen atom, and lead halogen
The nanocrystalline usual luminous efficiency low (PLQY < 30%) of perovskite, thermal stability are poor.Although the launch wavelength of lead bromine flaky nanocrystalline
Can be from green light blue shift to blue light, but the system is easy that orientation absorption occurs under light illumination, forms aggregation, blue light is caused to be sent out
Raw red shift.2, different halogen perovskites it is nanocrystalline between anion exchange reaction, although realize light emitting region from blue light to
The adjusting of feux rouges, but a series of problems such as spectral width, chromaticity drift are also brought simultaneously.3, lead halogen perovskite contains weight
Metallic lead has harmfulness to human body and environment, limits its following application in luminescence display field.Therefore, existing preparation
The technology of full-inorganic lead halogen perovskite nano material has yet to be improved and developed, and less toxic, efficient blue light nanometer material is urgently
It excavates.
Summary of the invention
In view of this, one of the objects of the present invention is to provide a kind of unleaded caesium copper iodine perovskite blue light of zero dimension is nanocrystalline
Preparation method；The second purpose is to provide a kind of unleaded caesium copper iodine perovskite blue light of zero dimension nanocrystalline.
In order to achieve the above objectives, the invention provides the following technical scheme:
1, a kind of nanocrystalline preparation method of the unleaded caesium copper iodine perovskite blue light of zero dimension, the method are as follows:
Cesium iodide and cuprous iodide are dissolved in n,N-Dimethylformamide or dimethyl sulfoxide, precursor solution is obtained,
Then the precursor solution is injected in organic solution, is centrifuged after 3-6min is stirred to react under the speed of 5000-9000rpm
After taking precipitating, washing.
Preferably, the mass volume ratio of the cesium iodide, cuprous iodide and n,N-Dimethylformamide or dimethyl sulfoxide
For 388-410:189-191:1, the unit of the mass volume ratio is mg:mg:mL.
Preferably, the cesium iodide and cuprous iodide are dissolved in n,N-Dimethylformamide or dimethyl sulfoxide specifically:
Cesium iodide and cuprous iodide are added in n,N-Dimethylformamide or dimethyl sulfoxide, stirred at 30-60 DEG C to cesium iodide
It is dissolved in N,N-dimethylformamide or dimethyl sulfoxide with cuprous iodide.
Preferably, the organic solution is one of toluene, chloroform or isopropanol.
Preferably, the centrifugation is specially to be centrifuged 3-6min with the speed of 5000-9000rpm.
Preferably, the washing is specially with organic solution washing 2-5 times.
2, the zero dimension leadless copper base perovskite blue light prepared by the method is nanocrystalline.
The beneficial effects of the present invention are: the present invention provides a kind of unleaded caesium copper iodine perovskite blue light of zero dimension it is nanocrystalline and
Preparation method, the unleaded caesium copper iodine perovskite blue light of the zero dimension is nanocrystalline not only to have good crystal structure, yield height, fluorescence
High-efficient and stable structure, and heavy metal lead is not contained, reduce the harm to human body and environment, has in terms of photoelectric device
Broad application prospect.This nanometer of crystal preparation method simply easily realize, and at low cost, can be pushed away in the industrial production
Extensively.
Other advantages, target and feature of the invention will be illustrated in the following description to a certain extent, and
And to a certain extent, based on will be apparent to those skilled in the art to investigating hereafter, Huo Zheke
To be instructed from the practice of the present invention.Target of the invention and other advantages can be realized by following specification and
It obtains.
Detailed description of the invention
To make the objectives, technical solutions, and advantages of the present invention clearer, the present invention is made below in conjunction with attached drawing excellent
The detailed description of choosing, in which:
Fig. 1 is the Cs prepared in embodiment 13Cu2I5Blue light nanocrystalline exciting light spectrogram and fluorescence spectra；
Fig. 2 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline photo under fluorescent lamp and UV light respectively of blue light；(Fig. 2
Middle a is the nanocrystalline photo under fluorescent light, and b is the nanocrystalline photo under w light in Fig. 2)
Fig. 3 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline X-ray diffractogram of blue light；
Fig. 4 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline scanning electron microscope diagram of blue light；
Fig. 5 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline transmission electron microscope figure of blue light and X-ray energy color
Astigmatism spectrogram；
Fig. 6 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline fluorescence efficiency test result figure of blue light；
Fig. 7 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline stability test result figure of blue light；
Fig. 8 is the Cs prepared in embodiment 23Cu2I5The nanocrystalline fluorescence spectra of blue light；
Fig. 9 is the Cs prepared in embodiment 23Cu2I5The nanocrystalline scanning electron microscope diagram of blue light；
Figure 10 is the Cs prepared in embodiment 33Cu2I5The nanocrystalline X-ray diffractogram of blue light；
Figure 11 is the Cs prepared in embodiment 33Cu2I5The nanocrystalline scanning electron microscope diagram of blue light.
Specific embodiment
Illustrate embodiments of the present invention below by way of specific specific example, those skilled in the art can be by this specification
Other advantages and efficacy of the present invention can be easily understood for disclosed content.The present invention can also pass through in addition different specific realities
The mode of applying is embodied or practiced, the various details in this specification can also based on different viewpoints and application, without departing from
Various modifications or alterations are carried out under spirit of the invention.
Embodiment 1
Prepare the unleaded caesium copper iodine (Cs of zero dimension3Cu2I5) perovskite blue light is nanocrystalline
389.72mg cesium iodide and 190.45mg cuprous iodide are added in 1mL n,N-Dimethylformamide, at 60 DEG C
Stirring to cesium iodide and cuprous iodide is dissolved in n,N-Dimethylformamide, obtains precursor solution, then infuses precursor solution
Enter in isopropanol, precipitating is taken with the speed of 6000rpm centrifugation 3min after being stirred to react 4min under the speed of 5000rpm, then with
Isopropanol washs 2 times, and Cs is made3Cu2I5Blue light is nanocrystalline.
Embodiment 2
Prepare the unleaded caesium copper iodine (Cs of zero dimension3Cu2I5) perovskite blue light is nanocrystalline
400mg cesium iodide and 189mg cuprous iodide are added in 1mL dimethyl sulfoxide, stirred at 60 DEG C to cesium iodide
It is dissolved in dimethyl sulfoxide with cuprous iodide, obtains precursor solution, then injects precursor solution in isopropanol,
After being stirred to react 6min under the speed of 7000rpm, precipitating is taken with the speed centrifugation 4min of 5000rpm, then with isopropanol washing 2
It is secondary, Cs is made3Cu2I5Blue light is nanocrystalline.
Embodiment 3
Prepare the unleaded caesium copper iodine (Cs of zero dimension3Cu2I5) perovskite blue light is nanocrystalline
410mg cesium iodide and 191mg cuprous iodide are added in 1mL n,N-Dimethylformamide, stirred at 50 DEG C to
Cesium iodide and cuprous iodide are dissolved in n,N-Dimethylformamide, obtain precursor solution, precursor solution is then injected toluene
In, after being stirred to react 3min under the speed of 9000rpm, precipitating is taken with the speed centrifugation 6min of 9000rpm, then wash with toluene
4 times, Cs is made3Cu2I5Blue light is nanocrystalline.
Fig. 1 is the Cs prepared in embodiment 13Cu2I5Blue light nanocrystalline exciting light spectrogram and fluorescence spectra, can by Fig. 1
Know, the nanocrystalline best excitation peak is about in 300nm, and optimal luminescent peak is in 446nm or so.
Fig. 2 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline photo under fluorescent lamp and UV light respectively of blue light, wherein
A is the nanocrystalline photo under fluorescent light in Fig. 2, and b is the nanocrystalline photo under w light in Fig. 2, as shown in Figure 2,
Under the excitation of UV light, the nanocrystalline blue light-emitting is corresponding with the fluorescence spectra in Fig. 1.
Fig. 3 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline X-ray diffractogram of blue light, from the figure 3, it may be seen that this is nanocrystalline
Diffraction maximum and Cs3Cu2I5Standard card (JCPDS No.79-0333) is corresponding, illustrates the Cs of preparation3Cu2I5With good crystal
Structure.
Fig. 4 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline scanning electron microscope diagram of blue light as shown in Figure 4 should
Nanocrystalline particle size is in 200nm or so.
Fig. 5 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline transmission electron microscope figure of blue light and X-ray energy color
Astigmatism spectrogram, as shown in Figure 5, the Cs3Cu2I5The nanocrystalline tri- kinds of elements of middle Cs, Cu, I of blue light are uniformly distributed.
Fig. 6 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline fluorescence efficiency test result figure of blue light, it will be appreciated from fig. 6 that
The Cs3Cu2I5The nanocrystalline luminous efficiency with higher of blue light.
Fig. 7 is the Cs prepared in embodiment 13Cu2I5The nanocrystalline stability test result figure of blue light, test condition are as follows: wet
Degree 75%, temperature 60 C, as shown in Figure 7, the Cs3Cu2I5The nanocrystalline stability with higher of blue light.
Fig. 8 is the Cs prepared in embodiment 23Cu2I5The nanocrystalline fluorescence spectra of blue light, as shown in Figure 8, this is nanocrystalline
Glow peak in 447nm or so.
Fig. 9 is the Cs prepared in embodiment 23Cu2I5The nanocrystalline scanning electron microscope diagram of blue light as shown in Figure 9 should
Nanocrystalline particle size is in 250nm or so.
Figure 10 is the Cs prepared in embodiment 33Cu2I5The nanocrystalline X-ray diffractogram of blue light, as shown in Figure 10, the nanometer
Brilliant diffraction maximum and Cs3Cu2I5Standard card (JCPDS No.79-0333) is corresponding.
Figure 11 is the Cs prepared in embodiment 33Cu2I5The nanocrystalline scanning electron microscope diagram of blue light, as shown in Figure 11,
The nanocrystalline particle size is in 300nm or so.
Finally, it is stated that the above examples are only used to illustrate the technical scheme of the present invention and are not limiting, although referring to compared with
Good embodiment describes the invention in detail, those skilled in the art should understand that, it can be to skill of the invention
Art scheme is modified or replaced equivalently, and without departing from the objective and range of the technical program, should all be covered in the present invention
Scope of the claims in.
Claims (7)
1. a kind of preparation method that the unleaded caesium copper iodine perovskite blue light of zero dimension is nanocrystalline, which is characterized in that the method is as follows:
Cesium iodide and cuprous iodide are dissolved in n,N-Dimethylformamide or dimethyl sulfoxide, obtain precursor solution, then
The precursor solution is injected in organic solution, centrifuging and taking is heavy after 3-6min is stirred to react under the speed of 5000-9000rpm
It forms sediment, after washing.
2. the method as described in claim 1, which is characterized in that the cesium iodide, cuprous iodide and n,N-Dimethylformamide
Or the mass volume ratio of dimethyl sulfoxide is 388-410:189-191:1, the unit of the mass volume ratio is mg:mg:mL.
3. the method as described in claim 1, which is characterized in that the cesium iodide and cuprous iodide are dissolved in N, N- dimethyl formyl
In amine or dimethyl sulfoxide specifically: cesium iodide and cuprous iodide are added in n,N-Dimethylformamide or dimethyl sulfoxide,
Stirring to cesium iodide and cuprous iodide is dissolved in N,N-dimethylformamide or dimethyl sulfoxide at 30-60 DEG C.
4. the method as described in claim 1, which is characterized in that the organic solution is one in toluene, chloroform or isopropanol
Kind.
5. the method as described in claim 1, which is characterized in that the centrifugation is specially to be centrifuged with the speed of 5000-9000rpm
3-6min。
6. method as claimed in claim 4, which is characterized in that the washing is specially with organic solution washing 2-5 times.
7. nanocrystalline by zero dimension leadless copper base perovskite blue light prepared by method described in any one of claims 1-6.
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| CN111139068A (en) * | 2019-12-03 | 2020-05-12 | 北京理工大学 | Zero-dimensional lead-free perovskite Cs3Cu2X5Preparation method and application of |
| CN111661867A (en) * | 2020-06-30 | 2020-09-15 | 重庆大学 | Preparation method of lead-free cesium copper chloride nanocrystalline and product and application thereof |
| CN111676014A (en) * | 2020-05-22 | 2020-09-18 | 中央民族大学 | Lead-free perovskite quantum dot and in-situ conversion synthesis method and application thereof |
| CN111792665A (en) * | 2020-07-17 | 2020-10-20 | 湘潭大学 | Method for high-pressure solid-phase synthesis of copper-cesium-iodide lead-free quantum dots |
| CN112048764A (en) * | 2020-08-17 | 2020-12-08 | 南京航空航天大学 | Zero-dimensional Cs3Cu2I5Perovskite scintillation crystal and application thereof |
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