CN105441074A - Preparation method based on regulating and controlling CsPbBr3 perovskite quantum dots from blue light to green light - Google Patents
Preparation method based on regulating and controlling CsPbBr3 perovskite quantum dots from blue light to green light Download PDFInfo
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- CN105441074A CN105441074A CN201510794092.XA CN201510794092A CN105441074A CN 105441074 A CN105441074 A CN 105441074A CN 201510794092 A CN201510794092 A CN 201510794092A CN 105441074 A CN105441074 A CN 105441074A
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- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/66—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing germanium, tin or lead
- C09K11/664—Halogenides
- C09K11/665—Halogenides with alkali or alkaline earth metals
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Abstract
The invention discloses a method for preparing CsPbBr3 quantum dots of which the photoluminescence changes from blue light to green light. The method comprises the following steps: preparing corresponding CsPbBr3 quantum dots at different temperatures in a temperature range of 100-160 DEG C, wherein the CsPbBr3 quantum dots prepared at different temperatures have different fluorescence spectrums; and combining the corresponding CsPbBr3 quantum dots to ensure that the fluorescence spectrums thereof change from blue light into green light gradually. The invention also specifically discloses preparation steps. The CsPbBr3 perovskite quantum dots prepared at different temperatures have different fluorescence spectrums and have high photoluminescence efficiency and excellent optical absorption, and the synthesized CsPbBr3 perovskite quantum dots are high in degree of crystallinity and stable in performance, and have extensive application prospects in light-emitting diodes and solar batteries.
Description
Technical field
The invention belongs to semiconductor-quantum-point luminescent material technical field, particularly one is based on to CsPbBr
3the preparation method that uhligite quantum dot regulates and controls from blue light to green glow.
Background technology
Original uhligite refers to CaTiO
3, belong to the oxide compound of cubic crystal system, found by Russian scientist Perrault Paderewski, after with the name of his surname, the English name of uhligite is Perovskite.The structure of uhligite generally can be measured by aristotype, and most of uhligite is ABX
3type cubic space group composition is in cubes crystal formation.Uhligite was referred to as with the material of perovskite crystal structure afterwards similar.
Uhligite nano material is with a wide range of applications in the field such as solar cell and photodiode with the optics of excellence and electric property.Organo-metallic muriate CH3NH3PbX
3the research of (X=Cl, Br, I) uhligite nano particle causes the huge interest of more and more scholar, application especially in solar cells, makes the photoelectric transformation efficiency of solar cell bring up to 20.1% from 3%.The people such as LoredanaProtesescu report a kind of synthesis CsPbX at " Nano.Lett.DOI:10.1021/nl5048779 "
3the method of (X=Cl, Br, I) nano particle, and the spectral range by regulating the haloid element of different ratios to prepare the whole visible region of covering, our comprehensive quantum dot research method feature, based on the basis of this kind of method, in single research building-up process, temperature is to CsPbBr
3the impact of quantum dot light photoluminescence.
Summary of the invention
In view of this, the object of the present invention is to provide a kind of based on to CsPbBr
3the preparation method that uhligite quantum dot regulates and controls from blue light to green glow, described method is mainly undertaken realizing by regulating and controlling temperature.
For achieving the above object, the invention provides following technical scheme:
A kind of based on to CsPbBr
3the preparation method that uhligite quantum dot regulates and controls from blue light to green glow, in 100 ~ 160 DEG C of temperature ranges, prepares corresponding CsPbBr under condition of different temperatures
3quantum dot, obtains the CsPbBr of the isometric system of different fluorescence spectrum by different temperature of reaction
3nano particle, the CsPbBr prepared under 100 DEG C of temperature condition
3quantum dot light photoluminescence is blue light, the CsPbBr prepared under 160 DEG C of temperature condition
3quantum dot light photoluminescence is green glow, the CsPbBr prepared from 100 DEG C ~ 160 DEG C conditions
3quantum dot light photoluminescence becomes green glow gradually by blue light.
Further, under the temperature condition of 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, corresponding CsPbBr is prepared respectively
3quantum dot, by 5 kinds of corresponding CsPbBr
3quantum dot combines.
To CsPbBr
3the preparation method that uhligite quantum dot regulates and controls from blue light to green glow, step is as follows:
1): by Cs
2cO
3, octadecylene, oleic acid for 100:4:0.6 Homogeneous phase mixing with mass volume ratio (mg:ml:ml), is heated to 120 DEG C and keeps 1 hour under nitrogen protection condition, fully dissolve the precursor solution forming oleic acid-caesium;
2): by PbBr
2with octadecylene with mass volume ratio (mg:ml) for 69:5 mixing, be heated to 120 DEG C under nitrogen protection condition and keep 1 hour, also control temperature is under 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C conditions respectively to take out 5 increment product, and injection oleic acid and oleyl amine are to dissolving completely respectively;
3) presoma of the oleic acid-caesium: by step 1) prepared is injected into step 2 respectively) in every part of mixing solutions having prepared, reaction 5s, centrifugal solid, washs with toluene solution, finally be dissolved in toluene and preserve, get up 5 parts of product mixes gained CsPbBr
3its photoluminescence of quantum dot gradually becomes green glow by blue light.
Further, step 1) middle Cs
2cO
3quality is 100mg, and octadecylene volume is 4mL, and oleic acid volume is 0.6mL; Step 2) in sample by 69mgPbBr
2form with 5mL octadecylene; Step 3) in get presoma 0.4mL and the step 2 of oleic acid-caesium) sample mix.
Beneficial effect of the present invention is: present invention finds synthesis temperature to CsPbBr
3quantum dot has impact, enters method synthesis quantum dot, obtained the CsPbBr of different fluorescence spectrum by different temperature of reaction by heat
3nano particle, its photoluminescence quantum efficiencies reaches as high as 67%.The present invention is that hot injection method prepares CsPbBr
3the improvement continuity of quantum dot method, demonstrating synthesis temperature can affect CsPbBr
3uhligite quantum dot light Photoluminescence Properties, illustrates CsPbBr
3quantum dot optical property is controlled, and the CsPbBr of preparation
3quantum dot photoluminescence efficiency is high, good stability, can realize CsPbBr3 uhligite quantum dot light photoluminescence gradually changing from blue light to green glow based on temperature adjusting.
Accompanying drawing explanation
In order to make object of the present invention, technical scheme and beneficial effect clearly, the invention provides following accompanying drawing and being described:
Fig. 1 is CsPbBr at differential responses temperature
3the photoluminescence spectra of quantum dot, wherein A is fluorescence color figure, B is the photoluminescence spectra recorded by fluorescence spectrophotometer;
Fig. 2 is CsPbBr at differential responses temperature
3the uv-visible absorption spectroscopy of quantum dot;
Fig. 3 is CsPbBr at differential responses temperature
3the X-ray powder diffraction of quantum dot;
In Fig. 4, A is CsPbBr under 120 DEG C of conditions
3the scanning electron microscope diagram sheet of quantum dot, B is high resolution scanning electron microscope picture;
In Fig. 5, A is CsPbBr under 140 DEG C of conditions
3the scanning electron microscope diagram sheet of quantum dot, B is high resolution scanning electron microscope picture;
In Fig. 6, A is CsPbBr under 150 DEG C of conditions
3the scanning electron microscope diagram sheet of quantum dot, B is high resolution scanning electron microscope picture.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
Prepare the CsPbBr of photoluminescence from blue light to green glow as follows
3quantum dot:
1) under churned mechanically environment, by 100mgCs
2cO
3be dissolved in 4mL octadecylene and 0.6mL oleic acid solutions, under nitrogen protection condition, be heated to 120 DEG C, keep 1 hour, fully dissolve, form the precursor solution of oleic acid-caesium;
2) by 69mgPbBr
2be dissolved in 5mL octadecylene solution, make 5 parts, under nitrogen protection condition, be heated to 120 DEG C; keep 1 hour, by five increment product difference control temperature under 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C conditions, inject 0.5mL oleic acid and 0.5mL oleyl amine respectively; to dissolving completely
3) step 1 is got respectively) the presoma 0.4mL of oleic acid-caesium that prepared is injected into step 2) in every part of mixing solutions having prepared, reaction 5s, within centrifugal 5 minutes under 8000rpm condition, obtain solid, three times are washed with toluene solution, finally be dissolved in toluene and preserve, 5 parts of product mixes are got up to become the CsPbBr that can cover whole visible region spectral range
3quantum dot.
By the CsPbBr of correspondence prepared under temperature is 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C conditions respectively
3quantum dot fluorescence spectrophotometer (PL) is carried out detecting and is obtained CsPbBr corresponding under often kind of temperature condition respectively
3quantum dot photoluminescence spectra, as shown in Figure 1, wherein A is fluorescence color figure, B is the photoluminescence spectra recorded by fluorescence spectrophotometer.Photoluminescence wavelength variation with temperature can be significantly found out, the CsPbBr of the correspondence prepared under temperature is 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C conditions respectively by Fig. 1
3its photoluminescence of quantum dot gradually becomes green glow by blue light.
By the CsPbBr of correspondence prepared under temperature is 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C conditions respectively
3quantum dot uv-visible absorption spectroscopy instrument (ABS.) carries out detecting and obtains CsPbBr corresponding under often kind of temperature condition respectively
3the uv-visible absorption spectroscopy of quantum dot, as shown in Figure 2, can be found out by Fig. 2, the CsPbBr under differing temps
3uhligite quantum dot is to the absorption characteristic of the light of different-waveband.
By the CsPbBr of correspondence prepared under temperature is 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C conditions respectively
3quantum dot carries out X-ray powder diffraction (XRD) analysis, and analytical results as shown in Figure 3, can be found out by Fig. 3, the CsPbBr under differing temps
3uhligite quantum dot crystal formation, size-grade distribution and main component are consistent, and they can not be different along with the change of temperature of reaction.
By the CsPbBr of correspondence prepared under temperature is 120 DEG C, 140 DEG C, 150 DEG C conditions respectively
3quantum dot carries out transmission electron microscope (TEM) analysis, and respectively as shown in Figure 4,5, 6, wherein A is CsPbBr
3the scanning electron microscope diagram sheet of quantum dot, B is high resolution scanning electron microscope picture, can be found out by figure, and grain diameter and overall pattern can change along with temperature.
What finally illustrate is, above preferred embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although by above preferred embodiment to invention has been detailed description, but those skilled in the art are to be understood that, various change can be made to it in the form and details, and not depart from claims of the present invention limited range.
Claims (4)
1. one kind based on to CsPbBr
3the preparation method that uhligite quantum dot regulates and controls from blue light to green glow, is characterized in that, in 100 ~ 160 DEG C of temperature ranges, prepares corresponding CsPbBr under condition of different temperatures
3quantum dot, obtains the CsPbBr of the isometric system of different fluorescence spectrum by different temperature of reaction
3nano particle, the CsPbBr prepared under 100 DEG C of temperature condition
3quantum dot light photoluminescence is blue light, the CsPbBr prepared under 160 DEG C of temperature condition
3quantum dot light photoluminescence is green glow, the CsPbBr prepared from 100 DEG C ~ 160 DEG C conditions
3quantum dot light photoluminescence becomes green glow gradually by blue light.
2. according to claim 1 based on to CsPbBr
3the preparation method that uhligite quantum dot regulates and controls from blue light to green glow, is characterized in that, prepares corresponding CsPbBr respectively under the temperature condition of 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C
3quantum dot, by 5 kinds of corresponding CsPbBr
3quantum dot combines.
3. according to claim 2 based on to CsPbBr
3the preparation method that uhligite quantum dot regulates and controls from blue light to green glow, it is characterized in that, step is as follows:
1): by Cs
2cO
3, octadecylene, oleic acid for 100:4:0.6 Homogeneous phase mixing with mass volume ratio (mg:ml:ml), is heated to 120 DEG C and keeps 1 hour under nitrogen protection condition, fully dissolve the precursor solution forming oleic acid-caesium;
2): by PbBr
2with octadecylene with mass volume ratio (mg:ml) for 69:5 mixing, be heated to 120 DEG C under nitrogen protection condition and keep 1 hour, also control temperature is under 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C conditions respectively to take out 5 increment product, and injection oleic acid and oleyl amine are to dissolving completely respectively;
3) presoma of the oleic acid-caesium: by step 1) prepared is injected into step 2 respectively) in every part of mixing solutions having prepared, reaction 5s, centrifugal solid, washs with toluene solution, finally be dissolved in toluene and preserve, get up 5 parts of product mixes gained CsPbBr
3its photoluminescence of quantum dot gradually becomes green glow by blue light.
4. according to claim 3 based on to CsPbBr
3the preparation method that uhligite quantum dot regulates and controls from blue light to green glow, is characterized in that, step 1) middle Cs
2cO
3quality is 100mg, and octadecylene volume is 4mL, and oleic acid volume is 0.6mL; Step 2) in sample by 69mgPbBr
2form with 5mL octadecylene; Step 3) in get presoma 0.4mL and the step 2 of oleic acid-caesium) sample mix.
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| CN105883905A (en) * | 2016-04-08 | 2016-08-24 | 长安大学 | Method for preparing photoelectric material CsPbBr3 |
| CN106010518A (en) * | 2016-06-01 | 2016-10-12 | 中国科学院新疆理化技术研究所 | Copper-doped all-inorganic halogen perovskite fluorescent material and preparation method and application thereof |
| CN106006722A (en) * | 2016-06-24 | 2016-10-12 | 中国科学院合肥物质科学研究院 | Preparing method and application of orthorhombic phase cesium-lead iodide monocrystal nanowire |
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| CN106590644A (en) * | 2016-11-09 | 2017-04-26 | 佛山科学技术学院 | Preparation method of cesium-lead-bromine quantum dot |
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| CN113233775A (en) * | 2021-06-17 | 2021-08-10 | 中国科学院上海光学精密机械研究所 | Nano-Ag reinforced CsPbBr3Quantum dot glass and preparation method thereof |
| CN113621369A (en) * | 2021-08-16 | 2021-11-09 | 浙江大学 | Preparation method of perovskite material with multiple emission peaks, product and application thereof |
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| CN114456800B (en) * | 2022-02-10 | 2023-07-21 | 齐鲁工业大学 | Preparation method and application of perovskite quantum dot-molecular imprinting fluorescent coding microsphere for detecting sudan red I |
| CN116804151A (en) * | 2023-05-31 | 2023-09-26 | 广东工业大学 | Blue light emission perovskite quantum dot and preparation method and application thereof |
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