CN105441074B - One kind is based on to CsPbBr3The preparation method that perovskite quantum dot regulates and controls from blue light to green glow - Google Patents
One kind is based on to CsPbBr3The preparation method that perovskite quantum dot regulates and controls from blue light to green glow Download PDFInfo
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- CN105441074B CN105441074B CN201510794092.XA CN201510794092A CN105441074B CN 105441074 B CN105441074 B CN 105441074B CN 201510794092 A CN201510794092 A CN 201510794092A CN 105441074 B CN105441074 B CN 105441074B
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- 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
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Abstract
The invention discloses a kind of CsPbBr for preparing its luminescence generated by light from blue light to green glow3The method of quantum dot, by the way that in 100~160 DEG C of temperature ranges, corresponding CsPbBr is prepared under condition of different temperatures3Quantum dot, the CsPbBr prepared under condition of different temperatures3Quantum dot has different fluorescence spectrums, by corresponding CsPbBr3Quantum dot its fluorescence spectrum that combines gradually becomes green glow from blue light.The invention further particularly discloses preparation process, the CsPbBr prepared at different temperatures3Perovskite quantum dot has different fluorescence spectrums, and has efficient photoluminescence efficiency and excellent optical absorption, the CsPbBr of synthesis3Perovskite quantum dot crystallinity is high, stable performance.Have wide practical use in light emitting diode, solar cell.
Description
Technical field
It is more particularly to a kind of to be based on to CsPbBr the invention belongs to semiconductor-quantum-point luminescent material technical field3Calcium titanium
The preparation method that ore deposit quantum dot regulates and controls from blue light to green glow.
Background technology
Original perovskite refers to CaTiO3, belong to the oxide of cubic crystal system, found by Russian scientist Perrault Paderewski,
Named afterwards with his surname, the English name of perovskite is Perovskite.The structure of perovskite is typically printed with jade-like stone sieve tincture silver chlorate
Phase method can be measured, and most of perovskite is ABX3Type cubic space group composition is in cube crystal formation.Later similar with calcium titanium
The material of ore deposit crystal structure is referred to as perovskite.
Perovskite nano material has with excellent optically and electrically performance in the field such as solar cell and light emitting diode
Have wide practical use.Organic metal chloride CH3NH3PbX3The research of (X=Cl, Br, I) perovskite nano particle causes
The huge interest of more and more scholars, application especially in solar cells so that the opto-electronic conversion effect of solar cell
Rate brings up to 20.1% from 3%.Loredana Protesescu et al. are in " Nano.Lett.DOI:10.1021/
Nl5048779 " reports a kind of synthesis CsPbX3The method of (X=Cl, Br, I) nano particle, and by adjusting different proportion
Halogen be prepared for covering the spectral region of whole visible region, we integrate quantum dot research method feature, are based on
On the basis of such a method, temperature is to CsPbBr in single research building-up process3The influence of quantum dot light photoluminescence.
The content of the invention
In view of this, it is an object of the invention to provide one kind to be based on to CsPbBr3Perovskite quantum dot is from blue light to green
The preparation method of light regulation and control, methods described are mainly what is realized by regulating and controlling temperature.
To reach above-mentioned purpose, the present invention provides following technical scheme：
One kind is based on to CsPbBr3The preparation method that perovskite quantum dot regulates and controls from blue light to green glow, at 100~160 DEG C
In temperature range, corresponding CsPbBr is prepared under condition of different temperatures3Quantum dot, obtained not by different reaction temperatures
With the CsPbBr of the cubic system of fluorescence spectrum3Nano particle, the CsPbBr prepared under 100 DEG C of temperature conditionss3The photic hair of quantum dot
Light is in blue light, the CsPbBr prepared under 160 DEG C of temperature conditionss3Quantum dot light photoluminescence is in green glow, from 100 DEG C~160 DEG C conditions
The CsPbBr of lower preparation3Quantum dot light photoluminescence gradually becomes green glow by blue light.
Further, corresponding to preparing respectively under 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C of temperature conditionss
CsPbBr3Quantum dot, by CsPbBr corresponding to 5 kinds3Quantum dot combines.
To CsPbBr3The preparation method that perovskite quantum dot regulates and controls from blue light to green glow, step are as follows：
1)：By Cs2CO3, octadecylene, oleic acid is with mass volume ratio (mg:ml:Ml it is) 100:4:0.6 uniformly mixing, nitrogen
120 DEG C are heated under protective condition and is kept for 1 hour, fully dissolving forms the precursor solution of oleic acid-caesium；
2)：By PbBr2With octadecylene with mass volume ratio (mg:Ml it is) 69:5 mix, and are heated under nitrogen protective condition
120 DEG C and keep 1 hour, take out 5 parts of samples simultaneously respectively control temperature in 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C of conditions
Under, oleic acid and oleyl amine are injected separately into being completely dissolved；
3)：The presoma for oleic acid-caesium that step 1) preparation is completed is injected separately into every part of step 2) preparation completion and mixed
Close in solution, react 5s, centrifuge to obtain solid, washed with toluene solution, be finally dissolved in toluene and preserve, by 5 parts of product mixes
Get up gained CsPbBr3Its luminescence generated by light of quantum dot gradually becomes green glow by blue light.
Further, Cs in step 1)2CO3Quality is 100mg, and octadecylene volume is 4mL, and oleic acid volume is 0.6mL；Step
2) sample is by 69mg PbBr in2Formed with 5mL octadecylenes；The presoma 0.4mL and step 2) of oleic acid-caesium are taken in step 3)
Sample mixes.
The beneficial effects of the present invention are：Present invention finds synthesis temperature to CsPbBr3Quantum dot has an impact, and passes through heat
Enter method synthesis quantum dot, the CsPbBr of different fluorescence spectrums is obtained by different reaction temperatures3Nano particle, its luminescence generated by light
Quantum efficiency reaches as high as 67%.The present invention is that hot injection method prepares CsPbBr3The improvement of quantum point methods continues, and demonstrates conjunction
CsPbBr can be influenceed into temperature3Perovskite quantum dot light Photoluminescence Properties, illustrate CsPbBr3Quantum dot optical property is controllable, and
And the CsPbBr prepared3Quantum dot light photoluminescence efficiency high, stability is good, and CsPbBr3 calcium titaniums can be realized based on temperature adjusting
Ore deposit quantum dot light photoluminescence gradually changing from blue light to green glow.
Brief description of the drawings
In order that the purpose of the present invention, technical scheme and beneficial effect are clearer, the present invention provides drawings described below and carried out
Explanation：
Fig. 1 is CsPbBr at a temperature of differential responses3The photoluminescence spectra of quantum dot, wherein A are fluorescence color figure, and B is
The photoluminescence spectra measured by XRF；
Fig. 2 is CsPbBr at a temperature of differential responses3The uv-visible absorption spectroscopy of quantum dot；
Fig. 3 is CsPbBr at a temperature of differential responses3The X-ray powder diffraction of quantum dot；
A is CsPbBr under the conditions of 120 DEG C in Fig. 43The scanning electron microscope diagram piece of quantum dot, B are high resolution scanning
Electron microscope picture；
A is CsPbBr under the conditions of 140 DEG C in Fig. 53The scanning electron microscope diagram piece of quantum dot, B are high resolution scanning
Electron microscope picture；
A is CsPbBr under the conditions of 150 DEG C in Fig. 63The scanning electron microscope diagram piece of quantum dot, B are high resolution scanning
Electron microscope picture.
Embodiment
Below in conjunction with accompanying drawing, the preferred embodiments of the present invention are described in detail.
It is prepared as follows CsPbBr of the luminescence generated by light from blue light to green glow3Quantum dot：
1) in the environment of mechanical agitation, by 100mg Cs2CO3It is dissolved in 4mL octadecylenes and 0.6mL oleic acid solutions, nitrogen
120 DEG C are heated under protective condition, is kept for 1 hour, fully dissolving, forms the precursor solution of oleic acid-caesium；
2) by 69mg PbBr2It is dissolved in 5mL octadecylene solution, makes 5 parts, 120 DEG C are heated under nitrogen protective condition,
Kept for 1 hour, control temperature to be noted respectively under the conditions of 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C respectively in five parts of samples
Enter 0.5mL oleic acid and 0.5mL oleyl amines, to being completely dissolved,
3) take step 1) to prepare the presoma 0.4mL for the oleic acid-caesium completed respectively and be injected into the every of step 2) preparation completion
In part mixed solution, 5s is reacted, solid is centrifuged 5 minutes to obtain under the conditions of 8000rpm, is washed three times with toluene solution, it is last molten
Solution preserves in toluene, and 5 parts of product mixes, which are got up, turns into the CsPbBr that can cover whole visible region spectral region3Quantum
Point.
The corresponding CsPbBr prepared under the conditions of will being respectively 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C in temperature3
Quantum dot carries out detection with XRF (PL) and respectively obtains corresponding CsPbBr under every kind of temperature conditionss3The photic hair of quantum dot
Light spectrum, as shown in figure 1, wherein A is fluorescence color figure, B is the photoluminescence spectra measured by XRF.Pass through figure
1 can significantly find out photoluminescence wavelength variation with temperature, respectively temperature be 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C,
The corresponding CsPbBr prepared under the conditions of 160 DEG C3Its luminescence generated by light of quantum dot gradually becomes green glow by blue light.
The corresponding CsPbBr prepared under the conditions of will being respectively 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C in temperature3
Quantum dot is carried out corresponding to detection respectively obtains under every kind of temperature conditionss with uv-visible absorption spectroscopy instrument (ABS.)
CsPbBr3The uv-visible absorption spectroscopy of quantum dot, as shown in Fig. 2 can be seen that by Fig. 2, the CsPbBr under different temperatures3
Absorption characteristic of the perovskite quantum dot to the light of different-waveband.
The corresponding CsPbBr prepared under the conditions of will being respectively 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C in temperature3
Quantum dot carries out X-ray powder diffraction (XRD) analysis, and analysis result by Fig. 3 as shown in figure 3, can be seen that, under different temperatures
CsPbBr3Perovskite quantum dot crystal formation, size distribution with main component be it is consistent, its will not with the change of reaction temperature and
It is different.
The corresponding CsPbBr prepared under the conditions of will being respectively 120 DEG C, 140 DEG C, 150 DEG C in temperature3Quantum dot carries out saturating
Electron microscope (TEM) analysis is penetrated, respectively as shown in Figure 4,5, 6, wherein A is CsPbBr3The SEM of quantum dot
Picture, B are high resolution scanning electron microscope picture, be can be seen that by figure, grain diameter and overall pattern can be with temperature
And change.
Finally illustrate, preferred embodiment above is merely illustrative of the technical solution of the present invention and unrestricted, although logical
Cross above preferred embodiment the present invention is described in detail, it is to be understood by those skilled in the art that can be
Various changes are made to it in form and in details, without departing from claims of the present invention limited range.
Claims (4)
1. one kind is based on to CsPbBr3The preparation method that perovskite quantum dot regulates and controls from blue light to green glow, it is characterised in that 100
In ~ 160 DEG C of temperature ranges, corresponding CsPbBr is prepared under condition of different temperatures3Quantum dot, pass through different reaction temperatures
Obtain the CsPbBr of the cubic system of different fluorescence spectrums3Nano particle, the CsPbBr prepared under 100 DEG C of temperature conditionss3Quantum dot
Luminescence generated by light is in blue light, the CsPbBr prepared under 160 DEG C of temperature conditionss3Quantum dot light photoluminescence is in green glow, from 100 DEG C ~ 160 DEG C
Under the conditions of the CsPbBr for preparing3Quantum dot light photoluminescence gradually becomes green glow by blue light；The step of preparation method, is as follows：
1）：By Cs2CO3, octadecylene, oleic acid is with mass volume ratio mg:ml:Ml is 100:4:0.6 uniformly mixing, nitrogen ceiling
120oC is heated under part and is kept for 1 hour, fully dissolving forms the precursor solution of oleic acid-caesium；
2）：By PbBr2With octadecylene with mass volume ratio mg:Ml is 69:5 are mixed, and 120 DEG C are heated to simultaneously under nitrogen protective condition
Kept for 1 hour, take out 5 parts of samples and control temperature respectively under the conditions of 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, respectively
Injection oleic acid and oleyl amine are to being completely dissolved；
3）：By step 1）The presoma for preparing the oleic acid-caesium completed is injected separately into step 2）It is molten to prepare the every part of mixing completed
In liquid, 5s is reacted, solid is centrifuged to obtain, is washed with toluene solution, be finally dissolved in toluene and preserve, 5 parts of product mixes are got up
Gained CsPbBr3Its luminescence generated by light of quantum dot gradually becomes green glow by blue light.
2. it is based on according to claim 1 to CsPbBr3The preparation method that perovskite quantum dot regulates and controls from blue light to green glow, its
It is characterised by, prepares corresponding CsPbBr under 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C of temperature conditionss respectively3Amount
It is sub-, by CsPbBr corresponding to 5 kinds3Quantum dot combines.
3. it is based on according to claim 2 to CsPbBr3The preparation method that perovskite quantum dot regulates and controls from blue light to green glow, its
It is characterised by, step is as follows：
1）：By Cs2CO3, octadecylene, oleic acid is with mass volume ratio mg:ml:Ml is 100:4:0.6 uniformly mixing, nitrogen ceiling
120oC is heated under part and is kept for 1 hour, fully dissolving forms the precursor solution of oleic acid-caesium；
2）：By PbBr2With octadecylene with mass volume ratio mg:Ml is 69:5 are mixed, and 120 DEG C are heated to simultaneously under nitrogen protective condition
Kept for 1 hour, take out 5 parts of samples and control temperature respectively under the conditions of 100 DEG C, 120 DEG C, 140 DEG C, 150 DEG C, 160 DEG C, respectively
Injection oleic acid and oleyl amine are to being completely dissolved；
3）：By step 1）The presoma for preparing the oleic acid-caesium completed is injected separately into step 2）It is molten to prepare the every part of mixing completed
In liquid, 5s is reacted, solid is centrifuged to obtain, is washed with toluene solution, be finally dissolved in toluene and preserve, 5 parts of product mixes are got up
Gained CsPbBr3Its luminescence generated by light of quantum dot gradually becomes green glow by blue light.
4. it is based on according to claim 3 to CsPbBr3The preparation method that perovskite quantum dot regulates and controls from blue light to green glow, its
It is characterised by, step 1）Middle Cs2CO3Quality is 100 mg, and octadecylene volume is 4 mL, and oleic acid volume is 0.6 mL；Step 2）In
Sample is by 69 mg PbBr2Formed with 5 mL octadecylenes；Step 3）In take the presoma 0.4mL of oleic acid-caesium and step 2）Sample
Product mix.
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