CN109761498A - A kind of KxCs1-xPbBr3Devitrified glass and preparation method thereof - Google Patents
A kind of KxCs1-xPbBr3Devitrified glass and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of K1‑xCsxPbBr3Quantum dot devitrified glass and preparation method thereof.The K1‑xCsxPbBr3Quantum dot devitrified glass uses B2O3‑SiO2Zno-based glass system, KxCs1‑ xPbBr3Quantum dot is evenly distributed on B2O3‑SiO2In zno-based glass system;The KxCs1‑xPbBr3Quantum dot devitrified glass is with B2O3、SiO2、ZnO、Cs2CO3、K2CO3、PbBr2, NaBr be prepared for raw material, wherein Cs2CO3、K2CO3、PbBr2, NaBr be quantum dot raw material, the mass percentage of each raw material component are as follows: B2O318.1-20.6%, SiO218.1-20.6%, ZnO 10.9-12.0%, Cs2CO39.9-21.2%, K2CO32.3-5.8%, PbBr217.3-19.1%, NaBr 10.9-12.0%.The K1‑xCsxPbBr3The preparation method of quantum dot devitrified glass follows the steps below: (1) mixing of glass raw material;(2) fusing of glass raw material;(3) it anneals;(4) it is heat-treated.K of the present invention1‑ xCsxPbBr3Quantum dot devitrified glass quantum efficiency is high and with good stability, third-order non-linear and upconversion mechanism, tool have been widely used.
Description
(1) technical field
The present invention relates to a kind of KxCs1-xPbBr3Quantum dot microcrystal glass material and preparation method thereof belongs to research quantum
Point microcrystal glass area.
(2) background technique
Currently, quanta point material has become one of the new material that current industry is paid close attention to the most, is widely used in photophore
The basic research and application and development in the fields such as part, solar battery, catalysis, biomarker and biomedicine.In quanta point material
In field, full-inorganic halide perovskite quantum dot has become the hot spot of focus concerned by people and research, and research achievement is such as
It emerges one after another as emerging rapidly in large numbersBamboo shoots after a spring rain.Full-inorganic halide perovskite quanta point material, due to having the very excellent characteristics of luminescence,
And become new research hotspot, compared with traditional rare earth fluorescent powder, perovskite quantum dot shows many excellent fluorescences
Matter, such as: narrow transmitting band, high quantum production rate, shine it is excellent, cover full spectrum the advantages that.This excellent characteristic will make it aobvious
Show, there is important application in the fields such as backlight, solid-state lighting, can be rated as with multiduty New Generation Optical electronic material.This
Studying the content being related to includes K1-xCsxPbBr3Synthesis, pattern control, performance characterization and the blue chip of perovskite nano material
White light LEDs of excitation etc..2014, Kovalenko [1] et al. synthesized CsPbX for the first time in the method for heat injection3(X
=Cl, Br, I) nanocrystalline passes through research discovery CsPbX3Light emitting region cover the range (410- of entire visible light
700nm), there is very high quantum yield, CsPbX3Perovskite is nanocrystalline to show excellent optical property.2017,
Jialong Zhao et al. successfully synthesizes Mn2+The CsPbCl of doping3QDs, Mn2+At concentrations up to 14%.The Mn of synthesis2+
The CsPbCl of doping3QDs shows Mn2+Characteristic luminescence peak.With doping Mn2+Concentration increase, quantum efficiency also exists
It gradually increases.Work as Mn2+Concentration be~3 ± 1% when, quantum efficiency is up to 60%.2017, Hongwei Song seminar
Synthesize CsPbCl1.5Br1.5:Yb3+,Ce3+QDs, since the QDs of synthesis has big absorption cross-section, weaker Electron Phonon coupling
It closes and high internal quantum efficiency (146%), the quantum dot can be used as the lower transition material of silica-based solar cell.And the battery
PCE is promoted to 21.5% from 18.1%.Next, the seminar is again successful in CsPbCl3Different rare earths is doped in QDs
Ion (Ce3+,Sm3+,Eu3+,Tb3+,Dy3+,Er3+,Yb3+).2018, Daniel Amgar seminar et al. successfully synthesized
The Rb of Rb doping1-xCsxPbBr3Perovskite is nanocrystalline, and the introducing of Rb2CO3 improves the ability of halide anion exchange, improves
The stability of its structure, Rb1-xCsxPbBr3Perovskite is nanocrystalline to compare CsPbBr3The nanocrystalline amount with higher of perovskite
Sub- efficiency, and the presence of rubidium ion is demonstrated by transmission electron microscope and EDS energy spectrum analysis.
(3) summary of the invention
Matter of utmost importance to be solved by this invention is to provide a kind of KxCs1-xPbBr3Quantum dot devitrified glass, quantum efficiency
High and with good stability, third-order non-linear and upconversion mechanism.
Second technical problem to be solved by this invention be to provide a kind of preparation process it is simple, it is at low cost, be easy to batch
The K of production1-xCsxPbBr3The method of quantum dot devitrified glass, makes KxCs1-xPbBr3Quantum dot is in B2O3-SiO2Zno-based glass
It generates and realizes in system and be uniformly distributed.
Technical solution used by the present invention solves the above problems is as follows:
On the one hand, the present invention provides a kind of K1-xCsxPbBr3Quantum dot devitrified glass, the K1-xCsxPbBr3Amount
Son point devitrified glass uses B2O3-SiO2Zno-based glass system, KxCs1-xPbBr3Quantum dot is evenly distributed on B2O3-SiO2-
In zno-based glass system;
The KxCs1-xPbBr3Quantum dot devitrified glass is with B2O3、SiO2、ZnO、Cs2CO3、K2CO3、 PbBr2、
NaBr is prepared for raw material, wherein Cs2CO3、K2CO3、PbBr2, NaBr be quantum dot raw material, the quality hundred of each raw material component
Divide content are as follows: B2O318.1-20.6%, SiO218.1-20.6%, ZnO 10.9-12.0%, Cs2CO39.9-21.2%,
K2CO32.3-5.8%, PbBr217.3-19.1%, NaBr 10.9-12.0%.
Preferably, with B2O3、SiO2The quality that feeds intake with ZnO is 100% meter, B2O3、SiO2Mass ratio with ZnO is
38.7-38.9%:38.7-38.9%:22.3-22.6%.
Preferably, B2O3And SiO2Feed intake identical in quality, feeding intake for ZnO and NaBr is identical in quality.
The mass percentage of the present invention most preferably each raw material component are as follows: B2O320.0%, SiO220.0%, ZnO
11.5%, Cs2CO311.3%, K2CO37.3%, PbBr218.5%, NaBr 11.5%.
The KxCs1-xPbBr3In quantum dot devitrified glass, with incorporation of the K in quantum dot, quantum dot devitrified glass
Quantum efficiency increase accordingly, when the doping of K be K/Cs=0.6/0.4 (i.e. x=0.6) when, XRD appearance is best, quantum effect
Rate highest.
Second aspect, the present invention provide a kind of KxCs1-xPbBr3The preparation method of quantum dot devitrified glass, according to following step
It is rapid to carry out:
(1) analysis pure raw material B is accurately weighed according to raw material proportioning2O3、SiO2、ZnO、Cs2CO3、K2CO3、 PbBr2, NaBr,
It is then placed in mortar, slight (purpose slightly ground is the original form in order to keep glass raw material) mixed grinding is uniform
It is placed in crucible;
(2) fusing of glass raw material: being put into crucible in high temperature resistance furnace, heat up to it, and fusion temperature is
1200-1300 DEG C, glass melt is poured on pig mold after reaching preset temperature, then after carrying out heat preservation to it 10-30 minutes;
(3) there will be the pig mold of glass melt to be placed in high temperature furnace to anneal, be protected in glass transformation temperature Tg temperature
It is 4-6 hours warm, it is then shut off high temperature furnace power supply and cools to room temperature automatically, take out glass;
(4) glass obtained to step (3) is heat-treated, and 600-700 DEG C of heat treatment temperature, the time is 5-15 hours,
Then room temperature is naturally rung to, K is obtainedxCs1-xPbBr3Quantum dot devitrified glass.
The preferred corundum crucible of crucible or platinum crucible used in step (1) of the present invention.
In step (2) of the present invention, the variation of fusion temperature will affect the uniformity of glass, and fusion temperature setting exists
Between 1200-1300 DEG C, temperature is too low, and glass raw material cannot sufficiently melt;Temperature is excessively high, in glass metal Br etc. it is volatile at
Branch is excessively lost, and it is relatively low to eventually lead to the concentration of quantum dot concentration in glass, and ideal experiment demand is not achieved.As
It is preferred that fusion temperature is 1300 DEG C, soaking time is 10-30 minutes.
In step (4) of the present invention, the variation of heat treatment temperature and time will affect KxCs1-xPbBr3The size of quantum dot
Size, to influence the position of its emission peak, the optical properties such as fluorescence intensity and life value must change.Preferably, heat treatment
Temperature is 600 DEG C, and heat treatment time is 8 hours.
K prepared by the present invention1-xCsxPbBr3The shape of quantum dot microcrystal glass material devitrified glass is plane, and can
It cut, polished, ground.
K prepared by the present inventionxCs1-xPbBr3Quantum dot devitrified glass can be used for preparing white light because of its good performance
LED can also prepare optical device using its third-order non-linear, apply also for photocatalysis, the fields such as upper conversion and scintillator.
Compared with prior art, the K that the present invention is preparedxCs1-xPbBr3Quantum dot microcrystal glass material, is mixed by K
Enter quantum dot, enhances CsPbBr3Stability, third-order non-linear and the upconversion mechanism of quantum dot devitrified glass simultaneously improve
Quantum efficiency.The KxCs1-xPbBr3Quantum dot microcrystal glass material have simple process, at low cost, photochemical properties are good
Equal outstanding advantages.
(4) Detailed description of the invention
Fig. 1 is the K of embodiment 1-5 preparationxCs1-xPbBr3The sample of quantum dot devitrified glass;
Fig. 2 is the K of embodiment 1-5 preparationxCs1-xPbBr3The XRD diagram and fluorogram of quantum dot devitrified glass
Fig. 3 is the K of embodiment 1-5 preparationxCs1-xPbBr3The life diagram of quantum dot devitrified glass, in left figure, from top to bottom
Be corresponding in turn to: K/Cs=0/1, K/Cs=0.2/0.8, K/Cs=0.4/0.6, K/Cs=0.6/0.4, K/Cs=0.8/0.2,
K/Cs=1/0;In right figure, 1-6 is respectively represented: K/Cs=0/1, K/Cs=0.2/0.8, K/Cs=0.4/0.6, K/Cs=
0.6/0.4, K/Cs=0.8/0.2, K/Cs=1/0.
Fig. 4 is K prepared by embodiment 40.6Cs0.4PbBr3Quantum Dot Glass carries out different crystallization processing, and what is obtained is glimmering
Light figure.
Fig. 5 is K prepared by embodiment 40.6Cs0.4PbBr3The third-order non-linear map of Quantum Dot Glass.
Fig. 6 is the upper conversion exciting light spectrogram of Quantum Dot Glass prepared by embodiment 1 and embodiment 4.
(5) specific embodiment
The present invention is specifically described with case study on implementation below, this narration is in order to further illustrate the invention, cannot
It regards as being limitation of the invention.Some nonessential modifications and adaptations can be made to foregoing invention content
Embodiment 1
(1) analysis pure raw material B is accurately weighed according to the raw material proportioning in table 12O3、SiO2、ZnO、Cs2CO3、 K2CO3、
PbBr2, NaBr, be then placed in mortar, slight mixed grinding 20min is placed in platinum crucible;
(2) fusing of glass raw material: being put into crucible in Muffle furnace, heat up to it, and fusion temperature is 1200 DEG C,
After reaching preset temperature, then it is kept the temperature and is after twenty minutes poured into glass melt on pig mold;
(3) there will be the pig mold of glass melt to be placed in high temperature furnace to anneal, be protected in glass transformation temperature Tg temperature
Temperature 5 hours is then shut off high temperature furnace power supply and cools to room temperature automatically, takes out glass;
(4) glass obtained to step (3) is heat-treated, and 600 DEG C of heat treatment temperature, the time is 8 hours, then certainly
Room temperature so is dropped to, obtains KxCs1-xPbBr3Quantum dot devitrified glass.
Table 1: glass formula and performance
Other glass appearances and performance characterization are as follows:
Fig. 1 is the K of embodiment 1-5 preparationxCs1-xPbBr3The sample of quantum dot devitrified glass, wherein upper stock layout product are purple
Fluorogram under outer 365nm excitation, lower stock layout product are the sample drawings under ordinary light, and sample is observed under ordinary light uniformly, in purple light
365nm excitation is lower to shine uniformly, shows KxCs1-xPbBr3Quantum dot is in B2O3-SiO2It is generated in zno-based glass system and real
Now it is uniformly distributed.
Fig. 2 is the K of embodiment 1-5 preparationxCs1-xPbBr3The XRD diagram and fluorogram of quantum dot devitrified glass.
Fig. 3 is the K of embodiment 1-5 preparationxCs1-xPbBr3The life diagram of quantum dot devitrified glass, with the increasing of K doping
Add, life value can reduce therewith, and provable K has been doped in CsPbBr3 quantum dot.Specifically, when the doping of K is 0
When, life value 71.14ns, when the doping of K increases therewith, life value is reduced therewith, because K enters the case of Cs, is reduced
CsPbBr3The surface defect of lattice, with reduction, the time that radiation transistion occurs for electronics shortens energy level trap, when fluorescence decay
Between shorten, i.e., life value reduce.
K prepared by embodiment 40.6Cs0.4PbBr3Quantum Dot Glass carry out different temperatures (420 DEG C, 440 DEG C, 460 DEG C,
490 DEG C, 520 DEG C) crystallization processing, the results showed that, as crystallization temperature increases, life value can be increased, fluorescence peak occur it is red
It moves, sees Fig. 4.
Fig. 5 is K prepared by embodiment 40.6Cs0.4PbBr3The nonlinear research of Quantum Dot Glass, it is seen that after mixing K
CsPbBr3With good third-order non-linear.
Fig. 6 is the upper conversion excitation spectrum of Quantum Dot Glass prepared by embodiment 1 and embodiment 4, is shown after mixing K,
Upper conversion excitation spectrum significantly increases.
Claims (8)
1. a kind of K1-xCsxPbBr3Quantum dot devitrified glass, the K1-xCsxPbBr3Quantum dot devitrified glass uses B2O3-
SiO2Zno-based glass system, KxCs1-xPbBr3Quantum dot is evenly distributed on B2O3-SiO2In zno-based glass system;
The KxCs1-xPbBr3Quantum dot devitrified glass is with B2O3、SiO2、ZnO、Cs2CO3、K2CO3、PbBr2, NaBr be original
Material is prepared, wherein Cs2CO3、K2CO3、PbBr2, NaBr be quantum dot raw material, the mass percentage of each raw material component are as follows:
B2O318.1-20.6%, SiO218.1-20.6%, ZnO 10.9-12.0%, Cs2CO39.9-21.2%, K2CO3 2.3-
5.8%, PbBr217.3-19.1%, NaBr 10.9-12.0%.
2. K as described in claim 11-xCsxPbBr3Quantum dot devitrified glass, it is characterised in that: with B2O3、SiO2With ZnO's
The quality that feeds intake is 100% meter, B2O3、SiO2Mass ratio with ZnO is 38.7-38.9%:38.7-38.9%:22.3-22.6%.
3. K as claimed in claim 1 or 21-xCsxPbBr3Quantum dot devitrified glass, it is characterised in that: B2O3And SiO2Feed intake
Identical in quality, feeding intake for ZnO and NaBr is identical in quality.
4. K as described in claim 11-xCsxPbBr3Quantum dot devitrified glass, it is characterised in that: the quality hundred of each raw material component
Divide content are as follows: B2O320.0%, SiO220.0%, ZnO 11.5%, Cs2CO311.3%, K2CO37.3%, PbBr2
18.5%, NaBr 11.5%.
5. a kind of K as described in claim 1xCs1-xPbBr3The preparation method of quantum dot devitrified glass, in accordance with the following steps into
Row:
(1) analysis pure raw material B is accurately weighed according to raw material proportioning2O3、SiO2、ZnO、Cs2CO3、K2CO3、PbBr2, NaBr, then
It is put into mortar, slight mixed grinding is uniformly placed in crucible;
(2) fusing of glass raw material: being put into crucible in high temperature resistance furnace, heat up to it, fusion temperature 1200-1300
DEG C, glass melt is poured on pig mold after reaching preset temperature, then after carrying out heat preservation to it 10-30 minutes;
(3) there will be the pig mold of glass melt to be placed in high temperature furnace to anneal, in glass transformation temperature Tg temperature 4-6
Hour, it is then shut off high temperature furnace power supply and cools to room temperature automatically, take out glass;
(4) glass obtained to step (3) is heat-treated, and 600-700 DEG C of heat treatment temperature, the time is 5-15 hours, then
Room temperature is naturally rung to, K is obtainedxCs1-xPbBr3Quantum dot devitrified glass.
6. preparation method as claimed in claim 5, it is characterised in that: the crucible used in step (1) is corundum crucible or platinum
Golden crucible.
7. preparation method as claimed in claim 5, it is characterised in that: in step (2), fusion temperature is 1300 DEG C, when heat preservation
Between be 10-30 minutes.
8. preparation method as claimed in claim 5, it is characterised in that: in step (4), heat treatment temperature is 600 DEG C, heat treatment
Time is 8 hours.
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CN112047636A (en) * | 2020-09-17 | 2020-12-08 | 昆明理工大学 | Preparation method and application of repairable inorganic perovskite quantum dot glass scintillator |
CN113831022A (en) * | 2021-10-18 | 2021-12-24 | 上海应用技术大学 | CsPbBr3:xDy3+Formula, preparation method and application of quantum dot glass |
CN114133141A (en) * | 2021-12-28 | 2022-03-04 | 海南大学 | Perovskite quantum dot glass ceramic and preparation method thereof |
CN114988707A (en) * | 2022-06-06 | 2022-09-02 | 武汉理工大学 | Lead-free halide nanocrystalline dispersion glass and application thereof |
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Cited By (6)
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CN112047636A (en) * | 2020-09-17 | 2020-12-08 | 昆明理工大学 | Preparation method and application of repairable inorganic perovskite quantum dot glass scintillator |
CN113831022A (en) * | 2021-10-18 | 2021-12-24 | 上海应用技术大学 | CsPbBr3:xDy3+Formula, preparation method and application of quantum dot glass |
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CN114988707A (en) * | 2022-06-06 | 2022-09-02 | 武汉理工大学 | Lead-free halide nanocrystalline dispersion glass and application thereof |
CN114988707B (en) * | 2022-06-06 | 2023-02-24 | 武汉理工大学 | Lead-free halide nanocrystalline dispersion glass and application thereof |
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