CN113354286B - GdF 3 :CsPbCl 1.5 Br 1.5 Quantum dot glass ceramic material and preparation method thereof - Google Patents
GdF 3 :CsPbCl 1.5 Br 1.5 Quantum dot glass ceramic material and preparation method thereof Download PDFInfo
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- 229910005690 GdF 3 Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
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- 239000011521 glass Substances 0.000 claims abstract description 40
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 claims abstract description 32
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims abstract description 26
- 239000002994 raw material Substances 0.000 claims abstract description 20
- 229910004298 SiO 2 Inorganic materials 0.000 claims abstract description 15
- 239000011780 sodium chloride Substances 0.000 claims abstract description 13
- 239000000463 material Substances 0.000 claims abstract description 11
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- DFGKGUXTPFWHIX-UHFFFAOYSA-N 6-[2-[4-[2-(2,3-dihydro-1H-inden-2-ylamino)pyrimidin-5-yl]piperazin-1-yl]acetyl]-3H-1,3-benzoxazol-2-one Chemical compound C1C(CC2=CC=CC=C12)NC1=NC=C(C=N1)N1CCN(CC1)CC(=O)C1=CC2=C(NC(O2)=O)C=C1 DFGKGUXTPFWHIX-UHFFFAOYSA-N 0.000 description 1
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- C—CHEMISTRY; METALLURGY
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- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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Abstract
The invention discloses a GdF 3 :CsPbCl 1.5 Br 1.5 Quantum dot microcrystalline glass material and preparation method thereof, gdF 3 :CsPbCl 1.5 Br 1.5 The quantum dot glass ceramic material is prepared from the following raw materials by a melt quenching method, wherein the raw materials comprise the following components in percentage by mol: b is 2 O 3 32.70‑32.00％，SiO 2 28.20‑28.00％，ZnO 14.23‑14.10％，Cs 2 CO 3 8.54‑8.45％，PbBr 2 2.47‑2.45％，PbCl 2 2.47‑2.45％，NaBr 5.56‑5.50％，NaCl 5.56‑5.50％，GdF 3 0.40-1.00%, the sum of all the components is 100%; wherein the mole percentage content meets the following conditions: pbBr 2 ＝PbCl 2 NaBr = NaCl; the GdF 3 :CsPbCl 1.5 Br 1.5 The micro-structural characteristic of the quantum dot microcrystalline glass material is GdF 3 :CsPbCl 1.5 Br 1.5 The quantum dots are embedded in the B 2 O 3 ‑SiO 2 -ZnO glass matrix. GdF prepared by the invention 3 :CsPbCl 1.5 Br 1.5 The quantum dot glass-ceramic material can emit blue light, obviously improves the optical performance after doping, and can generate amplified spontaneous emission.
Description
Technical Field
The invention belongs to the field of quantum dot glass ceramics, and particularly relates to GdF 3 :CsPbCl 1.5 Br 1.5 A quantum dot microcrystalline glass material and a preparation method thereof.
Background
In recent years, metal halide perovskites (CsPbX) 3 X = Cl, br and I) have attracted much attention due to their advantages of tunable emission wavelength, tunable optical gain, nearly uniform PLQYs, etc. Furthermore CsPbX 3 As a laser device, it has been applied to many emerging fields such as high definition display, optical communication, optical storage, bio-imaging, deep brillouin communication, and the like.
At present, the biggest problems of the existing metal halide perovskite are that the stability is poor, the application of the metal halide perovskite device is seriously hindered by fast luminescence quenching and poor hydrothermal stability, fortunately, fluorescent microcrystalline glass has short-term color stability and long-term material damage resistance, and can ensure good luminescence performance under high-flux laser irradiation and thermal shock, so that the fluorescent microcrystalline glass has great application prospects in the fields of power type white light LEDs and laser illumination display, and the research of fluorescent microcrystalline glass converters becomes a hotspot, and many well-known mechanisms at home and abroad are engaged in the research in the aspect.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a GdF 3 :CsPbCl 1.5 Br 1.5 Quantum dots (i.e., gdF) 3 Doped CsPbCl 1.5 Br 1.5 Quantum dot) microcrystalline glass material and preparation method thereof, and GdF 3 :CsPbCl 1.5 Br 1.5 The quantum dot glass-ceramic material can emit blue light, and the optical performance is obviously improved after doping.
The technical scheme adopted by the invention is as follows:
in a first aspect, the present invention provides a GdF 3 :CsPbCl 1.5 Br 1.5 The quantum dot glass ceramic material is prepared from the following raw materials by a melt quenching method, wherein the raw materials comprise the following components in percentage by mol: b is 2 O 3 32.70- 32.00％，SiO 2 28.20-28.00％，ZnO 14.23-14.10％，Cs 2 CO 3 8.54-8.45％，PbBr 2 2.47-2.45％，PbCl 2 2.47-2.45％，NaBr 5.56-5.50％，NaCl 5.56-5.50％，GdF 3 0.40-1.00%, the sum of all the components is 100%; wherein the mole percentage content meets the following conditions: pbBr 2 ＝PbCl 2 NaBr = NaCl; the GdF 3 :CsPbCl 1.5 Br 1.5 The micro-structural characteristic of the quantum dot microcrystalline glass material is GdF 3 :CsPbCl 1.5 Br 1.5 The quantum dots are embedded in the B 2 O 3 -SiO 2 -a ZnO glass matrix.
Preferably, the molar percentage content of the raw materials is as follows: b is 2 O 3 32.60-32.40％，SiO 2 28.10-28.00％，ZnO 14.18-14.12％，Cs 2 CO 3 8.50-8.47％，PbBr 2 2.46-2.45％， PbCl 2 2.46-2.45％，NaBr 5.54-5.52％，NaCl 5.54-5.52％，GdF 3 0.80-1.00%, and the sum of all the components is 100%. More preferably: b is 2 O 3 32.50％，SiO 2 28.01％，ZnO 14.14％，Cs 2 CO 3 8.48％，PbBr 2 2.46％，PbCl 2 2.46％，NaBr 5.53％，NaCl 5.53％，GdF 3 0.91 percent. By setting the raw material ratio in this way, gdF with higher quantum efficiency and narrower half-peak width can be obtained 3 :CsPbCl 1.5 Br 1.5 Quantum dot glass ceramics, and amplified spontaneous emission phenomenon can occur.
In a second aspect, the present invention provides a GdF 3 :CsPbCl 1.5 Br 1.5 The preparation method of the quantum dot microcrystalline glass material comprises the following steps:
(1) Weighing the raw materials according to the following mol percentage, and uniformly mixing and grinding the raw materials:
the molar percentage content of the raw materials is as follows: b 2 O 3 32.70-32.00％，SiO 2 28.20-28.00％， ZnO 14.23-14.10％，Cs 2 CO 3 8.54-8.45％，PbBr 2 2.47-2.45％，PbCl 2 2.47- 2.45％，NaBr 5.56-5.50％，NaCl 5.56-5.50％，GdF 3 0.40-1.00%, and the sum of all the components is 100%; wherein the mole percentage content meets the following conditions: pbBr 2 ＝PbCl 2 ，NaBr＝NaCl；
(2) Heating the mixed raw materials to 1100-1200 deg.C, holding the temperature for 5-20 min, pouring onto cast iron mold, annealing in high temperature furnace for 2-5 hr, cooling to a certain temperature (such as 50 deg.C), turning off the power supply, cooling to room temperature, and taking out glass to obtain GdF 3 :CsPbCl 1.5 Br 1.5 Quantum dot glass ceramics; the temperature of the cast iron mold and the annealing temperature are both set at the glass transition temperature (Tg temperature).
In step (1) of the present invention, since the present invention requires preparation of GdF 3 :CsPbCl 1.5 Br 1.5 Quantum dots, therefore, it is understood by those skilled in the art that PbBr is required to be used when designing the raw material ratio 2 With PbCl 2 The molar ratio of NaBr to NaCl was close to 1.
Preferably, the molar percentage content of the raw materials is as follows: b is 2 O 3 32.60-32.40％，SiO 2 28.10-28.00％，ZnO 14.18-14.12％，Cs 2 CO 3 8.50-8.47％，PbBr 2 2.46-2.45％， PbCl 2 2.46-2.45％，NaBr 5.54-5.52％，NaCl 5.54-5.52％，GdF 3 0.80-1.00 percent, and the sum of all the components is 100 percent; more preferably: b is 2 O 3 32.50％，SiO 2 28.01％，ZnO 14.14％，Cs 2 CO 3 8.48％，PbBr 2 2.46％，PbCl 2 2.46％，NaBr 5.53％，NaCl 5.53％，GdF 3 0.91 percent. By setting the raw material ratio in this way, gdF with higher quantum efficiency and narrower half-peak width can be obtained 3 :CsPbCl 1.5 Br 1.5 Quantum dot glass ceramics, and amplified spontaneous emission phenomenon can occur.
In the step (2) of the invention, the mixed raw materials are preferably placed in a corundum crucible or a platinum crucible, and then placed in a high-temperature resistance furnace, the temperature is raised to 1200 ℃, and the temperature is kept for 5min.
In the step (2) of the present invention, the glass transition temperature is 400 to 450 ℃.
Preferably, the preparation method further comprises the step (3): gdF obtained in step (2) 3 :CsPbCl 1.5 Br 1.5 The quantum dot microcrystalline glass is subjected to heat treatment crystallization at the temperature of 430-530 ℃, and the heat treatment crystallization time is 8-15h. The heat treatment devitrification step helps the further growth of quantum dots in the glass, thereby reducing GdF 3 :CsPbCl 1.5 Br 1.5 The quantum dot glass-ceramic emits the energy threshold of laser light (i.e., laser light can be emitted at a lower energy excitation), and the lower the energy threshold with an increase in the heat treatment temperature.
GdF prepared by the invention 3 :CsPbCl 1.5 Br 1.5 The shape of the quantum dot glass ceramic material can be plane, concave and convex, and can be cut, ground and polished.
The GdF of the invention 3 :CsPbCl 1.5 Br 1.5 The quantum dot glass-ceramic material can be applied to various lasers, such as: the picosecond laser can smash facial melanin, and can be used for treating freckle, chloasma, sunburn, etc.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention uses B 2 O 3 -SiO 2 -ZnO glass as matrix glass, adding Cs 2 CO 3 ,PbBr 2 , PbCl 2 ,NaBr,NaCl,GdF 3 Powder, preparation of GdF 3 :CsPbCl 1.5 Br 1.5 Quantum dot glass-ceramic material, 0.91% GdF 3 :CsPbCl 1.5 Br 1.5 The fluorescence emission wavelength of the quantum dot microcrystalline glass material is about 480nm, so that blue light can be effectively supplemented, and laser appears.
(2) GdF prepared by the invention 3 :CsPbCl 1.5 Br 1.5 Compared with undoped GdF, the quantum dot microcrystalline glass material 3 CsPbCl 1.5 Br 1.5 The quantum dot microcrystalline glass material has higher quantum efficiency and narrower half-peak width.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is within the scope of the present invention for those skilled in the art to obtain other drawings based on the drawings without inventive exercise.
FIG. 1 is a GdF prepared in examples 1-4 3 :CsPbCl 1.5 Br 1.5 The vitreous fluorescence map of quantum dots (365 nm excitation, 5 crack width);
FIG. 2 is a GdF prepared in examples 1-4 3 :CsPbCl 1.5 Br 1.5 A vitreous XRD pattern of the quantum dots;
FIG. 3 is GdF prepared in example 3 3 :CsPbCl 1.5 Br 1.5 An amplified spontaneous emission pattern of a vitreous body of quantum dots;
FIG. 4 is GdF prepared in example 4 3 :CsPbCl 1.5 Br 1.5 An amplified spontaneous emission pattern of a vitreous body of quantum dots;
FIG. 5 is GdF prepared in example 5 3 :CsPbCl 1.5 Br 1.5 An amplified spontaneous emission pattern of a vitreous body of quantum dots;
FIG. 6 is GdF prepared in example 6 3 :CsPbCl 1.5 Br 1.5 Amplified spontaneous emission pattern of the glass body of quantum dots.
Detailed Description
To make the objects, technical solutions and advantages of the present invention more apparent, the present invention will be described in further detail with reference to the accompanying drawings.
Examples 1 to 4
The raw materials were weighed out in the amounts shown in Table 1. Mixing and grinding for 30min, placing into a platinum crucible, placing into a high-temperature electromagnetic oven, heating to 1200 deg.C, maintaining for 5min, pouring into a cast iron mold set in advance at 420 deg.C, placing into the high-temperature electromagnetic oven, annealing, maintaining at 420 deg.C, and maintaining for 4h. Then cooling to 50 ℃ along with the furnace, closing the power supply of the high-temperature induction cooker, automatically cooling to room temperature, taking out the glass to obtain GdF 3 :CsPbCl 1.5 Br 1.5 Quantum dot glass ceramics. The glass products obtained in examples 1 to 4 were subjected to relevant performance tests, such asFig. 1 and 2 show the following.
The finished glass products of examples 2 and 3 were tested for their properties according to the following test methods: the prepared sample was fixed and then a 1nm spectral resolution fiber spectrometer was used to emit a laser beam that was focused on the sample surface through a cylindrical lens with a focal length of 10 cm. And then, the stripe length of the spot size is accurately controlled through the adjusted slit width, and whether amplified spontaneous emission appears in the sample is detected. The results show that: with the increase of the power density, the glass finished product of the embodiment 2 only has one straight line, and the phenomena that the output intensity is sharply increased and the output peak becomes sharp do not occur, which indicates that the glass of the embodiment 2 does not have the amplified spontaneous emission phenomenon and can not emit laser. While the results for the glass product of example 3 are shown in FIG. 3, with increasing watt density, gdF 3 :CsPbCl 1.5 Br 1.5 The output intensity of the quantum dot microcrystalline glass is sharply increased, the output peak becomes sharp, and the situation shows that the prepared GdF is 3 :CsPbCl 1.5 Br 1.5 The quantum dot glass ceramics has amplified spontaneous emission phenomenon, and the disordered laser is proved to be present.
TABLE 1
Example 4
GdF was obtained according to the preparation procedure of example 3 3 :CsPbCl 1.5 Br 1.5 And (3) carrying out 470 ℃ heat treatment crystallization treatment on the quantum dot microcrystalline glass for 10h. Then the treated GdF is treated 3 :CsPbCl 1.5 Br 1.5 Carrying out laser test on the quantum dot microcrystalline glass, wherein the test steps are as follows: the sample was fixed and then focused on the sample surface by transmitting a laser beam with a 1nm spectral resolution fiber optic spectrometer through a cylindrical lens with a focal length of 10 cm. Then the stripe of the spot size is accurately controlled by adjusting the width of the slitLength, and further detecting whether amplified spontaneous emission appears in the sample. As a result, as shown in FIG. 4, the sample exhibited an amplified spontaneous emission phenomenon, which confirmed that disordered lasing occurred, and that the energy threshold for disordered lasing occurred was lower than that of example 3.
Example 5
GdF was obtained according to the preparation procedure of example 3 3 :CsPbCl 1.5 Br 1.5 And (3) carrying out heat treatment crystallization treatment on the quantum dot microcrystalline glass at 500 ℃, wherein the treatment time is 10h. Then the treated GdF is treated 3 :CsPbCl 1.5 Br 1.5 Carrying out laser test on the quantum dot microcrystalline glass, wherein the test steps are as follows: the sample was fixed and then focused on the sample surface by transmitting a laser beam with a 1nm spectral resolution fiber optic spectrometer through a cylindrical lens with a focal length of 10 cm. And then, the stripe length of the spot size is accurately controlled through the adjusted slit width, and whether amplified spontaneous emission occurs in the sample is detected. As a result, as shown in FIG. 4, the sample exhibited an amplified spontaneous emission phenomenon, which confirmed that disordered lasing occurred, and that the energy threshold for disordered lasing was lower than that of examples 3 and 4.
Example 6
GdF was obtained according to the preparation procedure of example 3 3 :CsPbCl 1.5 Br 1.5 And (3) carrying out heat treatment crystallization treatment on the quantum dot microcrystalline glass at 530 ℃ for 10h. Then the treated GdF is treated 3 :CsPbCl 1.5 Br 1.5 Carrying out laser test on the quantum dot microcrystalline glass, wherein the test steps are as follows: the sample was fixed and then focused on the sample surface by a 1nm spectral resolution fiber spectrometer emitting a laser beam through a cylindrical lens with a focal length of 10 cm. And then, the stripe length of the spot size is accurately controlled through the adjusted slit width, and whether amplified spontaneous emission appears in the sample is detected. As a result, as shown in FIG. 4, the sample exhibited an amplified spontaneous emission phenomenon, and it was confirmed that disordered lasing occurred, and the energy threshold for the disordered lasing was lower than that of example 3, example 4, and example 5.
Comparative example 1
The formula of the glass comprises the following components in percentage by mole: b 2 O 3 30.3％，SiO 2 43.06％， ZnO 10.7％，Cs 2 CO 3 1.8％，PbBr 2 1.2％，PbI 2 2.5％，NaBr 3.21％，NaI 6.23％，GdF 3 1 percent. Otherwise the preparation was carried out as in example 1 to obtain GdF 3 :CsPbBr 1 I 2 Quantum dot glass ceramics.
And (3) carrying out performance test on the finished product, wherein the test method comprises the following steps: the prepared sample was fixed and then a 1nm spectral resolution fiber spectrometer was used to emit a laser beam that was focused on the sample surface through a cylindrical lens with a focal length of 10 cm. And then, the stripe length of the spot size is accurately controlled through the adjusted slit width, and whether amplified spontaneous emission occurs in the sample is detected. The results show that the GdF obtained by the preparation 3 :CsPbBr 1 I 2 The quantum dot glass ceramics can not generate amplified spontaneous radiation phenomenon, so the quantum dot glass ceramics can not be applied to the laser field.
Comparative example 2
The glass formula comprises the following components in percentage by mole: b 2 O 3 33.3％，SiO 2 40.06％， ZnO 10.7％，Cs 2 CO 3 3.6％，PbBr 2 5.4 percent of NaBr, 6.94 percent of NaBr. Otherwise the preparation was carried out as in example 1 to obtain GdF 3 :CsPbBr 3 Quantum dot glass ceramics.
And (3) carrying out performance test on the finished product, wherein the test method comprises the following steps: the prepared sample was fixed and then a 1nm spectral resolution fiber spectrometer was used to emit a laser beam that was focused on the sample surface through a cylindrical lens with a focal length of 10 cm. And then, the stripe length of the spot size is accurately controlled through the adjusted slit width, and whether amplified spontaneous emission occurs in the sample is detected. The results show that the GdF obtained by the preparation 3 :CsPbBr 3 The quantum dot glass ceramics can not generate amplified spontaneous emission, so the quantum dot glass ceramics can not be applied to the laser field.
Comparative example 3
The formula of the glass comprises the following components in percentage by mole: b 2 O 3 35.3％，SiO 2 38.06％， ZnO 12.7％，Cs 2 CO 3 3.9％，PbI 2 3.4 percent and NaI 6.64 percent. Other preparation conditions were the same as in example 1 to obtain GdF 3 :CsPbI 3 Quantum dot glass ceramics.
And (3) carrying out performance test on the finished product, wherein the test method comprises the following steps: the prepared sample was fixed and then a 1nm spectral resolution fiber spectrometer was used to emit a laser beam that was focused on the sample surface through a cylindrical lens with a focal length of 10 cm. And then, the stripe length of the spot size is accurately controlled through the adjusted slit width, and whether amplified spontaneous emission appears in the sample is detected. The results show that the GdF obtained by the preparation 3 :CsPbI 3 The quantum dot glass ceramics can not generate amplified spontaneous radiation phenomenon, so the quantum dot glass ceramics can not be applied to the laser field.
Claims (5)
1. GdF 3 :CsPbCl 1.5 Br 1.5 The quantum dot glass ceramic material is prepared from the following raw materials by a melt quenching method, wherein the raw materials comprise the following components in percentage by mol: b is 2 O 3 32.50%，SiO 2 28.01%，ZnO 14.14%，Cs 2 CO 3 8.48%，PbBr 2 2.46%，PbCl 2 2.46%，NaBr 5.53%，NaCl 5.53%，GdF 3 0.91 percent; the GdF 3 :CsPbCl 1.5 Br 1.5 The micro-structural characteristic of the quantum dot microcrystalline glass material is GdF 3 :CsPbCl 1.5 Br 1.5 The quantum dots are embedded in the B 2 O 3 -SiO 2 -ZnO glass matrix.
2. GdF according to claim 1 3 :CsPbCl 1.5 Br 1.5 The preparation method of the quantum dot glass ceramic material comprises the following steps:
(1) Weighing the raw materials according to the mol percentage of claim 1, and uniformly mixing and grinding:
(2) Heating the mixed raw materials to 1100-1200 ℃, preserving heat for 5-20 minutes, pouring the mixture onto a cast iron mold, then placing the cast iron mold in a high-temperature furnace for annealing for 2-5 hours, then cooling the cast iron mold to a certain temperature along with the furnace, turning off a power supply of the high-temperature furnace, automatically cooling the high-temperature furnace to room temperature, taking out glass to obtain GdF 3 :CsPbCl 1.5 Br 1.5 Quantum dot glass ceramics; the temperature of the cast iron mold and the annealing temperature are set to be glass transition temperatures.
3. The process according to claim 2, wherein the process further comprises the step (3): gdF obtained in step (2) 3 :CsPbCl 1.5 Br 1.5 The quantum dot microcrystalline glass is subjected to heat treatment crystallization at the temperature of 430-530 ℃, and the heat treatment crystallization time is 8-15h.
4. The method of claim 2, wherein: in the step (2), the mixed raw materials are placed in a corundum crucible or a platinum crucible, and are placed in a high-temperature resistance furnace, the temperature is raised to 1200 ℃, and the temperature is kept for 5min.
5. The method of claim 2, wherein: in the step (2), the glass transition temperature is 400 to 450 ℃.
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| CN109574506A (en) * | 2018-12-20 | 2019-04-05 | 温州大学 | A kind of CsPb1-xTixBr3Quantum dot devitrified glass and preparation method thereof |
| CN110540362A (en) * | 2019-09-25 | 2019-12-06 | 华南理工大学 | Perovskite quantum dot doped glass with reversible luminescence and preparation method thereof |
| CN112358190A (en) * | 2020-09-30 | 2021-02-12 | 温州大学 | GdF3:CsPbBrI2Preparation method of quantum dot microcrystalline glass material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109574506A (en) * | 2018-12-20 | 2019-04-05 | 温州大学 | A kind of CsPb1-xTixBr3Quantum dot devitrified glass and preparation method thereof |
| CN110540362A (en) * | 2019-09-25 | 2019-12-06 | 华南理工大学 | Perovskite quantum dot doped glass with reversible luminescence and preparation method thereof |
| CN112358190A (en) * | 2020-09-30 | 2021-02-12 | 温州大学 | GdF3:CsPbBrI2Preparation method of quantum dot microcrystalline glass material |
Non-Patent Citations (2)
| Title |
|---|
| "The preparation and up-conversion properties of full spectrum CsPbX3 (X=Cl,Br,I) quantum dot glasses";Huiling Zhang等;《Nanoscale》;20191010;全文 * |
| 超稳定CsPbX3量子点玻璃的激光上转换与光电性能的研究;张慧灵;《中国优秀硕士学位论文全文数据库 工程科技I 辑》;20210415;全文 * |
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Application publication date: 20210907 Assignee: GUANGDONG ODIMING PHOTOELECTRIC TECHNOLOGY CO.,LTD. Assignor: Wenzhou University Contract record no.: X2024330000059 Denomination of invention: A GdF3: CsPbCl1.5Br1.5quantum dot microcrystalline glass material and its preparation method Granted publication date: 20221021 License type: Exclusive License Record date: 20240516 |