CN113831022B - CsPbBr 3 ：xDy 3+ Quantum dot glass and preparation method and application thereof - Google Patents
CsPbBr 3 ：xDy 3+ Quantum dot glass and preparation method and application thereof Download PDFInfo
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- YLZOPXRUQYQQID-UHFFFAOYSA-N 3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)-1-[4-[2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidin-5-yl]piperazin-1-yl]propan-1-one Chemical compound N1N=NC=2CN(CCC=21)CCC(=O)N1CCN(CC1)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F YLZOPXRUQYQQID-UHFFFAOYSA-N 0.000 description 1
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- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
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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
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
- C03C14/006—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix the non-glass component being in the form of microcrystallites, e.g. of optically or electrically active material
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/10—Forming beads
- C03B19/1005—Forming solid beads
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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
- C03C12/00—Powdered glass; Bead compositions
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/77—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing rare earth metals
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- H01L33/502—
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B20/00—Energy efficient lighting technologies, e.g. halogen lamps or gas discharge lamps
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Abstract
The invention discloses CsPbBr 3 :xDy 3+ The quantum dot glass and the preparation method and the application thereof are characterized in that the weighed raw materials are fully ground, then the ground raw materials are dried and sintered at high temperature to obtain precursor glass, and the precursor glass is subjected to internal stress elimination and heat treatment process to finally obtain CsPbBr 3 :xDy 3+ Quantum dot glass using CsPbBr 3 :xDy 3+ The invention discloses a method for preparing a white light LED (light-emitting diode) device by using quantum dot glass, and Dy is firstly used in the method 2 O 3 Doping is carried out to prepare CsPbBr 3 :xDy 3+ The quantum dot glass and the prepared white light LED device can effectively improve CsPbBr 3 The quantum dot glass has high luminous efficiency, reduces the use of lead sources, and is a luminous material with strong stability, high crystallinity and environmental friendliness.
Description
Technical Field
The invention relates to the technical field of semiconductor luminescent materials, in particular to CsPbBr 3 ：xDy 3+ Quantum dot glass and a preparation method and application thereof.
Background
In recent years, all-inorganic cesium lead halide CsPbX 3 Perovskite Quantum Dots (QDs) have attracted considerable attention for their excellent optical properties, such as tunable emission wavelength, strong light absorption capability, high carrier mobility, and low trap state density. In addition, csPbX can be modulated by anion exchange reaction of halides 3 The emission wavelength of the quantum dots, thereby realizing full-spectrum emission of visible light. Based on the structure, the material has wide application prospect in the photoelectric fields of light emitting diodes, photoelectric detectors, lasers, solar cells and the like. However, due to CsPbX 3 The ionic nature and large surface energy of quantum dots severely affect their long-term stability, including: water, oxygen, thermal and chemical stability, which also severely limits its applications and development, commercialization, etc.
Through research, the CsPbX is discovered 3 The quantum dots are embedded in the inorganic oxide glass, so that CsPbX can be ensured 3 The physical and chemical properties of the quantum dots can effectively improve CsPbX 3 Stability of quantum dots. Among the inorganic glasses that have been used are tellurite glass, phosphate glass, germanate glass, silicate glass, and the like, but the most commonly used inorganic glass is silicate glass, the structure of which is continuous silicon tetrahedron. The stable Si-O tetrahedral structure helps to build the network structure of the glass, thereby providing a stable environment for the quantum dots. Although the quantum dots are embedded in the glass matrix to effectively solve the stability problem, the prepared quantum dot sample has low crystallinity in the glass matrix, and the luminous efficiency is very low compared with that of colloidal quantum dots. Later researchers found that CsPbX was 3 During the preparation of the quantum dot glass, csPbX is added 3 The components of the quantum dot raw material can increase CsPbX 3 The formation probability of quantum dots, and further improves CsPbX 3 The crystallinity of the quantum dots in the glass matrix improves the luminous efficiency. However, this requires the addition of an excessive amount of a lead source compound, and Pb as a heavy metal is not only a serious hazard to human health, but also is not very environment-friendly. Therefore, the method can effectively improve CsPbX 3 The crystallinity of the quantum dots in the glass matrix can be reduced, and the CsPbX used by the lead source compound can be reduced 3 Quantum dot glasses are currently in great demand.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The invention aims to provide CsPbBr 3 ：xDy 3+ Quantum dot glass, and preparation method and application thereof, aiming at solving the problem of CsPbBr mentioned in the background technology 3 The crystallinity of the quantum dots in the glass matrix is low, and the use of excessive lead source is not environment-friendly.
In order to realize the purpose, the invention provides CsPbBr 3 ：xDy 3+ A quantum dot glass comprising: dy with purity of more than or equal to 99 percent 2 O 3 Is CsPbBr 3 ：xDy 3+ The formation of quantum dots provides Dy element and Cs with the purity of more than or equal to 99.99 percent 2 CO 3 PbO not less than 99%, naBr not less than 99%, csPbBr 3 ：xDy 3+ The formation of quantum dots provides Cs, pb and Br elements, and the purity of Na is more than or equal to 99.5 percent 2 CO 3 BaCO not less than 99% 3 SiO of not less than 99.5% 2 99% or more ZnO and 99.5% or more H 3 BO 3 Mainly CsPbBr 3 ：xDy 3+ A glass matrix component of quantum dot glass, wherein the glass matrix and the dopant material are 5 to 10Na in terms of molar mass 2 CO 3 -20～30 ZnO-80～100 H 3 BO 3 -15～30 SiO 2 -10～30 BaCO 3 -x Dy 2 O 3 (x =0,0.1,0.3,0.5,0.7, 0.9mol%); the quantum dot raw material is 1.5-3 Cs by molar mass 2 CO 3 -3-6 PbO-9-18 NaBr.
CsPbBr 3 ：xDy 3+ The preparation method of the quantum dot glass comprises the following steps of mixing a doped compound Dy 2 O 3 Weighing raw materials of cesium source compound, lead source compound, halogen compound and compound forming glass matrix one by one, fully grinding the weighed raw materials, drying the ground raw materials, sintering the ground raw materials at high temperature to obtain precursor glass, and finally obtaining the CsPbBr after the precursor glass is subjected to internal stress elimination and heat treatment processes 3 ：xDy 3 + Quantum dot glass.
CsPbBr 3 ：xDy 3+ The application of quantum dot glass in a white light LED device is to prepare CsPbBr 3 ：xDy 3+ Further milling quantum dot glass into CsPbBr 3 ：xDy 3+ Quantum dot glass powder, and then CsPbBr 3 ：xDy 3+ Sieving quantum dot glass powder to obtain CsPbBr with substantially consistent particle size 3 ： xDy 3+ Quantum dot glass powder particles, followed by CsPbBr of substantially uniform particle size 3 ：xDy 3+ And encapsulating the quantum dot glass powder particles with commercial fluorescent powder, a blue light chip and glue to prepare the white light LED device.
Preferably, the specific operation steps of the further milling are: the prepared CsPbBr is added 3 ：xDy 3+ Putting the quantum dot glass block into an agate milling pot, and milling into CsPbBr3: the grinding time of the xDy3+ quantum dot glass powder is 5-10min.
Preferably, the specific operation steps of the sieving treatment are as follows: mixing the milled CsPbBr 3 ：xDy 3+ The quantum dot glass powder is sieved twice, firstly, a 400-mesh nylon net with the aperture size of 0.0385 mm is adopted, then the glass powder sieved for the first time is collected, then, the 500-mesh nylon net with the aperture size of 0.03 mm is adopted, and finally, the glass powder sieved for the second time is collected.
Preferably, the commercial phosphor is mainly commercial red phosphor, and the main component of the red phosphor is K 2 SiF 6 ：Mn 4+ The emission wavelength is mainly 630nm, and the fluorescent powder mainly provides a red component for packaging and preparing a white light LED.
Preferably, the blue light chip is mainly an InGaN blue light chip with an emission wavelength of 450nm, and the blue light chip mainly has two functions, one function is to provide a blue component for packaging and preparing a white light LED, and the other function is to be used as an excitation source for exciting CsPbBr 3 ：xDy 3+ Quantum dot glass powders and commercial phosphors.
Preferably, the glue is mainly LED organosilicon packaging glue, the glue is divided into a component A and a component B, wherein the main components of the component A comprise 60% -90% of epoxy resin and 10% -40% of benzyl alcohol, the main components of the component B comprise 95% -100% of triethylene triamine and 0-5% of water, when the white light LED is prepared and packaged, the component A and the component B need to be used simultaneously, and the use ratio of the two components is 1:1.
preferably, the method for packaging and preparing the white light LED device comprises the following specific steps: weighing CsPbBr in proportion 3 ：xDy 3+ Quantum dot glass powder and commercial phosphor, then 1:1, screw up the bottle lid with the sample collection bottle and put into the mixer stirring, the churning time is 90s, and the mixed composition with the stirring is through the mode of gluing afterwards, drips to the blue light chip, and follow-up through drying process to the good sample of gluing of counter point, and then obtains white light LED device.
Preferably, the baking process is mainly divided into two steps, firstly, the just-packaged sample is placed into an oven with the temperature of 80 ℃ for preheating for 30min, and then the pre-processed sample is placed into an oven with the temperature of 150 ℃ for baking for 180 min.
The invention provides a CsPbBr3: the xDy3+ quantum dot glass and the preparation method and the application thereof have the following beneficial effects.
1. The invention dopes rare earth element Dy into CsPbBr 3 In quantum dot glass, dy 3+ Ion entry to CsPbBr 3 Lattice of quantum dots, and Dy 3+ Ions can effectively replace CsPbBr 3 Part Pb of Quantum dots 2+ Ion, thereby forming CsPbBr 3 ：xDy 3+ Quantum dot glass. The invention effectively improves CsPbBr 3 ： xDy 3+ Crystallinity of quantum dots in glass matrix, csPbBr 3 The luminous efficiency of the quantum dot glass is improved from 35.9% to 62.5%.
2.CsPbBr 3 ：xDy 3+ The quantum dots become full in the glass matrix, so that the network structure of the glass becomes more compact, and Dy is doped after the quantum dots are soaked in deionized water for 1000 hours 2 O 3 The fluorescence efficiency of the quantum dot glass can be maintained at 95 percent of the original value, and Dy is not doped 2 O 3 The fluorescence efficiency of the quantum dot glass can only be maintained at 82% of the original fluorescence efficiency. This is due to CsPbBr 3 ：xDy 3+ The quantum dots become full and conductive in the glass matrixThe network structure of the glass becomes more compact, so that the stability of the whole quantum dot glass is improved.
3. Prepared CsPbBr 3 ：xDy 3+ The particle diameter of the quantum dot glass powder is more uniform based on CsPbBr 3 ： xDy 3+ White LED devices prepared from quantum dot glass powders exhibit a good wide color gamut, approximately 126.3% of the NTSC value.
Drawings
FIG. 1 shows CsPbBr prepared in example 1 3 ：xDy 3+ XRD spectrogram of the quantum dot glass powder;
FIG. 2 shows CsPbBr obtained in example 2 3 ：xDy 3+ A fluorescence absorption spectrum of the quantum dot glass powder;
FIG. 3 is a CsPbBr-based solution prepared in example 3 3 ：xDy 3+ An electroluminescence spectrum and a color coordinate graph of a white light LED device prepared from the quantum dot glass powder;
FIG. 4 shows two different Dys of comparative example 1 2 O 3 CsPbBr prepared by doping concentration 3 ：xDy 3+ TEM spectrogram of the quantum dot glass powder;
FIG. 5 shows four different Dys of comparative example 2 2 O 3 CsPbBr prepared by doping concentration 3 ：xDy 3+ Photoluminescence spectra of quantum dot glass powders.
Detailed Description
The present invention will be further described with reference to the following specific embodiments and accompanying drawings to assist in understanding the contents of the invention.
The invention provides CsPbBr 3 ：xDy 3+ A quantum dot glass comprising: dy with purity of more than or equal to 99 percent 2 O 3 Is CsPbBr 3 ：xDy 3+ The formation of quantum dots provides Dy element and Cs with the purity of more than or equal to 99.99 percent 2 CO 3 PbO not less than 99%, naBr not less than 99%, csPbBr 3 ：xDy 3+ The formation of quantum dots provides Cs, pb and Br elements, and the purity of Na is more than or equal to 99.5 percent 2 CO 3 BaCO not less than 99% 3 SiO of not less than 99.5% 2 99% or more ZnO and 99.5% or more H 3 BO 3 Mainly CsPbBr 3 ：xDy 3+ A glass matrix component of quantum dot glass, wherein the glass matrix and the dopant material are 5 to 10Na in terms of molar mass 2 CO 3 -20～30 ZnO-80～100 H 3 BO 3 -15～30 SiO 2 -10～30 BaCO 3 -x Dy 2 O 3 (x =0,0.1,0.3,0.5,0.7, 0.9mol%); the quantum dot raw material is 1.5-3 Cs by molar mass 2 CO 3 3 to 6 portions of PbO-9 to 18 portions of NaBr.
The invention provides CsPbBr 3 ：xDy 3+ The preparation method of the quantum dot glass comprises the following steps of mixing a doped compound Dy 2 O 3 Weighing raw materials such as cesium source compound, lead source compound, halogen compound and compound forming glass matrix one by one, fully grinding the weighed raw materials, drying the ground raw materials, sintering the ground raw materials at high temperature to obtain precursor glass, and finally obtaining CsPbBr after the precursor glass is subjected to internal stress elimination and heat treatment processes 3 ：xDy 3+ Quantum dot glass.
The invention provides CsPbBr 3 ：xDy 3+ The application of quantum dot glass in a white light LED device is to prepare CsPbBr 3 ：xDy 3+ Further grinding quantum dot glass into CsPbBr 3 ：xDy 3+ Quantum dot glass powder, and then CsPbBr 3 ：xDy 3+ Sieving quantum dot glass powder to obtain CsPbBr with substantially consistent particle size 3 ：xDy 3+ Quantum dot glass powder particles, followed by CsPbBr of substantially uniform particle size 3 ：xDy 3+ And packaging the quantum dot glass powder particles with commercial fluorescent powder, a blue light chip and glue to prepare the white light LED device.
The concrete operation steps of further grinding are as follows: the prepared CsPbBr is added 3 ：xDy 3+ Putting the quantum dot glass block into an agate milling pot, and milling into CsPbBr3: the grinding time of the xDy3+ quantum dot glass powder is 5-10min.
The specific operation steps of the sieving treatmentThe method comprises the following steps: mixing the milled CsPbBr 3 ：xDy 3+ The quantum dot glass powder is sieved twice, firstly, a 400-mesh nylon net with the aperture size of 0.0385 mm is carried out, then the glass powder sieved for the first time is collected, then, the 500-mesh nylon net with the aperture size of 0.03 mm is carried out, and finally, the glass powder sieved for the second time is collected.
The commercial fluorescent powder is mainly commercial red fluorescent powder, and the main component of the red fluorescent powder is K 2 SiF 6 ：Mn 4+ The emission wavelength is mainly 630nm, and the fluorescent powder mainly provides a red component for packaging and preparing a white light LED.
The blue light chip is mainly an InGaN blue light chip with the emission wavelength of 450nm, and has two main functions, one function is to provide blue components for packaging and preparing a white light LED, and the other function is to be used as an excitation source to excite CsPbBr 3 ：xDy 3+ Quantum dot glass powders and commercial phosphors.
The glue is mainly LED organic silicon packaging glue, and comprises a component A and a component B, wherein the main components of the component A comprise 60% -90% of epoxy resin and 10% -40% of benzyl alcohol, and the main components of the component B comprise 95% -100% of triethylene triamine and 0-5% of water, and when the white light LED is prepared and packaged, the component A and the component B need to be used simultaneously, and the use ratio of the two components is 1:1.
The method for packaging and preparing the white light LED device comprises the following specific steps: weighing CsPbBr in proportion 3 ：xDy 3+ Quantum dot glass powder and commercial phosphor powder, then add two kinds of components of glue according to 1:1 ratio, screw up the bottle lid with the sample collection bottle and put into the mixer stirring, the churning time is 90s, and the mixed component that will stir evenly afterwards drips to the blue light chip through the mode of gluing, and follow-up through drying process to the good sample of gluing, and then obtain white light LED device.
The drying treatment is mainly divided into two steps, firstly, the sample which is just packaged is placed into an oven with the temperature of 80 ℃ for preheating for 30min, and then the sample which is well pretreated is placed into the oven with the temperature of 150 ℃ for baking for 180 min.
Example 1
The purity of the raw materials used in the following implementation of the invention is as follows:
sodium carbonate (more than or equal to 99.5%), barium titanate (99%), silicon dioxide (99.5%), zinc oxide (99%), boric acid (more than or equal to 99.5%), dysprosium oxide (more than or equal to 99%), cesium carbonate (99.99%), lead oxide (more than or equal to 99%) and sodium bromide (99%). Glass matrix 5Na by molar mass 2 CO 3 -20ZnO-80H 3 BO 3 -15SiO 2 -10BaCO 3 Proportioning; doping material according to molar mass xDy 2 O 3 (x =0.3 mol%) are proportioned; the quantum dot raw material is 1.5Cs according to molar mass 2 CO 3 Proportioning the components of-3 PbO-9 NaBr.
CsPbBr is prepared as follows 3 ：xDy 3+ Quantum dot glass:
(1) The raw materials are weighed according to the molar mass, then added into an agate grinding pot in batches, and fully ground by using a grinding rod.
(2) And transferring the fully ground raw materials from the agate grinding pot to a corundum crucible, and then putting the corundum crucible filled with the raw materials into a muffle furnace at the temperature of 250 ℃ for drying treatment for 5min.
(3) And transferring the dried corundum crucible filled with the raw materials from a muffle furnace at 250 ℃ to a large muffle furnace at 1000 ℃ for high-temperature sintering for 10min.
(4) Pouring the sintered precursor glass onto a heating platform containing a copper mold plate at 220 ℃, maintaining the temperature of the heating platform for 2 hours, and then gradually reducing the temperature to room temperature.
(5) Putting the precursor glass with the internal stress eliminated into a porcelain boat, then placing the porcelain boat in a muffle furnace at the temperature of 430 ℃ for heat treatment for 3 hours, and then cooling the porcelain boat to room temperature along with the furnace. Thus obtaining CsPbBr 3 ： xDy 3+ Quantum dot glass.
(6) The obtained CsPbBr 3 ：xDy 3+ Grinding quantum dot glass block into CsPbBr 3 ：xDy 3+ Quantum dot glass powder and sieving.
By X-ray diffraction(ii) measurement of CsPbBr by X-ray diffraction (XRD) 3 ：xDy 3+ The XRD spectrum of the quantum dot glass powder is shown in figure 1, and the diffraction peak and CsPbBr appearing in the glass can be known from the graph 3 Substantially corresponds to the standard card PDF #54-0752, thereby proving that CsPbBr 3 The quantum dots are successfully precipitated in the glass matrix.
Example 2
The following raw materials used in the practice of the invention have the following purities:
sodium carbonate (more than or equal to 99.5%), barium titanate (99%), silicon dioxide (99.5%), zinc oxide (99%), boric acid (more than or equal to 99.5%), dysprosium oxide (more than or equal to 99%), cesium carbonate (99.99%), lead oxide (more than or equal to 99%) and sodium bromide (99%). Glass matrix 5Na by molar mass 2 CO 3 -20ZnO-80H 3 BO 3 -15SiO 2 -10BaCO 3 Proportioning; doping material according to molar mass xDy 2 O 3 (x =0.5 mol%) are proportioned; the quantum dot raw material is 1.5Cs by molar mass 2 CO 3 Proportioning the components of-3 PbO-9 NaBr.
CsPbBr is prepared as follows 3 ：xDy 3+ Quantum dot glass:
(1) The raw materials are weighed according to the molar mass, then added into an agate grinding pot in batches, and fully ground by using a grinding rod.
(2) And transferring the fully ground raw materials from an agate grinding pot to a corundum crucible, and then putting the corundum crucible filled with the raw materials into a muffle furnace at the temperature of 250 ℃ for drying treatment for 5min.
(3) And transferring the dried corundum crucible filled with the raw materials from a muffle furnace at 250 ℃ to a large muffle furnace at 1000 ℃ for high-temperature sintering for 10min.
(4) Pouring the sintered precursor glass onto a heating platform containing a copper mold plate at 220 ℃, maintaining the temperature of the heating platform for 2 hours, and then gradually reducing the temperature to room temperature.
(5) Putting the precursor glass with the internal stress eliminated into a porcelain boat, then placing the porcelain boat in a muffle furnace at the temperature of 430 ℃ for heat treatment for 3 hours, and then cooling the porcelain boat to room temperature along with the furnace. Thus obtaining a CsPbBr 3 ： xDy 3+ Quantum dot glass.
(6) The obtained CsPbBr 3 ：xDy 3+ Grinding quantum dot glass block into CsPbBr 3 ：xDy 3+ Quantum dot glass powder and sieving.
The obtained CsPbBr is analyzed by fluorescence spectrometer 3 ：xDy 3+ The fluorescence absorption spectrum obtained by measuring the quantum dot glass powder is shown in FIG. 2, and as can be seen from FIG. 2, under the excitation of 365nm, the emission wavelength is positioned in the 525nm wave band, which is consistent with the previous research result, and further proves that CsPbBr 3 The quantum dots are successfully precipitated in the glass matrix.
Example 3
The following raw materials used in the practice of the invention have the following purities:
glass matrix 5Na by molar mass 2 CO 3 -20ZnO-80H 3 BO 3 -15SiO 2 -10BaCO 3 Proportioning; doping material by molar mass xDy 2 O 3 (x =0.7 mol%) are proportioned; the quantum dot raw material is 1.5Cs by molar mass 2 CO 3 Proportioning the components of-3 PbO-9 NaBr. The glue is prepared from A/B glue, the component A and the component B are mixed according to the ratio of 1:1, and red commercial fluorescent powder with the emission wavelength of 630nm, the red commercial fluorescent powder and CsPbBr are used 3 ：xDy 3+ The quantum dot glass powder is mixed according to the ratio of 1: 3. A blue chip with the emission wavelength of 450nm is used, and the rated power of the blue chip is 1W.
CsPbBr is prepared as follows 3 ：xDy 3+ Quantum dot glass, and encapsulating it into a white light LED device:
(1) The raw materials are weighed according to the molar mass, then added into an agate grinding pot in batches, and fully ground by using a grinding rod.
(2) And transferring the fully ground raw materials from an agate grinding pot to a corundum crucible, and then putting the corundum crucible filled with the raw materials into a muffle furnace at the temperature of 250 ℃ for drying treatment for 5min.
(3) And transferring the dried corundum crucible filled with the raw materials from a muffle furnace at 250 ℃ to a large muffle furnace at 1000 ℃ for high-temperature sintering for 10min.
(4) The sintered precursor glass is poured onto a heating platform containing copper and the temperature of the mold plate is 220 ℃, the temperature of the heating platform is maintained for 2 hours, and then the temperature is gradually reduced to the room temperature.
(5) Putting the precursor glass with the internal stress eliminated into a porcelain boat, then placing the porcelain boat in a muffle furnace at the temperature of 430 ℃ for heat treatment for 3 hours, and then cooling the porcelain boat to room temperature along with the furnace. Thus obtaining CsPbBr 3 ： xDy 3+ Quantum dot glass.
(6) The obtained CsPbBr 3 ：xDy 3+ Grinding quantum dot glass block into CsPbBr 3 ：xDy 3+ Quantum dot glass powder and sieving.
(7) Reacting CsPbBr 3 ：xDy 3+ The quantum dot glass powder, the red commercial fluorescent powder and the glue are weighed according to the formula and put into a stirrer to be stirred for 90 seconds, so as to obtain the mixed component material.
(8) And (3) dropping the mixed component material onto the blue light chip in a dispensing manner, wherein the mixed component material needs to be uniformly coated on the blue light chip.
(9) Putting the coated chip into an oven for baking treatment to finally obtain the CsPbBr-based 3 ：xDy 3+ A white light LED device prepared from the quantum dot glass powder.
CsPbBr-based CsPbBr by adopting integrating sphere spectrometer 3 ：xDy 3+ The white light LED device prepared from the quantum dot glass is used for measuring relevant photoelectric performance parameters including color temperature, color coordinates and luminous efficiency. The obtained electroluminescence spectrum and color coordinate graph of the white light LED device are shown in FIG. 3, under the current drive of 40mA, the Correlated Color Temperature (CCT) of the white light LED device is 8705K, the color coordinate is (0.2881, 0.3001), the luminous efficacy is 98lm/W, and meanwhile, the white light LED device shows a good wide color gamut which is about 126.3% of the NTSC value.
Comparative example 1
The following raw materials used in the practice of the invention have the following purities:
sodium carbonate (more than or equal to 99.5%) and barium titanate(99%), silicon dioxide (99.5%), zinc oxide (99%), boric acid (99.5%), dysprosium oxide (99% or more), cesium carbonate (99.99%), lead oxide (99% or more) and sodium bromide (99%). Glass matrix 5Na by molar mass 2 CO 3 -20ZnO-80H 3 BO 3 -15SiO 2 -10BaCO 3 Proportioning; doped material xDy 2 O 3 Proportioning according to molar masses x =0mol% and x =0.7mol% respectively; the quantum dot raw material is 1.5Cs according to molar mass 2 CO 3 Proportioning the components of-3 PbO-9 NaBr.
Two different Dys were prepared as follows 2 O 3 Doping concentration CsPbBr 3 ：xDy 3+ Quantum dot glass:
(1) The raw materials are weighed according to the molar mass, then added into an agate grinding pot in batches, and fully ground by using a grinding rod.
(2) And transferring the fully ground raw materials from an agate grinding pot to a corundum crucible, and then putting the corundum crucible filled with the raw materials into a muffle furnace at the temperature of 250 ℃ for drying treatment for 5min.
(3) And transferring the dried corundum crucible filled with the raw materials from a muffle furnace at 250 ℃ to a large muffle furnace at 1000 ℃ for high-temperature sintering for 10min.
(4) Pouring the sintered precursor glass onto a heating platform containing a copper mold plate at 220 ℃, maintaining the temperature of the heating platform for 2 hours, and then gradually reducing the temperature to room temperature.
(5) Putting the precursor glass with the internal stress eliminated into a porcelain boat, then placing the porcelain boat in a muffle furnace at the temperature of 430 ℃ for heat treatment for 3 hours, and then cooling the porcelain boat to room temperature along with the furnace. Thus obtaining CsPbBr 3 ：xDy 3+ Quantum dot glass.
(6) The obtained CsPbBr 3 ：xDy 3+ Grinding quantum dot glass block into CsPbBr 3 ：xDy 3+ Quantum dot glass powder, and sieving.
Observation of CsPbBr with Transmission Electron Microscope (TEM) 3 ：xDy 3+ The TEM spectrum of the microstructure of the quantum dot glass powder is shown in FIG. 4It can be seen that the crystallinity on the right side is significantly better than that on the left side, which proves that Dy 2 O 3 The doping of CsPbBr can be effectively promoted 3 And (4) precipitation of the quantum dots in the glass matrix.
Comparative example 2
The following raw materials used in the practice of the invention have the following purities:
sodium carbonate (more than or equal to 99.5%), barium titanate (99%), silicon dioxide (99.5%), zinc oxide (99%), boric acid (more than or equal to 99.5%), dysprosium oxide (more than or equal to 99%), cesium carbonate (99.99%), lead oxide (more than or equal to 99%) and sodium bromide (99%). Glass matrix 5Na by molar mass 2 CO 3 -20ZnO-80H 3 BO 3 -15SiO 2 -10BaCO 3 Proportioning; doped material xDy 2 O 3 The mixture ratio is respectively according to molar masses x =0mol%, x =0.3mol%, x =0.7mol% and x =0.9 mol%; the quantum dot raw material is 1.5Cs by molar mass 2 CO 3 Proportioning the components of-3 PbO-9 NaBr.
Four different Dy's were prepared as follows 2 O 3 Doping concentration CsPbBr 3 ：xDy 3+ Quantum dot glass:
(1) The raw materials are weighed according to the molar mass, then added into an agate grinding pot in batches, and fully ground by using a grinding rod.
(2) And transferring the fully ground raw materials from an agate grinding pot to a corundum crucible, and then putting the corundum crucible filled with the raw materials into a muffle furnace at the temperature of 250 ℃ for drying treatment for 5min.
(3) And transferring the dried corundum crucible filled with the raw materials from a muffle furnace at 250 ℃ to a large muffle furnace at 1000 ℃ for high-temperature sintering for 10min.
(4) The sintered precursor glass is poured onto a heating platform containing copper and the temperature of the mold plate is 220 ℃, the temperature of the heating platform is maintained for 2 hours, and then the temperature is gradually reduced to the room temperature.
(5) And putting the precursor glass with the internal stress eliminated into a porcelain boat, then placing the porcelain boat in a muffle furnace at the temperature of 430 ℃ for heat treatment for 3 hours, and then cooling the porcelain boat to room temperature along with the furnace. To obtain CsPbBr 3 ：xDy 3+ Quantum dot glass.
(6) The obtained CsPbBr 3 ：xDy 3+ Grinding quantum dot glass block into CsPbBr 3 ：xDy 3+ Quantum dot glass powder and sieving.
Adopting a fluorescence spectrometer to obtain four different Dys 2 O 3 Doping concentration CsPbBr 3 ：xDy 3+ The quantum dot glass powder was subjected to photoluminescence spectroscopy (PL) measurement. The photoluminescence spectrum is shown in FIG. 5, along with Dy 2 O 3 Gradual increase of doping concentration, csPbBr 3 ：xDy 3+ The emission intensity of the quantum dot glass sample also gradually increases, but when the doping concentration is increased to a certain value, there is a tendency that the emission intensity decreases due to concentration quenching. Different Dy 2 O 3 The fluorescence efficiency corresponding to concentration doping is shown in Table 1, and preferred Dy 2 O 3 The doping concentration is 0.7mmol, and the fluorescence efficiency of the sample can reach 62.5%.
TABLE 1 fluorescence efficiency
| Dy 2 O 3 Doping concentration (mmol) | 0 | 0.3 | 0.7 | 0.9 |
| PLQY(％) | 35.9 | 45 | 62.5 | 53 |
The inventive concept is explained in detail herein using specific examples, which are only provided to help understanding the core idea of the present invention. It should be understood that any obvious modifications, equivalents and other improvements made by those skilled in the art without departing from the spirit of the present invention are included in the scope of the present invention.
Claims (10)
1. CsPbBr 3 ：xDy 3+ Quantum dot glass, characterized in that it comprises: dy with purity of more than or equal to 99 percent 2 O 3 Is CsPbBr 3 ：xDy 3+ The formation of quantum dots provides Dy element and Cs with the purity of more than or equal to 99.99 percent 2 CO 3 PbO not less than 99%, naBr not less than 99%, csPbBr 3 ：xDy 3+ The formation of quantum dots provides Cs, pb and Br elements, and the purity of Na is more than or equal to 99.5 percent 2 CO 3 BaCO not less than 99% 3 SiO of not less than 99.5% 2 99% or more ZnO and 99.5% or more H 3 BO 3 Mainly CsPbBr 3 ：xDy 3+ A glass matrix component of quantum dot glass, wherein the glass matrix and the dopant material are 5 to 10Na in terms of molar mass 2 CO 3 -20～30ZnO-80～100H 3 BO 3 -15～30SiO 2 -10～30BaCO 3 -x Dy 2 O 3 Proportioning, wherein x =0.1,0.3,0.5,0.7,0.9mo1%; the quantum dot raw material is 1.5-3 Cs by molar mass 2 CO 3 3 to 6 portions of PbO-9 to 18 portions of NaBr.
2. The CsPbBr of claim 1, wherein CsPbBr 3 ：xDy 3+ The preparation method of quantum dot glass is characterized in that a doping compound Dy is mixed according to the mixture ratio of claim 1 2 O 3 With a cesium source compound, a lead source compound, a halogen compound and a compound constituting a glass substrateWeighing the raw materials one by one, fully grinding the weighed raw materials, drying the ground raw materials, sintering the ground raw materials at high temperature to obtain precursor glass, and finally obtaining the CsPbBr after the precursor glass is subjected to internal stress elimination and heat treatment processes 3 ：xDy 3+ Quantum dot glass.
3. The CsPbBr of claim 1, wherein CsPbBr 3 ：xDy 3+ The application of the quantum dot glass in the white light LED device is characterized in that the prepared CsPbBr is 3 ：xDy 3+ Further grinding quantum dot glass into CsPbBr 3 ：xDy 3+ Quantum dot glass powder, and then CsPbBr 3 ：xDy 3+ Sieving quantum dot glass powder to obtain CsPbBr with substantially consistent particle size 3 ：xDy 3+ Quantum dot glass powder particles, followed by CsPbBr of substantially uniform particle size 3 ：xDy 3+ And encapsulating the quantum dot glass powder particles with commercial fluorescent powder, a blue light chip and glue to prepare the white light LED device.
4. A CsPbBr according to claim 3 3 ：xDy 3+ The application of the quantum dot glass in the white light LED device is characterized in that the specific operation steps of further grinding are as follows: the prepared CsPbBr is added 3 ：xDy 3+ Putting the quantum dot glass block into an agate milling pot, and milling the glass block into CsPbBr3: the grinding time of the xDy3+ quantum dot glass powder is 5-10min.
5. A CsPbBr according to claim 3 3 ：xDy 3+ The application of the quantum dot glass in the white light LED device is characterized in that the specific operation steps of the screening treatment are as follows: mixing the milled CsPbBr 3 ：xDy 3+ The quantum dot glass powder is sieved twice, firstly, a 400-mesh nylon net with the aperture size of 0.0385 mm is carried out, then the glass powder sieved for the first time is collected, then, the 500-mesh nylon net with the aperture size of 0.03 mm is carried out, and finally, the glass powder sieved for the second time is collected.
6. The CsPbBr of claim 3 3 ：xDy 3+ The application of the quantum dot glass in the white light LED device is characterized in that the commercial fluorescent powder is mainly commercial red fluorescent powder, and the main component of the red fluorescent powder is K 2 SiF 6 ：Mn 4+ The emission wavelength is mainly 630nm, and the fluorescent powder mainly provides a red component for packaging and preparing a white light LED.
7. A CsPbBr according to claim 3 3 ：xDy 3+ The application of the quantum dot glass in the white light LED device is characterized in that the blue light chip is mainly an InGaN blue light chip, the emission wavelength of the InGaN blue light chip is 450nm, the blue light chip mainly has two functions, one function is to provide a blue component for packaging and preparing the white light LED, and the other function is to serve as an excitation source for exciting CsPbBr 3 ：xDy 3+ Quantum dot glass powders and commercial phosphors.
8. A CsPbBr according to claim 3 3 ：xDy 3+ The application of quantum dot glass in a white light LED device is characterized in that glue is mainly LED organic silicon packaging glue and comprises a component A and a component B, wherein the main components of the component A comprise 60% -90% of epoxy resin and 10% -40% of benzyl alcohol, the main components of the component B comprise 95% -100% of triethylene triamine and 0-5% of water, when the white light LED is prepared and packaged, the component A and the component B need to be used simultaneously, and the using ratio of the two components is 1:1.
9. A CsPbBr according to claim 8 3 ：xDy 3+ The application of the quantum dot glass in the white light LED device is characterized in that the specific steps of packaging and preparing the white light LED device are as follows: weighing CsPbBr in proportion 3 ：xDy 3+ Quantum dot glass powder and commercial phosphor, then 1:1, screwing a bottle cover of a sample collection bottle, putting the bottle cover of the sample collection bottle into a stirrer, stirring uniformly for 90s, and then uniformly stirringThe mixed components are dripped onto a blue light chip in a dispensing mode, and then the samples subjected to dispensing are dried to obtain the white light LED device.
10. The CsPbBr of claim 9 3 ：xDy 3+ The application of the quantum dot glass in the white light LED device is characterized in that the drying treatment is mainly divided into two steps, firstly, a sample which is just packaged is placed into an oven with the temperature of 80 ℃ for preheating for 30min, and then the sample which is well pretreated is placed into the oven with the temperature of 150 ℃ for baking for 180 min.
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