CN110963711A - Composite quantum dot glass and preparation method thereof - Google Patents

Composite quantum dot glass and preparation method thereof Download PDF

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Publication number
CN110963711A
CN110963711A CN201911285596.3A CN201911285596A CN110963711A CN 110963711 A CN110963711 A CN 110963711A CN 201911285596 A CN201911285596 A CN 201911285596A CN 110963711 A CN110963711 A CN 110963711A
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quantum dot
glass
matrix
composite quantum
composite
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CN110963711B (en
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杨波波
梅时良
熊志勇
郭睿倩
张万路
解凤贤
叶怀宇
张国旗
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Southwest University of Science and Technology
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Shenzhen Third Generation Semiconductor Research Institute
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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
    • 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
    • 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
    • C03C4/00—Compositions for glass with special properties
    • C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
    • 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
    • C03C2214/00—Nature of the non-vitreous component
    • C03C2214/30—Methods of making the composites

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Dispersion Chemistry (AREA)
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  • Manufacturing & Machinery (AREA)
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Abstract

The invention discloses composite quantum dot glass and a preparation method thereof, wherein the composite quantum dot glass comprises a glass matrix and a quantum dot matrix, wherein the quantum dot matrix accounts for 10-20 mol% of the glass matrix; the quantum dot matrix is an inorganic perovskite-binary semiconductor composite quantum dot; the binary semiconductor in the quantum dot matrix is 5-10% mol of the inorganic perovskite. The inorganic perovskite-binary semiconductor composite quantum dot is a cesium halide lead perovskite-zinc sulfide composite quantum dot. The invention uses B2O3‑SiO2ZnO is used as a matrix glass system, the physical and chemical properties are stable, the ZnO can effectively reduce the melting temperature of the glass, the BaO can adjust the network structure of the glass, perovskite quantum dots can be easily grown in situ in the glass, and PbO in the quantum dot raw material can reduce the glassThe melting point and the addition of trace zinc sulfide can further improve the stability and the color purity of the perovskite quantum dot, and the addition of a proper amount of zinc sulfide enables the glass to simultaneously separate out the blue ZnS quantum dot under the annealing condition.

Description

Composite quantum dot glass and preparation method thereof
Technical Field
The invention relates to the technical field of quantum dot luminescent materials, in particular to composite quantum dot glass and a preparation method thereof.
Background
Recently, all-inorganic halides (CsPbX)3) The perovskite quantum dot has great potential application value in the fields of light-emitting diodes, lasers, polaroids, solar cells, photodetectors and the like by virtue of adjustable light-emitting wavelength, high fluorescence quantum efficiency and narrow emission peak. CsPbX3The quantum dots can be well dispersed in a plurality of non-polar solutions, and the oil phase perovskite quantum dots can be packaged into low-cost photoelectric devices. So far, the pure color CsPbX with the quantum size of 4-15nm, the luminous wavelength of which covers the whole visible spectrum (410 nm-700 nm), the luminous quantum efficiency of which reaches 90 percent3Quantum dots have been reported. However, the perovskite quantum dots synthesized by the liquid phase have poor stability in air and poor water resistance, and the packaged devices have poor performances in the aspects of heat resistance, light aging resistance and the like, so that the further development of the perovskite quantum dots in the fields of photoelectric materials and devices is hindered.
In order to improve the stability of perovskite quantum dots, researchers have tried various methods including ligand exchange, high molecular materials or organosilicon coated quantum dots, and the like. The Zeng group in 2016 embeds quantum dots into a high molecular material PMMA, and protects the excellent optical performance of the quantum dots. Liu and collaborators thereof use mesoporous silica to coat CsPbBr in nonpolar solution3Perovskite Quantum dots, Zhang and Rogach team Using organosilicon (3-aminopropyl) triethoxysilane and polyhedral Oligomerisation, respectivelyAnd the silsesquioxane is used as an end-capping agent, and the quantum dot/organic silicon composite material is generated through hydrolysis. Further, Mn is concerned2+:CsPbCl3/CsPbCl3Quantum dots, CsPbX3/ZnS heterostructure quantum dots, and phosphoric acid enhanced CsPbX3The quantum dots can be reported to improve the stability of the quantum dots. However, because of the high oxygen dispersion coefficient in the organic matter, these methods cannot ensure that the quantum dots can effectively avoid photooxidation. Therefore, the improvement of the stability of the quantum dot organic composite material under extreme conditions needs to be further researched, especially the thermal stability of the quantum dot organic composite material. So far, no quantum dot can prepare a high-efficiency device which is stable for a long time.
The traditional preparation process of the quantum dot film is directly prepared by coating a quantum dot solution or colloid on a substrate, the luminous stability of the traditional preparation process is limited by the stability of the quantum dot solution, the quantum efficiency of the traditional preparation process is greatly reduced, and the application of the traditional preparation process in a luminescent device is limited.
The glass in-situ growth of quantum dots is an effective way for preparing a quantum dot material with long-term stability, but in the preparation process of the quantum dot glass, halogen atoms, lead atoms, cesium atoms and the like are unevenly distributed in a glass precursor due to the fact that the internal and external temperatures of a glass melt are inconsistent in the cooling process, so that perovskite quantum dots precipitated in the heat treatment process are uneven, and the color purity of the quantum dot glass is not high.
In order to ensure the sufficient strength and transparency of the glass, the glass substrate is generally selected to be silicate glass, and the melting point of the silicon oxide raw material is high, so that the melting point of the quantum dot glass precursor is also high.
Disclosure of Invention
In order to solve the problems, the invention provides a composite quantum dot glass, which comprises a glass matrix and a quantum dot matrix, wherein the glass matrix is B2O3-SiO2-ZnO system said quantum dot matrix molar ratio is between 10% and 20% of said glass matrix; the quantum dot matrix is an inorganic perovskite-binary semiconductor composite quantum dot; the molar ratio of the binary semiconductor in the quantum dot matrix is 5 percent of that of the inorganic perovskite～10％。
Preferably, the inorganic perovskite-binary semiconductor composite quantum dot is a cesium-lead perovskite-zinc sulfide composite quantum dot.
Preferably, the glass substrate comprises 10-20 mol% of sodium oxide, 10-20 mol% of zinc oxide, 50 mol% of boron oxide, 20 mol% of silicon oxide and 5-10 mol% of barium oxide.
Preferably, the thickness of the quantum dot glass is 0.05mm-1.05 mm.
Preferably, the emission wavelength of the inorganic perovskite is 500mm-550nm, and the emission wavelength of the zinc sulfide is 430mm-500 nm.
Based on the same inventive concept, the invention provides a preparation method of composite quantum dot glass, which comprises the following steps
S1: adding the quantum dot matrix into the glass matrix and sintering to obtain a molten mass;
s2: casting and molding the molten mass to obtain transparent glass;
s3: and annealing and cooling the transparent glass to obtain the composite quantum dot glass.
Preferably, the sintering temperature in S1 is 1000-1350 ℃, and the sintering time is 5-30 min.
Preferably, the S2 is specifically that the melt is cast in a mold with the preheating temperature of 200-300 ℃ for molding, and the temperature is kept for 1-3 h.
Preferably, the annealing temperature of S3 is 400-450 ℃, and the annealing time is 3-10 h.
Preferably, the mold is an iron plate, a copper plate, or a stainless steel plate.
Preferably, the thickness of the quantum dot glass is 0.05mm-1.05 mm.
The invention also provides a preparation method of the composite quantum dot glass, which comprises the following steps
S1: adding quantum dot matrix into the glass matrix and sintering to obtain molten mass;
s2: casting and molding the molten mass to obtain transparent glass;
s3: and annealing and cooling the transparent glass to obtain the composite quantum dot glass.
Preferably, the sintering temperature in the S1 is 1000-1350 ℃, and the sintering time is 5-30 min.
Preferably, the S2 is specifically that the melt is cast in a mold with a preheating temperature of 200-300 ℃ for molding, and the temperature is kept for 1-3 hours.
Preferably, the annealing temperature of S3 is 400-450 ℃, and the annealing time is 3-10 h.
Preferably, the mold is an iron plate, a copper plate, or a stainless steel plate.
The invention has the beneficial effects that:
(1) the composite quantum dot glass of the invention is prepared by mixing B2O3-SiO2ZnO is used as a matrix glass system, borosilicate glass is high in transparency and stable in physical and chemical properties, meanwhile, ZnO can effectively reduce the melting temperature of the glass, BaO can adjust the structure of a glass network body, perovskite quantum dots can be easily grown in situ in the glass, PbO in quantum dot raw materials can reduce the melting point of the glass, the stability of the glass is improved, Pb can be provided as quantum dot raw materials, the perovskite quantum dots are separated from the glass under an annealing condition, the stability and the color purity of the perovskite quantum dots can be further improved by adding trace zinc sulfide, and blue ZnS quantum dots can be simultaneously separated from the glass under the annealing condition by adding proper amount of zinc sulfide.
(2) The preparation method of the composite quantum dot glass is simple, the raw materials of the matrix glass and the composite quantum dot raw materials are fully mixed according to a certain proportion, the precursor glass can be obtained by one-step sintering, and then the composite quantum dot glass can be obtained by low-temperature heat treatment. In particular, the invention can be used in LED and display technology.
Drawings
FIG. 1 is a fluorescence emission spectrum of the composite quantum dot prepared in example 1 of the present invention;
FIG. 2 is a coupling luminescence diagram of the composite quantum dot and the chip manufactured in example 1 of the present invention;
FIG. 3 is a fluorescence emission spectrum of the composite quantum dot prepared in example 2 of the present invention;
fig. 4 is a coupling luminescence diagram of the composite quantum dot and the chip manufactured in embodiment 2 of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and examples. It should be understood, however, that the description herein of specific embodiments is only intended to illustrate the invention and not to limit the scope of the invention.
The composite quantum dot glass provided by the invention comprises a glass matrix and a quantum dot matrix, wherein the quantum dot matrix accounts for 10-20 mol% of the glass matrix; the quantum dot matrix is an inorganic perovskite-binary semiconductor composite quantum dot; the binary semiconductor in the quantum dot matrix is 2-10 mol% of the inorganic perovskite. Wherein the inorganic perovskite-binary semiconductor composite quantum dots are cesium halide lead perovskite-zinc sulfide composite quantum dots. The thickness of the quantum dot glass is 0.05-1.05 mm. The emission wavelength of the inorganic perovskite is 500-550nm, and the emission wavelength of the zinc sulfide is 430-500 nm. The cesium-lead-perovskite halide component comprises: cesium carbonate, lead oxide, sodium bromide.
The first embodiment is as follows: the embodiment provides green light low-melting-point composite quantum dot glass
Will analyze pure Na2CO3、ZnO、B2O3、SiO2、BaCO3、Cs2CO3PbO, NaBr, ZnS in an amount of 10 mol% Na based on the base glass raw material2O,10mol％ZnO,50mol％B2O3,20mol％SiO210 mol% BaO; 10 wt% of quantum dot raw material, wherein each component of the quantum dot raw material is 10 mol% of Cs2CO3: 22 mol% PbO: 66 mol% NaBr: precisely weighing the molar fraction ratio of 2 mol% ZnS, placing the ZnS in an agate mortar, uniformly grinding the ZnS in the agate mortar, placing the ZnS in a corundum crucible, placing the corundum crucible in a muffle furnace at 1150 ℃ for heat preservation for 10min, taking out the glass solution, rapidly casting the glass solution in a mold with the preheating temperature of 250 ℃ for molding to obtain the transparent glassThe glass is exposed, the temperature is kept for 2h, and the internal stress is eliminated; and then transferring the glass to a muffle furnace for annealing at 430 ℃ for 5h, and naturally cooling to obtain the composite quantum dot glass.
The obtained composite quantum dot glass is measured by a fluorescence spectrometer (FLS920, Edinburgh Instruments, England) to obtain a spectrogram as shown in figure 1, under the excitation of 400nm wavelength, the emission wavelength is 525nm, the peak width at half height is 20nm, and the corresponding perovskite quantum dot CsPbBr is obtained3The composite quantum dot glass is coupled with a 400nm chip by using a Hangzhou remote STC4000 rapid spectrometer to emit bright green light, as shown in figure 2.
Example two: the embodiment provides a green light low-melting point composite quantum dot glass
Will analyze pure Na2CO3、ZnO、B2O3、SiO2、BaCO3、Cs2CO3PbO, NaBr, ZnS in an amount of 15 mol% Na based on the base glass raw material2O,10mol％ZnO,50mol％B2O3,20mol％SiO25 mol% BaO; 10 wt% of quantum dot raw material, wherein each component of the quantum dot raw material is 10 mol% of Cs2CO3: 20 mol% PbO: 64 mol% NaBr: accurately weighing the molar fraction ratio of 6 mol% ZnS, placing the ZnS in an agate mortar, grinding the ZnS in the agate mortar uniformly, placing the ZnS in a corundum crucible, placing the corundum crucible in a muffle furnace at 1150 ℃ for heat preservation for 10min, taking out a glass solution, quickly casting the glass solution in a mold with the preheating temperature of 250 ℃ for molding to obtain transparent glass, preserving the heat for 2h, and eliminating internal stress; then transferring the glass to a muffle furnace for annealing at 430 ℃ for 5h, and naturally cooling to obtain the composite quantum dot glass;
the obtained composite quantum dot glass is measured by a fluorescence spectrometer (FLS920, Edinburgh Instruments, England), the obtained spectrogram is shown in figure 3, under the excitation of 400nm wavelength, emission spectra show two peaks which are positioned at 510nm and 470nm and respectively correspond to perovskite quantum dots CsPbBr3And fluorescence emission of semiconductor quantum dot ZnS, coupling the composite quantum dot glass with 400nm blue light chip by Hangzhou remote STC4000 rapid spectrometer to emit bright cyan-green light, such asAs shown in fig. 4.
The foregoing is a further description of the invention with reference to preferred embodiments, and the examples described are some, but not all, examples of the invention. It will be apparent to those skilled in the art that various modifications, additions, substitutions, and other embodiments can be made without departing from the spirit and scope of the invention.

Claims (10)

1. A composite quantum dot glass is characterized in that: comprises a glass matrix and a quantum dot matrix, wherein the glass matrix is B2O3-SiO2-ZnO system, said quantum dot matrix molar ratio being between 10% and 20% of said glass matrix; the quantum dot matrix is an inorganic perovskite-binary semiconductor composite quantum dot; the molar ratio of the binary semiconductor in the quantum dot matrix is 5-10% of that of the inorganic perovskite.
2. A composite quantum dot glass according to claim 1, wherein: the inorganic perovskite-binary semiconductor composite quantum dot is a cesium halide lead perovskite-zinc sulfide composite quantum dot.
3. A composite quantum dot glass according to claim 2, wherein: the glass substrate comprises 10-20 mol% of sodium oxide, 10-20 mol% of zinc oxide, 50 mol% of boron oxide, 20 mol% of silicon oxide and 5-10 mol% of barium oxide.
4. A composite quantum dot glass according to claim 1, wherein: the thickness of the composite quantum dot glass is 0.05mm-1.05 mm.
5. A composite quantum dot glass according to claim 3, wherein: the emission wavelength of the inorganic perovskite is 500mm-550nm, and the emission wavelength of the zinc sulfide is 430mm-500 nm.
6. A method for preparing the composite quantum dot glass according to any one of claims 1 to 5, characterized in that: comprises that
S1: adding the quantum dot matrix into the glass matrix and sintering to obtain a molten mass;
s2: casting and molding the molten mass to obtain transparent glass;
s3: and annealing and cooling the transparent glass to obtain the composite quantum dot glass.
7. A method for preparing the composite quantum dot glass according to claim 6, characterized in that: the sintering temperature in the S1 is 1000-1350 ℃, and the sintering time is 5-30 min.
8. A method for preparing the composite quantum dot glass according to claim 6, characterized in that: and S2, specifically, casting the molten mass in a mold with a preheating temperature of 200-300 ℃ for molding, and keeping the temperature for 1-3 hours.
9. A method for preparing the composite quantum dot glass according to claim 6, characterized in that: the annealing temperature of S3 is 400-450 ℃, and the annealing time is 3-10 h.
10. A method for preparing the composite quantum dot glass according to claim 6, characterized in that: the die is an iron plate, a copper plate or a stainless steel plate.
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CN112759267A (en) * 2021-02-04 2021-05-07 中国科学院福建物质结构研究所 Perovskite nanocrystalline glass ceramic membrane laminated composite material
CN114213004A (en) * 2021-12-31 2022-03-22 云南大学 White light quantum dot luminescent glass and preparation method and application thereof
CN114716142A (en) * 2022-04-12 2022-07-08 中国计量大学上虞高等研究院有限公司 ZnS quantum dot doped luminescent glass and preparation method and application thereof
WO2022164412A1 (en) * 2021-01-27 2022-08-04 Yildiz Teknik Universitesi A solid state lighting device including cdse and cspbbr3 quantum dot-doped glass nanocomposite layers and production method thereof
CN114920460A (en) * 2022-05-02 2022-08-19 哈尔滨工程大学 Double-phase quantum dot glass ceramic and preparation method and application thereof
CN115161026A (en) * 2022-07-29 2022-10-11 厦门大学 Core-shell quantum dot luminescent material and preparation method thereof
CN115259663A (en) * 2022-08-15 2022-11-01 上海应用技术大学 All-inorganic perovskite quantum dot composite glass and preparation method thereof

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2022164412A1 (en) * 2021-01-27 2022-08-04 Yildiz Teknik Universitesi A solid state lighting device including cdse and cspbbr3 quantum dot-doped glass nanocomposite layers and production method thereof
CN112759267A (en) * 2021-02-04 2021-05-07 中国科学院福建物质结构研究所 Perovskite nanocrystalline glass ceramic membrane laminated composite material
CN114213004A (en) * 2021-12-31 2022-03-22 云南大学 White light quantum dot luminescent glass and preparation method and application thereof
CN114213004B (en) * 2021-12-31 2022-08-02 云南大学 White light quantum dot luminescent glass and preparation method and application thereof
CN114716142A (en) * 2022-04-12 2022-07-08 中国计量大学上虞高等研究院有限公司 ZnS quantum dot doped luminescent glass and preparation method and application thereof
CN114716142B (en) * 2022-04-12 2023-09-05 中国计量大学上虞高等研究院有限公司 ZnS-doped quantum dot luminescent glass and preparation method and application thereof
CN114920460A (en) * 2022-05-02 2022-08-19 哈尔滨工程大学 Double-phase quantum dot glass ceramic and preparation method and application thereof
CN114920460B (en) * 2022-05-02 2024-03-26 哈尔滨工程大学 Diphase quantum dot microcrystalline glass and preparation method and application thereof
CN115161026A (en) * 2022-07-29 2022-10-11 厦门大学 Core-shell quantum dot luminescent material and preparation method thereof
CN115259663A (en) * 2022-08-15 2022-11-01 上海应用技术大学 All-inorganic perovskite quantum dot composite glass and preparation method thereof

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