CN115259663A - A kind of all-inorganic perovskite quantum dot composite glass and preparation method thereof - Google Patents
A kind of all-inorganic perovskite quantum dot composite glass and preparation method thereof Download PDFInfo
- Publication number
- CN115259663A CN115259663A CN202210975525.1A CN202210975525A CN115259663A CN 115259663 A CN115259663 A CN 115259663A CN 202210975525 A CN202210975525 A CN 202210975525A CN 115259663 A CN115259663 A CN 115259663A
- Authority
- CN
- China
- Prior art keywords
- glass
- quantum dot
- inorganic perovskite
- perovskite quantum
- composite
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000011521 glass Substances 0.000 title claims abstract description 90
- 239000002096 quantum dot Substances 0.000 title claims abstract description 79
- 239000002131 composite material Substances 0.000 title claims abstract description 42
- 238000002360 preparation method Methods 0.000 title abstract description 7
- 239000011159 matrix material Substances 0.000 claims abstract description 29
- 238000000034 method Methods 0.000 claims abstract description 12
- 239000000758 substrate Substances 0.000 claims abstract description 12
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 claims description 18
- 239000002994 raw material Substances 0.000 claims description 15
- 239000011787 zinc oxide Substances 0.000 claims description 9
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 8
- 238000005245 sintering Methods 0.000 claims description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 229910007472 ZnO—B2O3—SiO2 Inorganic materials 0.000 claims description 3
- 238000000465 moulding Methods 0.000 claims description 3
- ZOXJGFHDIHLPTG-BJUDXGSMSA-N Boron-10 Chemical compound [10B] ZOXJGFHDIHLPTG-BJUDXGSMSA-N 0.000 claims description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052810 boron oxide Inorganic materials 0.000 claims description 2
- 238000005266 casting Methods 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- JKWMSGQKBLHBQQ-UHFFFAOYSA-N diboron trioxide Chemical compound O=BOB=O JKWMSGQKBLHBQQ-UHFFFAOYSA-N 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 2
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 claims description 2
- 229910001948 sodium oxide Inorganic materials 0.000 claims description 2
- 229910001220 stainless steel Inorganic materials 0.000 claims description 2
- 239000010935 stainless steel Substances 0.000 claims description 2
- 229910004298 SiO 2 Inorganic materials 0.000 abstract description 7
- 238000011065 in-situ storage Methods 0.000 abstract description 5
- 229910052792 caesium Inorganic materials 0.000 abstract description 4
- 238000010438 heat treatment Methods 0.000 abstract description 3
- 229910000287 alkaline earth metal oxide Inorganic materials 0.000 abstract 1
- 238000010791 quenching Methods 0.000 abstract 1
- 230000000171 quenching effect Effects 0.000 abstract 1
- 239000011734 sodium Substances 0.000 description 12
- JHJLBTNAGRQEKS-UHFFFAOYSA-M sodium bromide Chemical compound [Na+].[Br-] JHJLBTNAGRQEKS-UHFFFAOYSA-M 0.000 description 10
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 6
- 239000004570 mortar (masonry) Substances 0.000 description 6
- 229910052708 sodium Inorganic materials 0.000 description 6
- -1 cesium lead halide Chemical class 0.000 description 5
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 229910052796 boron Inorganic materials 0.000 description 3
- 229910052593 corundum Inorganic materials 0.000 description 3
- 239000010431 corundum Substances 0.000 description 3
- 230000008878 coupling Effects 0.000 description 3
- 238000010168 coupling process Methods 0.000 description 3
- 238000005859 coupling reaction Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 230000005284 excitation Effects 0.000 description 3
- 239000000156 glass melt Substances 0.000 description 3
- 229910052809 inorganic oxide Inorganic materials 0.000 description 3
- 239000000075 oxide glass Substances 0.000 description 3
- 239000011780 sodium chloride Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- HTUMBQDCCIXGCV-UHFFFAOYSA-N lead oxide Chemical compound [O-2].[Pb+2] HTUMBQDCCIXGCV-UHFFFAOYSA-N 0.000 description 2
- YEXPOXQUZXUXJW-UHFFFAOYSA-N lead(II) oxide Inorganic materials [Pb]=O YEXPOXQUZXUXJW-UHFFFAOYSA-N 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000005388 borosilicate glass Substances 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000006698 induction Effects 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000005693 optoelectronics Effects 0.000 description 1
- 239000005365 phosphate glass Substances 0.000 description 1
- 230000005622 photoelectricity Effects 0.000 description 1
- 239000006064 precursor glass Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- XHGGEBRKUWZHEK-UHFFFAOYSA-L tellurate Chemical compound [O-][Te]([O-])(=O)=O XHGGEBRKUWZHEK-UHFFFAOYSA-L 0.000 description 1
Images
Classifications
-
- 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
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
-
- 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
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/16—Special features of the melting process; Auxiliary means specially adapted for glass-melting furnaces
-
- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/062—Glass compositions containing silica with less than 40% silica by weight
- C03C3/07—Glass compositions containing silica with less than 40% silica by weight containing lead
- C03C3/072—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron
- C03C3/074—Glass compositions containing silica with less than 40% silica by weight containing lead containing boron containing zinc
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
Description
技术领域technical field
本发明涉及量子点发光材料技术领域，具体涉及一种复合量子点玻璃及其制备方法。The invention relates to the technical field of quantum dot luminescent materials, in particular to a composite quantum dot glass and a preparation method thereof.
背景技术Background technique
近年来，全无机钙钛矿CsPbX3(X＝Cl、Br、I)量子点吸引了大量的关注，在光电领域都展现了非凡的应用潜力，主要因为其具有独特的光学特性：发射波长可调、吸收宽、色域宽，量子效率高等。CsPbX3量子点制备工艺简单，通过简单离子交换即可实现全可见光范围调色，表面配体修饰获得高发光量子效率，基质包覆即可制备高亮度量子点薄膜和粉末。然而，由于CsPbX3量子点本征离子性质和具有低的形成能，其稳定性一直没能得到有效解决，尤其是制作成膜或者粉体后，量子效率迅速下降，这严重制约了自身在光电器件中的实际应用。In recent years, all-inorganic perovskite CsPbX 3 (X=Cl, Br, I) quantum dots have attracted a lot of attention, and have shown extraordinary application potential in the field of optoelectronics, mainly because of their unique optical properties: the emission wavelength can be tune, wide absorption, wide color gamut, high quantum efficiency, etc. The preparation process of CsPbX 3 quantum dots is simple, and the full range of visible light color can be realized by simple ion exchange. The surface ligand modification can obtain high luminous quantum efficiency, and the matrix coating can prepare high-brightness quantum dot films and powders. However, due to the intrinsic ionic properties and low formation energy of CsPbX 3 quantum dots, its stability has not been effectively solved, especially after the film or powder is made, the quantum efficiency drops rapidly, which seriously restricts its own photoelectricity. practical application of the device.
采用原位析晶法将CsPbX3量子点嵌入在无机氧化物玻璃中的制备方案被证明是一种简单而有效的提高量子点稳定性的策略。因为无机氧化物玻璃作为保护层阻止了内部量子点与外界的接触。许多低熔点的无机氧化物玻璃基质已被证实可以原位析出钙钛矿量子点，如硼硅酸盐玻璃、硼锗酸盐玻璃、碲酸盐玻璃、磷酸盐玻璃等等。不过，不同于胶体量子点的湿化学制备方法，在玻璃中原位生长CsPbX3量子点往往受到玻璃基质网络结构的制约作用，紧致的玻璃网络严重抑制了Cs+、Pb2+、X-等离子的扩散，致使CsPbX3量子点玻璃发光效率普遍较低。而且所报道的钙钛矿量子点玻璃制备方法往往需要两步法，再经过高温熔融制备前驱体玻璃后，需要后续热处理或者激光诱导等方式才能在玻璃内部析出钙钛矿量子点。The fabrication scheme of CsPbX QDs embedded in inorganic oxide glass by in situ crystallization was proved to be a simple and effective strategy to improve the stability of QDs. Because the inorganic oxide glass acts as a protective layer to prevent the internal quantum dots from contacting the outside world. Many inorganic oxide glass substrates with low melting point have been proved to be able to precipitate perovskite quantum dots in situ, such as borosilicate glass, borogermanate glass, tellurate glass, phosphate glass and so on. However, unlike the wet chemical preparation method of colloidal quantum dots, the in situ growth of CsPbX 3 quantum dots in glass is often restricted by the network structure of the glass matrix, and the compact glass network severely inhibits the Cs + , Pb 2+ , X - plasma The diffusion of CsPbX 3 quantum dot glass leads to generally low luminous efficiency. Moreover, the reported perovskite quantum dot glass preparation method often requires a two-step method. After the precursor glass is prepared by high-temperature melting, subsequent heat treatment or laser induction is required to precipitate perovskite quantum dots inside the glass.
发明内容Contents of the invention
为解决上述问题，本发明提供一种全无机钙钛矿量子点复合玻璃，包含玻璃基质、玻璃修饰氧化物和无机钙钛矿量子点基质，其中，所述玻璃基质为Na2O-ZnO-B2O3-SiO2体系，所述玻璃修饰氧化物为所述玻璃基质的5％-20％，所述全无机钙钛矿量子点基质摩尔比为所述玻璃基质的5％～30％。In order to solve the above problems, the present invention provides an all-inorganic perovskite quantum dot composite glass, comprising a glass matrix, a glass modified oxide and an inorganic perovskite quantum dot matrix, wherein the glass matrix is Na 2 O—ZnO— B 2 O 3 -SiO 2 system, the glass-modified oxide is 5%-20% of the glass matrix, and the molar ratio of the all-inorganic perovskite quantum dot matrix is 5%-30% of the glass matrix .
优选的，所述玻璃修饰氧化物可以为MgO、CaO、SrO和BaO中一种或多种Preferably, the glass modified oxide can be one or more of MgO, CaO, SrO and BaO
优选的，全无机钙钛矿量子点基质为卤化铅铯钙钛矿Cs2CO3-PbO-AX(A：Li，Na，K中一种或多种；X：Cl，Br，I中一种或多种)。Preferably, the all-inorganic perovskite quantum dot matrix is cesium lead halide perovskite Cs 2 CO 3 -PbO-AX (A: one or more of Li, Na, K; X: one of Cl, Br, I one or more species).
优选的，全无机钙钛矿量子点基质原料组成为Cs2CO3-PbO-AX(A：Li，Na，K中一种或多种；X：Cl，Br，I中一种或多种)。Preferably, the all-inorganic perovskite quantum dot matrix raw material is composed of Cs 2 CO 3 -PbO-AX (A: one or more of Li, Na, K; X: one or more of Cl, Br, I ).
优选的，所述玻璃基质包括10～20mol％氧化钠，10～30mol％氧化锌，40-60mol％氧化硼，10-30mol％氧化硅。Preferably, the glass matrix includes 10-20 mol% sodium oxide, 10-30 mol% zinc oxide, 40-60 mol% boron oxide, and 10-30 mol% silicon oxide.
优选的，所述全无机钙钛矿量子点复合玻璃厚度为0.05-3mm。Preferably, the thickness of the all-inorganic perovskite quantum dot composite glass is 0.05-3mm.
优选的，所述全无机钙钛矿发射波长为440-680nm。Preferably, the emission wavelength of the all-inorganic perovskite is 440-680nm.
基于同样的发明构思，本发明提供一种复合量子点玻璃的制备方法，包括Based on the same inventive concept, the present invention provides a method for preparing composite quantum dot glass, comprising
S1：在所述玻璃基质中加入所述玻璃修饰氧化物和全无机钙钛矿量子点基质原料烧结得熔融体；S1: adding the glass-modified oxide and all-inorganic perovskite quantum dot matrix raw materials into the glass matrix and sintering to obtain a melt;
S2：将所述熔融体浇铸成型，得到所述全无机钙钛矿量子点复合玻璃；S2: Casting the molten body to obtain the all-inorganic perovskite quantum dot composite glass;
优选的，所述S1中烧结温度为900℃-1350℃，烧结时间为5～60min。Preferably, the sintering temperature in S1 is 900°C-1350°C, and the sintering time is 5-60min.
优选的，所述S2具体为将所述熔融体浇铸在预热温度为200～300℃的模具中成型，保温0.5～3h，然后自然冷却。Preferably, the S2 is specifically to cast the melt into a mold with a preheating temperature of 200-300° C., keep it warm for 0.5-3 hours, and then cool it down naturally.
优选的，所述模具为铁板，铜板，或不锈钢板。Preferably, the mold is an iron plate, a copper plate, or a stainless steel plate.
本发明的有益效果：Beneficial effects of the present invention:
(1)本发明全无机钙钛矿量子点复合玻璃通过以Na2O-ZnO-B2O3-SiO2作为基质玻璃体系，硼硅体系玻璃透明度高，物理化学性能稳定，同时，Na2O和ZnO能有效降低玻璃的熔融温度，玻璃修饰氧化物能够调节玻璃网络结构维度，使玻璃网络更加松软，使得全无机钙钛矿量子点在玻璃中更易原位析出，全无机钙钛矿量子点基质原料中PbO既能降低玻璃熔点，又能作为提供钙钛矿所需Pb元素，进一步促进了全无机钙钛矿量子点的形成。(1) The all-inorganic perovskite quantum dot composite glass of the present invention uses Na 2 O-ZnO-B 2 O 3 -SiO 2 as the matrix glass system. The borosilicate system glass has high transparency and stable physical and chemical properties. At the same time, Na 2 O and ZnO can effectively reduce the melting temperature of glass, and glass-modified oxides can adjust the dimension of the glass network structure, making the glass network softer, making it easier for all-inorganic perovskite quantum dots to be precipitated in situ in the glass. PbO in the dot matrix material can not only reduce the melting point of glass, but also serve as the Pb element required for perovskite, which further promotes the formation of all-inorganic perovskite quantum dots.
(2)本发明中全无机钙钛矿量子点复合玻璃的制备方法简单，使用基质玻璃的原料、玻璃修饰氧化物和全无机钙钛矿量子点原料按照一定配比充分混合，一次烧结即可得到全无机钙钛矿量子点复合玻璃，操作工序简单，量子点复合玻璃稳定性好，发射光谱窄，物理化学性质稳定，且量子点发光性能可通过熔融条件和原料组分有效调节，应用于发光器件。特别的，本发明可用于LED和显示技术。(2) The preparation method of the all-inorganic perovskite quantum dot composite glass in the present invention is simple, and the raw material of the matrix glass, the glass modified oxide and the all-inorganic perovskite quantum dot raw material are fully mixed according to a certain proportion, and one-time sintering is enough The all-inorganic perovskite quantum dot composite glass is obtained, the operation process is simple, the quantum dot composite glass has good stability, narrow emission spectrum, stable physical and chemical properties, and the quantum dot luminescence performance can be effectively adjusted by melting conditions and raw material components. Light emitting devices. In particular, the invention can be used in LED and display technology.
附图说明Description of drawings
图1为本发明实施例1制得的全无机钙钛矿量子点复合玻璃的荧光发射光谱图；Fig. 1 is the fluorescence emission spectrogram of the all-inorganic perovskite quantum dot composite glass obtained in Example 1 of the present invention;
图2为本发明实施例1制得的全无机钙钛矿量子点复合玻璃与芯片耦合发光图；Fig. 2 is the all-inorganic perovskite quantum dot composite glass and the chip coupling luminescent diagram that the
图3为本发明实施例2制得的全无机钙钛矿量子点复合玻璃的荧光发射光谱图；Fig. 3 is the fluorescence emission spectrogram of the all-inorganic perovskite quantum dot composite glass obtained in Example 2 of the present invention;
图4为本发明实施例2制得的全无机钙钛矿量子点复合玻璃与芯片耦合发光图；Fig. 4 is the all-inorganic perovskite quantum dot composite glass and the chip coupling luminescent diagram that the embodiment 2 of the present invention makes;
图5为本发明实施例2制得的全无机钙钛矿量子点复合玻璃的荧光发射光谱图；Fig. 5 is the fluorescence emission spectrogram of the all-inorganic perovskite quantum dot composite glass prepared in Example 2 of the present invention;
图6为本发明实施例2制得的全无机钙钛矿量子点复合玻璃与芯片耦合发光图Fig. 6 is the coupling luminescence diagram of the all-inorganic perovskite quantum dot composite glass and the chip prepared in Example 2 of the present invention
具体实施方式Detailed ways
为使本发明的目的、技术方案和优点更加清楚明了，下面通过附图及实施例，对本发明进行进一步详细说明。但是应该理解，此处所描述的具体实施例仅用以解释本发明，并不用于限制本发明的范围。In order to make the object, technical solution and advantages of the present invention clearer, the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. However, it should be understood that the specific embodiments described here are only used to explain the present invention, and are not intended to limit the scope of the present invention.
本发明提供的全无机钙钛矿量子点复合玻璃，包含玻璃基质、玻璃修饰氧化物和全无机钙钛矿量子点基质，其中，所述玻璃修饰氧化物为所述玻璃基质的5％-20wt％，所述全无机钙钛矿量子点基质为所述玻璃基质的5％～30wt％；量子点玻璃厚度为0.05-3mm。全无机钙钛矿发射波长为440-680nm。所述玻璃修饰氧化物可以为MgO、CaO、SrO和BaO中一种或多种；所述卤化铅铯钙钛矿组分包括：Cs2CO3-PbO-AX(A：Li，Na，K中一种或多种；X：Cl，Br，I中一种或多种)。The all-inorganic perovskite quantum dot composite glass provided by the present invention comprises a glass matrix, a glass-modified oxide and an all-inorganic perovskite quantum dot matrix, wherein the glass-modified oxide is 5%-20wt of the glass matrix %, the all-inorganic perovskite quantum dot matrix is 5%-30wt% of the glass matrix; the thickness of the quantum dot glass is 0.05-3mm. The emission wavelength of the all-inorganic perovskite is 440-680nm. The glass-modified oxide can be one or more of MgO, CaO, SrO and BaO; the cesium lead halide perovskite component includes: Cs 2 CO 3 -PbO-AX (A: Li, Na, K One or more of them; X: one or more of Cl, Br, I).
实施例一：本实施例提供一种绿光钙钛矿量子点复合玻璃Embodiment 1: This embodiment provides a green light perovskite quantum dot composite glass
将分析纯的Na2CO3、ZnO、B2O3、SiO2、SrCO3、Cs2CO3、PbO、NaBr，按照基质玻璃原料10mol％Na2O,15mol％ZnO,55mol％B2O3,20mol％SiO2,；10wt％SrO，20wt％量子点原料，其中量子点原料各组分按10mol％Cs2CO3：20mol％PbO：70mol％KBr的摩尔分数配比精确称量后置于玛瑙研钵中，在玛瑙研钵中并研磨均匀后置于刚玉坩埚中，放入1050℃的马弗炉中保温10min，而后，将玻璃溶体取出快速浇铸在预热温度为250℃的模具中成型，保温1h，然后自然冷却，即可得到绿光钙钛矿量子点复合玻璃。Analytical pure Na 2 CO 3 , ZnO, B 2 O 3 , SiO 2 , SrCO 3 , Cs 2 CO 3 , PbO, NaBr, according to the matrix glass raw material 10mol% Na 2 O, 15mol% ZnO, 55mol% B 2 O 3 , 20mol% SiO 2 ,; 10wt% SrO, 20wt% quantum dot raw material, wherein each component of the quantum dot raw material is accurately weighed according to the molar ratio of 10mol% Cs 2 CO 3 : 20mol% PbO: 70mol% KBr In the agate mortar, grind evenly in the agate mortar, place it in a corundum crucible, put it in a muffle furnace at 1050°C and keep it warm for 10 minutes, then take out the glass melt and quickly cast it in a mold with a preheating temperature of 250°C Molding in medium temperature, heat preservation for 1h, and then natural cooling, the green light perovskite quantum dot composite glass can be obtained.
采用荧光光谱仪(FLS920，英国爱丁堡Instruments公司)对上述所得的量子点复合玻璃进行测定，所得的谱图如图1所示，在365nm波长激发下，它的发射波长位于515nm，半高峰宽为27nm，对应钙钛矿量子点CsPbBr3的荧光发射，利用杭州远方STC4000快速光谱仪将复合量子点玻璃与365nm的芯片耦合，发出明亮的绿光，如图2所示。Adopt fluorescence spectrometer (FLS920, U.K. Edinburgh Instruments company) to measure the quantum dot composite glass of above-mentioned gained, the spectrogram of gained is as shown in Figure 1, and under 365nm wavelength excitation, its emission wavelength is positioned at 515nm, half peak width is 27nm , corresponding to the fluorescence emission of perovskite quantum dots CsPbBr 3 , using Hangzhou Yuanfang STC4000 fast spectrometer to couple the composite quantum dot glass with a 365nm chip to emit bright green light, as shown in Figure 2.
实施例二：本实施例提供一种蓝光钙钛矿量子点复合玻璃Embodiment 2: This embodiment provides a blue light perovskite quantum dot composite glass
将分析纯的Na2CO3、ZnO、B2O3、SiO2、BaCO3、Cs2CO3、PbO、NaBr、NaCl，按照基质玻璃原料15mol％Na2O,15mol％ZnO,50mol％B2O3,20mol％SiO2；10wt％CaO；20wt％钙钛矿原料，其中钙钛矿原料各组分按10mol％Cs2CO3：20mol％PbO：25mol％NaBr：45mol％NaCl的摩尔分数配比精确称量后置于玛瑙研钵中，在玛瑙研钵中并研磨均匀后置于刚玉坩埚中，放入1100℃的马弗炉中保温15min，而后，将玻璃溶体取出快速浇铸在预热温度为200℃的模具中成型，保温2h，然后自然冷却，即可得到复合量子点玻璃；Analytical pure Na 2 CO 3 , ZnO, B 2 O 3 , SiO 2 , BaCO 3 , Cs 2 CO 3 , PbO, NaBr, NaCl, according to the matrix glass raw material 15mol% Na 2 O, 15mol% ZnO, 50mol% B 2 O 3 , 20mol% SiO 2 ; 10wt% CaO; 20wt% perovskite raw material, wherein each component of the perovskite raw material is based on the mole fraction of 10mol% Cs 2 CO 3 : 20mol% PbO: 25mol% NaBr: 45mol% NaCl The ratio is accurately weighed and placed in an agate mortar, ground evenly in the agate mortar, placed in a corundum crucible, placed in a muffle furnace at 1100°C for 15 minutes, and then the glass melt is taken out and quickly cast in a pre- Molded in a mold with a heating temperature of 200°C, kept warm for 2 hours, and then cooled naturally to obtain composite quantum dot glass;
采用荧光光谱仪(FLS920，英国爱丁堡Instruments公司)对上述所得的复合量子点玻璃进行测定，所得的谱图如图3所示，在365nm波长激发下，发射波长位于450nm，半高峰宽为21nm，对应钙钛矿量子点CsPb(Br,Cl)3的荧光发射，利用杭州远方STC4000快速光谱仪将复合量子点玻璃与365nm的紫外光芯片耦合，发出明亮的蓝光，如图4所示。Adopt fluorescence spectrometer (FLS920, Instruments company of Edinburgh, U.K.) to measure the composite quantum dot glass of above-mentioned gained, the spectrogram of gained is as shown in Figure 3, under the excitation of 365nm wavelength, emission wavelength is positioned at 450nm, half peak width is 21nm, corresponding For the fluorescence emission of perovskite quantum dots CsPb(Br,Cl) 3 , the composite quantum dot glass is coupled with a 365nm ultraviolet chip by using Hangzhou Yuanfang STC4000 fast spectrometer to emit bright blue light, as shown in Figure 4.
实施例三：本实施例提供一种红光钙钛矿量子点复合玻璃Embodiment 3: This embodiment provides a red light perovskite quantum dot composite glass
将分析纯的Na2CO3、ZnO、B2O3、SiO2、BaCO3、Cs2CO3、PbO、NaBr、NaCl，按照基质玻璃原料15mol％Na2O,15mol％ZnO,50mol％B2O3,20mol％SiO2；10wt％BaO；20wt％钙钛矿原料，其中钙钛矿原料各组分按7.5mol％Cs2CO3：15mol％PbO：30mol％NaBr：47.5mol％LiI的摩尔分数配比精确称量后置于玛瑙研钵中，在玛瑙研钵中并研磨均匀后置于刚玉坩埚中，放入1150℃的马弗炉中保温10min，而后，将玻璃溶体取出快速浇铸在预热温度为300℃的模具中成型，保温0.5h，然后自然冷却，即可得到复合量子点玻璃；Analytical pure Na 2 CO 3 , ZnO, B 2 O 3 , SiO 2 , BaCO 3 , Cs 2 CO 3 , PbO, NaBr, NaCl, according to the matrix glass raw material 15mol% Na 2 O, 15mol% ZnO, 50mol% B 2 O 3 , 20mol% SiO 2 ; 10wt% BaO; 20wt% perovskite raw material, wherein each component of the perovskite raw material is based on 7.5mol% Cs 2 CO 3 : 15mol% PbO: 30mol% NaBr: 47.5mol% LiI The mole fraction ratio is accurately weighed and placed in an agate mortar, ground evenly in the agate mortar, placed in a corundum crucible, placed in a muffle furnace at 1150°C for 10 minutes, and then the glass melt is taken out and quickly cast Forming in a mold with a preheating temperature of 300°C, holding the temperature for 0.5h, and then cooling naturally, the composite quantum dot glass can be obtained;
采用荧光光谱仪(FLS920，英国爱丁堡Instruments公司)对上述所得的复合量子点玻璃进行测定，所得的谱图如图5所示，在365nm波长激发下，发射波长位于619nm，半高峰宽为36nm，对应钙钛矿量子点CsPb(Br,I)3的荧光发射，利用杭州远方STC4000快速光谱仪将复合量子点玻璃与365nm的紫外光芯片耦合，发出明亮的红光，如图6所示。Adopt fluorescence spectrometer (FLS920, Instruments company of Edinburgh, U.K.) to measure the composite quantum dot glass of the above-mentioned gained, the spectrogram of gained is as shown in Figure 5, under the excitation of 365nm wavelength, emission wavelength is positioned at 619nm, half peak width is 36nm, corresponding For the fluorescence emission of perovskite quantum dots CsPb(Br,I) 3 , the composite quantum dot glass is coupled with a 365nm ultraviolet light chip by using Hangzhou Yuanfang STC4000 fast spectrometer to emit bright red light, as shown in Figure 6.
以上内容是结合优选技术方案对本发明所做的进一步说明，所描述的实例是本发明的一部分实例，而不是全部实例。对于本发明所属技术领域的研究人员来说，在不脱离构思的前提下还可以做出简单推演和替换，在没有做出创造性劳动前提下所获得的其他实例，都属于本发明保护的范围。The above content is a further description of the present invention in conjunction with the preferred technical solutions, and the described examples are part of the examples of the present invention, not all examples. For researchers in the technical field to which the present invention belongs, simple deduction and substitution can be made without departing from the idea, and other examples obtained without creative work all belong to the protection scope of the present invention.
Claims (8)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210975525.1A CN115259663A (en) | 2022-08-15 | 2022-08-15 | A kind of all-inorganic perovskite quantum dot composite glass and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210975525.1A CN115259663A (en) | 2022-08-15 | 2022-08-15 | A kind of all-inorganic perovskite quantum dot composite glass and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN115259663A true CN115259663A (en) | 2022-11-01 |
Family
ID=83750278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202210975525.1A Pending CN115259663A (en) | 2022-08-15 | 2022-08-15 | A kind of all-inorganic perovskite quantum dot composite glass and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN115259663A (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116282927A (en) * | 2023-04-07 | 2023-06-23 | 上海应用技术大学 | A dual-emission color-tunable composite glass-ceramic and its preparation method and application |
| CN117142763A (en) * | 2023-09-05 | 2023-12-01 | 昆明理工大学 | A method to enhance the luminescence of perovskite quantum dot glass |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194593A (en) * | 2019-05-08 | 2019-09-03 | 杭州电子科技大学 | A method of full-inorganic perovskite quantum dot crystallization in glass is promoted by addition fluoride |
| CN110294597A (en) * | 2019-05-28 | 2019-10-01 | 华南农业大学 | A kind of width colour gamut, which show, uses caesium lead bromine perovskite quantum dot fluorescence glass and its preparation method and application |
| CN110963711A (en) * | 2019-12-13 | 2020-04-07 | 深圳第三代半导体研究院 | A kind of composite quantum dot glass and preparation method thereof |
| KR20200139329A (en) * | 2019-06-04 | 2020-12-14 | 부산대학교 산학협력단 | Perovskite quantum dot based on M13 bacteriophage, method for preparing thereof, and display device using thereof |
| CN113831022A (en) * | 2021-10-18 | 2021-12-24 | 上海应用技术大学 | A kind of formula, preparation method and application of CsPbBr3:xDy3+ quantum dot glass |
-
2022
- 2022-08-15 CN CN202210975525.1A patent/CN115259663A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110194593A (en) * | 2019-05-08 | 2019-09-03 | 杭州电子科技大学 | A method of full-inorganic perovskite quantum dot crystallization in glass is promoted by addition fluoride |
| CN110294597A (en) * | 2019-05-28 | 2019-10-01 | 华南农业大学 | A kind of width colour gamut, which show, uses caesium lead bromine perovskite quantum dot fluorescence glass and its preparation method and application |
| KR20200139329A (en) * | 2019-06-04 | 2020-12-14 | 부산대학교 산학협력단 | Perovskite quantum dot based on M13 bacteriophage, method for preparing thereof, and display device using thereof |
| CN110963711A (en) * | 2019-12-13 | 2020-04-07 | 深圳第三代半导体研究院 | A kind of composite quantum dot glass and preparation method thereof |
| CN113831022A (en) * | 2021-10-18 | 2021-12-24 | 上海应用技术大学 | A kind of formula, preparation method and application of CsPbBr3:xDy3+ quantum dot glass |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116282927A (en) * | 2023-04-07 | 2023-06-23 | 上海应用技术大学 | A dual-emission color-tunable composite glass-ceramic and its preparation method and application |
| CN117142763A (en) * | 2023-09-05 | 2023-12-01 | 昆明理工大学 | A method to enhance the luminescence of perovskite quantum dot glass |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN110294597B (en) | Cesium-lead-bromine perovskite quantum dot fluorescent glass for wide color gamut display and preparation method and application thereof | |
| CN105523715B (en) | Transparent fluorescent glass of a kind of low melting point and preparation method thereof and the application in white light LEDs | |
| CN115259663A (en) | A kind of all-inorganic perovskite quantum dot composite glass and preparation method thereof | |
| CN101381204B (en) | CaO-MgO-SiO2 series fluorescent glass-ceramics and preparation method thereof | |
| CN111574062B (en) | A kind of nitride red light glass and its application | |
| CN102121591A (en) | White LED light source and manufacturing method of phosphor thereof | |
| Xu et al. | High refractive index coating of phosphor-in-glass for enhanced light extraction efficiency of white LEDs | |
| CN103496852A (en) | Glass ceramic for blue light-excited white-light LED (Light-Emitting Diode), and preparation method thereof | |
| CN114394753B (en) | A high luminescence quantum efficiency CsPbBr3 perovskite quantum dot glass and its preparation method and application | |
| CN109592907B (en) | Borobismuthate glass-based Ce:YAG glass-ceramic for white light LED and preparation method thereof | |
| CN107500529B (en) | YAG fluorescent glass, preparation method thereof and application thereof in white light LED | |
| CN105236750A (en) | Rare earth-doped white-light fluorescent phosphate glass ceramics material and preparation method thereof | |
| CN101857423B (en) | Light-emitting low-temperature co-fired ceramic powder, preparation method thereof and light-emitting low-temperature co-fired ceramic | |
| CN106698933B (en) | A kind of devitrified glass and its preparation method and application of transparent low melting point | |
| CN202048398U (en) | White-light LED (light-emitting diode) light source | |
| CN105819696A (en) | Low temperature glass-phosphor composite material and preparation method thereof | |
| Li et al. | Low-temperature sintering coating of phosphor in TeO2–SiO2–B2O3–ZnO glass for enhanced luminous efficacy of white LED | |
| CN102092952A (en) | Transparent glass ceramic with tunable light emitting colors and preparation technique thereof | |
| CN108585482A (en) | A kind of white light LEDs fluorescent glass piece and preparation method thereof | |
| CN114276012B (en) | A rare earth element Dy-doped fluoroborate luminescent glass and its preparation method | |
| CN116535205B (en) | A double-layer composite structure fluorescent ceramic material for laser lighting and its preparation method | |
| CN104986956A (en) | Oxide glass with rare earth ion single-doped white up-conversion luminescence and preparation method thereof | |
| CN104529170B (en) | A kind of transparent Ce：YAG devitrified glass and its application in white light LEDs | |
| CN110590158A (en) | A kind of borate fluorescent glass and its preparation method and application | |
| CN111099896A (en) | Dysprosium-doped potassium sodium niobate-based transparent ceramic for white light LED and preparation method thereof |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination |