CN115124247A - All-inorganic perovskite quantum dot glass ceramic material and preparation method thereof - Google Patents
All-inorganic perovskite quantum dot glass ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an all-inorganic perovskite quantum dot glass ceramic material and a preparation method thereof, wherein the chemical formula of the all-inorganic perovskite quantum dot glass ceramic material is CsPb (A) x B 1‑x ) 3 Wherein A, B is one or two of Cl, Br or I, x is more than or equal to 0 and less than or equal to 1, and the components and the molar content of the precursor glass matrix are as follows: 40-60 mol% GeO 2 ，20‑40 mol% B 2 O 3 ，3‑10 mol% ZnO，3‑10 mol% CaO，3‑10 mol% PbO，5‑10 mol% CsCO 3 0-14 mol% of NaCl, 0-14 mol% of NaBr and 0-14 mol% of NaI, wherein the total mol amount of the components is 100 mol%. The perovskite quantum dot microcrystalline glass material disclosed by the invention is simple in preparation process and good in luminescence property, can realize high-efficiency down-conversion luminescence in the whole visible light range under the excitation of an ultraviolet lamp, and has an important application prospect in the field of solid-state illumination.
Description
Technical Field
The invention relates to the field of optical functional materials, in particular to an all-inorganic perovskite quantum dot glass ceramic material and a preparation method thereof.
Background
In recent years, the problem of energy crisis is increasingly prominent, and energy depletion is a common problem facing the world at present. The consumption of light illumination on energy is huge, and the global illumination electricity consumption accounts for nearly 20% of the total world electricity consumption according to statistics. In order to save energy, green illumination light sources with environmental protection and energy saving are actively popularized in various countries. White light LED is a new solid-state light source, and has a series of advantages such as high efficiency, energy saving, environmental protection, long service life, stable light emitting performance, and small size, so it is considered as a new generation of green light source, and has been widely used in the fields of illumination, display, landscape decoration, etc. The luminescent material is one of key technologies for preparing the LED with excellent performance, and the performance of the luminescent material can directly influence important parameters such as luminous efficiency, luminous intensity and the like of the LED. At present, a commercial white light LED mainly adopts a combination of yellow fluorescent powder and a blue light chip, however, the white light LED lacks a red light component, and the problems of high white light color temperature, low color rendering index and the like are easily caused; in addition, the silica gel used for packaging is easy to age under high-power light radiation or higher use temperature, so that light attenuation, color cast and the like of products are caused. Compared with the traditional fluorescent material for the white light LED, the all-inorganic perovskite quantum dot CsPbX 3 (X = Cl, Br, I), due to its unique optical properties, such as narrow emission band, high quantum yield, adjustable color, etc., has attracted more and more attention of researchers, becoming a promising luminescent material for next generation lighting and display devices. But all-inorganic perovskite quantum dot CsPbX 3 There still exist some disadvantages that moisture, oxygen, etc. in the environment cause their degradation and their properties deteriorate rapidly due to low energy of quantum dot formation and high surface activity, so that their practical applications are limited. Therefore, if the defect of poor physical stability of perovskite quantum dots can be overcome and the advantage of excellent luminescence property is exerted, the all-inorganic perovskite quantum dots CsPbX are expected to be realized 3 The LED can replace the traditional fluorescent material to obtain a high-performance LED, thereby realizing environmental protection and energy saving.
Inorganic oxide glass has excellent thermal and physicochemical stability, and has been widely used as a matrix of various nano/micro crystals (such as fluoride, oxide, quantum dots, and the like), and the core of the inorganic oxide glass lies in the careful design of a glass network structure and the control of crystalline phase nucleation/growth. The quantum dots are embedded into the inorganic glass, so that the excellent optical performance of the quantum dots can be effectively exerted, and the problem of poor stability of the quantum dots can be solved.
Disclosure of Invention
The invention aims to provide an all-inorganic perovskite quantum dot glass ceramic material and a preparation method thereof, quantum dot glass presents efficient down-conversion luminescence in the whole visible light range (410-700 nm) under the excitation of ultraviolet light, and the all-inorganic perovskite quantum dot glass ceramic material can be used in the field of solid-state lighting.
In order to realize the purpose, the invention adopts the following technical scheme:
an all-inorganic perovskite quantum dot glass ceramic material with a chemical formula of CsPb (A) x B 1-x ) 3 Wherein A, B is one or two of Cl, Br or I, x is more than or equal to 0 and less than or equal to 1, and the precursor glass matrix of the perovskite quantum dot glass ceramic material comprises the following components in molar content: 40-60 mol% GeO 2 ，20-40 mol% B 2 O 3 ，3-10 mol% ZnO，3-10 mol% CaO，3-10 mol% PbO，5-10 mol% CsCO 3 0-14 mol% of NaCl, 0-14 mol% of NaBr and 0-14 mol% of NaI, wherein the total mol amount of the components is 100 mol%.
Preferably, the molar contents of the components are as follows: 40-50 mol% GeO 2 ，20-30 mol% B 2 O 3 ，3-5 mol% ZnO，3-5 mol% CaO，3-5mol% PbO ，5-8 mol% CsCO 3 ，0-14 mol% NaCl，0-14 mol% NaBr，0-14 mol% NaI。
The preparation method of the all-inorganic perovskite quantum dot glass ceramic material comprises the following steps:
(1) adding GeO 2 、B 2 O 3 、ZnO、CaO、PbO、CsCO 3 Weighing powder raw materials of NaCl, NaBr and NaI in an agate mortar according to a molar ratio, mixing and fully grinding to obtain mixed powder;
(2) placing the obtained mixed powder into an alumina crucible, placing the alumina crucible into a high-temperature box-type furnace, heating and preserving heat for a period of time to melt the mixed powder, quickly pouring the molten liquid into a preheated copper mold, and cooling and forming to obtain precursor glass;
(3) and carrying out high-temperature stress removal treatment and high-temperature heat treatment on the precursor glass to obtain the perovskite quantum dot glass ceramics.
In the step (2), the heating and melting temperature in the high-temperature box furnace is 900-1000 ℃, preferably 950-1000 ℃, and the heat preservation time is 10-30 min, preferably 15-20 min.
In the step (3), the temperature of the high-temperature stress relief treatment is 300-400 ℃, and the stress relief time is 3-5 h; the high-temperature heat treatment temperature of the precursor glass after the stress relief treatment is 480-560 ℃, and the heat treatment time is 10-30 h. Obtaining a full series of fully inorganic CsPbX 3 The color of the perovskite quantum dot glass is changed from light green to dark red.
The perovskite quantum dot glass ceramics can be applied to white light LEDs.
The invention has the following remarkable advantages: the preparation method is simple and convenient, the glass matrix structure is stable, the obtained microcrystalline glass material has good transparency, and the glass matrix contains uniformly distributed perovskite quantum dots CsPbX 3 The (X = Cl, Br, I) nanocrystalline phase has fluorescence emission performance covering the whole visible light range (410-700 nm) under the excitation of ultraviolet light, and has important application prospects in the field of solid-state lighting.
Drawings
FIG. 1 is an all-inorganic CsPbX 3 Photograph of perovskite quantum dot glass ceramics (CsPbCl from left to right respectively) 3 、CsPb(Br/Cl) 3 、CsPbBr 3 、CsPb(Br/I) 3 And CsPbI 3 A quantum dot glass photo, wherein the first line is precursor glass, the second line is quantum dot glass ceramics corresponding to the first line under the irradiation of natural light, and the third line is quantum dot glass ceramics corresponding to the first line under the irradiation of ultraviolet light);
FIG. 2 is an X-ray diffraction pattern (XRD) of all-inorganic perovskite quantum dot glass ceramics with different halogen contents;
FIG. 3 is an emission spectrum of all-inorganic perovskite quantum dot glass ceramics with different halogen contents under ultraviolet excitation;
FIG. 4 shows CsPb (Br/I) under different heat treatment temperature conditions 3 An X-ray diffraction pattern of the quantum dot glass ceramics;
FIG. 5Is CsPb (Br/I) under the condition of heat treatment temperature of 520 ℃/10 h 3 TEM image of quantum dot glass ceramics;
FIG. 6 shows CsPb (Br/I) under different heat treatment temperature conditions 3 The fluorescence emission spectrum of the quantum dot microcrystalline glass is shown in an inset as a normalized spectrum;
FIG. 7 shows CsPb (Br/I) under different heat treatment temperature conditions 3 A PLQY dot diagram of quantum dot glass ceramics;
FIG. 8 is a picture of blue light excited perovskite quantum dot glass white light LED luminescence.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but the scope of the present invention is not limited to the description.
Example 1
Adding GeO 2 、B 2 O 3 、ZnO、CaO、PbO、CsCO 3 And NaCl in 40GeO 2 -30B 2 O 3 -3ZnO-3CaO-4PbO-6CsCO 3 Weighing 14NaCl (molar ratio), mixing in an agate mortar, fully grinding uniformly, placing in a crucible, placing in a high-temperature box furnace, heating to 1000 ℃ at a speed of 10 ℃/min, and preserving heat for 20 min to melt; then quickly pouring the molten liquid into a preheated copper mold grinding tool for cooling and forming to obtain transparent block precursor glass; finally, the glass after the stress removal treatment for 4 hours at 400 ℃ is heated to 520 ℃, and the temperature is preserved for 10 hours to obtain CsPbCl 3 Transparent glass ceramics (as the leftmost sample of fig. 1). X-ray diffraction data indicate CsPbCl precipitation in the glass matrix 3 The perovskite cubic phase (the uppermost first curve in fig. 2). The sample was polished and its room temperature emission spectrum was measured using an FLS1000 fluorescence spectrometer. The luminescence spectrum result shows that the microcrystalline glass emits stronger blue-violet light under the excitation of 365 nm ultraviolet light, the peak value is 412 nm, the half-peak width is 17 nm, and the peak value corresponds to CsPbCl 3 Exciton recombination emission of the nanocrystals is shown in fig. 3.
Example 2
Adding GeO 2 、B 2 O 3 、ZnO、CaO、PbO、CsCO 3 Powder raw material of NaBr and NaClAccording to 50GeO 2 -20B 2 O 3 -3ZnO-3CaO-4PbO-6CsCO 3 Weighing the mixture ratio of-10 NaCl to 4NaBr (molar ratio), mixing in an agate mortar, fully grinding uniformly, placing in a crucible, placing in a high-temperature box furnace, heating to 1000 ℃ at the speed of 10 ℃/min, and preserving heat for 20 min to melt; then quickly pouring the molten liquid into a preheated copper mold grinding tool for cooling and forming to obtain transparent block precursor glass; finally, the glass after the stress removal treatment for 4 hours at 400 ℃ is heated to 520 ℃ and is kept warm for 10 hours to obtain CsPb (Br/Cl) 3 Transparent glass ceramics (as the left two sample pictures in figure 1). X-ray diffraction data indicate that the cubic perovskite phase is precipitated in the glass matrix. The sample was polished and its room temperature emission spectrum was measured using an FLS1000 fluorescence spectrometer. The luminescence spectrum result shows that the microcrystalline glass emits stronger blue-violet light under the excitation of the ultraviolet light of 365 nm, the peak value is 454 nm, the half-peak width is 20 nm, and the peak value corresponds to CsPb (Br/Cl) 3 Exciton recombination emission of the nanocrystals is shown in fig. 3.
Example 3
Adding GeO 2 、B 2 O 3 、ZnO、CaO、PbO、CsCO 3 And NaBr powder raw material according to 40GeO 2 -30B 2 O 3 -3ZnO-3CaO-4PbO-6CsCO 3 Weighing 14NaBr (molar ratio), mixing in an agate mortar, fully grinding uniformly, placing in a crucible, placing in a high-temperature box furnace, heating to 1000 ℃ at a speed of 10 ℃/min, and keeping the temperature for 25 min to melt; then quickly pouring the molten liquid into a preheated copper mold grinding tool for cooling and forming to obtain transparent block precursor glass; finally, the glass after being stress-removed for 3 hours at 400 ℃ is heated to 520 ℃ and is kept warm for 10 hours to obtain CsPbBr 3 Transparent glass ceramics (as the 4 th sample picture in figure 1). X-ray diffraction data show that CsPbBr is precipitated in the glass matrix 3 Cubic perovskite phase (fourth XRD spectrum of fig. 2). The sample emits stronger green light under the excitation of the ultraviolet light 365 nm, the peak value is 524 nm, the half-peak width is 24 nm, and the half-peak width corresponds to CsPbBr 3 Exciton recombination emission of the nanocrystal.
Example 4
Adding GeO 2 、B 2 O 3 、ZnO、CaO、PbO、CsCO 3 Powder raw materials of NaBr and NaI according to the formula of 40GeO 2 -30B 2 O 3 -3ZnO-3CaO-4PbO-6CsCO 3 Weighing the mixture ratio of-4 NaBr to 10NaI (molar ratio), mixing in an agate mortar, fully grinding uniformly, placing in a crucible, placing in a high-temperature box furnace, heating to 950 ℃, and preserving heat for 30 min to melt; then quickly pouring the molten liquid into a copper mold grinding tool for cooling and forming to obtain transparent block precursor glass; finally, the glass after the stress removal treatment at 400 ℃ for 5 hours is subjected to heat treatment at 480-560 ℃, and the temperature is kept for 10 hours to obtain CsPb (Br/I) 3 Transparent glass ceramics (figure 1, 6 th picture). FIG. 4 shows X-ray diffraction data under different heat treatment conditions (480 ℃ -560 ℃), Precursor Glass (PG) is a typical amorphous peak, the increase of the diffraction peak with the increase of the heat treatment temperature shows that a corresponding perovskite cubic phase is precipitated in the glass matrix, and a TEM image of a sample with the heat treatment temperature of 520 ℃ is shown in FIG. 5, which shows that perovskite quantum dots are more uniformly precipitated in the glass matrix. The sample emits stronger red light under the excitation of the ultraviolet light of 365 nm, the peak value is 624 nm-640 nm, the half-peak width is 36 nm, and the peak value corresponds to CsPb (Br/I) 3 Exciton recombination emission of the nanocrystals (fig. 6), fluorescence quantum efficiency (PLQY) under different heat treatment temperature conditions as shown in fig. 7, it is evident that PLQY (38.24%) is higher in the sample after heat treatment at 520 ℃. A blue light LED chip with the central wavelength of 460 nm is selected as an excitation light source, and green CsPbBr is added 3 Quantum dot glass and red CsPb (Br/I) 3 Quantum dot glass combined with blue LED to make white LED (FIG. 8), CIE color coordinates (0.3150, 0.3023), confirmation CsPb (Br/I) 3 The perovskite quantum dot glass can be made into a white light LED.
Example 5
Adding GeO 2 、B 2 O 3 Powder raw materials of ZnO, CaO, PbO, CsCO and NaI according to the proportion of 45GeO 2 -25B 2 O 3 -3ZnO-5CaO-3PbO-5CsCO 3 Weighing the proportion of-14 NaI (molar ratio), mixing in an agate mortar, fully grinding uniformly, placing in a crucible, and heating in a high-temperature box type furnaceMelting at 950 deg.C for 30 min; then quickly pouring the molten liquid into a copper mold grinding tool for cooling and forming to obtain transparent block precursor glass; finally, the glass after the stress removal treatment at 400 ℃ for 4 hours is subjected to heat treatment at 500 ℃, and the temperature is kept for 10 hours to obtain CsPbI 3 Transparent glass ceramics. The sample emits stronger red light under the excitation of the ultraviolet light of 365 nm, the peak value is located at 698 nm, the half-peak width is 35 nm, and the emission intensity corresponds to CsPbI 3 Exciton recombination emission of the nanocrystals (fig. 3).
Claims (8)
1. The all-inorganic perovskite quantum dot glass ceramics are characterized in that the chemical formula is CsPb (A) x B 1-x ) 3 Wherein A, B is one or two of Cl, Br or I, x is more than or equal to 0 and less than or equal to 1, and the precursor glass matrix of the perovskite quantum dot glass ceramics comprises the following components in molar content: 40-60 mol% GeO 2 ，20-40 mol% B 2 O 3 ，3-10 mol% ZnO，3-10 mol% CaO，3-10 mol% PbO，5-10 mol% CsCO 3 0-14 mol% of NaCl, 0-14 mol% of NaBr and 0-14 mol% of NaI, wherein the total mol amount of the components is 100 mol%.
2. The all-inorganic perovskite quantum dot glass ceramic according to claim 1, wherein the precursor glass matrix of the perovskite quantum dot glass ceramic comprises the following components in molar content: 40-50 mol% GeO 2 ，20-30 mol% B 2 O 3 ，3-5 mol% ZnO，3-5 mol% CaO，3-5mol% PbO ，5-8 mol% CsCO 3 ，0-14 mol% NaCl，0-14 mol% NaBr，0-14 mol% NaI。
3. The all-inorganic perovskite quantum dot glass ceramic according to claim 1, wherein the perovskite quantum dot glass ceramic exhibits down-conversion luminescence in a visible light range of 410-700 nm under the excitation of ultraviolet light.
4. A preparation method of the all-inorganic perovskite quantum dot glass ceramics according to any one of claims 1 to 3, characterized by comprising the following steps:
(1) adding GeO 2 、B 2 O 3 、ZnO、CaO、PbO、CsCO 3 Weighing powder raw materials of NaCl, NaBr and NaI in an agate mortar according to a molar ratio, mixing and fully grinding to obtain mixed powder;
(2) placing the obtained mixed powder into an alumina crucible, placing the alumina crucible into a high-temperature box-type furnace, heating and preserving heat for a period of time to melt the mixed powder, quickly pouring the molten liquid into a preheated copper mold, and cooling and forming to obtain precursor glass;
(3) and carrying out high-temperature stress relief treatment and high-temperature heat treatment on the precursor glass to obtain the perovskite quantum dot glass ceramics.
5. The preparation method of the all-inorganic perovskite quantum dot glass ceramics according to claim 4, characterized in that in the step (2), the heating and melting temperature in a high-temperature box furnace is 900-1000 ℃, and the heat preservation time is 10-30 min.
6. The preparation method of the all-inorganic perovskite quantum dot glass ceramic according to claim 4, wherein in the step (3), the temperature of the high-temperature stress relief treatment is 300-400 ℃, and the stress relief time is 3-5 h.
7. The preparation method of the all-inorganic perovskite quantum dot glass ceramic according to claim 4, wherein in the step (3), the temperature of the high-temperature heat treatment is 480-560 ℃, and the heat treatment time is 10-30 h.
8. The use of the all-inorganic perovskite quantum dot glass ceramics according to any one of claims 1 to 3 in white light LEDs.
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| CN116239305A (en) * | 2023-03-22 | 2023-06-09 | 武汉理工大学 | Alkali metal alkaline earth metal halide perovskite nanocrystalline dispersion glass and application thereof |
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| CN116239305A (en) * | 2023-03-22 | 2023-06-09 | 武汉理工大学 | Alkali metal alkaline earth metal halide perovskite nanocrystalline dispersion glass and application thereof |
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