CN114394753B - High-luminous quantum efficiency CsPbBr 3 Perovskite quantum dot glass and preparation method and application thereof - Google Patents
High-luminous quantum efficiency CsPbBr 3 Perovskite quantum dot glass and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses a CsPbBr 3 Perovskite quantum dot glass and a preparation method thereof. The quantum dot glass comprises the following components: 20 to 35 percent of SiO 2 ，10～25％ZnO，30～50％B 2 O 3 ，3～8％SrCO 3 ，1～5％K 2 CO 3 ，0.5～3％BaCO 3 ，0.1～2％Sb 2 O 3 ，1～5％Cs 2 CO 3 Or 2-10% CsBr, 1-10% PbBr 2 Or PbO, 1-10% NaBr or KBr; the sum of the mole percentages of the components is 100 percent. The preparation method comprises the following steps: s1, weighing raw materials according to the glass composition, fully and uniformly mixing the raw materials, and pouring the raw materials into a graphite mold after high-temperature melting to obtain precursor glass; s2, transferring the obtained precursor glass into a muffle furnace for annealing treatment; s3, placing the annealed precursor glass into a muffle furnace for heat treatment. The quantum dot glass prepared by the invention has a main emission peak at 526nm under blue light excitation, a half-peak width of 23nm, and high luminous quantum efficiency, and in addition, the quantum dot glass can also resist high-temperature baking, and has good application prospect in the field of wide color gamut display.
Description
Technical Field
The invention belongs to the technical field of all-inorganic perovskite quantum dot display, and particularly relates to a high-luminous quantum efficiency CsPbBr 3 Perovskite quantum dot glass, and a preparation method and application thereof.
Background
CsPbBr 3 Is considered to be an ideal green material for wide color gamut display due to its advantages of high luminescence quantum efficiency and narrow emission band, however due to its lower formation energyAnd ionic character, making it relatively sensitive to water, oxygen, light, heat, etc., limiting its practical application. In order to solve the problem of poor luminescence stability, continuous efforts are made in industry and academia, such as coating or doping, which can solve the problem of luminescence stability to a certain extent, but not thoroughly. In addition, device packaging often requires high temperature baking, most of the CsPbBr available 3 The modified composite material cannot bear the weight, so that the light-emitting performance is seriously deteriorated, and meanwhile, the large-scale preparation is one of the main problems faced by the modified composite material. CsPbBr production by in situ crystallization in inorganic glass 3 Perovskite quantum dot glasses are believed to address CsPbBr 3 One of the important ways of poor luminescence stability is that the water resistance of the material depends on the stability of the glass matrix, and the luminescence thermal stability and the light stability of the material are obviously improved due to the isolation of water and oxygen.
However, csPbBr is currently available 3 Perovskite quantum dot glasses still face the following problems: (1) The glass composition is not properly selected, so that the moisture resistance and the weather resistance of the glass are poor; (2) quantum efficiency is generally not high under blue light excitation; (3) The high rigidity of the glass network structure or the small network gap limits the growth of perovskite quantum dots, so that the surface defects are more, and the luminous quantum efficiency is generally lower.
Disclosure of Invention
In order to solve the problems of the prior art, the invention provides a CsPbBr with high luminous quantum efficiency 3 Perovskite quantum dot glass, and a preparation method and application thereof. The invention has the advantages of easily available raw materials, simple preparation process, strong repeatability and easy large-scale preparation. CsPbBr prepared by the invention 3 The perovskite quantum dot glass has a main emission peak at 526nm, a half-peak width of 23nm, a quantum efficiency of 86% under 365nm ultraviolet excitation, a quantum efficiency of 53% under 455nm blue excitation, good luminescence stability, moisture and heat resistance and weather resistance, and potential application value in the field of wide color gamut display.
The aim of the invention is achieved by the following technical scheme:
high-luminous quantum efficiency CsPbBr 3 Perovskite quantum dot glassGlass, csPbBr 3 The perovskite quantum dot glass consists of the following components in mole percent: 20 to 35 percent of SiO 2 ，10～25％ZnO,30～50％B 2 O 3 ，3～8％SrCO 3 ，1～5％K 2 CO 3 ，0.5～3％BaCO 3 ，0.1～2％Sb 2 O 3 ，1～5％Cs 2 CO 3 Or 2-10% CsBr, 1-10% PbBr 2 Or PbO, 1-10% NaBr or KBr; the sum of the mole percentages of the components is 100 percent.
Preferably, the CsPbBr 3 The perovskite quantum dot glass consists of the following components in mole percent: the CsPbBr 3 The perovskite quantum dot glass consists of the following components in mole percent: 22-28% SiO 2 ，15～20％ZnO，35～45％B 2 O 3 ，5～7％SrCO 3 ，2～3％K 2 CO 3 ，1～2％BaCO 3 ，0.2～1.5％Sb 2 O 3 ，1.5～4.5％Cs 2 CO 3 Or 4 to 6 percent of CsBr,3 to 7 percent of PbBr 2 Or PbO, 3-7% NaBr or KBr; the sum of the mole percentages of the components is 100 percent.
Further, the CsPbBr 3 The main emission peak of the perovskite quantum dot glass is at 526nm, the half-width is 23nm, the quantum efficiency is up to 86% under the excitation of 365nm ultraviolet light, and the quantum efficiency is up to 53% under the excitation of 455nm blue light.
Further, the CsPbBr 3 The average size particle diameter of the quantum dots in the perovskite quantum dot glass is 25-30 nm.
The high luminous quantum efficiency CsPbBr 3 The preparation method of the perovskite quantum dot glass comprises the following operation steps:
s1, weighing raw materials according to the glass composition of claim 1, fully and uniformly mixing the raw materials, and pouring the raw materials into a graphite mold after high-temperature melting to obtain precursor glass;
s2, transferring the precursor glass obtained in the step S1 into a muffle furnace for annealing treatment so as to eliminate internal stress;
s3, placing the precursor glass subjected to the annealing treatment in the step S2 into a muffle furnaceIs subjected to heat treatment to obtain CsPbBr 3 Perovskite quantum dot glass.
Preferably, the high temperature melting temperature in the step S1 is 1050-1300 ℃, and the high temperature melting time is 10-60 min.
Preferably, the temperature of the annealing treatment in the step S2 is 250-400 ℃, and the time of the annealing treatment is 3-15 h.
Preferably, the temperature of the heat treatment in the step S3 is 450-580 ℃, and the time of the heat treatment is 7-20 h.
The high luminous quantum efficiency CsPbBr 3 The perovskite quantum dot glass is applied to the field of wide color gamut display, and comprises LED backlight source display, mini LED display, laser display and the like.
Compared with the prior art, the invention has the following advantages:
(1) Compared with the prior literature, the CsPbBr provided by the invention 3 The quantum efficiency of the perovskite quantum dot glass under 365nm ultraviolet light excitation reaches 86%, and the quantum efficiency under 455nm blue light excitation reaches 53%, which is higher than that reported in literature;
(2) The wavelength requirement of the wide color gamut display device for green light is 532nm, and the emission main peak of most perovskite quantum dot glasses is located around 515 nm. The traditional method adopts a mode of replacing Br by part I to realize the red shift of the emission spectrum, but brings about the steep decline of the luminous quantum efficiency. The CsPbBr provided by the invention 3 The perovskite quantum dot glass has a main emission peak at 526nm under the excitation of blue light, and can obtain emission with longer wavelength without I doping, so that the advantage is obvious.
(3) The CsPbBr provided by the invention 3 The perovskite quantum dot glass has higher thermal stability, and the luminous performance (comprising emission intensity, emission main peak, half-peak width and the like) has complete restorability in the range of room temperature to 140 ℃; in addition, good thermal stability enables it to withstand high temperature baking during device packaging.
(4) The CsPbBr provided by the invention 3 The perovskite quantum dot glass has higher water-oxygen stability and weather resistance, and light attenuation is smaller under blue light and ultraviolet light irradiation;
(5) The CsPbBr provided by the invention 3 The perovskite quantum dot glass is easy to prepare in large scale;
(6) The CsPbBr provided by the invention 3 The perovskite quantum dot glass can be used for various different types of wide color gamut display devices, such as LED backlight display, mini LED display, laser display and the like.
Drawings
FIG. 1 shows CsPbBr after heat treatment of the glass precursor and the glass precursor at different temperatures in example 1 3 XRD pattern of perovskite quantum dot glass sample.
FIG. 2 is CsPbBr in example 1 3 TEM image of perovskite quantum dot glass.
FIG. 3 is CsPbBr in example 2 3 Photo of perovskite quantum dot glass block and powder under sunlight and ultraviolet light.
FIG. 4 is CsPbBr in example 3 3 Emission spectrum diagram of perovskite quantum dot glass.
FIG. 5 is CsPbBr in example 4 3 Fluorescence lifetime decay curve of perovskite quantum dot glass.
FIG. 6 is CsPbBr in example 4 3 And (3) researching the cyclic thermal stability of perovskite quantum dot glass.
FIG. 7 is CsPbBr in example 4 3 Moisture resistance studies of perovskite quantum dot glasses.
FIG. 8 is CsPbBr in example 4 3 The perovskite quantum dot glass is applied to a wide color gamut display backlight device.
FIG. 9 is CsPbBr in example 4 3 And preparing a mini LED physical image by perovskite quantum dot glass.
FIG. 10 is CsPbBr in example 5 3 The internal quantum efficiency of the perovskite quantum dot fluorescent glass under 455nm excitation.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but embodiments of the present invention are not limited thereto.
Unless specifically stated otherwise, the reagents, methods and apparatus employed in the present invention are those conventional in the art. The reagents and materials used in the present invention are commercially available unless otherwise specified.
Example 1:
this example CsPbBr 3 The perovskite quantum dot glass comprises the following chemical compositions in mol percent: 35SiO 2 -16ZnO-34B 2 O 3 -2K 2 CO 3 -7SrCO 3 -1BaCO 3 -5Cs 2 CO 3 -10PbBr 2 -10NaBr
TABLE 1 CsPbBr in example 1 3 Raw material composition of perovskite quantum dot glass
| Raw materials | SiO 2 | ZnO | B 2 O 3 | SrCO 3 | K 2 CO 3 | BaCO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 3.0421 | 1.4951 | 3.2132 | 1.4318 | 0.3998 | 0.2854 | 1.3213 | 2.9767 | 0.8345 |
Analytically pure Silica (SiO) was precisely weighed according to Table 1 2 ) Zinc oxide (ZnO), boron oxide (B) 2 O 3 ) Strontium carbonate (SrCO) 3 ) Potassium carbonate (K) 2 CO 3 ) Barium carbonate (BaCO) 3 ) Cesium carbonate (Cs) 2 CO 3 ) Lead bromide (PbBr) 2 ) Sodium bromide (NaBr). The precisely weighed raw materials are placed in an agate mortar for full grinding, the materials are placed in a corundum crucible after being uniformly mixed, the materials are melted for 15min in a muffle furnace at 1150 ℃, then, the glass melt is taken out and rapidly poured into a preheated graphite mold for molding, the block precursor glass is obtained, and the obtained precursor glass is placed in the muffle furnace for annealing for 3h at 350 ℃ to eliminate internal stress, so that the block glass is obtained. Placing the bulk glass in a muffle furnace for heat treatment, performing heat treatment at 470-570 ℃ for 7h, and then cooling to room temperature to obtain CsPbBr 3 Perovskite quantum dot glass. FIG. 1 shows XRD patterns of a glass precursor and samples thereof after heat treatment at different temperatures, and it can be seen from the figure that the glass precursor exhibits hump characteristics of glass, and shows a remarkable diffraction peak with increasing heat treatment temperature, and is in contact with cubic phase CsPbBr 3 Is a standard card match of CsPbBr 3 The nanocrystalline quantum dots are successfully separated out in the glass system. FIG. 2 is a TEM image of a sample after heat treatment at 540℃for 10 hours, from which precipitation of quantum dots is clearly observed, with an average size particle diameter of 27.39nm.
Example 2:
example CsPbBr 3 The perovskite quantum dot glass comprises the following chemical compositions in mol percent: 34SiO 2 -16ZnO-36B 2 O 3 -2K 2 CO 3 -7SrCO 3 -1BaCO 3 -4CsBr-10PbO-10NaBr
TABLE 2 CsPbBr in example 2 3 Raw material composition of perovskite quantum dot glass
| Raw materials | SiO 2 | ZnO | B 2 O 3 | SrCO 3 | K 2 CO 3 | BaCO 3 | CsBr | PbO | NaBr |
| Quality (g) | 8.4112 | 5.1432 | 8.8836 | 3.9564 | 1.1056 | 0.7904 | 3.6492 | 8.2208 | 2.3048 |
Analytically pure Silica (SiO) was precisely weighed according to Table 2 2 ) Zinc oxide (ZnO), boron oxide (B) 2 O 3 ) Strontium bromide (SrCO) 3 ) Potassium carbonate (K) 2 CO 3 ) Barium carbonate (BaCO) 3 ) Cesium bromide (CsBr), lead oxide (PbO), sodium bromide (NaBr). And (3) fully grinding the precisely weighed raw materials in a ball mill, uniformly mixing, placing in a corundum crucible, melting in a muffle furnace at 1100 ℃ for 18min, taking out the glass melt, rapidly pouring the glass melt into a preheated graphite mold for molding to obtain bulk precursor glass, and placing the obtained precursor glass into the muffle furnace for annealing at 250 ℃ for 10h to eliminate internal stress to obtain bulk glass. Placing the bulk glass in a muffle furnace for heat treatment, performing heat treatment at 480 ℃ for 10 hours, and then cooling to room temperature to obtain CsPbBr 3 Perovskite quantum dot glass. FIG. 3 shows the CsPbBr produced 3 From the physical photograph of polished perovskite quantum dot glass, csPbBr can be seen from the figure 3 The perovskite quantum dot glass still keeps high transparency, and the body color is yellow green, and emits bright green light under an ultraviolet lamp.
Example 3:
this example CsPbBr 3 The perovskite quantum dot glass comprises the following chemical compositions in mol percent: 26SiO 2 -16ZnO-43B 2 O 3 -2K 2 CO 3 -7SrCO 3 -1BaCO 3 -2.5Cs 2 CO 3 -6PbBr 2 -6NaBr
TABLE 3 CsPbBr in example 3 3 Raw material composition of perovskite quantum dot glass
| Raw materials | SiO 2 | ZnO | B 2 O 3 | SrCO 3 | K 2 CO 3 | BaCO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.3414 | 2.9634 | 8.3258 | 2.838 | 0.7924 | 0.5659 | 2.619 | 5.9004 | 1.654 |
Analytically pure Silica (SiO) was precisely weighed according to Table 3 2 ) OxygenZinc oxide (ZnO) and boron oxide (B) 2 O 3 ) Strontium carbonate (SrCO) 3 ) Potassium carbonate (K) 2 CO 3 ) Barium carbonate (BaCO) 3 ) Cesium carbonate (Cs) 2 CO 3 ) Lead bromide (PbBr) 2 ) Sodium bromide (NaBr). The precisely weighed raw materials are placed in an agate mortar for full grinding, the materials are placed in a corundum crucible after being uniformly mixed, the materials are melted for 10min in a muffle furnace at 1250 ℃, then, the glass melt is taken out and rapidly poured into a preheated graphite mold for molding, the block precursor glass is obtained, and the obtained precursor glass is placed in the muffle furnace for annealing for 5h at 370 ℃ to eliminate internal stress, so that the block glass is obtained. Placing the bulk glass in a muffle furnace for heat treatment, performing heat treatment at 470-570 ℃ for 10h, and then cooling to room temperature to obtain CsPbBr 3 Perovskite quantum dot glass. In FIG. 4, csPbBr was prepared 3 As can be seen from the emission spectrum graph of the perovskite quantum dot glass, the main luminescence peak position of the quantum dot glass is about 526nm, and the average half-peak width is 23nm, which shows that the CsPbBr 3 The perovskite quantum dot glass is suitable for ultraviolet, near ultraviolet and blue light LED chips, and the luminous characteristics of the perovskite quantum dot glass are the same as those of the traditional colloid CsPbBr 3 The luminescence properties of the quantum dots are similar, indicating that CsPbBr 3 Perovskite quantum dots were successfully precipitated in the glass.
Example 4:
this example CsPbBr 3 The perovskite quantum dot glass comprises the following chemical compositions in mol percent: 26SiO 2 -16ZnO-43B 2 O 3 -2K 2 CO 3 -7SrCO 3 -1BaCO 3 -0.3Sb 2 O 3 -2.4Cs 2 CO 3 -6PbBr 2 -6KBr
TABLE 4 CsPbBr in example 4 3 Raw material composition of perovskite quantum dot glass
| Raw materials | SiO 2 | ZnO | B 2 O 3 | SrCO 3 | K 2 CO 3 | BaCO 3 | Sb 2 O 3 | Cs 2 CO 3 | PbBr 2 | KBr |
| Quality (g) | 9.9070 | 6.7625 | 19.0000 | 6.4765 | 1.8085 | 1.2910 | 0.5610 | 5.9765 | 13.4645 | 3.9705 |
Analytically pure Silica (SiO) was precisely weighed according to Table 4 2 ) Zinc oxide (ZnO), boron oxide (B) 2 O 3 ) Strontium carbonate (SrCO) 3 ) Potassium carbonate (K) 2 CO 3 ) Barium carbonate (BaCO) 3 ) Tellurium oxide (Sb) 2 O 3 ) Cesium carbonate (Cs) 2 CO 3 ) Lead bromide (PbBr) 2 ) Potassium bromide (KBr). And (3) fully grinding the precisely weighed raw materials in a ball mill, uniformly mixing, placing in a corundum crucible, melting for 30min in a muffle furnace at 1300 ℃, taking out a glass melt, rapidly pouring the glass melt into a preheated graphite mold for molding to obtain bulk precursor glass, and placing the obtained precursor glass into the muffle furnace for annealing at 400 ℃ for 8h to eliminate internal stress to obtain bulk glass. Placing the bulk glass in a muffle furnace for heat treatment, performing heat treatment at 510 ℃ for 5h,10h and 20h, and then cooling to room temperature to obtain CsPbBr 3 Perovskite quantum dot glass. FIG. 5 shows the preparation of CsPbBr 3 The fluorescence lifetime decay curve of the perovskite quantum dot glass fits its lifetime to about 20.3ns. Fig. 6 shows the study of the temperature-changing spectral properties of the prepared samples at room temperature to 140 ℃, and it can be seen from the graph that as the temperature increases, the luminous intensity decreases, the temperature returns to room temperature, and the luminous intensity can return to the initial value. This phenomenon can be maintained through multiple cycle testing, due to CsPbBr 3 The perovskite quantum dots are precipitated by heat treatment at 510 ℃ and are effectively protected by the glass matrix, so that decomposition and degradation do not occur. FIG. 8 shows the preparation of CsPbBr 3 Perovskite quantum dot fluorescent glass combination K 2 SiF 6 :Mn 4+ And calculating the electrochromic spectrogram of the wide color gamut display backlight source prepared by the red fluorescent powder and the blue LED chip, wherein the color gamut area of the device is larger than 100% NTSC.
Example 5:
this example CsPbBr 3 The perovskite quantum dot glass comprises the following chemical compositions in mol percent: 26SiO 2 -16ZnO-43B 2 O 3 -2K 2 CO 3 -7SrCO 3 -1BaCO 3 -2.5Cs 2 CO 3 -8PbO-6KBr。
TABLE 5 CsPbBr in example 5 3 Perovskite quantum dot glassComposition of raw materials
| Raw materials | SiO 2 | ZnO | B 2 O 3 | SrCO 3 | K 2 CO 3 | BaCO 3 | Cs 2 CO 3 | PbO | KBr |
| Quality (g) | 1.8142 | 1.2382 | 3.4787 | 1.1858 | 0.3311 | 0.2363 | 1.0943 | 4.9305 | 0.6911 |
Analytically pure Silica (SiO) was precisely weighed according to Table 5 2 ) Zinc oxide (ZnO), boron oxide (B) 2 O 3 ) Strontium carbonate (SrCO) 3 ) Potassium carbonate (K) 2 CO 3 ) Barium carbonate (BaCO) 3 ) Cesium carbonate (Cs) 2 CO 3 ) Lead oxide (PbO), potassium bromide (KBr). The precisely weighed raw materials are placed in an agate mortar for full grinding, the materials are placed in a corundum crucible after being uniformly mixed, the materials are melted for 45min in a muffle furnace at 1150 ℃, then, the glass melt is taken out and rapidly poured into a preheated graphite mould for molding, the block precursor glass is obtained, and the obtained precursor glass is placed in the muffle furnace for annealing at 270 ℃ for 12h to eliminate internal stress, so that the block glass is obtained. Placing the bulk glass in a muffle furnace for heat treatment, performing heat treatment at 510 ℃ for 10 hours, and then cooling to room temperature to obtain CsPbBr 3 Perovskite quantum dot glass. FIG. 10 shows the preparation of CsPbBr 3 As a result of quantum efficiency test of perovskite quantum dot glass under 455nm excitation, the internal quantum efficiency of the sample under blue light excitation is as high as 53.08%.
The above examples are preferred embodiments of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other changes, modifications, substitutions, combinations, and simplifications that do not depart from the spirit and principle of the present invention should be made in the equivalent manner, and the embodiments are included in the protection scope of the present invention.
Claims (6)
1. High-luminous quantum efficiency CsPbBr 3 Perovskite quantum dot glass, its characterized in that: the CsPbBr 3 The perovskite quantum dot glass consists of the following components in mole percent: 20-35% SiO 2 ，10～25% ZnO, 30～50% B 2 O 3 ，3～8% SrCO 3 ，1～5% K 2 CO 3 ，0.5～3% BaCO 3 ，0.1～2% Sb 2 O 3 ，1～5% Cs 2 CO 3 Or 2-10% CsBr, 1-10% PbBr 2 Or PbO, 1-10% NaBr or KBr; the sum of the mole percentages of the components is100%；
The CsPbBr 3 The main emission peak of the perovskite quantum dot glass is 526nm, the half-peak width is 23nm, the quantum efficiency is 86% under 365nm ultraviolet excitation, and the quantum efficiency is 53% under 455nm blue excitation;
the CsPbBr 3 The average size particle diameter of the quantum dots in the perovskite quantum dot glass is 25-30 nm;
the high luminous quantum efficiency CsPbBr 3 The preparation method of the perovskite quantum dot glass comprises the following operation steps:
s1, weighing raw materials according to the glass composition, fully and uniformly mixing the raw materials, and pouring the raw materials into a graphite mold after high-temperature melting to obtain precursor glass;
s2, transferring the precursor glass obtained in the step S1 into a muffle furnace for annealing treatment so as to eliminate internal stress;
s3, placing the precursor glass subjected to the annealing treatment in the step S2 into a muffle furnace for heat treatment to obtain CsPbBr 3 Perovskite quantum dot glass.
2. A high luminescence quantum efficiency CsPbBr according to claim 1 3 Perovskite quantum dot glass, its characterized in that: the CsPbBr 3 The perovskite quantum dot glass consists of the following components in mole percent: 22-28% SiO 2 ，15～20% ZnO，35～45% B 2 O 3 ，5～7% SrCO 3 ，2～3% K 2 CO 3 ，1～2% BaCO 3 ，0.2～1.5% Sb 2 O 3 ，1.5～4.5% Cs 2 CO 3 Or 4 to 6 percent of CsBr,3 to 7 percent of PbBr 2 Or PbO, 3-7% NaBr or KBr; the sum of the mole percentages of the components is 100 percent.
3. A high luminescence quantum efficiency CsPbBr according to claim 1 3 Perovskite quantum dot glass, its characterized in that: the high-temperature melting temperature in the step S1 is 1000-1300 ℃, and the high-temperature melting time is 5-60 min.
4. The method according to claim 1High-luminous quantum efficiency CsPbBr 3 Perovskite quantum dot glass, its characterized in that: the temperature of the annealing treatment in the step S2 is 200-450 ℃, and the time of the annealing treatment is 3-20 h.
5. A high luminescence quantum efficiency CsPbBr according to claim 1 3 Perovskite quantum dot glass, its characterized in that: the temperature of the heat treatment in the step S3 is 400-600 ℃, and the time of the heat treatment is 5-24 h.
6. A high luminescent quantum efficiency CsPbBr as defined in any one of claims 1 to 5 3 The application of perovskite quantum dot glass in the wide color gamut display field is characterized in that: the LED backlight display device comprises LED backlight display, mini LED display and laser display.
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