CN112062474A - Preparation method and application of near-infrared perovskite quantum dot glass - Google Patents
Preparation method and application of near-infrared perovskite quantum dot glass Download PDFInfo
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- C03C10/00—Devitrified glass ceramics, i.e. glass ceramics having a crystalline phase dispersed in a glassy phase and constituting at least 50% by weight of the total composition
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Abstract
The invention relates to a preparation method and application of near-infrared perovskite quantum dot glass, and belongs to the technical field of optical glass preparation. High purity B of the invention2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2NaI and Pr4O7The mixed powder is put into an air atmosphere at the temperature of 1150-1250 ℃ for high-temperature melting for 8-20 min, and then is poured, cooled and formed to obtain precursor glass, and the precursor glass is put into a furnace to be heated and melted for 8-20 minSequentially carrying out high-temperature stress relief treatment and high-temperature heat treatment on the glass to obtain the fully inorganic perovskite CsPbI3:Pr3+Quantum dot glass. The CsPbI of the invention3:Pr3+The quantum dot glass has excellent near-infrared emission characteristics under the excitation of red light, and can be used for lighting facilities such as plants and the like which require red light for near-infrared coupling.
Description
Technical Field
The invention relates to a preparation method and application of near-infrared perovskite quantum dot glass, and belongs to the technical field of optical glass preparation.
Background
Light plays a key role in the plant growth process, wherein the basic light requirements of red light (600-. The absorption spectrum of the red light and the dominant photosynthetic pigment chlorophyll and carotenoid is well matched, the red light/far-red light is mainly absorbed by photosensitive cell photosensitive pigment protein, and the germination, development and maturation processes of the plant are regulated through the photosensitive intensity, photosensitive quality, photosensitive direction and photosensitive period of the photosensitive cell to the surrounding environment. Biological activity state PRAnd active state PFRAre two types of photosensitive pigment proteins which mainly absorb 600-700nm red light (the peak value is 660nm) and 600-780nm red light/FR light (the center is about 730 nm) respectively. Under far-red light irradiation, PFRWill be converted into PRResult in PFR/PRTo a threshold level, thereby promoting flowering stimulation in short-day plants, and vice versa. In addition, photosynthetic bacteria are widely distributed in oil, water and plant tissues, promote plant growth by absorbing near infrared (NIR, 715-1050nm) light, promote synthesis of nutrients, and assist biological nitrogen fixation. Therefore, it is reasonable to promote the growth of crops by supplementing light and lighting in the photoperiod to achieve the purpose of improving the yield and quality of crops.
However, the design of the current LED plant lighting phosphor is not perfect. The current research is mainly focused on blue chips and ultraviolet chips excited blue and red phosphors, such as A3MgSi2O8：Pr3+，Mn2+And Sr reported by Wang's team2SiO4：Pr2+-Ba3MgSi2O8：Pr2+，Mn2+A dual-response type phosphor. Except for a small amount of doped Mn4+Ionic titanates, and Ce in phosphates3+And Pr3+Outside the reports of ion mixing, little attention has been paid to phosphors with R and FR emission for plant growth.
The LED plant lighting phosphor is mostly composed of uv or blue light chip excitation, which indicates that the coordination of multiple phosphors is required if the adjustment of red and near infrared light needs to be designed. The method not only brings the problem of chromatic aberration caused by different thermal quenching of different fluorescent powder, but also is difficult to avoid blue light in the spectrum. Therefore, a near-infrared substance excited by a red light chip is searched for regulating the P of the plant growth stageRAnd PFR。
Disclosure of Invention
Aiming at the problems of low light conversion efficiency and single and unadjustable spectrum of the existing red light excited near-infrared fluorescent material, the invention provides a preparation method and application of near-infrared perovskite quantum dot glass, and CsPbI3:Pr3+The quantum dot glass has strong red light conversion efficiency, excellent quantum efficiency and Pr3+The doping can effectively adjust the peak position of emitting near infrared light, and can utilize red to excite Pr of far-red light3+Doped CsPbI3Quantum dot glass is made into the LED lamp with high luminous efficiency and high stability for plant growth.
A preparation method of near-infrared perovskite quantum dot glass comprises the following specific steps:
(1) mixing high-purity B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2NaI and Pr2O3Grinding to obtain mixed powder;
(2) melting the mixed powder in the step (1) at 1150-1250 ℃ in an air atmosphere at high temperature for 8-20 min, pouring, cooling and forming to obtain precursor glass;
(3) sequentially carrying out high-temperature stress relief treatment and high-temperature heat treatment on the precursor glass in the step (2) to obtain the fully inorganic perovskite CsPbI3:Pr3+A quantum dot glass scintillator.
The step (1) B2O3、SiO2ZnO and SrCO3Is a glass matrix, Cs2CO3、PbI2NaI and Pr2O3As a microcrystalline material, with B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2The total molar amount of NaI is 100 percent, B in the mixed powder2O330～40％、SiO235～45％、ZnO 10～20％、SrCO 35～10％、Pr4O70.1～4.0％、Cs2CO38～12％、PbI23-5% and 6-9% of NaI.
The temperature of the high-temperature stress relief treatment in the step (3) is 400-450 ℃, and the stress relief time is 3-5 h.
The temperature of the high-temperature heat treatment in the step (3) is 480-590 ℃, and the heat treatment time is 10-28 h.
The near-infrared perovskite quantum dot glass is used for preparing an encapsulating material of an LED lamp for plant growth.
The basic principle that the red light excited near-infrared perovskite quantum dot can be excited by the red light is as follows: from CsPbI3The absorption spectrum of the quantum dot can be seen, CsPbI3The absorption range of the quantum dots is from ultraviolet to red, and in addition, the material can convert red light into near infrared light; due to the characteristics of the perovskite structure, the material has excellent light conversion performance and narrow spectrum at half height, and can ensure the color purity of an emission spectrum, so that the emission spectrum is easier to tune for plants; in addition, the near-infrared perovskite quantum dot glass has high luminous quantum yield, high absorption efficiency and high stability.
The invention has the beneficial effects that:
(1) the CsPbI of the invention3:Pr3+The quantum dot glass has excellent performance of exciting near infrared rays by red light, and meanwhile, Pr3+The doping of the LED can effectively coordinate the near-infrared emission spectrum, and is beneficial to manufacturing the LED lamp with high luminous efficiency for plant growth;
(2) the CsPbI of the invention3:Pr3+The quantum dot glass has the characteristics of ultrahigh stability, high visible light transmittance, simple preparation process, low cost and the like.
Drawings
FIG. 1 shows example 1 without doping Pr3+The differential thermal spectrum of the glass-ceramic of (a);
FIG. 2 shows different Pr3+XRD pattern of the doping concentration microcrystalline glass;
FIG. 3 shows Pr doping in example 23+TEM and EDS of the glass-ceramics illustrate the main composition and element distribution of the crystallites;
FIG. 4 shows different Pr3+Photoluminescence spectrum of the microcrystalline glass with doping concentration;
FIG. 5 shows CsPbI of example 23:Pr3+Quantum dot glass and no doped Pr3+The quantum efficiency of the glass ceramics;
FIG. 6 is a comparison of plant lighting with natural light for example 2.
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: a preparation method of a red light excited near-infrared perovskite quantum dot comprises the following specific steps:
(1) mixing high-purity B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2NaI and Pr2O3Grinding to obtain mixed powder; wherein B is2O3、SiO2ZnO and SrCO3Is a glass matrix, Cs2CO3、PbI2NaI as microcrystalline material and B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2The total molar amount of NaI is 100 percent, B in the mixed powder2O330％、SiO232％、ZnO 12％、SrCO 37％、Cs2CO311％、PbI 23% and NaI 5%;
(2) melting the mixed powder in the step (1) at 1150 ℃ and high temperature in an air atmosphere for 20min, pouring the melted mixed powder onto a copper plate preheated to 450 ℃, and cooling and forming to obtain precursor glass;
(3) sequentially carrying out high-temperature stress relief treatment and high-temperature heat treatment on the precursor glass in the step (2) to obtain the fully inorganic perovskite CsPbI3The high-temperature stress relief treatment temperature is 420 ℃, the stress relief time is 3h, the high-temperature heat treatment temperature is 500 ℃, and the heat treatment time is 22 h;
not doped with Pr3+The microcrystalline glass is not doped with Pr3+The differential thermogram of the glass-ceramic of (1) is shown in FIG. 1, which shows that the glass transition temperature (Tg) is about 465 ℃ and the crystallization temperature (Tc) is about 588 ℃; thus heating at a temperature of 590 ℃ can produce CsPbI3And (4) quantum dots.
Example 2: a preparation method of all-inorganic perovskite quantum dot glass comprises the following specific steps:
(1) mixing high-purity B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2NaI and Pr2O3Grinding to obtain mixed powder; wherein B is2O3、SiO2ZnO and SrCO3Is a glass matrix, Cs2CO3、PbI2NaI and Pr2O3As a microcrystalline material, with B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2The total molar amount of NaI is 100 percent, B in the mixed powder2O332％、SiO235％、ZnO 10％、SrCO 35％、Cs2CO39％、PbI 23% and 6% of NaI, Pr2O3(1.0％)；
(2) Melting the mixed powder in the step (1) at 1250 ℃ in air for 10min at high temperature, pouring the molten powder onto a copper plate preheated to 450 ℃, and cooling and forming to obtain precursor glass;
(3) sequentially carrying out high-temperature stress relief treatment and high-temperature heat treatment on the precursor glass in the step (2) to obtain the fully inorganic perovskite CsPbI3The high-temperature stress relief treatment temperature is 400 ℃, the stress relief time is 5h, the high-temperature heat treatment temperature is 590 ℃, and the heat treatment time is 10 h;
doped Pr3+TEM and EDS of glass-ceramics show that the main components and element distribution of the glass-ceramics are shown in FIG. 3, and Si, O, B, Na, Cs, Pb, I, Zn and Pr are detected from the EDS spectrum of FIG. 3, indicating that Pr is successfully grown in the glass matrix3+Doped CsPbI3Quantum dots, and in addition, the strong signal of Cu comes from the TEM grid; different Pr3+The photoluminescence spectrum of the glass ceramics with doping concentration is shown in fig. 4, and it is known from fig. 4 that the luminescence shows a trend of increasing first and then decreasing with the increase of doping concentration, and the luminescence is the best when the concentration is 1.0%; CsPbI in contrast to quantum efficiency3:Pr3+Quantum dot glass and no doped Pr3+The quantum efficiency of the glass ceramics is shown in FIG. 5, and from FIG. 5, CsPbI doped with 1.0% is shown3The quantum yield of the quantum dot glass is 49.11%, and the undoped quantum dot glass is only 14.28, which is nearly 3.4 times increased; the phenomenon of the material is shown in figure 6 in a plant irradiation experiment after being packaged, and compared with a plant irradiated by natural light, 1.0 percent of CsPbI is doped3The growth condition of the quantum dot glass is better, the growth vigor is uniform, and the length of the root is far longer than that of natural light irradiation.
Example 3: a preparation method of all-inorganic perovskite quantum dot glass comprises the following specific steps:
(1) mixing high-purity B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2NaI and Pr2O3Grinding to obtain mixed powder; wherein B is2O3、SiO2ZnO and SrCO3Is a glass matrix, Cs2CO3、PbI2NaI and Pr2O3As a microcrystalline material, with B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2The total molar amount of NaI is 100 percent, B in the mixed powder2O332％、SiO235％、ZnO 10％、SrCO 35％、Cs2CO39％、PbI 23% and 6% of NaI, Pr2O32.0％；
(2) Melting the mixed powder in the step (1) at 1200 ℃ in an air atmosphere for 15min at a high temperature, pouring the molten powder onto a copper plate preheated to 450 ℃, and cooling and forming to obtain precursor glass;
(3) sequentially carrying out high-temperature stress relief treatment and high-temperature heat treatment on the precursor glass in the step (2) to obtain the fully inorganic perovskite CsPbI3The high-temperature stress relief treatment temperature is 420 ℃, the stress relief time is 3h, the high-temperature heat treatment temperature is 550 ℃, and the heat treatment time is 22 h;
doping different Pr3+The XRD pattern of the concentration microcrystalline glass is shown in FIG. 2, due to CsPbI3The quantum dot size is small, and the diffraction peak is not obvious due to the coating of the glass, however, the (002) diffraction peak can be matched with a standard PDF card; in-situ precipitated spherical CsPbI3The average diameter of the quantum dots is about 7.0nm, and the quantum dots are uniformly distributed in the glass matrix; at the same time, the corresponding transmission electron microscope and fast Fourier transform images show that the lattice spacing is about 0.301nm, and the cubic CsPbI3The (002) planes are consistent; this is consistent with XRD observations.
While the present invention has been described in detail with reference to the specific embodiments thereof, it will be apparent to one skilled in the art that various changes and modifications can be made therein without departing from the spirit and scope thereof.
Claims (5)
1. A preparation method of near-infrared perovskite quantum dot glass is characterized by comprising the following specific steps:
(1) mixing high-purity B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2NaI and doped Pr4O7Grinding to obtain mixed powder;
(2) melting the mixed powder in the step (1) at 1150-1250 ℃ in an air atmosphere at high temperature for 8-20 min, pouring, cooling and forming to obtain precursor glass;
(3) sequentially carrying out high-temperature stress relief treatment and high-temperature heat treatment on the precursor glass in the step (2) to obtain the fully inorganic perovskite CsPbI3:Pr3+A quantum dot glass scintillator.
2. The method for preparing the near-infrared perovskite quantum dot glass according to claim 1, which is characterized in that: with B2O3、SiO2、ZnO、SrCO3、Cs2CO3、PbI2The total molar amount of NaI is 100 percent, B in the mixed powder2O330～40％、SiO235～45％、ZnO 10～20％、SrCO35～10％、Pr4O70.1～4.0％、Cs2CO38～12％、PbI23-5% and 6-9% of NaI.
3. The method for preparing the near-infrared perovskite quantum dot glass according to claim 1, which is characterized in that: the temperature of the high-temperature stress relief treatment in the step (3) is 400-450 ℃, and the stress relief time is 3-5 h.
4. The method for preparing the near-infrared perovskite quantum dot glass according to claim 1, which is characterized in that: the temperature of the high-temperature heat treatment in the step (3) is 480-590 ℃, and the heat treatment time is 10-28 h.
5. The near-infrared perovskite quantum dot glass prepared by the preparation method of any one of claims 1 to 4 is used for preparing an encapsulating material of an LED lamp for plant growth.
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| US20070010390A1 (en) * | 2005-07-05 | 2007-01-11 | Margaryan Alfred A | Bismuth containing fluorophosphate glass and method for making thereof |
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| CN101618945A (en) * | 2008-07-03 | 2010-01-06 | 中国科学院福建物质结构研究所 | Near-infrared quantum-cutting down-conversion luminescent transparent glass ceramic and preparation method and application thereof |
| CN102674688A (en) * | 2012-05-25 | 2012-09-19 | 中国科学院上海光学精密机械研究所 | Praseodymium-doped borophosphate base near-infrared ultra wide band luminescent glass and preparation method thereof |
| CN110642515A (en) * | 2019-09-29 | 2020-01-03 | 昆明理工大学 | Preparation method and application of all-inorganic perovskite quantum dot glass |
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| US20070010390A1 (en) * | 2005-07-05 | 2007-01-11 | Margaryan Alfred A | Bismuth containing fluorophosphate glass and method for making thereof |
| CN101618945A (en) * | 2008-07-03 | 2010-01-06 | 中国科学院福建物质结构研究所 | Near-infrared quantum-cutting down-conversion luminescent transparent glass ceramic and preparation method and application thereof |
| CN101318773A (en) * | 2008-07-04 | 2008-12-10 | 华东理工大学 | Pr3+doped high-density scintillation glass and preparation method thereof |
| CN102674688A (en) * | 2012-05-25 | 2012-09-19 | 中国科学院上海光学精密机械研究所 | Praseodymium-doped borophosphate base near-infrared ultra wide band luminescent glass and preparation method thereof |
| CN110642515A (en) * | 2019-09-29 | 2020-01-03 | 昆明理工大学 | Preparation method and application of all-inorganic perovskite quantum dot glass |
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