CN113233775B - Nano Ag enhanced CsPbBr 3 Quantum dot glass and preparation method thereof - Google Patents
Nano Ag enhanced CsPbBr 3 Quantum dot glass and preparation method thereof Download PDFInfo
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Abstract
Nano-Ag enhanced CsPbBr 3 Quantum dot glass and a preparation method thereof. The method is through Ag + ‑Na + Ag nanoparticles are formed by an ion exchange method and a heat treatment process, and CsPbBr is enhanced by plasma formed by Ag 3 Photoluminescence and scintillation luminescence intensity of quantum dot glass. The invention relates to nano Ag enhanced CsPbBr 3 The specific mol percentage of the quantum dot glass is as follows: 8 to 23mol% of P 2 O 5 2 to 11mol% of Na 2 O,0 to 10mol% of K 2 O, znO 7-16 mol%, al 5-12 mol% 2 O 3 35 to 65mol% of B 2 O 3 3 to 14mol% of Cs 2 O, 1-8 mol% of PbBr 2 1 to 10mol percent of NaBr. The glass has the characteristics of high photoluminescence intensity, high flicker luminous intensity and good stability.
Description
Technical Field
The invention relates to the technical field of fluorescent glass and novel scintillating glass for a white light emitting diode, in particular to nano Ag enhanced CsPbBr 3 Quantum dot glass and a preparation method thereof.
Background
Inorganic cesium lead halide CsPbX 3 (X = Cl, br, I) perovskite quantum dots have received great attention due to their excellent optical properties, such as broad wavelength tunability with controllable band gap, full width at half maximum of emission band, and high photoluminescence quantum efficiency, which indicates that they have great potential applications in the field of white Light Emitting Diodes (LEDs). Recently, lead cesium halide perovskites have become a new type of scintillating material for applications in ultrasensitive X-ray detectors and low dose radiography. When they are scaled down to the size range of quantum dots, excellent scintillation performance comparable to commercial single crystals (e.g., luAG: ce) has been achieved due to exciton confinement effects. Only the anion component is needed to be adjusted, and the attractive twinkling luminescence which cannot be imagined by the traditional scintillation crystal and can be adjusted in color can be obtained. Thus, csPbX 3 The perovskite quantum dot is expected to be applied to the fields of medical diagnosis, safety inspection, basic scientific research, dosimetry and the like. However,although perovskite quantum dots have excellent photoluminescence and scintillation properties, poor stability limits their practical applications. Research reports, inorganic CsPbX 3 Perovskite quantum dots can be precipitated in different oxide glass systems by melt quenching methods, such as borosilicate, germanoborate, phosphoborate, phosphosilicate, and tellurite borate glasses. Since the oxide glass matrix can effectively prevent the degradation of the metal halide quantum dots, the stability of these glass-embedded quantum dots is significantly improved and they still show good optical properties inside the glass. However, quantum dot glasses have a problem that the scintillation efficiency is generally low among the above glasses.
Furthermore, photoluminescence of some materials can be enhanced by local surface plasmon effect caused by added noble metal nanoparticles, and thus, we also try to improve luminescence and scintillation efficiency of perovskite nanoparticles therein by appropriately introducing plasmon nanostructures into glass ceramics containing the perovskite nanoparticles. Noble metal nanoparticles do not produce strong fluorescent emissions, but they can interact strongly with light of a particular wavelength. The collective oscillation of free electrons caused by the periodic variation of the external electromagnetic field greatly enhances the absorption and scattering of electromagnetic waves in a specific wavelength range by the nanoparticles, and also greatly enhances the nearby local electromagnetic field. In some cases, the near-field enhancement of Ag nanoparticle plasmon resonance can greatly increase the fluorescence emission intensity of the sample. The silver nanoparticles can be introduced into the glass matrix in different ways, and compared with other ways, the ion exchange method has the advantages of low cost, large-scale production, uniform particle distribution, doping amount improvement and the like, so that CsPbBr is added in the method 3 Quantum dot glass to Ag + -Na + Ion exchange and heat treatment to form Ag nanoparticles, thereby significantly enhancing photoluminescence and scintillation of the glass and having superior stability, especially scintillation, indicating that CsPbBr incorporated into Ag by the ion exchange method 3 The quantum dot glass has huge commercial application potential in the field of novel scintillating materials.
Disclosure of Invention
The invention aims to provide a nano Ag enhanced CsPbBr 3 The quantum dot glass has the characteristics of high photoluminescence intensity, high scintillation luminous intensity and good stability.
The technical scheme adopted by the invention is as follows:
Nano-Ag enhanced CsPbBr 3 The quantum dot glass ceramics comprise the following components in percentage by mole:
the nano Ag enhanced CsPbBr 3 The preparation method of the quantum dot glass comprises the following steps:
(1) the nano-Ag enhanced CsPbBr of claim 1 3 The composition and mole percentage of the quantum dot glass are selected, the mass of each corresponding glass composition is calculated, each raw material is accurately weighed, and the weight P is 2 O 5 From NaPO 3 、KPO 3 And Al (PO) 3 ) 3 Introduction of, na 2 O and K 2 O is respectively prepared from NaPO 3 And KPO 3 Introduction of B 2 O 3 From H 3 BO 3 Introduction of, cs 2 O is formed by Cs 2 CO 3 Introducing;
(2) grinding the weighed raw materials in a corundum mortar, and uniformly mixing to form a mixture;
(3) putting the mixture into a covered alumina crucible to be melted in a high-temperature furnace, taking out the crucible after the mixture is completely melted, and pouring clear molten glass on a preheated stainless steel mold to obtain transparent glass;
(4) rapidly transferring the glass to a muffle furnace with the temperature being 30-50 ℃ lower than Tg for annealing treatment, carrying out heat preservation for 4-8 hours, then cooling along with the furnace, taking out the glass, and then cutting and polishing to form polished glass;
(5) immersing the polished glass into AgNO with different molar concentrations 3 ：NaNO 3 Molten saltMedium, agNO 3 The concentration of the sodium hydroxide is 0.1-20 mol%, exchange is carried out for 1-48 h at the temperature of 360 ℃, and the sodium hydroxide is cleaned by absolute ethyl alcohol and deionized water;
(6) carrying out heat treatment on the cleaned glass again, wherein the heat treatment temperature is 400-490 ℃, the heat treatment time is 1-48 h, and naturally cooling to obtain the nano Ag reinforced CsPbBr 3 Quantum dot glass.
The invention has the technical effects that:
the nano Ag enhanced CsPbBr prepared by the invention 3 Quantum dot glass, and the existence of CsPbBr in the glass is confirmed by X-ray diffraction test analysis, raman test and TEM image 3 Quantum dots and Ag nanoparticles. The silver nano-particles not only have absorption peaks at 420-470 nm, but also lead CsPbBr to pass through the local plasma effect 3 The quantum dots enhanced 3-fold and 7-fold in photoluminescence center near 520nm and scintillation near 540nm, respectively.
In addition, the fluorescence lifetime of the glass samples of the invention after ion exchange was reduced to 132cm compared to the glass without ion exchange -1 The intensity of the Raman vibration peak is improved by about 8 times.
The invention relates to nano Ag reinforced CsPbBr 3 The quantum dot glass has high light yield, short attenuation life and high stability, and the nano Ag enhanced CsPbBr is added 3 The quantum dot glass is used for preparing white light emitting diodes, illumination and other fields and becomes a possibility of a new generation of scintillation materials.
Drawings
FIG. 1 shows a nano Ag-enhanced CsPbBr of the present invention 3 Photoluminescence spectra of quantum dot glass example 1# and example 4# are compared.
FIG. 2 shows the CsPbBr enhanced by nano Ag in the invention 3 Comparative scintillation luminescence spectra of quantum dot glass example 1# and example 4 #.
Detailed Description
The present invention will be further described with reference to the following examples and drawings, but the scope of the present invention should not be limited thereto.
The invention relates to nano Ag enhanced CsPbBr 3 QuantumThe 16 embodied glass compositions of the dot glass are shown in the following table:
the invention concretely implements 16 nano Ag enhanced CsPbBr 3 Quantum dot glass compositions, wherein the glass samples prepared from component 9 were subjected to Ag + -Na + Ion exchange and heat treatment, specific 15 embodiments are shown below:
example 1#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment manufacturing processes 3 The concentration, ion exchange time, heat treatment temperature and time of (b) are shown in Table 2,
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 0mol％ | 0h | 430℃ | 3h |
The preparation process comprises the following steps:
firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the glass sample was heat-treated at 430 ℃ for 3 hours and naturally cooled to obtain Ag-free CsPbBr 3 The quantum dot glass has a transparent sample and a yellowish green color. The photoluminescence spectrum of a sample measured by an FLS920 instrument of Edinburgh company in England is shown as a solid line in figure 1, and the scintillation spectrum of the sample measured by an X-ray source with the tube voltage of 100KV and the tube current of 1mA is shown as a solid line in figure 2 by matching with an SBP-300 spectrum instrument of Touhahan light.
Example 2#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment manufacturing processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in Table 2,
table 1:
table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 0.25mol％ | 4h | 430℃ | 3h |
The preparation process comprises the following steps: firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving the heat for 4 hours, then cooling the glass to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 Molar concentration ratio of 0.25:99.75 in molten salt, exchanging for 4 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at a temperature of 430 ℃ for 3 hours and naturally cooled.
Example 3#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in Table 2,
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the design | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 0.5mol％ | 4h | 430℃ | 3h |
The preparation method comprises the following specific steps:
firstly, according to the table 1, the weighed raw materials are put into a corundum mortar to be uniformly mixed to obtainMixing; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving the heat for 4 hours, then cooling the glass to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 Molar concentration ratio of 0.5:99.5 in molten salt, exchanging for 4 hours at the temperature of 360 ℃, and cleaning with absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at a temperature of 430 ℃ for 3 hours and naturally cooled.
Example 4#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 4h | 430℃ | 3h |
Firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, exchanging for 4 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; carrying out heat treatment on the cleaned glass sample at the temperature of 430 ℃ for 3 hours and naturally cooling to obtain the Ag-containing CsPbBr 3 The quantum dot glass has the advantages of relatively transparent sample and green color. The photoluminescence spectrum of a sample measured by an FLS920 instrument of Edinburgh company in England is shown as a dotted line in figure 1, and the scintillation spectrum of the sample measured by an X-ray source with the tube voltage of 100KV and the tube current of 1mA is shown as a dotted line in figure 2 by matching with an SBP-300 spectrum instrument of Zoehan light.
Ke Zhang et al reported that Ag was added to the starting material 2 O, preparing CsPbBr containing Ag nano particles by adopting a melt quenching method and a heat treatment process 3 Quantum dot glass, and undoped Ag 2 Glass samples doped with O0.1mol% of Ag 2 The sample of O enhanced photoluminescence by 2.37 times by a plasma formed by Ag nanometers, located near 520 nm. YInsheng Xu et al reported the preparation of CsPbBr by melt quenching and heat treatment 3 Quantum dot glass with scintillation intensity of commercial scintillation material Bi 4 Ge 3 O 12 (BGO). The existing known literature has no CsPbBr enhanced by nano Ag 3 Report of scintillation luminescence of quantum dot glass, compared with Ag-free CsPbBr in example 1# 3 Quantum dot glass, csPbBr containing Ag nanoparticles in this embodiment 3 The photoluminescence intensity and the scintillation intensity of the quantum dot glass are respectively enhanced by about 3 times and 7 times, and particularly, the scintillation intensity is about 70 percent of BGO.
Example 5#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the design | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.5mol％ | 4h | 430℃ | 3h |
Firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1.5: exchanging in 98.5 fused salt for 4 hours at 360 ℃, and cleaning with absolute ethyl alcohol and deionized water; the cleaned glass sample was heat treated at a temperature of 430 ℃ for 3 hours and naturally cooled.
Example 6#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the design | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Heat treatment ofTime management |
| Numerical value | 3.0mol％ | 4h | 430℃ | 3h |
Firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving the heat for 4 hours, then cooling the glass to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 3:97, exchanging for 4 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at a temperature of 430 ℃ for 3 hours and naturally cooled.
Example 7#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 2h | 430℃ | 3h |
Firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, exchanging for 2 hours at the temperature of 360 ℃, and cleaning with absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at a temperature of 430 ℃ for 3 hours and naturally cooled.
Example 8#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (A) are shown in Table 2The preparation process comprises the following steps:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 6h | 430℃ | 3h |
Firstly, according to table 1, putting weighed raw materials into a corundum mortar, and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, 6 small exchanges at 360 DEG CIn the process, absolute ethyl alcohol and deionized water are used for cleaning; the cleaned glass sample was heat-treated at a temperature of 430 ℃ for 3 hours and naturally cooled.
Example 9#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 10h | 430℃ | 3h |
Firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting the mixture in a silicon carbide rod electric furnace at 1000 ℃, and melting the glass after 13 minutesLiquid is poured on a stainless steel die preheated to 350 ℃; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, exchanging for 10 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at a temperature of 430 ℃ for 3 hours and naturally cooled.
Example 10#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment manufacturing processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 4h | 400℃ | 3h |
Firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, exchanging for 4 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at a temperature of 400 ℃ for 3 hours and naturally cooled.
Example 11#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 4h | 460℃ | 3h |
Firstly, according to table 1, putting weighed raw materials into a corundum mortar, and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, exchanging for 4 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at 460 ℃ for 3 hours and naturally cooled.
Example 12#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Mass (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 4h | 490℃ | 3h |
Firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving the heat for 4 hours, then cooling the glass to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, exchanging for 4 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; the cleaned glass sample was heat treated at 490 c for 3 hours and allowed to cool naturally.
Example 13#:
9 th glass raw material groupAs shown in Table 1, in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 4h | 430℃ | 1h |
Firstly, according to table 1, putting the weighed raw materials into a corundum mortar and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing, and processing into rulerA glass block of 10X 2mm in size. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, exchanging for 4 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at a temperature of 430 ℃ for 1 hour and naturally cooled.
Example 14#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment manufacturing processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the design | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 4h | 430℃ | 5h |
Firstly, the methodPutting the weighed raw materials into a corundum mortar and uniformly mixing according to the table 1 to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, exchanging for 4 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at a temperature of 430 ℃ for 5 hours and naturally cooled.
Example 15#:
the composition of the 9 th glass raw material is shown in Table 1 in Ag + -Na + AgNO in ion exchange and heat treatment processes 3 The concentration, ion exchange time, heat treatment temperature and time of (a) are shown in table 2, and the specific preparation process is as follows:
table 1:
| components | NaPO 3 | KPO 3 | ZnO | Al 2 O 3 | Al(PO 3 ) 3 | H 3 BO 3 | Cs 2 CO 3 | PbBr 2 | NaBr |
| Quality (g) | 4.5 | 5.22 | 3.6 | 3.76 | 3.88 | 21.84 | 10.08 | 4.86 | 2.28 |
Table 2:
| factors of the fact | AgNO 3 Concentration of (2) | Ion exchange time | Temperature of heat treatment | Time of heat treatment |
| Numerical value | 1.0mol％ | 4h | 430℃ | 7h |
Firstly, according to table 1, putting weighed raw materials into a corundum mortar, and uniformly mixing to obtain a mixture; putting the mixture into a covered alumina crucible, melting in a silicon carbide rod electric furnace at 1000 ℃, and pouring molten glass on a stainless steel mold preheated to 350 ℃ after 13 minutes; rapidly transferring the glass to an annealing furnace which is heated to 350 ℃ for annealing, preserving heat for 4 hours, cooling to room temperature along with the furnace, and taking out a glass sample after complete cooling to obtain colorless and transparent glass; cutting, polishing and processing into glass blocks with the size of 10 multiplied by 2 mm. Subsequently, the processed glass samples were immersed in AgNO according to table 2 3 And NaNO 3 The molar concentration ratio is 1:99 in molten salt, exchanging for 4 hours at the temperature of 360 ℃, and cleaning by using absolute ethyl alcohol and deionized water; the cleaned glass sample was heat-treated at a temperature of 430 ℃ for 7 hours and naturally cooled.
Claims (1)
1. Nano-Ag enhanced CsPbBr 3 The quantum dot glass is characterized in that the composition mole percentage of the glass is as follows:
the nano Ag enhanced CsPbBr 3 The preparation method of the quantum dot glass comprises the following steps:
(1) the CsPbBr 3 Selecting the mol percent of the components and the mol percent of the quantum dot glass, calculating the mass of each corresponding glass component, accurately weighing each raw material, and obtaining the P 2 O 5 From NaPO 3 、KPO 3 And Al (PO) 3 ) 3 Introduction of Na 2 O and K 2 O is respectively made of NaPO 3 And KPO 3 Introduction of B 2 O 3 From H 3 BO 3 Introduction of, cs 2 O is formed by Cs 2 CO 3 Introducing;
(2) grinding the weighed raw materials in a corundum mortar, and uniformly mixing to form a mixture;
(3) putting the mixture into a covered alumina crucible, melting in a high-temperature furnace, taking out the crucible after complete melting, and pouring clear molten glass on a preheated stainless steel mold to obtain transparent glass;
(5) immersing the polished glass into AgNO with different molar concentrations 3 ：NaNO 3 In a molten salt, said AgNO 3 The concentration of the resin is 0.1 to 20mol%, the resin is exchanged for 1 to 48 hours at the temperature of 360 ℃, and the resin is washed by absolute ethyl alcohol and deionized water;
(6) and (3) carrying out heat treatment on the cleaned glass at the temperature of 400-490 ℃ for 1-48h, and naturally cooling to obtain the nano Ag reinforced CsPbBr 3 Quantum dot glass.
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