CN109437562B - 2-micron ultra-wideband tunable rare earth-doped laser glass capable of emitting light to separate out quantum dots and preparation method thereof - Google Patents
2-micron ultra-wideband tunable rare earth-doped laser glass capable of emitting light to separate out quantum dots and preparation method thereof Download PDFInfo
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- CN109437562B CN109437562B CN201811368104.2A CN201811368104A CN109437562B CN 109437562 B CN109437562 B CN 109437562B CN 201811368104 A CN201811368104 A CN 201811368104A CN 109437562 B CN109437562 B CN 109437562B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
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- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B25/00—Annealing glass products
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/076—Glass compositions containing silica with 40% to 90% silica, by weight
- C03C3/102—Glass compositions containing silica with 40% to 90% silica, by weight containing lead
- C03C3/105—Glass compositions containing silica with 40% to 90% silica, by weight containing lead containing aluminium
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Abstract
The invention discloses rare earth-doped laser glass with 2 mu m ultra-wide band and tunable luminescence precipitated quantum dots and a preparation method thereof. The glass comprises the following components in percentage by mole: SiO 22 45‑60%；NaCO3 30‑40%；Al2O3 3‑7%；ZnO 5‑10%；ZnS 1‑4%；PbO 0.5‑2%；Tm2O30.05-4 percent. The invention is prepared by a melting cooling method, and quantum dots are precipitated after heat treatment. The quantum dots in the glass prepared by the invention are PbS, and the size is 1.7-5.1 nm. Tm can be obtained simultaneously under the pump of 808nm laser diode3+And PbS is positioned in the ultra-wide band fluorescence of 2 mu m wave band, the emission wavelength range is 1400-2600 nm, the tuning range is up to 1200 nm, and the method is suitable for the preparation and the application of 2 mu m broadband tunable laser glass optical fiber and optical fiber laser.
Description
Technical Field
The invention belongs to the field of optical materials, and particularly relates to 2-micrometer ultra-wideband tunable luminescent rare earth-doped laser glass for separating out quantum dots and a preparation method thereof.
Background
The 2-micron optical fiber laser has wide application prospect and great commercial value in remote sensing, minimally invasive surgery, military and national defense and the like. The laser glass is used as a core gain medium of the optical fiber laser and fundamentally determines the performance of the optical fiber laser. At present, the rare earth ions for realizing 2 mu m luminescence mainly have Tm3+Ion sum Ho3+Ion wherein Tm is3+The ions have an absorption peak at 808nm, so that a common 808nm semiconductor laser can be adopted for pumping. Applicants have found that to achieve Tm 3+2 μm ofBroadband tunable luminescence, usually by simultaneous introduction of Ho3+The ion method can realize the light emission of 1400-2200 nm, but the light emission range is still relatively limited. Compared with rare earth ions, quantum dots with a narrow band gap, such as PbS and the like, can realize 2-micron luminescence through a proper heat treatment process, so that the combination of the rare earth ions and the quantum dots in laser glass is expected to realize wider 2-micron adjustable luminescence, and the quantum dots can be used as matrix glass of a 2-micron tunable optical fiber laser.
Disclosure of Invention
The invention aims to provide rare earth-doped laser glass with 2 mu m ultra-wide band tunable luminescence precipitated quantum dots and a preparation method thereof, wherein the quantum dots are introduced into the rare earth-doped laser glass, so that the luminescence range of 2 mu m wave bands can be greatly widened, the luminescence wave bands and the tuning range of the laser glass are enlarged, and the rare earth-doped laser glass can be used for 2 mu m broadband tunable laser glass optical fibers and optical fiber lasers.
The purpose of the invention is realized by the following technical scheme.
A2 μm ultra-wideband tunable rare earth-doped laser glass capable of emitting light to separate out quantum dots comprises the following components in percentage by weight: SiO 22：45-60%，NaCO3：30-40%，Al2O3：3-7%，ZnO：5-10%，ZnS：1-4%，PbO：0.5-2%，Tm2O3: 0.05-4 percent. The sum of the above mole percentages is 100%.
The preparation method of the rare earth-doped laser glass for separating out the quantum dots comprises the following steps:
(1) accurately weighing raw materials (wherein Na) according to composition and proportion2O is NaCO3Introduced in the form of (1);
(2) mixing the raw materials obtained in the step (1) in an agate mortar to form a batch;
(3) transferring the batch in the step (2) into a corundum crucible (with an alumina crucible cover), placing the corundum crucible in a high-temperature smelting furnace for heating and heat preservation, and obtaining transparent and uniform glass liquid without bubbles and stones after melting, clarification and homogenization;
(4) pouring the clarified molten glass on a preheated stainless steel iron plate for molding to obtain a transparent glass block;
(5) and (3) rapidly transferring the formed transparent glass to a muffle furnace for annealing, preserving heat to remove the internal stress of the glass, and then cooling to room temperature along with the furnace to obtain the rare earth-doped laser glass without quantum dot precipitation, namely the matrix glass.
(6) And (3) preserving the heat of the transparent glass cooled to room temperature at different heat treatment temperatures, and then cooling to room temperature to obtain the rare earth-doped laser glass for separating out the quantum dots.
Preferably, the temperature in the step (3) is raised from room temperature to 1400-1500 ℃, and the temperature is kept for 30-60 minutes.
Preferably, the annealing temperature in the step (5) is 350-400 ℃.
Preferably, the heat preservation time in the step (5) is 2-4 hours.
Preferably, the cooling rate in the step (5) is 10-20 ℃/min.
Preferably, the temperature of the cooling heat treatment in the step (6) is 490-530 ℃.
Preferably, the cooling in the step (6) has a heat preservation time of 5-30 hours.
Compared with the prior art, the invention has the following technical effects:
the rare earth-doped laser glass for separating out the quantum dots has high transparency and excellent thermal stability, the quantum dots are PbS, and the size is 1.7-5.1 nm. Tm can be obtained simultaneously in the glass after heat treatment under the pump of a 808nm Laser Diode (LD)3+And PbS is positioned in the ultra-wideband fluorescence of 2 mu m wave band, the emission wavelength range is 1400-2600 nm, the tuning range is up to 1200 nm, and the method is very suitable for the preparation and the application of 2 mu m broadband tunable laser glass optical fiber and optical fiber laser.
Drawings
FIG. 1 is a comparison of the luminescence spectra of the mother glass obtained by the present invention and the rare earth-doped laser glass from which quantum dots are precipitated in example 1, wherein each curve represents the mother glass and the samples heat-treated at 490 deg.C, 500 deg.C, 510 deg.C, 520 deg.C and 530 deg.C for 10 hours;
FIG. 2 is a comparison of the absorption spectra of the resulting mother glass of the present invention and rare earth-doped laser glass from which quantum dots were precipitated in example 1, with the inset being the transmission curve;
FIG. 3 is a transmission electron micrograph and a size distribution of the rare earth-doped laser glass from which quantum dots are precipitated in example 1;
FIG. 4 is a graph of the fluorescence decay of the parent glass and the sample of example 1 heat treated at 530 ℃ for 10 hours with an excitation wavelength of 808nm and a monitored emission wavelength of 1810 nm.
Detailed Description
The embodiments of the present invention will be further described below with reference to specific examples and drawings, but the embodiments of the present invention are not limited thereto.
Table 1 shows the heat treatment process parameters of 10 embodiments of the present invention, and the glass composition and the ratio are as follows: SiO 22：49.8%，Na2O：34%，Al2O3：5%，ZnO：8%，ZnS：2%，PbO：1%，Tm2O3：0.2%。
TABLE 1
| Glass component (mol%) | SiO2 | Na2O | Al2O3 | ZnO | ZnS | PbO | Tm2O3 |
| Example 1 | 49.8 | 34 | 5 | 8 | 2 | 1 | 0.2 |
| Example 2 | 45 | 35 | 6 | 6 | 3 | 0.8 | 0.1 |
| Example 3 | 60 | 35 | 3 | 7 | 4 | 2 | 1 |
| Example 4 | 55 | 30 | 7 | 5 | 1 | 0.5 | 1.5 |
| Example 5 | 45 | 40 | 3 | 5 | 3.5 | 1.5 | 2 |
| Example 6 | 50 | 30 | 4 | 10 | 3 | 1 | 2 |
| Example 7 | 52 | 32 | 4 | 5 | 2 | 1 | 4 |
The preparation steps of the rare earth-doped laser glass for precipitating the quantum dots in the embodiment 1 are as follows:
(1) accurately weighing raw materials (Na) according to composition and proportion2O is NaCO3In the form of) 50g of SiO2：18.13g，NaCO3：21.83g，Al2O3：3.09g，ZnO：3.95g，ZnS：1.18g，PbO：1.35g，Tm2O3：0.47g。
(2) Mixing the raw materials obtained in the step (1) in an agate mortar to form a batch;
(3) transferring the batch in the step (2) into a corundum crucible (with an alumina crucible cover), and placing the corundum crucible into a high-temperature melting furnace to melt for 30 minutes at 1400 ℃ to obtain a transparent and uniform glass liquid without bubbles and stones;
(4) pouring the clarified molten glass on a stainless steel iron plate for molding to obtain a transparent glass block;
(5) and (3) rapidly transferring the formed transparent glass to a muffle furnace at the temperature of 350 ℃ for annealing, preserving the heat for 2 hours to remove the internal stress of the glass, and then cooling the glass to room temperature along with the furnace at the cooling rate of 10 ℃/minute to obtain the rare earth-doped laser glass without quantum dot precipitation.
(6) And (3) preserving the heat of the transparent glass cooled to room temperature at 490 ℃, 500 ℃, 510 ℃, 520 ℃ and 530 ℃ for 10 hours, and then cooling to room temperature to obtain the rare earth-doped laser glass for separating out the quantum dots.
The preparation steps of the rare earth-doped laser glass for precipitating the quantum dots in the embodiment 2 are as follows:
(1) accurately weighing raw materials (Na) according to composition and proportion2O is NaCO3In the form of) 50g of SiO2：16.85g，NaCO3：23.12g，Al2O3：3.81g，ZnO：3.04g，ZnS：1.82g，PbO：1.11g，Tm2O3：0.24g。
(2) Mixing the raw materials obtained in the step (1) in an agate mortar to form a batch;
(3) transferring the batch in the step (2) into a corundum crucible (with an alumina crucible cover), and placing the corundum crucible into a high-temperature melting furnace to melt for 30 minutes at 1400 ℃ to obtain a transparent and uniform glass liquid without bubbles and stones;
(4) pouring the clarified molten glass on a stainless steel iron plate for molding to obtain a transparent glass block;
(5) and (3) rapidly transferring the formed transparent glass to a muffle furnace at the temperature of 350 ℃ for annealing, preserving the heat for 2 hours to remove the internal stress of the glass, and then cooling the glass to room temperature along with the furnace at the cooling rate of 10 ℃/minute to obtain the rare earth-doped laser glass without quantum dot precipitation.
(6) And (3) preserving the heat of the transparent glass cooled to room temperature at 490 ℃, 500 ℃, 510 ℃, 520 ℃ and 530 ℃ for 5 hours, and then cooling to room temperature to obtain the rare earth-doped laser glass for separating out the quantum dots.
The preparation steps of the rare earth-doped laser glass for precipitating the quantum dots in the embodiment 3 are as follows:
(1) accurately weighing raw materials (Na) according to composition and proportion2O is NaCO3In the form of) 50g of SiO2：19.15g，NaCO3：19.71g，Al2O3：1.62g，ZnO：3.03g，ZnS：2.07g，PbO：2.37g，Tm2O3：2.05g。
(2) Mixing the raw materials obtained in the step (1) in an agate mortar to form a batch;
(3) transferring the batch in the step (2) into a corundum crucible (with an alumina crucible cover), and placing the corundum crucible into a high-temperature melting furnace to melt at 1500 ℃ for 60 minutes to obtain bubble-free, stone-free, transparent and uniform glass liquid;
(4) pouring the clarified molten glass on a stainless steel iron plate for molding to obtain a transparent glass block;
(5) and (3) quickly transferring the formed transparent glass to a muffle furnace at the temperature of 400 ℃ for annealing, preserving the heat for 3 hours to remove the internal stress of the glass, and then cooling the glass to room temperature along with the furnace at the cooling rate of 20 ℃/minute to obtain the rare earth-doped laser glass without quantum dot precipitation.
(6) And (3) preserving the heat of the transparent glass cooled to room temperature at 490 ℃, 500 ℃, 510 ℃, 520 ℃ and 530 ℃ for 15 hours, and then cooling to room temperature to obtain the rare earth-doped laser glass for separating out the quantum dots.
The preparation steps of the rare earth-doped laser glass for precipitating the quantum dots in the embodiment 4 are as follows:
(1) accurately weighing raw materials (Na) according to composition and proportion2O is NaCO3In the form of) 50g of SiO2：19.69g，NaCO3：18.94g，Al2O3：4.25g，ZnO：2.42g，ZnS：0.58g，PbO：0.66g，Tm2O3：3.45g。
(2) Mixing the raw materials obtained in the step (1) in an agate mortar to form a batch;
(3) transferring the batch in the step (2) into a corundum crucible (with an alumina crucible cover), and placing the corundum crucible into a high-temperature melting furnace to melt for 40 minutes at 1450 ℃ to obtain bubble-free, stone-free, transparent and uniform glass liquid;
(4) pouring the clarified molten glass on a stainless steel iron plate for molding to obtain a transparent glass block;
(5) and (3) quickly transferring the formed transparent glass to a muffle furnace at the temperature of 380 ℃ for annealing, preserving the heat for 2 hours to remove the internal stress of the glass, and then cooling the glass to room temperature along with the furnace at the cooling rate of 15 ℃/minute to obtain the rare earth-doped laser glass without quantum dot precipitation.
(6) And (3) preserving the heat of the transparent glass cooled to room temperature at 490 ℃, 500 ℃, 510 ℃, 520 ℃ and 530 ℃ for 20 hours, and then cooling to room temperature to obtain the rare earth-doped laser glass for separating out the quantum dots.
The preparation steps of the rare earth-doped laser glass for precipitating the quantum dots in the embodiment 5 are as follows:
(1) accurately weighing raw materials (Na) according to composition and proportion2O is NaCO3In the form of) 50g of SiO2：19.15g，NaCO3：19.71g，Al2O3：1.62g，ZnO：3.03g，ZnS：2.07g，PbO：2.37g，Tm2O3：2.05g。
(2) Mixing the raw materials obtained in the step (1) in an agate mortar to form a batch;
(3) transferring the batch in the step (2) into a corundum crucible (with an alumina crucible cover), and placing the corundum crucible into a high-temperature melting furnace to melt at 1450 ℃ for 35 minutes to obtain bubble-free, stone-free, transparent and uniform glass liquid;
(4) pouring the clarified molten glass on a stainless steel iron plate for molding to obtain a transparent glass block;
(5) and (3) quickly transferring the formed transparent glass to a muffle furnace at the temperature of 350 ℃ for annealing, preserving the heat for 3 hours to remove the internal stress of the glass, and then cooling the glass to room temperature along with the furnace at the cooling rate of 20 ℃/minute to obtain the rare earth-doped laser glass without quantum dot precipitation.
(6) And (3) preserving the heat of the transparent glass cooled to room temperature at 490 ℃, 500 ℃, 510 ℃, 520 ℃ and 530 ℃ for 25 hours, and then cooling to room temperature to obtain the rare earth-doped laser glass for separating out the quantum dots.
The preparation steps of the rare earth-doped laser glass for precipitating the quantum dots in the embodiment 6 are as follows:
(1) accurately weighing raw materials (Na) according to composition and proportion2O is NaCO3In the form of) 50g of SiO2：17.28g，NaCO3：18.29g，Al2O3：2.35g，ZnO：4.68g，ZnS：1.68g，PbO：1.28g，Tm2O3：4.44g。
(2) Mixing the raw materials obtained in the step (1) in an agate mortar to form a batch;
(3) transferring the batch in the step (2) into a corundum crucible (with an alumina crucible cover), and placing the corundum crucible into a high-temperature melting furnace to melt at 1500 ℃ for 60 minutes to obtain bubble-free, stone-free, transparent and uniform glass liquid;
(4) pouring the clarified molten glass on a stainless steel iron plate for molding to obtain a transparent glass block;
(5) and (3) quickly transferring the formed transparent glass to a muffle furnace at the temperature of 400 ℃ for annealing, preserving the heat for 4 hours to remove the internal stress of the glass, and then cooling the glass to room temperature along with the furnace at the cooling rate of 20 ℃/minute to obtain the rare earth-doped laser glass without quantum dot precipitation.
(6) And (3) preserving the heat of the transparent glass cooled to room temperature at 490 ℃, 500 ℃, 510 ℃, 520 ℃ and 530 ℃ for 30 hours, and then cooling to room temperature to obtain the rare earth-doped laser glass for separating out the quantum dots.
The preparation steps of the rare earth-doped laser glass for precipitating the quantum dots in the embodiment 7 are as follows:
(1) accurately weighing raw materials (Na) according to composition and proportion2O is NaCO3In the form of) 50g of SiO2：16.81g，NaCO3：18.25g，Al2O3：2.19g，ZnO：2.19g，ZnS：1.05g，PbO：1.20g，Tm2O3：8.30g。
(2) Mixing the raw materials obtained in the step (1) in an agate mortar to form a batch;
(3) transferring the batch in the step (2) into a corundum crucible (with an alumina crucible cover), and placing the corundum crucible into a high-temperature melting furnace to melt at 1500 ℃ for 60 minutes to obtain bubble-free, stone-free, transparent and uniform glass liquid;
(4) pouring the clarified molten glass on a stainless steel iron plate for molding to obtain a transparent glass block;
(5) and (3) quickly transferring the formed transparent glass to a muffle furnace at the temperature of 400 ℃ for annealing, preserving the heat for 4 hours to remove the internal stress of the glass, and then cooling the glass to room temperature along with the furnace at the cooling rate of 20 ℃/minute to obtain the rare earth-doped laser glass without quantum dot precipitation.
(6) And (3) preserving the heat of the transparent glass cooled to room temperature at 490 ℃, 500 ℃, 510 ℃, 520 ℃ and 530 ℃ for 30 hours, and then cooling to room temperature to obtain the rare earth-doped laser glass for separating out the quantum dots.
FIG. 1 is an emission spectrum of example 1, showing 2 μm luminescence under excitation of a 808nm laser diode from a mother glass and a sample heat-treated at 490 deg.C, 500 deg.C, 510 deg.C, 520 deg.C and 530 deg.C for 10 hours, and it can be seen that fluorescence gradually broadens with increasing heat treatment temperature and the luminescence bandwidth reaches a maximum at 530 deg.C. FIG. 2 is an absorption spectrum of example 1, showing 2 μm luminescence of a mother glass and a sample heat-treated at 490, 500, 510, 520 and 530 ℃ for 10 hours, and it can be seen that the absorption coefficient of the sample at 808nm gradually increases with the increase of the heat-treatment temperature, which is advantageous for obtaining a high absorption coefficient. The inset shows the transmission spectrum, and it can be seen that the transmittance of the glass sample is maintained above 70%, and the glass sample has high transparency. FIG. 3 is a transmission electron micrograph and a size distribution of a rare earth-doped laser glass from which quantum dots are precipitated in example 1, showing, from bottom to top, the distribution of the quantum dots in the samples heat-treated at 490 deg.C, 500 deg.C, 510 deg.C, 520 deg.C and 530 deg.C for 10 hours, respectively, corresponding to the results of the different heat treatment temperatures in step (6)And (3) distribution and size, the quantum dot size is continuously increased in the increase of the heat treatment temperature, and the distribution is relatively uniform. FIG. 4 is a graph showing the fluorescence decay curve of the sample of example 1 heat-treated at 530 ℃ for 10 hours, showing a fluorescence lifetime of about 574. mu.s. The rare earth-doped laser glass for separating out the quantum dots prepared in the above embodiment has high transparency, the quantum dots are PbS, and the size is 1.7-5.1 nm. Tm can be obtained simultaneously in the glass after heat treatment under the pump of a 808nm Laser Diode (LD)3+And PbS is positioned in the ultra-wideband fluorescence of 2 mu m wave band, the emission wavelength range is 1400-2600 nm, the tuning range is up to 1200 nm, and the method is very suitable for the preparation and the application of 2 mu m broadband tunable laser glass optical fiber and optical fiber laser.
Claims (1)
1. The rare earth-doped laser glass capable of emitting light with an ultra-wide band of 2 microns and separating out quantum dots is characterized by comprising the following components in percentage by mole: SiO 22 52％，Na2CO3 32％，Al2O3 4％，ZnO 5％，ZnS 2％，PbO 1％，Tm2O34%, the luminescence wavelength of the glass can realize the luminescence of 2600nm wave band, and the preparation method of the laser glass comprises the following steps:
(1) accurately weighing 50g of raw materials according to the composition and the proportion, wherein SiO2：16.81g，Na2CO3：18.25g，Al2O3：2.19g，ZnO：2.19g，ZnS：1.05g，PbO：1.20g，Tm2O3：8.30g；
(2) Mixing the raw materials obtained in the step (1) in an agate mortar to form a batch;
(3) transferring the batch in the step (2) into a corundum crucible, and placing the corundum crucible in a high-temperature melting furnace to melt at 1500 ℃ for 60 minutes to obtain bubble-free, stone-free, transparent and uniform glass liquid;
(4) pouring the clarified molten glass on a stainless steel iron plate for molding to obtain a transparent glass block;
(5) rapidly transferring the formed transparent glass to a muffle furnace at the temperature of 400 ℃ for annealing, preserving the heat for 4 hours to remove the internal stress of the glass, and then cooling the glass to room temperature along with the furnace at the cooling rate of 20 ℃/minute to obtain the rare earth-doped laser glass without quantum dot precipitation;
(6) and (3) preserving the heat of the transparent glass cooled to room temperature at 490 ℃, 500 ℃, 510 ℃, 520 ℃ and 530 ℃ for 30 hours, and then cooling to room temperature to obtain the rare earth-doped laser glass for separating out the quantum dots.
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| Lead Chalcogenide Quantum Dot‐Doped Glasses for Photonic Devices;Chao Liu;《International Journal of Applied Glass Science》;20130527;第4卷(第3期);第163-173页 * |
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