CN112028480A - Preparation method of praseodymium and ytterbium co-doped fluorine-aluminum glass with 3.5-micrometer luminescence broadband - Google Patents
Preparation method of praseodymium and ytterbium co-doped fluorine-aluminum glass with 3.5-micrometer luminescence broadband Download PDFInfo
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- -1 fluorine-aluminum Chemical compound 0.000 title claims abstract description 47
- 239000011521 glass Substances 0.000 title claims abstract description 40
- 229910052777 Praseodymium Inorganic materials 0.000 title claims abstract description 34
- 229910052769 Ytterbium Inorganic materials 0.000 title claims abstract description 29
- PUDIUYLPXJFUGB-UHFFFAOYSA-N praseodymium atom Chemical compound [Pr] PUDIUYLPXJFUGB-UHFFFAOYSA-N 0.000 title claims abstract description 24
- NAWDYIZEMPQZHO-UHFFFAOYSA-N ytterbium Chemical compound [Yb] NAWDYIZEMPQZHO-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 238000004020 luminiscence type Methods 0.000 title claims abstract description 18
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 239000000126 substance Substances 0.000 claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000001816 cooling Methods 0.000 claims abstract description 4
- 229910052802 copper Inorganic materials 0.000 claims abstract description 4
- 239000010949 copper Substances 0.000 claims abstract description 4
- 238000000227 grinding Methods 0.000 claims abstract description 4
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 4
- 238000005303 weighing Methods 0.000 claims abstract description 4
- 238000010304 firing Methods 0.000 claims abstract description 3
- 238000002844 melting Methods 0.000 claims abstract description 3
- 230000008018 melting Effects 0.000 claims abstract description 3
- 238000000034 method Methods 0.000 claims description 10
- 230000003287 optical effect Effects 0.000 claims description 7
- KLZUFWVZNOTSEM-UHFFFAOYSA-K Aluminum fluoride Inorganic materials F[Al](F)F KLZUFWVZNOTSEM-UHFFFAOYSA-K 0.000 claims description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 238000005498 polishing Methods 0.000 claims description 3
- IRPGOXJVTQTAAN-UHFFFAOYSA-N 2,2,3,3,3-pentafluoropropanal Chemical compound FC(F)(F)C(F)(F)C=O IRPGOXJVTQTAAN-UHFFFAOYSA-N 0.000 claims description 2
- 239000005383 fluoride glass Substances 0.000 claims description 2
- 238000010521 absorption reaction Methods 0.000 abstract description 13
- 239000013307 optical fiber Substances 0.000 abstract description 6
- 230000005540 biological transmission Effects 0.000 abstract description 5
- 230000009467 reduction Effects 0.000 abstract description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 3
- 238000010923 batch production Methods 0.000 abstract description 2
- 238000002834 transmittance Methods 0.000 abstract description 2
- 238000001228 spectrum Methods 0.000 abstract 1
- 239000000835 fiber Substances 0.000 description 15
- 238000005086 pumping Methods 0.000 description 11
- 239000000463 material Substances 0.000 description 8
- 229910052691 Erbium Inorganic materials 0.000 description 6
- 239000005371 ZBLAN Substances 0.000 description 6
- 230000008569 process Effects 0.000 description 6
- 238000012546 transfer Methods 0.000 description 4
- 230000005281 excited state Effects 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 239000004065 semiconductor Substances 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 2
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 2
- 230000005283 ground state Effects 0.000 description 2
- 238000001748 luminescence spectrum Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- WCWKKSOQLQEJTE-UHFFFAOYSA-N praseodymium(3+) Chemical compound [Pr+3] WCWKKSOQLQEJTE-UHFFFAOYSA-N 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 230000003595 spectral effect Effects 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- 238000000411 transmission spectrum Methods 0.000 description 2
- 101100136092 Drosophila melanogaster peng gene Proteins 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- PJHIYISBDSWHHA-UHFFFAOYSA-N [Ho].[Pr] Chemical compound [Ho].[Pr] PJHIYISBDSWHHA-UHFFFAOYSA-N 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000005372 fluoroaluminate glass Substances 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- LXDXBIJPSAUNBJ-UHFFFAOYSA-N holmium ytterbium Chemical compound [Ho][Yb] LXDXBIJPSAUNBJ-UHFFFAOYSA-N 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 230000010355 oscillation Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000002250 progressing effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004611 spectroscopical analysis Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B5/00—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture
- C03B5/06—Melting in furnaces; Furnaces so far as specially adapted for glass manufacture in pot furnaces
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B19/00—Other methods of shaping glass
- C03B19/02—Other methods of shaping glass by casting molten glass, e.g. injection moulding
-
- 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
- C03C3/32—Non-oxide glass compositions, e.g. binary or ternary halides, sulfides or nitrides of germanium, selenium or tellurium
- C03C3/325—Fluoride glasses
-
- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
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Abstract
The invention relates to a preparation method of praseodymium and ytterbium co-doped fluorine-aluminum glass with a 3.5 micron luminescence broadband, which comprises the steps of weighing and preparing chemical raw materials according to molar percentage, and then fully grinding and mixing the chemical raw materials; putting the mixed raw materials into a crucible, and melting and firing the mixed raw materials in a glove box through a high-temperature furnace at 930 ℃; and pouring the molten liquid into a copper plate mold preheated at 370 ℃, keeping for 3 hours, and then slowly cooling to room temperature to obtain the praseodymium and ytterbium co-doped fluoaluminum glass with different concentrations. The glass prepared by the invention has good deliquescence resistance; the preparation process is simple, and batch production can be realized; the optical fiber has good spectrum transmission width and transmission performance, and no obvious visible transmittance reduction condition exists at the water molecule absorption position; the laser has the luminous performance of a broadband of 3.5 microns, and can realize the luminescence by using a simple and reliable 976nm laser pump; has important application prospect in the field of realizing high-power 3.5 mu m optical fiber laser.
Description
Technical Field
The invention belongs to the fields of mid-infrared glass luminescence, mid-infrared fiber laser and the like, and particularly relates to a preparation method of praseodymium and ytterbium co-doped fluorine-aluminum glass with a 3.5-micrometer luminescence broadband.
Background
Mid-infrared lasers in the 3-5 μm range have received widespread domestic and foreign attention because of their minimal window of atmospheric attenuation. And a plurality of absorption peaks of gases and organic molecules are in the region, so that the application of the mid-infrared laser in the fields of space communication, atmospheric monitoring, spectroscopy, national defense and the like is ensured. Currently, there are two main techniques for generating mid-infrared laser light: the first is based on nonlinear optical effects including optical parametric oscillation and difference frequency generation. Such lasers are generally complex in structure, low in electro-optical efficiency, and complex in crystal preparation process of the optical parametric oscillator. The second is realized by gain materials such as quantum well semiconductors and transition metal doped II-IV semiconductors. Solid-state lasers based on these materials have been intensively studied and commercialized, but they also have other technical drawbacks such as difficulty in achieving high power and obtaining good beam quality, and a great reduction in laser output efficiency at higher ambient temperatures.
Compared with the technology, the mid-infrared rare earth doped fiber laser has remarkable advantages in the aspects of spectral range, pumping efficiency, stability, portability and the like. The most commonly used optical fiber in mid-infrared lasers is ZBLAN (ZrF)4-BaF2-LaF3-AlF3NaF)) optical fiber, which has been widely studied since 1985. The use of ZBLAN fibers has been in various fields and is still under constant development. However, ZBLAN fibers present serious deliquescence problems that limit their use in many applications. Fluoroaluminium glasses and optical fibers are another fluoride material for visible-near-infrared-mid-infrared laser applications, which are similar in structure and phonon energy to ZBLAN glasses, but are much more moisture resistant than ZBLAN. In 2010, yellow visible laser was implemented in dysprosium-doped fluoroaluminium fibers. In 2000, neodymium-doped fluor-aluminum fibers were found to be useful in 1.3 μm fiber amplifiers. 2014 found that the holmium-ytterbium co-doped fluorine-aluminum glass can be used for 2.85 μm luminescence. In addition, the holmium praseodymium codope fluorine aluminum fiber laser developed in 2019 also shows that the fluorine aluminum glass has good application in the field of mid-infrared lasersAnd (4) potential.
Most of 3.5-micron mid-infrared fiber lasers are realized by using erbium ion-doped fibers at present, but due to the energy level characteristic of erbium ions, the pumping efficiency of 638-nm lasers is low, so that the luminous efficiency of 3.5-micron lasers is low. In order to improve the pumping efficiency, 976nm and 1976nm dual-wavelength pumps are generally adopted as pumping sources. In 2017, the solar curing Peng and the like realize the 3.52-3.68 mu m adjustable mid-infrared fiber laser of the erbium-doped ZBLAN fiber, and the passive Q-switch and the mode-locked pulse laser at the 3.5 mu m wave band are realized by adding a black phosphorus saturated absorption mirror and utilizing an experimental device of a dual-wavelength pump. Jobin et al used a similar dual wavelength pump to implement a gain switched fiber laser for the first time in 2018. On the other hand, the research on single-wavelength pumping erbium ions started as early as 1992, but its research has been progressing slowly due to the high cost of dye lasers or semiconductor lasers and the limitations of the conditions of use. Although theoretical analysis finds some methods for improving the pumping efficiency, the erbium ion-doped 3.5 μm fiber laser still has the problems of high cost and complex installation. Meanwhile, F.Maes et al also find that the dual-wavelength pump erbium ion doped fiber laser has quenching behavior due to excited state absorption of erbium ions.
Therefore, based on the technical problems, we propose for the first time that praseodymium and ytterbium are doped into a fluorine-aluminum material together, and 3.5 μm luminescence of a broadband can be realized under the pumping of a cheap 976nm laser diode, so that the fluorine-aluminum material has high innovation and frontier performance, and the core technology is shown to people in the patent. Meanwhile, the preparation method of the praseodymium and ytterbium co-doped fluorine-aluminum glass with the light emitting bandwidth of 3.5 microns based on the invention has a certain inspiring effect on the realization of 3.5 microns middle infrared laser of a fluorine-aluminum material.
Disclosure of Invention
The invention aims to solve the problem of realizing mid-infrared luminescence with a broadband of 3.5 mu m in a glass material, and the glass with good performance is obtained by selecting a proper glass material and proper rare earth ions.
A preparation method of praseodymium and ytterbium co-doped fluorine-aluminum glass with a 3.5 micron luminescence broadband comprises the following steps:
step 1: weighing and preparing chemical raw materials according to a certain molar percentage, and then fully grinding and mixing in an agate mortar;
step 2: putting the mixed raw materials into a crucible, and melting and firing the mixed raw materials in a glove box through a high-temperature furnace at 930 ℃;
and step 3: pouring the molten liquid into a copper plate mould preheated at 370 ℃, keeping for 3 hours, and then slowly cooling to room temperature to obtain praseodymium and ytterbium co-doped aluminum fluoride glass with different concentrations;
and 4, step 4: and polishing the surface of the praseodymium and ytterbium co-doped fluorine-aluminum glass sample to optical quality to obtain a final glass sample capable of realizing broadband 3.5 mu m luminescence.
The chemical raw materials comprise the following components in percentage by mole:
30AlF3-15BaF2-(20-x-y)YF3-25PbF2-10MgF2-xPrF3-yYbF3wherein x and y are each any positive number less than 20.
The invention has the beneficial effects that:
(1) the glass prepared by the invention has simple preparation process and can realize batch production;
(2) the glass prepared by the invention has good spectral transmission width and transmission performance, and has no obvious visible transmittance reduction condition at the water molecule absorption position;
(3) the glass prepared by the invention has the luminescent property of a broadband of 3.5 mu m, and the luminescence can be realized by a simple and reliable 976nm laser pump;
(4) the glass prepared by the invention has important application prospect in the field of realizing high-power 3.5 mu m optical fiber laser.
Drawings
FIG. 1 is a 3.5 μm broadband luminescence spectrum of a fluorine-aluminum glass doped with praseodymium and ytterbium ions with different concentrations;
FIG. 2 is a graph of absorption transmission spectra of various concentrations of praseodymium and ytterbium ions doped fluorine aluminum glass;
fig. 3 is an energy transfer diagram of fluoroaluminium glasses doped with different concentrations of praseodymium and ytterbium ions.
Detailed Description
The following further describes embodiments of the present invention with reference to the accompanying drawings:
a preparation method of praseodymium and ytterbium co-doped fluorine-aluminum glass with a 3.5 micron luminescence broadband comprises the following steps:
step 1: weighing and preparing the chemical raw materials according to the following mol percentage, and then fully grinding and mixing the raw materials in an agate mortar: 30AlF3-15BaF2-(20-x-y)YF3-25PbF2-10MgF2-xPrF3-yYbF3(x＝0、0.1、0.2、0.3、0.5、1、2、3；y＝1).
Step 2: the mixed raw materials are filled into a crucible and melted and fired in a glove box through a high-temperature furnace at 930 ℃.
And step 3: and pouring the molten liquid into a copper plate mold preheated at 370 ℃, keeping for 3 hours, and then slowly cooling to room temperature to obtain the praseodymium and ytterbium co-doped fluoaluminum glass with different concentrations.
And 4, step 4: and polishing the surface of the praseodymium and ytterbium co-doped fluorine-aluminum glass sample to optical quality to obtain a final glass sample capable of realizing broadband 3.5 mu m luminescence.
Further optical tests were performed on the glass samples prepared above.
FIG. 1 is a broad-band 3.5 μm luminescence spectrum of the fluorine-aluminum glass doped with praseodymium and ytterbium ions of different concentrations detected by a Zolix Omni-lambda 300i fluorescence spectrometer under the condition of 976nm laser diode pumping. When the molar ratio of ytterbium ion to praseodymium ion is 1 to 0.3, the light emission of 3.5 μm reaches the maximum intensity and the widest light emission range, and the whole light emission range can cover 2.6 μm to 4.1 μm. The light-emitting position shown in fig. 1 corresponds to two energy transfer processes of praseodymium ions:1G4→3F4(center position 2.92 μm) and1G4→3F3(center position 3.46 μm), and in the luminescence of the latter, the full width at half maximum is 363.64 nm.
FIG. 2 shows the absorption spectra measured by a Perkin Elmer Lambda750 spectrophotometer (measurement range 250-2500nm) and the transmission spectra measured by a Perkin Elmer FT-IR spectrometer (measurement range 2500-10000nm) for samples of fluoroaluminium glass doped with different concentrations of praseodymium and ytterbium ions. (a) The absorption peaks in the figure correspond to the transition of praseodymium ions and ytterbium ions from the ground state to the excited state, the position and the shape of the 980nm absorption peak are not obviously different along with the change of the concentration of the praseodymium ions, and the overlapped peaks near 980nm indicate that the cheap 980nm commercial laser diode can be a pumping source of praseodymium and ytterbium co-doped glass. The very weak absorption peak of hydroxyl groups around 3 μm is shown in (b), indicating that the water absorption of the fluoroaluminate glass we prepared is very low. The average transmission before 5 μm was about 92% and the infrared cut-off wavelength was 9 μm, demonstrating that this glass can be used for mid-infrared applications.
FIG. 3 is a graph of the energy transfer mechanism of our glass under 976nm laser diode pumping conditions. Although praseodymium ions can directly absorb photons of about 980nm, the praseodymium ions do not have a specific structure because of the specific structure of the praseodymium ions3H4→1G4The absorption transition of (a) is a spin-forbidden band, so the efficiency is low. Ytterbium ions have only two energy levels, and can effectively absorb 980nm photon energy through the Ground State Absorption (GSA) process. Through co-doping of ytterbium ions and praseodymium ions, the energy of the ytterbium ions can be sensitized to the praseodymium ions through an energy transfer process (ET). In praseodymium ion pumping to1G4After the energy level, 3.5 μm light emission can be obtained in the relaxation process from this energy level to other energy levels below. At the same time, is located at1G4Praseodymium ion at an energy level can absorb another photon and is excited to a higher level by an excited state absorption process (ESA)1P6、3P1、3P0And an upper energy level. Finally, through the process of radiationless relaxation and Cross Relaxation (CR), praseodymium ions at higher energy level will return to1G4The energy level increases the particle number of the energy level, thereby leading to more effective 3.5 mu m luminescence, and the ion is doped into the fluorine-aluminum glass, thereby providing a new research idea for developing the mid-infrared laser.
The above description is directed to the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any changes or substitutions that may be easily made by those skilled in the art within the technical scope of the present invention will be included in the present invention. The specific protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (2)
1. A preparation method of praseodymium and ytterbium co-doped fluorine-aluminum glass with a 3.5 micron luminescence broadband is characterized by comprising the following steps:
step 1: weighing and preparing chemical raw materials according to molar percentage, and then fully grinding and mixing in an agate mortar;
step 2: putting the mixed raw materials into a crucible, and melting and firing the mixed raw materials in a glove box through a high-temperature furnace at 930 ℃;
and step 3: pouring the molten liquid into a copper plate mould preheated at 370 ℃, keeping for 3 hours, and then slowly cooling to room temperature to obtain praseodymium and ytterbium co-doped aluminum fluoride glass with different concentrations;
and 4, step 4: and polishing the surface of the praseodymium and ytterbium co-doped fluorine-aluminum glass sample to optical quality to obtain the praseodymium and ytterbium co-doped fluorine-aluminum glass with a light emitting bandwidth of 3.5 microns.
2. The method for preparing praseodymium and ytterbium co-doped fluorine-aluminum glass with 3.5 micron luminescence of broadband according to claim 1, wherein the method comprises the following steps: the chemical raw materials comprise the following components in percentage by mole:
30AlF3-15BaF2-(20-x-y)YF3-25PbF2-10MgF2-xPrF3-yYbF3wherein x and y are each any positive number less than 20.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112960905A (en) * | 2021-03-11 | 2021-06-15 | 哈尔滨工程大学 | Ho3+Doped fluoroaluminium glasses |
| CN113480172A (en) * | 2021-07-05 | 2021-10-08 | 哈尔滨工程大学 | Preparation method of holmium and neodymium co-doped fluorine-aluminum glass capable of realizing 3.9 micron luminescence |
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2020
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|---|
| R. I. WOODWARD等: "Towards diode-pumped mid-infrared praseodymium-ytterbium-doped fluoride fiber lasers" * |
| 周小等: "Pr3+/Yb3+共掺1.3μm锆系氟化物玻璃光纤的研制" * |
| 黄琦等: "Pr3+/Yb3+共掺光纤放大器中的能量转移过程" * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112960905A (en) * | 2021-03-11 | 2021-06-15 | 哈尔滨工程大学 | Ho3+Doped fluoroaluminium glasses |
| CN113480172A (en) * | 2021-07-05 | 2021-10-08 | 哈尔滨工程大学 | Preparation method of holmium and neodymium co-doped fluorine-aluminum glass capable of realizing 3.9 micron luminescence |
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