CN113402166A - Erbium-doped phosphate laser glass, preparation method and optical element - Google Patents
Erbium-doped phosphate laser glass, preparation method and optical element Download PDFInfo
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- CN113402166A CN113402166A CN202110783082.1A CN202110783082A CN113402166A CN 113402166 A CN113402166 A CN 113402166A CN 202110783082 A CN202110783082 A CN 202110783082A CN 113402166 A CN113402166 A CN 113402166A
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- glass
- erbium
- doped phosphate
- doped
- phosphate laser
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- 239000000087 laser glass Substances 0.000 title claims abstract description 17
- 229910019142 PO4 Inorganic materials 0.000 title claims abstract description 15
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 title claims abstract description 15
- 239000010452 phosphate Substances 0.000 title claims abstract description 15
- 230000003287 optical effect Effects 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims description 15
- 239000011521 glass Substances 0.000 claims abstract description 34
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 14
- 238000000137 annealing Methods 0.000 claims abstract description 13
- 239000010431 corundum Substances 0.000 claims abstract description 13
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 238000000034 method Methods 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims description 19
- 239000002243 precursor Substances 0.000 claims description 12
- 239000011812 mixed powder Substances 0.000 claims description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 239000004570 mortar (masonry) Substances 0.000 claims description 6
- 238000005303 weighing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 230000009477 glass transition Effects 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 2
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims 2
- 229910052697 platinum Inorganic materials 0.000 claims 1
- 239000000843 powder Substances 0.000 claims 1
- 238000004321 preservation Methods 0.000 claims 1
- 239000005365 phosphate glass Substances 0.000 abstract description 9
- 239000013307 optical fiber Substances 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 abstract description 4
- 230000008859 change Effects 0.000 abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- ILRRQNADMUWWFW-UHFFFAOYSA-K aluminium phosphate Chemical compound O1[Al]2OP1(=O)O2 ILRRQNADMUWWFW-UHFFFAOYSA-K 0.000 abstract 1
- 238000004020 luminiscence type Methods 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 229910001018 Cast iron Inorganic materials 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 238000010309 melting process Methods 0.000 description 4
- 239000006060 molten glass Substances 0.000 description 4
- 238000007493 shaping process Methods 0.000 description 4
- 239000012856 weighed raw material Substances 0.000 description 4
- 239000000835 fiber Substances 0.000 description 3
- 239000003607 modifier Substances 0.000 description 3
- 238000003723 Smelting Methods 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 238000009472 formulation Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- 230000003321 amplification Effects 0.000 description 1
- 238000000295 emission spectrum Methods 0.000 description 1
- XFULIUKARWFBDF-UHFFFAOYSA-K erbium(3+);phosphate Chemical compound [Er+3].[O-]P([O-])([O-])=O XFULIUKARWFBDF-UHFFFAOYSA-K 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000009022 nonlinear effect Effects 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- -1 rare earth ions Chemical class 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910052714 tellurium Inorganic materials 0.000 description 1
- PORWMNRCUJJQNO-UHFFFAOYSA-N tellurium atom Chemical compound [Te] PORWMNRCUJJQNO-UHFFFAOYSA-N 0.000 description 1
Images
Classifications
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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
- C03C3/12—Silica-free oxide glass compositions
- C03C3/16—Silica-free oxide glass compositions containing phosphorus
- C03C3/17—Silica-free oxide glass compositions containing phosphorus containing aluminium or beryllium
-
- 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
- C03C4/00—Compositions for glass with special properties
-
- 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
- C03C4/0071—Compositions for glass with special properties for laserable glass
-
- G—PHYSICS
- G02—OPTICS
- G02B—OPTICAL ELEMENTS, SYSTEMS OR APPARATUS
- G02B1/00—Optical elements characterised by the material of which they are made; Optical coatings for optical elements
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Geochemistry & Mineralogy (AREA)
- General Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Physics & Mathematics (AREA)
- Optics & Photonics (AREA)
- Manufacturing & Machinery (AREA)
- General Physics & Mathematics (AREA)
- Glass Compositions (AREA)
Abstract
An erbium-doped phosphate laser glass is prepared by controlling (RO + R) in phosphate glass2O)/P2O5To change Er3+Covalent bonding and asymmetry of the ions, thereby adjusting the luminescence properties thereof. The phosphate glass main body of the invention is aluminum phosphate glass, and the molar components are as follows: 39 to 50 mol% of P2O520 to 31 mol% of RO (R is Mg, Ca, Ba), 5 to 15 mol% of Al2O315 to 25 mol% of Ra2O (Ra is Na and K) and doped Er with the concentration of 1-10 mol percent2O3. The method adopts a corundum crucible to prepare glass liquid, then cools the glass in a preheated mold, and then puts the glass into a muffle furnace for annealing. Tong (Chinese character of 'tong')Over-control (RO + R)2O)/P2O5The content of (a) enables the fluorescence bandwidth of the erbium-doped phosphate glass to be widened to 1609-1627 nm. The phosphate glass has the advantages of good optical performance, easy processing and the like, and has great application prospect in laser glass and optical fibers.
Description
Technical Field
The invention relates to the technical field of rare earth luminescent glass and laser glass, in particular to erbium-doped phosphate laser glass for an L + band optical amplifier, a preparation method and an optical element.
Technical Field
Ultra-wideband fiber amplifiers have a greater number of channels and a greater bandwidth, and are therefore of great interest in the field of optical communications. Er3+Ions are widely used as optical amplification media because they are in the lowest loss window of single-mode optical fibers. But commonly used L-band Er-doped3+The working wavelength of the optical fiber amplifier is 1570-1603 nm, and the optical fiber amplifier is not expanded to an L + wave band (1603 nm-1627 nm).
The current novel host material optical fiber amplifier comprises Er-doped3+The tellurium-based fiber amplifier (EDTFA) can work in a C + L wave band or an L wave band (1581-1616 nm). The gain bandwidth of EDTFA in the L band is large, but the high refractive index of EDTFA causes high nonlinear effect, and the raw material cost is high. The phosphate glass has high solubility to rare earth ions, large gain per unit length, low cost of raw materials, good fiber forming performance and suitability for civil communication, and is used for small optical fiber amplifiers. The invention proposes a method for modifying (RO + R) in phosphate glasses2O)/P2O5To expand Er3+To 1627nm and provides a preparation flow.
Disclosure of Invention
The invention aims to provide erbium-doped phosphate laser glass which has the advantages of low cost, easiness in preparation, high doping concentration and the like, and a corresponding preparation method.
The technical solution of the invention is as follows:
the composition of an erbium-doped phosphate laser glass is described as follows:
r ═ Mg, Ca, Ba, Ra ═ Na, K, where (RO + Ra)2O)/P2O5Greater than or equal to 0.8. The luminous intensity at 1627nm is greater than 1/2 which is the magnitude of luminous intensity at 1603 nm.
The invention also provides a preparation method of the erbium-doped phosphate laser glass, which comprises the following steps:
calculating and weighing raw materials according to the composition and the mole percentage of the erbium phosphate laser glass in claim 1, and putting the raw materials into an agate mortar for fully grinding to form mixed powder;
placing the mixed powder obtained by grinding in the step I into a corundum crucible, putting the corundum crucible into a 1100-1200 ℃ smelting furnace, and smelting for 60-70 min to obtain glass liquid;
thirdly, pouring the glass liquid on a preheated iron mold to obtain a transparent and uniform glass precursor;
fourthly, transferring the glass precursor into a muffle furnace for annealing treatment, wherein the annealing temperature is the glass transition temperature (T)g) After preserving heat for 3-24 hours, cooling to room temperature at a cooling rate of 0.1-10 ℃/h, and taking out a glass precursor;
and fifthly, processing the glass precursor obtained in the step IV into a glass sheet with the thickness of 1-2 mm.
The glass sheet may be ground or polished to obtain optical elements such as lenses and prisms.
The invention has the technical effects that:
the invention controls Er3+(RO + R) in phosphate-doped glass2O)/P2O5To increase Er3+Local field strength of the ion, thereby increasing Er3+Stark splitting and asymmetry of (1), and ultimately Er3+The fluorescence bandwidth of the ions is extended. RO and R2O as a component of the glass network modifier acts to break or accumulate the glass network, and the glass network modifier P is modified by the change of the O and the network modifier2O5The proportion of Er can be easily changed3+The degree of order of the lattice sites. Er3+The lower the degree of order of the local environment, the larger the difference of the stark energy levelsThe wider the fluorescence line. In addition, the glass has the advantages of low cost, easy preparation, high doping concentration and the like, and can be used in high-power high-energy pulse laser media.
Drawings
FIG. 1 shows Er at room temperature in example 1#, example 2#, example 3#, and example 4# of the present invention3+The fluorescence spectrum of (1) is illustrated by Er in each example3+Change in the ratio of fluorescence intensity at 1627nm and 1603 nm.
FIG. 2 shows example 3 of the present invention, Er of another erbium-doped phosphate glass and erbium-doped quartz glass at room temperature3+The emission spectrum of (a).
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The components of the examples of erbium-doped phosphate laser glass of the present invention are as follows:
table 1: formulation of the example Components
Example 1 #:
the raw materials are shown in table 1, and the specific preparation process is as follows:
weighing raw materials (70 g in total):
placing the weighed raw materials in an agate mortar for fully grinding to form mixed powder, placing the ground mixed powder in a corundum crucible, placing the corundum crucible in a high-temperature furnace at 1150 ℃ for melting for 55min, and raising the temperature to 1200 DEG CAnd keeping the temperature for about 10 min. Thereafter, the homogeneous molten glass is cast on a preheated cast iron mould, which is transferred rapidly to an annealing furnace after its shaping, at about TgAnnealing at temperature for 180min followed by cooling to room temperature at a rate of about 1 deg.C/min. In the melting process, a corundum crucible is required to be covered, so that the volatilization of raw materials is reduced. The prepared glass precursor is processed into a glass sheet with the thickness of 1 mm.
Example 2 #:
the raw materials are shown in table 1, and the specific preparation process is as follows:
weighing raw materials (70 g in total):
the weighed raw materials are placed in an agate mortar to be fully ground to form mixed powder, the mixed powder obtained by grinding is placed in a corundum crucible, and is placed in a high-temperature furnace at 1150 ℃ to be melted for 55min, and then the temperature is raised to 1200 ℃ and is kept for 10 min. Thereafter, the homogeneous molten glass is cast on a preheated cast iron mould, which is transferred rapidly to an annealing furnace after its shaping, at about TgAnnealing at temperature for 180min followed by cooling to room temperature at a rate of about 1 deg.C/min. In the melting process, a corundum crucible is required to be covered, so that the volatilization of raw materials is reduced. The prepared glass precursor is processed into a glass sheet with the thickness of 1 mm.
Example 3 #:
the raw materials are shown in table 1, and the specific preparation process is as follows:
weighing raw materials (70 g in total):
the weighed raw materials are placed in an agate mortar to be fully ground to form mixed powder, the mixed powder obtained by grinding is placed in a corundum crucible, and is placed in a high-temperature furnace at 1150 ℃ to be melted for 55min, and then the temperature is raised to 1200 ℃ and is kept for 10 min. Thereafter, the homogeneous molten glass is cast in a preheated stateOn cast iron moulds, and after shaping, rapidly transferring to an annealing furnace at about TgAnnealing at temperature for 180min followed by cooling to room temperature at a rate of about 1 deg.C/min. In the melting process, a corundum crucible is required to be covered, so that the volatilization of raw materials is reduced. The prepared glass precursor is processed into a glass sheet with the thickness of 1 mm.
Example 4 #:
the raw materials are shown in table 1, and the specific preparation process is as follows:
weighing raw materials (70 g in total):
the weighed raw materials are placed in an agate mortar to be fully ground to form mixed powder, the mixed powder obtained by grinding is placed in a corundum crucible, and is placed in a high-temperature furnace at 1150 ℃ to be melted for 55min, and then the temperature is raised to 1200 ℃ and is kept for 10 min. Thereafter, the homogeneous molten glass is cast on a preheated cast iron mould, which is transferred rapidly to an annealing furnace after its shaping, at about TgAnnealing at temperature for 180min followed by cooling to room temperature at a rate of about 1 deg.C/min. In the melting process, a corundum crucible is required to be covered, so that the volatilization of raw materials is reduced. The prepared glass precursor is processed into a glass sheet with the thickness of 1 mm. The glass sheet may be ground or polished to obtain optical elements such as lenses and prisms.
Effect embodiment:
FIG. 1 shows Er in the example3+Fluorescence spectrum in the wavelength band of 1600 to 1635 nm. As can be seen from the inset, Er at room temperature is observed in example 1#, example 2#, example 3#, and example 4#3+The fluorescence intensity ratios at 1627nm and 1603nm are 0.5402, 0.5640, 0.5862 and 0.6038 respectively, which are all higher than 0.5. As can be seen, the fluorescence bandwidth of the invention in the L + band is flatter.
Formulation of other matrix components and Er at room temperature3+The ratio of fluorescence intensity at 1627nm and 1603nm is as follows:
comparative example 1:
phosphate saltsGlass: 72P2O5-8Al2O3-20BaO-0.5Er2O3，I1627/I1603＝0.3538
Comparative example 2:
quartz: 0.05Er2O3-0.5Al2O3-99.45SiO2，I1627/I1603＝0.5283
As shown in FIG. 2, Er of example 3#3+The normalized fluorescence intensity ratio at 1627nm and 1603nm was 0.5862, Er of the erbium-doped quartz glass of comparative example 13+The normalized fluorescence intensity ratio at 1627nm and 1603nm was 0.5283, Er for the erbium-doped phosphate glass of comparative example 23+The normalized fluorescence intensity ratio at 1627nm and 1603nm was 0.3538. In contrast, example 3# has a much flatter spectrum in the L + band.
Claims (5)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110783082.1A CN113402166A (en) | 2021-07-12 | 2021-07-12 | Erbium-doped phosphate laser glass, preparation method and optical element |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202110783082.1A CN113402166A (en) | 2021-07-12 | 2021-07-12 | Erbium-doped phosphate laser glass, preparation method and optical element |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116675437A (en) * | 2023-05-24 | 2023-09-01 | 之江实验室 | Nonlinear optical glass and its preparation method and application |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3731226A (en) * | 1971-11-10 | 1973-05-01 | American Optical Corp | Laser using phosphate base laser glass |
| CN1583627A (en) * | 2004-06-01 | 2005-02-23 | 中国科学院上海光学精密机械研究所 | Method for manufacturing phosphate glass optical waveguide |
| CN105347674A (en) * | 2015-11-19 | 2016-02-24 | 成都光明光电有限责任公司 | Phosphate neodymium glass with high thermal conductivity |
| CN109081579A (en) * | 2018-09-17 | 2018-12-25 | 成都光明光电股份有限公司 | phosphate laser neodymium glass |
| CN110807292A (en) * | 2019-10-30 | 2020-02-18 | 华南理工大学 | A kind of preparation method of laser glass material with specific laser performance |
-
2021
- 2021-07-12 CN CN202110783082.1A patent/CN113402166A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3731226A (en) * | 1971-11-10 | 1973-05-01 | American Optical Corp | Laser using phosphate base laser glass |
| CN1583627A (en) * | 2004-06-01 | 2005-02-23 | 中国科学院上海光学精密机械研究所 | Method for manufacturing phosphate glass optical waveguide |
| CN105347674A (en) * | 2015-11-19 | 2016-02-24 | 成都光明光电有限责任公司 | Phosphate neodymium glass with high thermal conductivity |
| CN109081579A (en) * | 2018-09-17 | 2018-12-25 | 成都光明光电股份有限公司 | phosphate laser neodymium glass |
| CN110807292A (en) * | 2019-10-30 | 2020-02-18 | 华南理工大学 | A kind of preparation method of laser glass material with specific laser performance |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN116675437A (en) * | 2023-05-24 | 2023-09-01 | 之江实验室 | Nonlinear optical glass and its preparation method and application |
| CN116675437B (en) * | 2023-05-24 | 2026-01-23 | 之江实验室 | Nonlinear optical glass and preparation method and application thereof |
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Application publication date: 20210917 |