CN102211872A - 3 mu m luminous rare earth ion doped fluorophosphates laser glass and preparation method thereof - Google Patents
3 mu m luminous rare earth ion doped fluorophosphates laser glass and preparation method thereof Download PDFInfo
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- CN102211872A CN102211872A CN2011100702621A CN201110070262A CN102211872A CN 102211872 A CN102211872 A CN 102211872A CN 2011100702621 A CN2011100702621 A CN 2011100702621A CN 201110070262 A CN201110070262 A CN 201110070262A CN 102211872 A CN102211872 A CN 102211872A
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Abstract
The invention relates to 3 mu m luminous rare earth ion doped fluorophosphates laser glass and a preparation method thereof. The glass comprises the following components by molar percent: 15-20% of Al(PO3)3, 13-17% of MgF2, 5-25% of CaF2, 5-25% of SrF2, 17-22% of BaF2, 18-22% of NaF and 3-5% of RF3 (R can be rare-earth elements such as Er, Pr, Tm, Ho, or Nd). The glass is prepared by using a platinum crucible and a silicon carbide rod electric furnace fusion method. The glass in the invention is transparent, has no crystallization, has high infrared transmissivity at the vicinity of 3 mu m wave band, good physical and chemical properties and stability parameter delta T of more than or equal to 150 DEG C and can obtain strong 3 mu m fluorescence under the pumping of a laser diode with a wavelength of 980 nm, and the method is suitable for preparation and application of 3 mu m luminous rare earth ion doped special glass and optical fiber materials.
Description
Technical field
The present invention relates to a kind of fluorphosphate glass that 3 mu m luminous multiple rare earth ions are mixed altogether and preparation method thereof of realizing.
Background technology
In recent years, the solid statelaser of rear-earth-doped 3 μ m output has caused people's attention because of its extensive use.Because the absorption peak of 3 μ m laser and water is very approaching, and biological tissue is moisture more than 70%, therefore near the laser the 3 μ m is called as the gold laser of Dermatology Department, surgery, dentistry; In addition, 3 mu m waveband lasers also can be applicable to remote sensing chemical sensitisation, air pollution control (in the environment 10
-9The detection of the obnoxious flavoures such as formaldehyde, nitrogen protoxide, nitrogen peroxide, hydrogen sulfide, arsenous hydride of level content) aspect such as; Moreover, 3 mu m waveband lasers are positioned at atmospheric 2 transmission windows (1-3 μ m, 3-5 μ m, 8-14 μ m) in, many important characterization of molecules spectral lines have been covered, therefore, in remote sensing, range finding, environment measuring, biotechnology and medical treatment and be used for all having important application aspect the pumping source of new middle-infrared band laser.
The output of 3 μ m laser at first obtains by the Er doped crystal.Bagdasarov reported first in 1980 in the adulterated yttrium aluminum garnet of Er (YAG) crystal, obtain the 100mJ laser output of 3 mu m wavebands.At present abroad a lot of to the research that obtains 3 μ m output by rear-earth-doped crystal, but large-size crystals is difficult to shortcomings such as preparation, rear-earth-doped concentration be little, has limited its application.And rear-earth-doped glass optical fiber can be avoided these shortcomings of crystalline well.1988, the Pollack reported first the adulterated ZBLAN fluoride fiber of Er because Er
3+:
4I
11/2→
4I
13/2Transition obtains centre wavelength at 2.78 μ m, and the output energy is the laser output of 75J.Although the phonon energy of fluoride glass is low, the relatively poor and harsh preparation condition of its chemical stability and physical strength has also limited its application in 3 μ m outputs.
Fluorphosphate glass is a kind of comparatively ideal substrate material, it combines the advantage of fluoride glass and phosphate glass, glass ingredient adjustability has in a big way been brought the adjustability of a series of optical properties, lower nonlinear refractive index and higher stimulated emission cross section make it be expected to become the superpower laser laser glass, and it has the fluorescence linewidth of broad and higher rare earth ion solubleness simultaneously.On preparation technology, it is than the easier preparation of fluoride glass in addition, and technology is ripe more, and this drawing for high quality, low loss fiber provides guarantee.But, at present both at home and abroad the research that realizes 3 mu m luminous fluorphosphate glasses also seldom is seen in report.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of 3 mu m luminous rare earth ion doped fluophosphate laser glass and preparation method thereof, this glass has good thermostability, infrared transmission performance can obtain 3 very strong μ m fluorescence down the laser diode-pumped of 980nm wavelength preferably.
The concrete technical solution of the present invention is as follows:
A kind of 3 mu m luminous rare earth ion doped fluophosphate laser glass, its characteristics are that its molar percentage consists of:
Wherein: R is a rare earth element er, Tm, Ho, Nd, Pr, Yb.
Described rare earth ion doped mode has: Er singly mixes, Er-Pr two mixes, Er-Tm twoly mixes, Er-Nd twoly mixes, Er-Ho twoly mixes, Er-Tm-Ho three mixes, Er-Tm-Pr three mixes, Er-Yb-Pr three mixes, Er-Nd-Pr three mixes, Er-Nd-Ho three mixes.
The preparation method of 3 above-mentioned mu m luminous rare earth ion doped fluophosphate laser glass comprises the following steps:
1. selected described glass is formed and molar percentage, calculates the weight that corresponding each glass is formed, and accurately takes by weighing each raw material, mixes the formation compound;
2. compound is put into platinum crucible and melted in 1050～1120 ℃ globars electric furnace, the clarification of fusing back is 10～15 minutes fully, glass metal is cast in the mould of preheating;
3. glass is moved into rapidly and has been warming up to glass transformation temperature (T
g) in the following 10 ℃ retort furnace, be incubated 3～4 hours, reduce to room temperature with 10 ℃/hour speed again, glass sample is taken out in the cooling back fully.
Technique effect of the present invention is as follows:
The present invention is rare earth ion doped by many kinds of Er/Pr/Yb/Tm/Ho/Nd, can obtain 3 mu m luminous rare earth ion doped fluorphosphate glasses, glass transparent, no crystallization, near infrared transmittivity height 3 μ m, excellent in physical and chemical performance, stability parameter Δ T 〉=150 ℃.3 very strong μ m fluorescence be can obtain down the laser diode-pumped of 980nm wavelength, the preparation and the application of 3 μ m laser glasses and fiber optic materials are applicable to.
Description of drawings
The differential thermal curve of the 3 mu m luminous rare earth ion doped fluophosphate laser glass that Fig. 1 is obtained for embodiment 1#.
The infrared permeation spectrum of the 3 mu m luminous rare earth ion doped fluophosphate laser glass that Fig. 2 is obtained for embodiment 1#.
The fluorescence spectrum of the 3 mu m luminous rare earth ion doped fluophosphate laser glass that Fig. 3 is obtained for embodiment 1# under 980nm wavelength laser diode-pumped.
Embodiment
The glass ingredient of 10 specific embodiments of the present invention's 3 mu m luminous rare earth ion doped fluophosphate laser glass is as shown in table 1:
Table 1: the glass formula of concrete 10 embodiment
Embodiment 1#:
Composition is shown in 1# in the table 1, and concrete preparation process is as follows:
According to the molar percentage that 1# glass in the table 1 is formed, calculate corresponding each weight of forming, take by weighing each raw material and mix; Compound is put into platinum crucible melt in 1050 ℃ globars electric furnace, the clarification of fusing back is 15 minutes fully, glass metal is cast in the mould of preheating; Glass is moved into rapidly in the retort furnace that has been warming up to 420 ℃, is incubated 3 hours, reduce to room temperature with 10 ℃/hour speed again, glass sample is taken out in the cooling back fully.
Test result to this glass is as follows:
Get a little sample after the annealing, wear into fine powdered, carry out the differential thermal analysis test with agate mortar.The differential thermal curve of the present invention's 3 mu m luminous rare earth ion doped fluophosphate laser glass as shown in Figure 1.
The sheet glass that sample after the annealing is processed into 10 * 20 * 1.0 millimeters also polishes, and tests its infrared permeation spectrum, at laser diode-pumped its fluorescence spectrum of test down of 980nm wavelength.The infrared permeation spectrum of the present invention's 3 mu m luminous rare earth ion doped fluophosphate laser glass as shown in Figure 2.The fluorescence spectrum of the present invention's 3 mu m luminous rare earth ion doped fluophosphate laser glass under 980nm wavelength laser diode-pumped as shown in Figure 3.Experiment shows, glass transparent, no crystallization, near infrared transmittivity height 3 μ m, excellent in physical and chemical performance, stability parameter Δ T 〉=150 ℃.Can obtain 3 very strong μ m fluorescence down the laser diode-pumped of 980nm wavelength.
Embodiment 2#:
Composition is shown in 2# in the table 1, and concrete preparation process is as follows:
According to the molar percentage that 2# glass in the table 1 is formed, calculate corresponding each weight of forming, take by weighing each raw material and mix; Compound is put into platinum crucible melt in 1050 ℃ globars electric furnace, the clarification of fusing back is 13 minutes fully, glass metal is cast in the mould of preheating; Glass is moved into rapidly in the retort furnace that has been warming up to 430 ℃, is incubated 3.5 hours, reduce to room temperature with 10 ℃/hour speed again, glass sample is taken out in the cooling back fully.
Test result to this glass is as follows:
Get a little sample after the annealing, wear into fine powdered, carry out the differential thermal analysis test with agate mortar.
The sheet glass that sample after the annealing is processed into 10 * 20 * 1.0 millimeters also polishes, at laser diode-pumped its fluorescence spectrum of test down of 980nm wavelength.
Embodiment 3#:
Composition is shown in 3# in the table 1, and concrete preparation process is as follows:
According to the molar percentage that 3# glass in the table 1 is formed, calculate corresponding each weight percent of forming, take by weighing each raw material and mix; Compound is put into platinum crucible melt in 1080 ℃ globars electric furnace, the clarification of fusing back is 15 minutes fully, glass metal is cast in the mould of preheating; Glass is moved into rapidly in the retort furnace that has been warming up to 440 ℃, is incubated 4 hours, reduce to room temperature with 10 ℃/hour speed again, glass sample is taken out in the cooling back fully.
Test result to this glass is as follows:
Get a little sample after the annealing, wear into fine powdered, carry out the differential thermal analysis test with agate mortar.
The sheet glass that sample after the annealing is processed into 10 * 20 * 1.0 millimeters also polishes, at laser diode-pumped its fluorescence spectrum of test down of 980nm wavelength.
Embodiment 4#:
Composition is shown in 4# in the table 1, and concrete preparation process is as follows:
According to the molar percentage that 4# glass in the table 1 is formed, calculate corresponding each weight percent of forming, take by weighing each raw material and mix; Compound is put into platinum crucible melt in 1120 ℃ globars electric furnace, the clarification of fusing back is 15 minutes fully, glass metal is cast in the mould of preheating; Glass is moved into rapidly in the retort furnace that has been warming up to 440 ℃, is incubated 4 hours, reduce to room temperature with 10 ℃/hour speed again, glass sample is taken out in the cooling back fully.
Test result to this glass is as follows:
Get a little sample after the annealing, wear into fine powdered, carry out the differential thermal analysis test with agate mortar.
The sheet glass that sample after the annealing is processed into 10 * 20 * 1.0 millimeters also polishes, at laser diode-pumped its fluorescence spectrum of test down of 980nm wavelength.
Embodiment 5# is to 10#:
Composition as 5# in the table 1 to shown in the 10#, concrete preparation process such as embodiment 1#.
As follows to 5# to the test result of 10# glass:
Get a little sample after the annealing, wear into fine powdered, carry out the differential thermal analysis test with agate mortar.
The sheet glass that sample after the annealing is processed into 10 * 20 * 1.0 millimeters also polishes, at laser diode-pumped its fluorescence spectrum of test down of 980nm wavelength.
The foregoing description test shows all has the similar results of Fig. 1, Fig. 2 of the 3 mu m luminous rare earth ion doped fluophosphate laser glass that embodiment 1 obtained, differential thermal curve shown in Figure 3, infrared permeation spectrum and the fluorescence spectrum under 980nm wavelength laser diode-pumped.It is rare earth ion doped that experiment shows that the present invention passes through many kinds of Er/Pr/Yb/Tm/Ho/Nd, can obtain 3 mu m luminous rare earth ion doped fluorphosphate glasses, glass transparent, no crystallization, near infrared transmittivity height 3 μ m, excellent in physical and chemical performance, stability parameter Δ T 〉=150 ℃.3 very strong μ m fluorescence be can obtain down the laser diode-pumped of 980nm wavelength, the preparation and the application of 3 μ m laser glasses and fiber optic materials are applicable to.
Claims (3)
1. mu m luminous rare earth ion doped fluophosphate laser glass is characterized in that its molar percentage consists of:
Wherein: R is a rare earth element er, Tm, Ho, Nd, Pr, Yb.
2. according to claim 13 mu m luminous rare earth ion doped fluophosphate laser glass is characterized in that described rare earth ion doped mode has: Er singly mixes, Er-Pr two mixes, Er-Tm twoly mixes, Er-Nd twoly mixes, Er-Ho twoly mixes, Er-Tm-Ho three mixes, Er-Tm-Pr three mixes, Er-Yb-Pr three mixes, Er-Nd-Pr three mixes, Er-Nd-Ho three mixes.
3. the preparation method of the fluorphosphate glass of the described rare earth ion codoped of claim 1 is characterized in that this preparation method comprises the following steps:
1. selected described glass is formed and molar percentage, calculates the weight that corresponding each glass is formed, and accurately takes by weighing each raw material, mixes the formation compound;
2. compound is put into platinum crucible and melted in 1050～1120 ℃ globars electric furnace, the clarification of fusing back is 10～15 minutes fully, glass metal is cast in the mould of preheating;
3. glass is moved into rapidly and has been warming up to glass transformation temperature (T
g) in the following 10 ℃ retort furnace, be incubated 3～4 hours, reduce to room temperature with 10 ℃/hour speed again, glass sample is taken out in the cooling back fully.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183472A (en) * | 2013-03-30 | 2013-07-03 | 中国计量学院 | Erbium and terbium co-doped fluoride halide phosphate laser glass as well as preparation method and application thereof |
| CN103723919A (en) * | 2013-12-17 | 2014-04-16 | 中国科学院上海光学精密机械研究所 | Oxyfluoride glass with low hydroxyl content and preparation method of oxyfluoride glass |
| CN103820858A (en) * | 2014-02-28 | 2014-05-28 | 中国科学院福建物质结构研究所 | Er- or Ho-activated ABC3O7 type intermediate infrared ultrafast laser crystal |
| CN105293932A (en) * | 2015-11-09 | 2016-02-03 | 苏州优康通信设备有限公司 | Yb-Er co-doped fluorophosphate optical fiber preform glass and preparation method thereof |
| CN105293931A (en) * | 2015-11-09 | 2016-02-03 | 苏州优康通信设备有限公司 | Erbium-doped fluorphosphate glass optical fiber and preparation method thereof |
| CN105384340A (en) * | 2015-11-09 | 2016-03-09 | 苏州优康通信设备有限公司 | Erbium-doped fluorophosphate optical fiber preform glass and preparation method thereof |
| CN105384351A (en) * | 2015-11-09 | 2016-03-09 | 苏州优康通信设备有限公司 | Ytterbium-erbium co-doped fluorophosphate glass optical fiber and preparation method thereof |
| CN105384352A (en) * | 2015-11-09 | 2016-03-09 | 苏州优康通信设备有限公司 | Fluorophosphate cladding glass optical fiber and preparation method thereof |
| CN105601106A (en) * | 2016-01-13 | 2016-05-25 | 中国科学院上海光学精密机械研究所 | Neodymium-doped fluorophosphate glass and preparation method thereof |
| CN112028480A (en) * | 2020-09-09 | 2020-12-04 | 哈尔滨工程大学 | Preparation method of praseodymium and ytterbium co-doped fluorine-aluminum glass with 3.5-micrometer luminescence broadband |
| CN114180835A (en) * | 2021-11-08 | 2022-03-15 | 宁波大学 | Rare earth doped glass with ultra-wideband near-infrared fluorescence emission and preparation method and application thereof |
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103183472A (en) * | 2013-03-30 | 2013-07-03 | 中国计量学院 | Erbium and terbium co-doped fluoride halide phosphate laser glass as well as preparation method and application thereof |
| CN103183472B (en) * | 2013-03-30 | 2014-12-17 | 中国计量学院 | Erbium and terbium co-doped fluoride halide phosphate laser glass as well as preparation method and application thereof |
| CN103723919A (en) * | 2013-12-17 | 2014-04-16 | 中国科学院上海光学精密机械研究所 | Oxyfluoride glass with low hydroxyl content and preparation method of oxyfluoride glass |
| CN103820858A (en) * | 2014-02-28 | 2014-05-28 | 中国科学院福建物质结构研究所 | Er- or Ho-activated ABC3O7 type intermediate infrared ultrafast laser crystal |
| CN105384340A (en) * | 2015-11-09 | 2016-03-09 | 苏州优康通信设备有限公司 | Erbium-doped fluorophosphate optical fiber preform glass and preparation method thereof |
| CN105293931A (en) * | 2015-11-09 | 2016-02-03 | 苏州优康通信设备有限公司 | Erbium-doped fluorphosphate glass optical fiber and preparation method thereof |
| CN105293932A (en) * | 2015-11-09 | 2016-02-03 | 苏州优康通信设备有限公司 | Yb-Er co-doped fluorophosphate optical fiber preform glass and preparation method thereof |
| CN105384351A (en) * | 2015-11-09 | 2016-03-09 | 苏州优康通信设备有限公司 | Ytterbium-erbium co-doped fluorophosphate glass optical fiber and preparation method thereof |
| CN105384352A (en) * | 2015-11-09 | 2016-03-09 | 苏州优康通信设备有限公司 | Fluorophosphate cladding glass optical fiber and preparation method thereof |
| CN105384352B (en) * | 2015-11-09 | 2018-07-06 | 苏州优康通信设备有限公司 | A kind of fluorophosphate Caldding glass optical fiber and preparation method thereof |
| CN105601106A (en) * | 2016-01-13 | 2016-05-25 | 中国科学院上海光学精密机械研究所 | Neodymium-doped fluorophosphate glass and preparation method thereof |
| CN105601106B (en) * | 2016-01-13 | 2017-12-12 | 中国科学院上海光学精密机械研究所 | Neodymium-doped fluorphosphate glass and preparation method thereof |
| CN112028480A (en) * | 2020-09-09 | 2020-12-04 | 哈尔滨工程大学 | Preparation method of praseodymium and ytterbium co-doped fluorine-aluminum glass with 3.5-micrometer luminescence broadband |
| CN114180835A (en) * | 2021-11-08 | 2022-03-15 | 宁波大学 | Rare earth doped glass with ultra-wideband near-infrared fluorescence emission and preparation method and application thereof |
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Application publication date: 20111012 |