CN101486530A - 2-micron luminous rare earth ion-doped germanate laser glass and preparation method thereof - Google Patents
2-micron luminous rare earth ion-doped germanate laser glass and preparation method thereof Download PDFInfo
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- CN101486530A CN101486530A CNA200910046761XA CN200910046761A CN101486530A CN 101486530 A CN101486530 A CN 101486530A CN A200910046761X A CNA200910046761X A CN A200910046761XA CN 200910046761 A CN200910046761 A CN 200910046761A CN 101486530 A CN101486530 A CN 101486530A
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- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 34
- 239000000087 laser glass Substances 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 150000002910 rare earth metals Chemical class 0.000 title claims description 3
- 239000011521 glass Substances 0.000 claims abstract description 39
- 239000000835 fiber Substances 0.000 claims abstract description 7
- 229910001404 rare earth metal oxide Inorganic materials 0.000 claims abstract description 4
- 229910052797 bismuth Inorganic materials 0.000 claims description 7
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 6
- 150000001875 compounds Chemical class 0.000 claims description 6
- 238000002844 melting Methods 0.000 claims description 6
- 230000008018 melting Effects 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 239000002994 raw material Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 5
- 229910016036 BaF 2 Inorganic materials 0.000 claims description 4
- 229910005793 GeO 2 Inorganic materials 0.000 claims description 3
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 claims description 3
- 238000005273 aeration Methods 0.000 claims description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 3
- 238000005352 clarification Methods 0.000 claims description 3
- 229910001882 dioxygen Inorganic materials 0.000 claims description 3
- 230000004927 fusion Effects 0.000 claims description 3
- 238000000265 homogenisation Methods 0.000 claims description 3
- 239000004615 ingredient Substances 0.000 claims description 3
- 229910052751 metal Inorganic materials 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000001301 oxygen Substances 0.000 claims description 3
- 229910052760 oxygen Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims description 2
- 229910052731 fluorine Inorganic materials 0.000 claims description 2
- 239000011737 fluorine Substances 0.000 claims description 2
- 150000001621 bismuth Chemical class 0.000 claims 1
- 230000009466 transformation Effects 0.000 claims 1
- -1 rare earth ion Chemical class 0.000 abstract description 21
- 238000002189 fluorescence spectrum Methods 0.000 abstract description 4
- 238000012360 testing method Methods 0.000 abstract description 4
- 239000013307 optical fiber Substances 0.000 abstract description 3
- 229910052775 Thulium Inorganic materials 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract description 2
- 238000004020 luminiscence type Methods 0.000 abstract description 2
- 238000002834 transmittance Methods 0.000 abstract description 2
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 abstract 2
- 229910052689 Holmium Inorganic materials 0.000 abstract 1
- 229910052769 Ytterbium Inorganic materials 0.000 abstract 1
- 229910001632 barium fluoride Inorganic materials 0.000 abstract 1
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 abstract 1
- 229910052746 lanthanum Inorganic materials 0.000 abstract 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 6
- 238000005086 pumping Methods 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000007704 transition Effects 0.000 description 3
- 206010070834 Sensitisation Diseases 0.000 description 2
- 239000000382 optic material Substances 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 230000008313 sensitization Effects 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 229910004379 HoF 3 Inorganic materials 0.000 description 1
- 229910017768 LaF 3 Inorganic materials 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000002419 bulk glass Substances 0.000 description 1
- 238000005253 cladding Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000005357 flat glass Substances 0.000 description 1
- 239000003365 glass fiber Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 238000001356 surgical procedure Methods 0.000 description 1
- FRNOGLGSGLTDKL-UHFFFAOYSA-N thulium atom Chemical compound [Tm] FRNOGLGSGLTDKL-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
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Abstract
A2 μm luminous rare earth ion doped germanate laser glass and a preparation method thereof are disclosed, wherein the glass comprises the following components in percentage by mol: GeO2：60～65％，BaF2：15～20％，Ga2O3：2～13％，Re2O3/ReF3: 2-13%, wherein Re is rare earth elements La, Yb, Tm and Ho. The rare earth ion doping mode of the glass is as follows: tm single doping, Yb-Tm double doping, Yb-Ho double doping, Tm-Ho double doping or Yb-Tm-Ho triple doping, and rare earth ions are introduced by rare earth oxides or rare earth fluorides, so that the glass with stability and excellent luminescence property can be obtained. Experimental results show that the germanate glass has high transmittance and wide transmission range. Fluorescence spectrum tests show that the germanate laser glass can obtain good fluorescence emission close to 2 mu m. The laser glass of the invention is also suitable for preparing the fiber core of the 2 mu m optical fiber preform.
Description
Technical field
The present invention relates to bismuth germanate glass, particularly a kind of 2 mu m luminous rare earth ion doped germanate laser glass and preparation method thereof.
Background technology
For wavelength is the mid-infrared laser of 2 μ m, in fields such as medical surgery operation, optical communication, gas-monitoring, environmental pollution check and analysis and eye-safe lidars and the pumping source that is used for new middle-infrared band laser all have important application.Tm
3+And Ho
3+Obtained a large amount of research as the active ions of laser in the various different substrates in 2 μ m zone.Doping Tm
3+And Ho
3+The ionic optical fiber laser is the strong candidate as the all-solid state laser source of compact efficient.
Employing along with high power semiconductor lasers and cladding pumping mode, the performance of thulium-doped fiber laser also is greatly improved (referring to technology formerly: Jianfeng Wu, Zhidong Yao, Jie Zong et al.Highlyefficient high-power thulium doped germinate glass fiber laser, Opt.Lett., 2007,32 (6): 638-640.).Another noticeable rare earth ion is Ho
3+, very special advantages is arranged at medical laser device and lidar field.To Ho
3+Because the metastable state life-span is very long, is suitable for making pulsed laser.Ho
3+The subject matter that the doped fiber laser apparatus exists then is to lack effective pumping source.In order better to improve Ho
3+The laser activity of 2 μ m generally adopts the mode of ion co-doped with sensitized to improve its luminescent properties.The most common a kind of sensitization mode is to pass through Tm
3+Sensitization Ho
3+Realize 2 mu m luminous (referring to technology: Dong Shufu formerly, Chen Guofu, Wang Xianhua etc. " Tm
3+: Ho
3+Mix the experimental study of silica fibre laser apparatus altogether ", photon journal, 2004,33 (2): 129-132.).Utilize commercial laser pumping source in order further to expand, the researchist also attempts adopting Yb/Tm/Ho three doping way to realize that 2 is mu m luminous, and many useful results have been obtained (referring to technology formerly: Bo Peng, TetsuroIzumitani.Optical properties, fluorescence mechanisms and energy transfer in Tm
3+, Ho
3+And Tm
3+-Ho
3+Doped near-infrared laser glasses, sensitized by Yb
3+, Opt.Mater., 1995,4:797-810.).
At quartz substrate middle-weight rare earths ionic radiationless transition meeting restriction lasing efficiency, the luminosity of therefore studying the glass matrix with low phonon energy is significant.Bismuth germanate glass has relatively low phonon energy, and becomes glass properties good, is suitable for preparing preform and drawing optical fiber.Traditional bismuth germanate glass component all is that oxide compound constitutes, by introduce the effect that extra-network ion and rare earth ion can play minimizing glass internal hydroxyl groups to a certain extent with the form of fluorochemical.Therefore it is very necessary exploring suitable glass ingredient and analyze effective rare earth ion sensitized luminescence mode.
Summary of the invention
The invention provides a kind of 2 mu m luminous rare earth ion doped germanate laser glass and preparation method thereof.This glass has good one-tenth glass properties, infrared transmission performance and good luminosity, is applicable to the preparation and the application of rare-earth-ion-doped extraordinary laser glass of 2 μ m and fiber optic materials.
The concrete technical solution of the present invention is as follows:
A kind of 2 mu m luminous rare earth ion doped bismuth germanate glasses and preparation method thereof is characterized in that extra-network ion is with BaF
2Introduce, several rare earth ions can Tm be singly mixed, Yb-Tm twoly mixes, Yb-Ho twoly mixes, Tm-Ho twoly mixes, Yb-Tm-Ho three modes of mixing are introduced in the glass, and the introducing mode of rare earth ion is mixed the component China and foreign countries divided by rare earth oxide and can also the rare earth fluorine mode be introduced in the glass ingredient.
Described 2 mu m luminous rare earth ion doped germanate laser glass, its characteristics are that its compositing range is as follows:
Form mol%
GeO
2 65～70
BaF
2 15～20
Ga
2O
3 2～13
Re
2O
3/ ReF
3, Re=La/Yb/Tm/Ho rare earth element wherein, 2～13
A kind of preparation method of 2 mu m luminous rare earth ion doped bismuth germanate glasses may further comprise the steps:
1. the molar percentage of forming by above-mentioned glass (mol%) calculates weight of glass per-cent, takes by weighing raw material then, mixes the formation compound;
2. described compound is put into platinum crucible, place 1350～1400 ℃ silicon carbon rod electric furnace fusion, melting time was controlled at 45～60 minutes;
3. behind the glass melting, be cooled to 1300 ℃, feed high purity oxygen gas and dewater, what of raw material aeration time be decided by;
4. stop logical oxygen, glass metal is warmed up to 1450 ℃ carries out clarification and homogenization, be cooled to 1400 ℃ and stir, a straight-through pure oxygen carries out atmosphere protection in this process;
5. fast glass is put into the retort furnace that is warming up to transition temperature (Tg), is incubated after 2 hours, be annealed to 380～420 ℃ with 10 ℃/hour speed,, and then be annealed to 80 ℃ with 20 ℃/hour speed, close retort furnace, be cooled to room temperature.
Technique effect of the present invention
2 mu m luminous rare earth ion doped germanate laser glass of the present invention's preparation have the very wide scope that sees through in middle-infrared band.
The present invention's 2 mu m luminous rare earth ion doped germanate laser glass can obtain excellent luminosity, can potentially be applied to prepare polycomponent laser bulk glass and the fiber optic materials of realizing 2 μ m laser.
Description of drawings
Fig. 1 is the infrared transmittivity of the present invention 2 mu m luminous rare earth ion doped germanate laser glass embodiment 1, and thickness of sample is 2mm.
Fig. 2 is 2 μ m fluorescence spectrum figure of the embodiment of the invention 1.
Embodiment
Table 1 has provided glass formula and the partial test result of 10 embodiment of the present invention.
Table 1: the glass formula of concrete 10 embodiment
| Component (mol%) | 1# | 2# | 3# | 4# | 5# | 6# | 7# | 8# | 9# | 10# |
| GeO 2 | 65 | 70 | 65 | 70 | 65 | 65 | 65 | 65 | 65 | 65 |
| BaF 2 | 20 | 15 | 20 | 15 | 20 | 20 | 20 | 20 | 20 | 20 |
| Ga 2O 3 | 2 | 2 | 2 | 6 | 6 | 13 | 9 | 6 | 6 | 4 |
| La 2O 3 | 5 | 5 | 3 | 6 | ||||||
| LaF 3 | 5 | 5 | 5 | 5 | ||||||
| Yb 2O 3 | 6 | 6 | 3 | 4 | 3 | 3 | ||||
| YbF 3 | 6 | |||||||||
| Tm 2O 3 | 1 | 1 | 2 | 1 | ||||||
| TmF 3 | 1 | 2 | 4 | 1 | 4 | |||||
| Ho 2O 3 | 1 | 1 | 1 | |||||||
| HoF 3 | 1 | 1 | 1 | 1 | 1 | |||||
| Pumping wavelength (nm) | 980 | 980 | 980 | 980 | 980 | 808 | 808 | 980 | 980 | 808 |
| Peak luminous wavelength (μ m) | ～2 | ～2 | ～2 | ～2 | ～2 | ～2 | ～1.8 | ～1.8 | ～2 | ～2 |
| Luminous intensity | High | High | High | In | In | Difference | High | Difference | Difference | High |
Embodiment 1 to embodiment 10, all adopts identical glass smelting technology, and its concrete preparation process is as follows:
1. the molar percentage of forming by the glass of embodiment (mol%) calculates weight of glass per-cent, takes by weighing raw material then, mixes;
2. compound is put into platinum crucible, place 1350～1400 ℃ silicon carbon rod electric furnace fusion, melting time was controlled at 45～60 minutes;
3. behind the glass melting, be cooled to 1300 ℃, feed high purity oxygen gas and dewater, what of raw material aeration time be decided by;
4. stop logical oxygen, glass metal is warmed up to 1450 ℃ carries out clarification and homogenization, be cooled to 1400 ℃ and stir.A straight-through pure oxygen carries out atmosphere protection in this process.
5. fast glass is put into and be warming up to transition temperature (T
g) retort furnace in, be incubated 2 hours, be annealed to 380～420 ℃ with 10 ℃/hour speed, and then after being annealed to 80 ℃ with 20 ℃/hour speed, close retort furnace, be cooled to room temperature.
Sample after the annealing is processed into the thick sheet glass of 2mm of six mirror polish, test infrared permeation spectrum and nearly 2 μ m fluorescence.Experimental result shows that the present invention's 2 mu m luminous rare earth ion doped germanate laser glass have higher transmittance and the very wide scope that sees through.Adopt the fluorescence spectrum of 808nm laser diode LD and 980nmLD pumping specimen respectively, described in the fluorescence intensity result such as table 1 of test.Fig. 1 is the infrared transmittivity of the present invention 2 mu m luminous rare earth ion doped germanate laser glass embodiment 1, and thickness of sample is 2mm.Fig. 2 is 2 μ m fluorescence spectrum figure of the embodiment of the invention 1.Adopt the bismuth germanate glass of the multiple doping way of multiple rare earth ion can obtain good nearly 2 μ m fluorescent emission among the present invention.
Claims (5)
1, a kind of 2 mu m luminous rare earth ion doped germanate laser glass is characterized in that its molar percentage consists of:
Form mol%
GeO
2 65～70
BaF
2 15～20
Ga
2O
3 2～13
Re
2O
3/ ReF
32～13, Re=La/Yb/Tm/Ho rare earth element wherein.
2, the preparation method of described 2 mu m luminous rare earth ion doped germanate laser glass of claim 1 is characterized in that this method comprises the following steps:
Molar percentage 1. selected and that form by the described glass of claim 1 calculates weight of glass per-cent, takes by weighing raw material then, mixes the formation compound;
2. compound is put into platinum crucible, place 1350～1400 ℃ silicon carbon rod electric furnace fusion, melting time was controlled at 45～60 minutes;
3. behind the glass melting, be cooled to 1300 ℃, feed high purity oxygen gas and dewater, what of raw material aeration time be decided by;
4. stop logical oxygen, glass metal is warmed up to 1450 ℃ carries out clarification and homogenization, be cooled to 1400 ℃ and stir, a straight-through pure oxygen carries out atmosphere protection in this process;
5. fast glass is put into the retort furnace that is warming up to this glass transformation temperature, be incubated after 2 hours, be annealed to 380～420 ℃ with 10 ℃/hour speed, and then be annealed to 80 ℃, close retort furnace, be cooled to room temperature with 20 ℃/hour speed.
3, the preparation method of 2 mu m luminous rare earth ion doped germanate laser glass according to claim 2 is characterized in that the introducing mode of described rare earth element: Tm singly mixes, Yb-Tm twoly mixes, Yb-Ho twoly mixes, Tm-Ho is two mixes or Yb-Tm-Ho three mixes.
4, the preparation method of 2 mu m luminous rare earth ion doped germanate laser glass according to claim 2 is characterized in that described rare earth element is with in rare earth oxide or the rare earth fluorine introducing glass ingredient.
5,2 mu m luminous rare earth ion doped germanate laser glass according to claim 1 is characterized in that this bismuth germanate glass is applicable to the preparation of 2 μ m laser fiber preform core.
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|---|---|---|---|
| CNA200910046761XA CN101486530A (en) | 2009-02-27 | 2009-02-27 | 2-micron luminous rare earth ion-doped germanate laser glass and preparation method thereof |
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|---|---|---|---|
| CNA200910046761XA CN101486530A (en) | 2009-02-27 | 2009-02-27 | 2-micron luminous rare earth ion-doped germanate laser glass and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN101486530A true CN101486530A (en) | 2009-07-22 |
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|---|---|---|---|
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| CN102211873A (en) * | 2011-03-23 | 2011-10-12 | 中国科学院上海光学精密机械研究所 | 3-micron luminescent rare earth ion-doped fluorogermanate laser glass and preparation method thereof |
| CN103230601A (en) * | 2013-04-16 | 2013-08-07 | 浙江大学 | Rare earth doped gallium oxide drug-loading body preparation method |
| CN104140203A (en) * | 2014-07-10 | 2014-11-12 | 中国科学院上海光学精密机械研究所 | Germanate glass for 2micron laser output, and preparation method thereof |
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