CN103241948B - Method for preparing oxygen fluorine chlorine tellurate glass with intermediate infrared fluorescence output at 4 mu m - Google Patents

Method for preparing oxygen fluorine chlorine tellurate glass with intermediate infrared fluorescence output at 4 mu m Download PDF

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CN103241948B
CN103241948B CN201310153356.4A CN201310153356A CN103241948B CN 103241948 B CN103241948 B CN 103241948B CN 201310153356 A CN201310153356 A CN 201310153356A CN 103241948 B CN103241948 B CN 103241948B
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glass
doping
fluorine chlorine
oxygen fluorine
tellurate
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CN103241948A (en
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戎亮
林健
任军江
张文俊
贾玉洁
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CETC 23 Research Institute
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Abstract

The invention relates to the technical field of intermediate infrared rare earth doped luminescent glass application, and aims at solving the technical problem of providing a method for preparing oxygen fluorine chlorine tellurate glass with intermediate infrared fluorescence output at 4 mu m. The glass is good in glass forming property, high in infrared light transmission rate, good in luminescence property and beneficial to output of fluorescence and laser of 4 mu m. The oxygen fluorine chlorine tellurate glass prepared by using a fusion method is tellurate glass which contains zinc fluoride and zinc chloride, and due to the appropriate amount of contains zinc fluoride and zinc chloride, the hydroxyl content and the phonon energy in the system are greatly reduced, so that the forming capability of the glass is effectively improved, the doping amount of rare earth ions is increased, and the fluorescence service lives of the rare earth ions are prolonged. By adopting the doping amount of the external doping rare earth ions, namely, Ho<3+> and Yb<3+>, the pumping efficiency of 980nm is greatly improved, and tests show that the oxygen fluorine chlorine tellurate glass has remarkable fluorescence output at 4 mu m.

Description

There is the oxygen fluorine chlorine tellurate glass implementation method that in 4 μm, Infrared fluorescence exports
Technical field
Infrared rare earth doped luminescent glass applied technical field in the present invention relates to.
Technical background
4 μm of mid-infrared fiber lasers, because of its special output wavelength and good beam quality, have a wide range of applications in fields such as military affairs, atmospheric communication, biologic medicals.Rare earth ion doped crystalline material can realize the output of mid-infrared laser, as in all solid state laser that works at normal temperatures, and Pr 3+: LaCl 3(phonon energy is about 210cm to crystal -1) pulse laser that most long wavelength is 7.24 μm can be sent, but this crystal very easily deliquescence.4 μm of laser apparatus need glass host material to have low phonon energy.At present, fluorochemical and chalcogenide glass is mainly contained for rare earth ion doped low phonon energy glass material system.In all optical fiber lasers, only have fluoride fiber to achieve wavelength and be greater than 3 μm of mid-infrared lasers outputs, and need could realize in the cooling condition.Fluoride glass fiber can support the laser generation of 3.9-4.5 mum wavelength, but is not widely used because of its poor stability.Chalcogenide glass has lower phonon energy than fluoride glass, also can at middle infrared wavelength place Emission Lasers, but the problem that the same existence and stability of this kind of material is poor, is difficult to prepare large size and can the mid-infrared laser material of steady operation.By contrast, oxide glass preparation technology is simple, have good physical and mechanical properties, and has good chemical stability, and therefore, the rear-earth-doped oxide glass system finding Infrared fluorescence or laser in a kind of can transmitting becomes an inevitable choice.The Tellurite Glasses belongs to a kind of heavy metal oxide glass, and (maximum phonon energy is about 750cm to have comparatively low phonon energy -1), there is wider infrared light transmission scope (until 6 mum wavelengths), more excellent optical property (having extremely low optical loss from wavelength 0.4 ~ 5.5 μm), lower glass melting temperature, high dielectric constant, large emission cross section, higher specific refractory power (about 2.0) and comparatively high non-linearity specific refractory power, the advantage such as solubilize rare earth ions is good, thermostability is better.
U.S. patent Nos US7551348B2 discloses a kind of tellurate glass for optical waveguides and light amplification field, 25 ~ 90%TeO 2, 1 ~ 40%WO 3, 1 ~ 55%MoO 3, 0 ~ 35%ZnO, 0 ~ 20%Bi 2o 3, 0 ~ 35%Li 2o/Na 2o/K 2o, this glass has good light wide-band amplify effect at 1.5 μm of near infrareds.
Chinese invention patent CN1803686A discloses a kind of erbium-doped tellurate glass and the preparation method with high IR pumping efficiency.Utilize multi-phonon relaxation principle, introducing phonon in glass can about 1200cm -1p 2o 5, keep that 1.5 μm of quantum yielies of launching are impregnable increases substantially fluorescence intensity simultaneously.
Chinese invention patent CN101224947A discloses a kind of oxyhalide tellurite glass of 2 mu m waveband luminescences.Maximum phonon can lower than 760cm -1, Δ T (thermostability parameter) higher than 100 DEG C, glass forming ability and water resistance good.
Chinese invention patent CN1686885A discloses a kind of sulphur tellurate glass for fiber amplifier field.This glass has higher stability, can drawing optic fibre, has larger small-signal gain and larger amplified broad band.
Above reported be all the tellurate glass of 1.5 ~ 2 mu m waveband luminescences, and have no report at the tellurate glass of 3 ~ 5 mu m waveband luminescences.Therefore, when keeping phonon energy low and thermostability is good, the tellurate glass that exploitation long wave 4 μm is launched has important using value.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of implementation method with the oxygen fluorine chlorine tellurate glass that Infrared fluorescence exports in 4 μm, and this glass glass forming ability is good, infrared transmittivity is high, good luminous performance, be conducive to the output realizing 4 μm of fluorescence and laser.
For solving the problems of the technologies described above, technical solution of the present invention is:
There is an implementation method for the oxygen fluorine chlorine tellurate glass that Infrared fluorescence exports in 4 μm, it is characterized in that:
The component of described oxygen fluorine chlorine tellurate glass is as follows:
Outer doping: Holmium trioxide+holmium fluoride and Ho 2o 3+ HoF 3doping is the 0.02mol% ~ 0.25mol% of aforementioned basic raw material composition;
Outer doping: ytterbium oxide+fluoridize ytterbium and Yb 2o 3+ YbF 3doping is the 0.5mol% ~ 3mol% of aforementioned basic raw material composition;
Making step is as follows:
Step one: clayed into power by the material of above-mentioned whole glass component, fully to mix material powder in its ratio and is placed on the dry 5h of loft drier;
Step 2: loaded in the gold crucible of adding a cover by above-mentioned compound, and be placed in electric furnace melting, atmosphere is air, melt temperature is 760 DEG C ~ 900 DEG C, and melting time is 15 ~ 20min;
Step 3: melts step 2 obtained is cast on the copper coin of 250 ~ 280 DEG C or stainless punching block shaping, the 2h that then anneals at 260 DEG C of temperature to eliminate internal stress, furnace cooling afterwards.
The present invention can bring following beneficial effect:
The oxygen fluorine chlorine tellurate glass of the present invention's design is a kind of tellurate glass containing zinc fluoride and zinc chloride, appropriate zinc fluoride and zinc chloride can make the hydroxy radical content in system and phonon significantly to reduce, thus effectively improve the Forming ability of glass, improve rare earth ion doping in glass, and improve the fluorescence lifetime of rare earth ion.The oxygen fluorine chlorine tellurate glass adopting the present invention to be prepared by scorification has good thermostability, does not occur crystallization, can meet drawing process requirement prepared by optical fiber in the moulding process of glass.By adjusting outer doping with rare-earth ions Ho 3+, Yb 3+doping, can significantly improve the pumping efficiency of 980nm, show after tested, this kind of oxygen fluorine chlorine tellurate glass has obvious fluorescence and exports at 4 μm of places.
Accompanying drawing explanation
Fig. 1 is Infrared fluorescence spectrogram under 980nm laser pumping 4 μm of 7 groups of embodiments of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the present invention is described in further detail.
Table 1 is basic raw material composition (mol%) of glass of the present invention.
Table 1
TeO 2 50～80
WO 3 5～10
GeO 2 0～5
ZnO 5～20
ZnF 2+ZnCl 2 10～20
Ho 2o 3+ HoF 3and Yb 2o 3+ YbF 3introduced by the form of outer doping.Wherein Ho 2o 3+ HoF 3doping be above-mentioned basic raw material composition 0.02mol% ~ 0.25mol%, Yb 2o 3+ YbF 3doping be above-mentioned basic raw material composition 0.5mol% ~ 3mol%.
Table 2 lists Infrared fluorescence in the present invention 4 μm and exports the formula of oxygen fluorine chlorine tellurate glass 7 groups of specific embodiments.
Table 2
Fig. 1 is Infrared fluorescence spectrogram under 980nm laser pumping 4 μm of 7 groups of embodiments of the present invention; Wherein, rare earth Ho 2o 3, HoF 3, Yb 2o 3, YbF 3the form of doping (mol%) beyond doping is all introduced in formula.
Embodiment 1:
Whole components of glass are: TeO 2: 80mol%, WO 3: 5mol%, ZnO:5mol%, ZnCl 2: 10mol%, Ho 2o3:0.02mol%, Yb 2o 3: 0.5mol%, its middle-weight rare earths Ho 2o 3, Yb 2o 3the form of doping is all introduced, according to formula accurate calculation, weighing, mixing.Loaded in the gold crucible of adding a cover by above-mentioned compound, and be placed in electric furnace melting, atmosphere is air, and melt temperature is 760 ~ 900 DEG C, and melting time is 15 ~ 20min; Glass metal is poured on the copper coin of 250 ~ 280 DEG C or stainless punching block shaping, then at 260 DEG C of annealing 2h to eliminate internal stress, furnace cooling afterwards.Thermostability parameter Δ T (DEG C) of sample prepared by embodiment 1 reaches 102 DEG C, and glass glass forming ability is good, and fluorescence spectrum is shown in Fig. 1.
Embodiment 2:
Whole components of glass are: TeO 2: 75mol%, WO 3: 5mol%, GeO 2: 5mol%, ZnO:5mol%, ZnF 2: 10mol%, Ho 2o 3: 0.02mol%, HoF 3: 0.02mol%, Yb 2o 3: 0.25mol%, YbF 3: 0.25mol%, its middle-weight rare earths Ho 2o 3, HoF 3, Yb 2o 3, YbF 3the form of doping is all introduced, according to formula accurate calculation, weighing, mixing.Loaded in the gold crucible of adding a cover by above-mentioned compound, and be placed in electric furnace melting, atmosphere is air, and melt temperature is 760 ~ 900 DEG C, and melting time is 15 ~ 20min; Glass metal is poured on the copper coin of 250 ~ 280 DEG C or stainless punching block shaping, then at 260 DEG C of annealing 2h to eliminate internal stress, furnace cooling afterwards.Thermostability parameter Δ T (DEG C) of sample prepared by embodiment 2 reaches 105 DEG C, and glass glass forming ability is good, and fluorescence spectrum is shown in Fig. 1.
Embodiment 3:
Whole components of glass are: TeO 2: 70mol%, WO 3: 10mol%, ZnO:5mol%, ZnF 2: 10mol%, ZnCl 2: 5mol%, HoF 3: 0.1mol%, YbF 3: 1.5mol%, its middle-weight rare earths HoF 3, YbF 3the form of doping is all introduced, according to formula accurate calculation, weighing, mixing.Loaded in the gold crucible of adding a cover by above-mentioned compound, and be placed in electric furnace melting, atmosphere is air, and melt temperature is 760 ~ 900 DEG C, and melting time is 15 ~ 20min; Glass metal is poured on the copper coin of 250 ~ 280 DEG C or stainless punching block shaping, then at 260 DEG C of annealing 2h to eliminate internal stress, furnace cooling afterwards.Thermostability parameter Δ T (DEG C) of sample prepared by embodiment 3 reaches 110 DEG C, and glass glass forming ability is good, and fluorescence spectrum is shown in Fig. 1.
Embodiment 4:
Whole components of glass are: TeO 2: 65mol%, WO 3: 7mol%, GeO 2: 3mol%, ZnO:10mol%, ZnF 2: 10mol%, ZnCl 2: 5mol%, Ho 2o 3: 0.04mol%, HoF 3: 0.08mol%, Yb 2o 3: 0.5mol%, YbF 3: 1.5mol%, its middle-weight rare earths Ho 2o 3, HoF 3, Yb 2o 3, YbF 3the form of doping is all introduced, according to formula accurate calculation, weighing, mixing.Loaded in the gold crucible of adding a cover by above-mentioned compound, and be placed in electric furnace melting, atmosphere is air, and melt temperature is 760 ~ 900 DEG C, and melting time is 15 ~ 20min; Glass metal is poured on the copper coin of 250 ~ 280 DEG C or stainless punching block shaping, then at 260 DEG C of annealing 2h to eliminate internal stress, furnace cooling afterwards.Thermostability parameter Δ T (DEG C) of sample prepared by embodiment 4 reaches 108 DEG C, and glass glass forming ability is good, and fluorescence spectrum is shown in Fig. 1.
Embodiment 5:
Whole components of glass are: TeO 2: 60mol%, WO 3: 10mol%, GeO 2: 5mol%, ZnO:10mol%, ZnF 2: 5mol%, ZnCl 2: 10mol%, Ho 2o 3: 0.1mol%, HoF 3: 0.1mol%, Yb 2o 3: 1mol%, YbF 3: 1.5mol%, its middle-weight rare earths Ho 2o 3, HoF 3, Yb 2o 3, YbF 3the form of doping is all introduced, according to formula accurate calculation, weighing, mixing.Loaded in the gold crucible of adding a cover by above-mentioned compound, and be placed in electric furnace melting, atmosphere is air, and melt temperature is 760 ~ 900 DEG C, and melting time is 15 ~ 20min; Glass metal is poured on the copper coin of 250 ~ 280 DEG C or stainless punching block shaping, then at 260 DEG C of annealing 2h to eliminate internal stress, furnace cooling afterwards.Thermostability parameter Δ T (DEG C) of sample prepared by embodiment 5 reaches 113 DEG C, and glass glass forming ability is good, and fluorescence spectrum is shown in Fig. 1.
Embodiment 6:
Whole components of glass are: TeO 2: 55mol%, WO 3: 10mol%, GeO 2: 5mol%, ZnO:15mol%, ZnF 2: 5mol%, ZnCl 2: 10mol%, Ho 2o 3: 0.05mol%, HoF 3: 0.2mol%, Yb 2o 3: 0.5mol%, YbF 3: 2mol%, its middle-weight rare earths Ho 2o 3, HoF 3, Yb 2o 3, YbF 3the form of doping is all introduced, according to formula accurate calculation, weighing, mixing.Loaded in the gold crucible of adding a cover by above-mentioned compound, and be placed in electric furnace melting, atmosphere is air, and melt temperature is 760 ~ 900 DEG C, and melting time is 15 ~ 20min; Glass metal is poured on the copper coin of 250 ~ 280 DEG C or stainless punching block shaping, then at 260 DEG C of annealing 2h to eliminate internal stress, furnace cooling afterwards.Thermostability parameter Δ T (DEG C) of sample prepared by embodiment 6 reaches 112 DEG C, and glass glass forming ability is good, and fluorescence spectrum is shown in Fig. 1.
Embodiment 7:
Whole components of glass are: TeO 2: 50mol%, WO 3: 10mol%, ZnO:20mol%, ZnF 2: 10mol%, ZnCl 2: 10mol%, Ho 2o 3: 0.05mol%, HoF 3: 0.2mol%, Yb 2o 3: 0.5mol%, YbF 3: 2.5mol%, its middle-weight rare earths Ho 2o 3, HoF 3, Yb 2o 3, YbF 3the form of doping is all introduced, according to formula accurate calculation, weighing, mixing.Loaded in the gold crucible of adding a cover by above-mentioned compound, and be placed in electric furnace melting, atmosphere is air, and melt temperature is 760 ~ 900 DEG C, and melting time is 15 ~ 20min; Glass metal is poured on the copper coin of 250 ~ 280 DEG C or stainless punching block shaping, then at 260 DEG C of annealing 2h to eliminate internal stress, furnace cooling afterwards.Thermostability parameter Δ T (DEG C) of sample prepared by embodiment 1 reaches 115 DEG C, and glass glass forming ability is good, and fluorescence spectrum is shown in Fig. 1.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.

Claims (1)

1. there is an implementation method for the oxygen fluorine chlorine tellurate glass that Infrared fluorescence exports in 4 μm, it is characterized in that:
The component of described oxygen fluorine chlorine tellurate glass is as follows:
Outer doping: Holmium trioxide+holmium fluoride and Ho 2o 3+ HoF 3doping is the 0.02mol% ~ 0.25mol% of aforementioned basic raw material composition;
Outer doping: ytterbium oxide+fluoridize ytterbium and Yb 2o 3+ YbF 3doping is the 0.5mol% ~ 3mol% of aforementioned basic raw material composition;
Making step is as follows:
Step one: clayed into power by the material of above-mentioned whole glass component, fully to mix material powder in its ratio and is placed on the dry 5h of loft drier;
Step 2: loaded in the gold crucible of adding a cover by above-mentioned compound, and be placed in electric furnace melting, atmosphere is air, melt temperature is 760 DEG C ~ 900 DEG C, and melting time is 15 ~ 20min;
Step 3: melts step 2 obtained is cast on the copper coin of 250 ~ 280 DEG C or stainless punching block shaping, the 2h that then anneals at 260 DEG C of temperature to eliminate internal stress, furnace cooling afterwards.
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CN106186679A (en) * 2016-07-06 2016-12-07 中国计量大学 Er ions mid-infrared luminescence fluorine chlorine phosphorus glass and preparation method thereof
CN107601857B (en) * 2017-09-29 2019-11-26 中国计量大学 One kind mixing infrared glass and preparation method thereof in thulium tellurium germanate
CN107640893B (en) * 2017-09-29 2019-11-26 中国计量大学 Infrared tellurium germanate glass and preparation method in a kind of high er-doped
CN110272206B (en) * 2018-03-14 2022-03-04 湘潭大学 Application of zinc fluoride, zinc fluoride/tellurate glass with medium-infrared wide transmission waveband and preparation thereof
CN108587627B (en) * 2018-06-01 2020-03-17 苏州大学 Eu3+Ion-activated bismuth fluorochlorotelluroate and preparation method and application thereof
CN109678334B (en) * 2019-01-24 2020-06-12 中国科学院西安光学精密机械研究所 Multi-core composite material optical fiber with chalcogenide glass core layer/tellurate glass cladding layer and preparation method thereof
CN112110648B (en) * 2020-09-23 2022-12-30 中国计量大学 Holmium-ytterbium co-doped oxyhalide system mid-infrared glass and preparation method thereof

Citations (2)

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CN101224947A (en) * 2008-02-04 2008-07-23 中国科学院上海光学精密机械研究所 2mum band light-emitting oxyhalide tellurite glasses
CN101239783A (en) * 2008-03-12 2008-08-13 中国科学院上海光学精密机械研究所 Rear earth doping oxygen-fluorine tellurate microcrystalline glass and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101224947A (en) * 2008-02-04 2008-07-23 中国科学院上海光学精密机械研究所 2mum band light-emitting oxyhalide tellurite glasses
CN101239783A (en) * 2008-03-12 2008-08-13 中国科学院上海光学精密机械研究所 Rear earth doping oxygen-fluorine tellurate microcrystalline glass and preparation method thereof

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