CN100513339C - Rare earth doped gallium germanium bismuth lead luminous glass material and its preparation method and uses - Google Patents

Rare earth doped gallium germanium bismuth lead luminous glass material and its preparation method and uses Download PDF

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CN100513339C
CN100513339C CNB2006100335138A CN200610033513A CN100513339C CN 100513339 C CN100513339 C CN 100513339C CN B2006100335138 A CNB2006100335138 A CN B2006100335138A CN 200610033513 A CN200610033513 A CN 200610033513A CN 100513339 C CN100513339 C CN 100513339C
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glass
rare earth
preparation
molfraction
lead
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CN1807310A (en
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张勤远
杨钢锋
石冬梅
姜中宏
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South China University of Technology SCUT
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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
    • C03C3/23—Silica-free oxide glass compositions containing halogen and at least one oxide, e.g. oxide of boron
    • 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
    • C03C3/253—Silica-free oxide glass compositions containing germanium

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
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  • Glass Compositions (AREA)

Abstract

The disclosed Ga-Ge-Bi-Pb fluorescent glass material doped with rare earth is prepared by: mixing and fusing the Ga2O3, Bi2O3, GeO2, lead-contained compound and rare earth compound to obtain the fused glass liquor; clearing and pouring the liquor into the mold to obtain the glass; putting the glass rapidly into a muffle furnace with temperature as the glass transformation temperature for heat preservation; finally, cooling to room temperature. This product can be manufactured into different shape, and has wide application as the gain medium.

Description

Rare earth doped gallium germanium bismuth lead luminous glass material and its production and application
Technical field
The present invention relates to a kind of luminous glass material, particularly a kind of rare earth doped gallium germanium bismuth lead luminous glass material.
The invention still further relates to the preparation method of above-mentioned luminous glass material.
The invention still further relates to the application of above-mentioned luminous glass material.
Background technology
What dense wave division multipurpose (DWDM) technology and broad band amplifier combined at present is the trend of optical communication development.(1530-1565nm) have only covered the part of the low loss window of quartzy single-mode fiber, have limited the number of channel that can utilize transmission wavelength to be used for the amplification wave band of er-doped silica-based optical fiber amplifier (EDFA) of wavelength-division multiplex (WDM) technical transmission system now.Therefore, searching has the direction that bandwidth is wide, gain height and thermostability and the good er-doped host glass of machining property are still people's effort at 1.5 mu m wavebands; On the other hand, (1450～1650nm), the 1.47 mu m waveband fiber amplifiers (TDFA) of mixing thulium become another target that people pay close attention to for the low loss window that makes full use of silica-based optical fiber.How to select suitable substrate material to become the focus of research once again with the luminosity that improves 1.47 μ m.There is huge economic and social benefit in the research in above-mentioned field for, high capacity communication long-range in order to satisfy and seek the common carrier of the fiber amplifier substrate material that loss is low, function is strong, performance is high and can be highly integrated.In addition, along with technology rapid development such as information processing, data storage, underwater communication, video demonstration and surface treatments, demand to high-level efficiency, low price, high performance visible wavelength Laser Devices is more and more urgent, can significantly improve the print speed and the resolving power of existing laser printer as the bluish-green laser device.In addition, the bluish-green laser device also demonstrates its huge commerce and Military Application prospect at aspects such as optical communication, Fibre Optical Sensor and laser medicines.In addition, prior art also has urgent demand to some special wave band luminous, as 2.0 mu m wavebands are luminous extremely important using value is arranged in medical diagnosis.
As seen the different rare earth ion that mixes in various substrate materials can realize-near-infrared band luminous, and the host glass material that is used for above-mentioned luminescent device device in the prior art has: conventional oxide glass, fluoride glass, chalcogenide glass, chloride glass etc.In these glass, the substrate material that is used for up-conversion luminescence and 1.47 mu m waveband light-emitting devices is fluoride glass normally.But fluoride glass is its chemical stability and bad mechanical strength as rare-earth doped optical fibre substrate material disadvantage, and because easily crystallization and more difficult drawing optical fiber, this has limited its application greatly.And chemical stability and physical strength all preferably conventional oxide glass be difficult to obtain high efficiency up-conversion luminescence, in addition Tm because the phonon energy height 3+Ion in the glass of high phonon energy because the influence of multi-phonon relaxation and difficultly observe the luminous of 1.47 mu m wavebands.In addition,, compare, also have bigger gap with nonoxide glass though the up-conversion luminescence efficient of rare earth ion in tellurate glass is higher than conventional oxide glass such as borate, silicate and phosphoric acid salt far away; The anti-crystallization stability of tellurate glass is relatively poor in addition, in fiber draw process, be easy to generate crystallization and make it be difficult to obtain practicability [referring to U.S.patent 6356387, date of publication on March 12nd, 2002, name is called TELLURITE GLASS, OPTICAL AMPLIFIER, AND LIGHTSOURCE].
Compare with above-mentioned glass system, do not contain the Ga of any conventional oxide glass-former 2O 3-Bi 2O 3-PbO glass has just caused the great interest of people since finding.This glass system contains germanium oxide, plumbous oxide, bismuth oxide, two or more heavy metal oxide such as gallium oxide has high specific refractory power, good mechanical properties, good thermostability, high chemical stability and splendid infrared transmission scope excellent properties such as (～8 μ m).The phonon energy of heavy metal oxide glass is lower and specific refractory power is higher, and this helps improving the luminous efficiency and the emission cross section of doping with rare-earth ions, is suitable as the substrate material of solid statelaser and amplifier.Compare with chalcogenide glass with fluoride glass, the physical strength that the gallium germanium bismuth lead glass system is high, chemical stability, anti-crystallization ability and the performance that is easy to drawing optical fiber make it have its special advantages; And make it can be used as doping Er well below the characteristic of conventional oxide glass phonon energy 3+, Tm 3+, Nd 3+, Sm 3+, Eu 3+, Tb 3+Realize the luminous of visible-a plurality of wave bands of near infrared etc. the substrate material of multiple rare earth ion, thereby in light-emitting devices such as fiber amplifier, optical waveguides, laser apparatus and upconverter spare, be used widely.Thereby because having big nonlinear optics specific refractory power, fast time of response and little uptake factor, heavy metal oxide glass becomes one of candidate material of full optical switch device in addition.Therefore self unique advantage was indicating that this glass system had broad application prospects at optoelectronic areas to heavy metal oxide glass in that above each side has.
Summary of the invention
The present invention has overcome the deficiencies in the prior art, and a kind of rare earth doped gallium germanium bismuth lead luminous glass material is provided, and described material has the advantages that physico-chemical property is good, machining property good, luminous efficiency is high.
A kind of preparation method and application thereof of above-mentioned materials have been another object of the present invention is to provide.
Rare earth doped gallium germanium bismuth lead luminous glass material of the present invention is by Ga 2O 3, Bi 2O 3, GeO 2, lead-containing compounds, rare earth compound make, Ga wherein 2O 3, Bi 2O 3, GeO 2, lead-containing compounds the molfraction sum be 100, the molfraction of each component is as follows:
Ga 2O 3 0～30
Bi 2O 3 15～50
GeO 2 0～70
Lead-containing compounds 0～60
Rare earth compound 0～4.
Preferred plumbous oxide compound of described lead-containing compounds and/or plumbous halogenide, the halid molfraction of described lead is 0～45.
A kind of or more than one mixtures in the oxide compound of the preferred terbium of described rare earth compound (Tb), dysprosium (Dy), holmium (Ho), erbium (Er), thulium (Tm), ytterbium (Yb).
Er wherein 2O 3And Yb 2O 3Molfraction be 0～2.5, Tm 2O 3Molfraction be 0～1.5, Ho 2O 3, Dy 2O 3And Tb 2O 3Molfraction be 0～2.
Rare earth doped gallium germanium bismuth lead luminous glass material of the present invention can adopt the preparation of prior art method in common, also can adopt preparation method of the present invention, comprises the steps:
(1) will found after each component mixing, glass melting temperature is 900～1100 ℃, and melting time is 15～30 minutes, obtains melten glass liquid;
(2) after the melten glass liquid clarification it is poured into and obtains glass in the mould, put into the retort furnace insulation 1 hour that is warming up to this glass transformation temperature, be cooled to 100 ℃ with 5～10 ℃/hour speed then after, close the retort furnace power supply and be cooled to room temperature naturally.
Material of the present invention is made bulk, sheet, bar-shaped or fibrous, can be applicable to prepare the gain media of light-emitting devices such as full optical switch device, optical fiber laser, waveguide laser, large screen color display or fiber amplifier, have the advantage of cheapness, efficient, integrated and miniaturization.
For example, the glass after the annealing is made bulk, sheet, bar-shaped or fibrous, be used to prepare the gain media of light-emitting devices such as laser diode-pumped laser apparatus, amplifier.
With doping Tm of the present invention 3+Or Tm 3+And Yb 3+Or Ho 3+The glass material of mixing altogether is as the gain media of blue upconversion laser, and it is blue up-conversion luminous to observe intensive under 980nm is laser diode-pumped.
With doping Er of the present invention 3+Or Er 3+And Yb 3+The glass material of mixing altogether can be observed the green up-conversion luminescence of intensive as the gain media of green upconversion laser under 980nm is laser diode-pumped.
With doping Tm of the present invention 3+Or Tm 3+With Yb 3+, Tb 3+, Dy 3+Or Ho 3+The glass material of mixing altogether is laser diode-pumped down at 800nm, it is luminous to observe intensive 1.47 mu m wavebands, the luminous low loss window of silica based telecommunication optical fiber 1450～1650nm that makes of this wave band is fully used, for realizing that the S-band amplifier is extremely beneficial.
With doping Er of the present invention 3+Perhaps Er 3+With Yb 3+The glass material of mixing altogether can be observed the luminous of intensive 1.53 mu m wavebands under 980nm is laser diode-pumped, help realizing 1.53 mu m waveband amplifiers of wide bandwidth, high gain.
Compared with prior art, the present invention has following advantage:
(1) the highest phonon energy and the fluoride glass of material of the present invention are suitable, but chemical stability, physical strength and devitrification resistance can be higher than fluoride glass far away, and preparation technology is also quite simple.
(2) material of the present invention is compared with tellurate glass, has advantages such as machining property and anti-crystallization stability are good.
(3) material of the present invention and conventional oxide glassy phase ratios such as silicate, borate, phosphoric acid salt have advantages such as last efficiency of conversion height, emission wavelength are many.
(4) material of the present invention can be realized the luminous of bluish-green luminous, 1.47 mu m wavebands of conversion, 1.53 mu m wavebands and 2.0 mu m wavebands.
(5) material of the present invention can be made into bulk, sheet, bar-shaped or fibrous, be applied to light-emitting devices such as full optical switch device, optical fiber laser, waveguide laser, large screen color display or fiber amplifier, help realizing optics, the photonic device of cheapness, efficient, integrated and miniaturization.
Description of drawings
Fig. 1 is the differential thermal analysis curve figure of 1 prepared material of embodiment;
Fig. 2 is the up-conversion luminescence spectrogram of 1 prepared material of embodiment;
Fig. 3 is the up-conversion luminescence spectrogram of 2 prepared materials of embodiment;
Fig. 4 is the luminescent spectrum figure of 3 prepared materials of embodiment;
Fig. 5 is the up-conversion luminescence spectrogram of 4 prepared materials of embodiment;
Fig. 6 is the differential thermal analysis curve figure of 5 prepared materials of embodiment;
Fig. 7 is the luminescent spectrum figure of 5 prepared materials of embodiment.
Embodiment
Below in conjunction with embodiment the present invention is described in detail, the present invention is not limited to this.
Embodiment 1
(1) takes by weighing the component 20g of following molar content, put into the platinum crucible of lid after mixing and place silicon carbon rod electric furnace to found, temperature of fusion is 1100 ℃, melting time is to obtain glass melting liquid in 30 minutes, after treating fused solution clarification, it is cast in the stainless steel mould of preheating obtains glass;
(2) above-mentioned glass is put into be warming up to the material transition temperature T fast gInsulation is 1 hour in the retort furnace of (344 ℃), is cooled to 100 ℃ with 10 ℃/hour speed then, and powered-down is cooled to room temperature automatically, can obtain luminous glass material of the present invention.
Each component and molar content thereof are:
Ga 2O 3 0；?GeO 2 70； Bi 2O 3 15； PbO 10；
PbF 2 5；?Er 2O 3 1.5；?Yb 2O 3 1.0。
The small part sample of getting after the annealing ground to form 80 purpose fine powders with agate mortar, got 10 milligrams and carried out differential thermal analysis, and differential thermal analysis curve as shown in Figure 1.Record the T of sample by differential thermal analysis gBe 344 ℃, T xBe 468 ℃, the parameter Δ T that calculates the anti-crystallization stability of sample in view of the above is 124 ℃, and this is very favourable to fibre-optical drawing.
All the other samples are processed into the sheet glass of 15mm * 15mm * 2mm, two big mirror polish, recording its uv-absorbing cutoff wavelength through spectrum test is 413nm, the LD that adopts 977nm is as pump light source, at room temperature can obtain very strong going up and change green glow, its up-conversion luminescence spectrogram as shown in Figure 2.
Embodiment 2
(1) takes by weighing the component 20g of following molar content, put into the platinum crucible of lid after mixing and place silicon carbon rod electric furnace to found, temperature of fusion is 900 ℃, melting time is to obtain glass melting liquid in 30 minutes, after treating fused solution clarification, it is cast in the stainless steel mould of preheating obtains glass;
(2) above-mentioned glass is put into be warming up to the material transition temperature T fast gInsulation is 1 hour in the retort furnace of (357 ℃), is cooled to 100 ℃ with 5 ℃/hour speed then, and powered-down is cooled to room temperature automatically, can obtain luminous glass material of the present invention.
Each component and molar content thereof are:
Ga 2O 3 30；?GeO 2 0； Bi 2O 3 20； PbO 5；
PbF 2 45；?Tm 2O 3 1.5；?Yb 2O 3 2。
The small part sample of getting after the annealing ground to form 80 purpose fine powders with agate mortar, got 10 milligrams and carried out differential thermal analysis.Record the T of sample by differential thermal analysis gBe 357 ℃, T xBe 481 ℃, the parameter Δ T that calculates the anti-crystallization stability of sample in view of the above is 124 ℃, and this is very favourable to fibre-optical drawing.
All the other samples are processed into the sheet glass of 15mm * 15mm * 2mm, two big mirror polish, recording its uv-absorbing cutoff wavelength through spectrum test is 424nm, the LD that adopts 977nm is as pump light source, at room temperature can obtain very strong last converting blue light, its up-conversion luminescence spectrogram as shown in Figure 3.
Embodiment 3
(1) takes by weighing the component 20g of following molar content, put into the platinum crucible of lid after mixing and place silicon carbon rod electric furnace to found, temperature of fusion is 1000 ℃, melting time is to obtain glass melting liquid in 20 minutes, after treating fused solution clarification, it is cast in the stainless steel mould of preheating obtains glass;
(2) above-mentioned glass is put into be warming up to the material transition temperature T fast gInsulation is 1 hour in the retort furnace of (357 ℃), is cooled to 100 ℃ with 8 ℃/hour speed then, and powered-down is cooled to room temperature automatically, can obtain luminous glass material of the present invention.
Each component and molar content thereof are:
Ga 2O 3 15； GeO 2 20； Bi 2O 3 50； PbO 15；
PbF 2 0； Tm 2O 3 0.2；?Ho 2O 3 2。
Get the sheet glass that sample after the annealing is processed into 15mm * 15mm * 2mm, two big mirror polish, recording its uv-absorbing cutoff wavelength through spectrum test is 424nm, the LD that adopts 808nm is as pump light source, at room temperature can obtain the luminous of 1.47 very wide mu m wavebands, the fluorescence halfwidth reaches 123nm, help preparing broadband S-band fiber amplifier, its luminescent spectrum figure as shown in Figure 4.
Embodiment 4
(1) takes by weighing the component 20g of following molar content, put into the platinum crucible of lid after mixing and place silicon carbon rod electric furnace to found, temperature of fusion is 1050 ℃, melting time is to obtain glass melting liquid in 15 minutes, after treating fused solution clarification, it is cast in the stainless steel mould of preheating obtains glass;
(2) above-mentioned glass is put into be warming up to the material transition temperature T fast gInsulation is 1 hour in the retort furnace of (412 ℃), is cooled to 100 ℃ with 10 ℃/hour speed then, and powered-down is cooled to room temperature automatically, can obtain luminous glass material of the present invention.
Each component and molar content thereof are:
GeO 2 20； Bi 2O 3 20； PbO 30； PbF 2 30；
Er 2O 3 1.5；?Yb 2O 3 0.5。
Sample after the annealing is processed into the sheet glass of 15mm * 15mm * 2mm, two big mirror polish, recording its uv-absorbing cutoff wavelength through spectrum test is 399nm, the LD that adopts 977nm is as pump light source, at room temperature can obtain very strong going up and change green glow, its up-conversion luminescence spectrogram as shown in Figure 5.
Embodiment 5
(1) takes by weighing the component 20g of following molar content, put into the platinum crucible of lid after mixing and place silicon carbon rod electric furnace to found, temperature of fusion is 1100 ℃, melting time is to obtain glass melting liquid in 15 minutes, after treating fused solution clarification, it is cast in the stainless steel mould of preheating obtains glass;
(2) above-mentioned glass is put into be warming up to the material transition temperature T fast gInsulation is 1 hour in the retort furnace of (437 ℃), is cooled to 100 ℃ with 5 ℃/hour speed then, and powered-down is cooled to room temperature automatically, can obtain luminous glass material of the present invention.
Each component and molar content thereof are:
GeO 2 62； Bi 2O 3 25； PbO 13；
Er 2O 3 0.5；?Yb 2O 3 0.5。
The small part sample of getting after the annealing ground to form 80 purpose fine powders with agate mortar, got 10 milligrams and carried out differential thermal analysis, and differential thermal analysis curve as shown in Figure 6.Record the T of sample by differential thermal analysis gBe 437 ℃, T xBe 528 ℃, the parameter Δ T that calculates the anti-crystallization stability of sample in view of the above is 91 ℃, can satisfy the requirement of fibre-optical drawing.
All the other samples are processed into the sheet glass of 15mm * 15mm * 2mm, two big mirror polish, recording its uv-absorbing cutoff wavelength through spectrum test is 404nm, the LD that adopts 977nm is as pump light source, at room temperature can obtain 1.53 mu m wavebands luminous of broad, the fluorescence halfwidth reaches 60nm, help preparing the C-band fiber amplifier of broadband, high gain, its luminescent spectrum figure as shown in Figure 7.

Claims (8)

1, a kind of rare earth doped gallium germanium bismuth lead luminous glass material is characterized in that by Ga 2O 3, Bi 2O 3, GeO 2, lead-containing compounds, rare earth compound make, Ga wherein 2O 3, Bi 2O 3, GeO 2, lead-containing compounds the molfraction sum be 100, the molfraction of each component is as follows:
Ga 2O 3 0～30
Bi 2O 3 15～50
GeO 2 0～70
Lead-containing compounds 0～60
Rare earth compound 1.0～3.5;
Described lead-containing compounds is plumbous oxide compound and plumbous halid mixture, the halid molfraction of described lead is 0～45, the molfraction of plumbous oxide compound is 5,10,13,15 or 30, and described rare earth compound is the two or more mixtures in the oxide compound of terbium, dysprosium, holmium, erbium, thulium, ytterbium.
2, material according to claim 1 is characterized in that, wherein Er 2O 3And Yb 2O 3Molfraction be 0～2.5, Tm 2O 3Molfraction be 0～1.5, Ho 2O 3, Dy 2O 3And Tb 2O 3Molfraction be 0～2.
3, the described material of one of a kind of claim 1～2 is characterized in that its preparation method comprises the steps:
(1) will found after each component mixing, glass melting temperature is 900～1100 ℃, and melting time is 15～30 minutes, obtains melten glass liquid;
(2) after the melten glass liquid clarification, it is poured into obtains glass in the mould, put into the retort furnace insulation 1 hour that is warming up to this glass transformation temperature, be cooled to 100 ℃ with 5～10 ℃/hour speed then after, close the retort furnace power supply and be cooled to room temperature naturally.
4, the application of the described material of one of claim 1～2 in the gain media of the full optical switch device of preparation.
5, the application of the described material of one of claim 1～2 in the gain media of preparation optical fiber laser.
6, the application of the described material of one of claim 1～2 in the gain media of preparation waveguide laser.
7, the application of the described material of one of claim 1～2 in the gain media of preparation large screen color display.
8, the application of the described material of one of claim 1～2 in the gain media of preparation fiber amplifier.
CNB2006100335138A 2006-02-10 2006-02-10 Rare earth doped gallium germanium bismuth lead luminous glass material and its preparation method and uses Expired - Fee Related CN100513339C (en)

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CN101182121B (en) * 2007-11-02 2010-08-25 中国科学院上海光学精密机械研究所 Bismuth-nickel co-doped transparent silicate glass-ceramics and preparation method thereof
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CN104926118B (en) * 2015-07-09 2017-09-22 盐城工学院 One kind mixes Yb3+Bi2O3‑GeO2Based laser glass and preparation method
CN105776858B (en) * 2016-04-19 2018-08-17 盐城工学院 Mix Er3+Bi2O3-GeO2Based laser glass and preparation method thereof
CN107162412A (en) * 2017-05-26 2017-09-15 云南师范大学 A kind of alkali metal gallate glass and preparation method thereof
CN108147660A (en) * 2017-12-13 2018-06-12 上海应用技术大学 A kind of fiber amplifier is co-doped with bismuthates laser glass and preparation method thereof with thulium dysprosium
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