CN110357422A - Middle infrared band luminous host material-germanium gallium bismuthate glass - Google Patents
Middle infrared band luminous host material-germanium gallium bismuthate glass Download PDFInfo
- Publication number
- CN110357422A CN110357422A CN201810307477.2A CN201810307477A CN110357422A CN 110357422 A CN110357422 A CN 110357422A CN 201810307477 A CN201810307477 A CN 201810307477A CN 110357422 A CN110357422 A CN 110357422A
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- CN
- China
- Prior art keywords
- glass
- infrared
- bismuthate
- germanium gallium
- infrared band
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000011521 glass Substances 0.000 title claims abstract description 64
- GYHNNYVSQQEPJS-UHFFFAOYSA-N Gallium Chemical compound [Ga] GYHNNYVSQQEPJS-UHFFFAOYSA-N 0.000 title claims abstract description 19
- 229910052733 gallium Inorganic materials 0.000 title claims abstract description 19
- 229910052732 germanium Inorganic materials 0.000 title claims abstract description 19
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052593 corundum Inorganic materials 0.000 claims abstract description 6
- 239000010431 corundum Substances 0.000 claims abstract description 6
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 claims abstract description 4
- YBMRDBCBODYGJE-UHFFFAOYSA-N germanium dioxide Chemical compound O=[Ge]=O YBMRDBCBODYGJE-UHFFFAOYSA-N 0.000 claims abstract description 4
- VQCBHWLJZDBHOS-UHFFFAOYSA-N erbium(III) oxide Inorganic materials O=[Er]O[Er]=O VQCBHWLJZDBHOS-UHFFFAOYSA-N 0.000 claims abstract description 3
- QZQVBEXLDFYHSR-UHFFFAOYSA-N gallium(III) oxide Inorganic materials O=[Ga]O[Ga]=O QZQVBEXLDFYHSR-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000000463 material Substances 0.000 claims abstract 2
- 239000000203 mixture Substances 0.000 claims description 22
- 238000001816 cooling Methods 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 8
- 229910052751 metal Inorganic materials 0.000 claims description 5
- 239000002184 metal Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 230000004927 fusion Effects 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000009466 transformation Effects 0.000 claims description 2
- 239000000835 fiber Substances 0.000 abstract description 5
- 239000000126 substance Substances 0.000 abstract description 5
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 4
- 229910003439 heavy metal oxide Inorganic materials 0.000 abstract description 3
- 239000000382 optic material Substances 0.000 abstract description 3
- 239000000075 oxide glass Substances 0.000 abstract description 3
- 238000000034 method Methods 0.000 abstract description 2
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 229910052691 Erbium Inorganic materials 0.000 description 13
- UYAHIZSMUZPPFV-UHFFFAOYSA-N erbium Chemical compound [Er] UYAHIZSMUZPPFV-UHFFFAOYSA-N 0.000 description 12
- 238000002189 fluorescence spectrum Methods 0.000 description 5
- 239000005371 ZBLAN Substances 0.000 description 4
- 238000000137 annealing Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 239000005357 flat glass Substances 0.000 description 4
- 238000005498 polishing Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 230000005540 biological transmission Effects 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000087 laser glass Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 150000002978 peroxides Chemical class 0.000 description 2
- -1 rare earth ion Chemical class 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- CWCCJSTUDNHIKB-UHFFFAOYSA-N $l^{2}-bismuthanylidenegermanium Chemical compound [Bi]=[Ge] CWCCJSTUDNHIKB-UHFFFAOYSA-N 0.000 description 1
- 241000013355 Mycteroperca interstitialis Species 0.000 description 1
- 238000001069 Raman spectroscopy Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- LNTHITQWFMADLM-UHFFFAOYSA-N gallic acid Chemical compound OC(=O)C1=CC(O)=C(O)C(O)=C1 LNTHITQWFMADLM-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 239000013307 optical fiber Substances 0.000 description 1
- 238000005086 pumping Methods 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- XHGGEBRKUWZHEK-UHFFFAOYSA-L tellurate Chemical compound [O-][Te]([O-])(=O)=O XHGGEBRKUWZHEK-UHFFFAOYSA-L 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- C03C3/00—Glass compositions
- C03C3/12—Silica-free oxide glass compositions
- C03C3/253—Silica-free oxide glass compositions containing germanium
-
- 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
- C03C4/12—Compositions for glass with special properties for luminescent glass; for fluorescent glass
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Manufacturing & Machinery (AREA)
- Glass Compositions (AREA)
Abstract
A kind of middle infrared band host material germanium gallium bismuthate glass, the molar percentage compositing range of the glass are as follows: Bi2O3: 30~40%, GeO2: 30~50%, Ga2O3: 3~20%, Na2O2: 5~16%, Er2O3: 0~3%.It is prepared using corundum crucible and Elema electric furnace melting method.Glass of the present invention is high in middle infrared band transmitance, excellent in physical and chemical performance, stability parameter T >=160 DEG C, rare earth ion doped good luminous performance, the application of the heavy metal oxide glass rare earth ion doped suitable for middle infrared band and fiber optic materials.
Description
Technical field
The present invention relates to a kind of middle infrared band luminous host material-germanium gallium bismuthate glasses.
Background technique
In recent years, for the solid state lasers of 3 μm of output infrared in erbium ion-doped because of the absorption peak of its wavelength and water
It is very close, it attracts attention.Therefore, the solid state laser of 3 μm of output of Er ions is in remote sensing, ranging, environment inspection
It surveys, all have in terms of bioengineering and medical treatment and pumping source for new middle infrared band laser and highly important apply valence
Value.Report within 1967 3 μm of pulse and continuous laser output for the first time in LiYF4 crystal.At present both at home and abroad to passing through rare earth
There are many researchs that doped crystal obtains 3 μm of outputs, but crystal because large scale is difficult to prepare, rear-earth-doped concentration small the disadvantages of due to
Limit its application.And rear-earth-doped glass optical fiber can avoid these disadvantages of crystal well.1988, Pollack
The ZBLAN fluoride fiber for reporting Er doping for the first time, due to Er3+:4I11/2→4I13/2Transition obtains central wavelength in 2.78 μ
M, the laser that output energy is 75J export.2008, Zhu etc. obtained a watt grade laser output in ZBLAN fluoride fiber, it
Obtain nearly 10 watts of laser output in succession afterwards.Hereafter, Tokita in 2009 etc. obtains 24 watts in ZBLAN under the conditions of liquid cooling and swashs
Light output.But the thermal stability and chemical stability due to ZBLAN glass are poor, limit its power in 3 μm of outputs
It improves and applies.
Heavy metal oxide glass has lower phonon energy such as germanate glass, tellurate glass, bismuthate glass
Amount, while rare earth ion solubility is high, refractive index is high, and transition temperature is higher, and has preferable infrared transmission performance.These property
Matter provides guarantee as infrared 2.7 mu m luminous realizations in erbium ion for heavy metal oxide glass.In bismuth germanium gallate glass
In glass melting process, to glass, the transmitance at 2.7 μm is affected for the control of atmosphere.The present invention is by introducing peroxide
Na2O2, infrared transmission and Er in preferable can be obtained under conditions of obstructed oxygen3+The good luminescent properties of ion.It is domestic at present
There has been no report in this respect outside.
Summary of the invention
The technical problem to be solved in the present invention is that provide it is a kind of prepare have good stability in infrared 2.7 mu m luminous erbium from
Sub- doped germanium gallium bismuthate glass, the glass have excellent thermal stability, preferable infrared transmission performance, in 980nm wavelength
It is laser diode-pumped it is lower can obtain it is very strong in infrared 2.7 μm of fluorescent emissions.
The specific technical solution of the present invention is as follows:
Infrared 2.7 mu m luminous erbium ion-doped germanium gallium bismuthate glass in one kind, it is characterized in that its molar percentage forms
Are as follows:
Form mol%
Bi2O330~40,
GeO230~50,
Ga2O33~20,
Na2O25~16,
Er2O30~1.
The preparation method of infrared 2.7 mu m luminous erbium ion-doped germanium gallium bismuthate glass in above-mentioned, including the following steps:
1. selecting the glass composition and its molar percentage, the weight of corresponding each glass composition is calculated, is accurately weighed
Each raw material is uniformly mixed and forms mixture；
It is melted in 1200~1250 DEG C of Elema electric furnace 2. mixture is put into corundum crucible, fusing time is 15~20
Minute；
3. reducing fusion temperature to 1100~1150 DEG C, homogenizing is 10~15 minutes cooling, and glass metal is cast in the mold of preheating
In；
It has warmed up 4. glass is moved into rapidly to lower than glass transformation temperature (Tg) in 10 DEG C of Muffle furnace, heat preservation 8~12 is small
When, then room temperature is down to 10 DEG C/h of rate, glass sample is taken out after cooling completely.
Technical effect of the invention is as follows:
Infrared 2.7 mu m luminous erbium ion-doped germanium gallium bismuthate glass in the present invention, by introducing peroxide Na2O2Improve glass
The atmosphere stability of glass, realization obtained under the conditions of obstructed oxygen in very strong it is infrared 2.7 mu m luminous, near infrared 2.7 μm
Infrared transmittivity is high, excellent in physical and chemical performance, stability parameter T >=160 DEG C.In the laser diode of 980nm wavelength
Infrared 2.7 μm of fluorescence in very strong can be obtained under Pu, be suitable in infrared 2.7 μm of laser glasses and fiber optic materials preparation and
Using.
Specific embodiment
The glass ingredient of 13 specific embodiments of infrared 2.7 mu m luminous erbium ion-doped germanium gallium bismuthate glass is such as in the present invention
Shown in table 1:
Table 1: the glass formula of specific 13 embodiments
Embodiment 1#:
Composition is as 1 in table 1#Shown, specific preparation process is as follows:
According in table 11#The molar percentage of glass composition, calculates the weight respectively formed accordingly, weighs each raw material and mix
Uniformly；Mixture is put into corundum crucible and is melted in 1200~1250 DEG C of Elema electric furnace, temperature near 1100~
1150 DEG C, homogenizing is 15 minutes cooling, and glass metal is cast in the mold of preheating；Glass is moved into rapidly and is had warmed up to 420
DEG C Muffle furnace in, keep the temperature 10 hours, then room temperature be down to 10 DEG C/h of rate, take out glass sample after completely cooling.
To the glass, test result is as follows:
Sample after annealing is processed into sheet glass and the polishing of 20 × 10 × 1.0mm, tests its infrared penetrates and compose, in 980nm
Laser diode-pumped lower its fluorescence spectrum of test of wavelength.Infrared 2.7 mu m luminous erbium ion-doped germanium gallium bismuthic acid in the present invention
The infrared of salt glass penetrates spectrum as shown in Figure 1.In the present invention infrared 2.7 mu m luminous erbium ion-doped germanium gallium bismuthate glass
980nm wavelength it is laser diode-pumped under fluorescence spectrum it is as shown in Figure 2.Experiment shows glass near infrared 2.7 μm
Infrared transmittivity is high, excellent in physical and chemical performance, stability parameter T >=160 DEG C.In the laser diode of 980nm wavelength
Infrared 2.7 μm of fluorescence in very strong can be obtained under Pu.
Embodiment 2#:
Composition is as 2 in table 1#Shown, specific preparation process is as follows:
According in table 12#The molar percentage of glass composition, calculates the weight respectively formed accordingly, weighs each raw material and mix
Uniformly；Mixture is put into corundum crucible and is melted in 1200~1250 DEG C of Elema electric furnace, temperature near 1100~
1150 DEG C, homogenizing is 15 minutes cooling, and glass metal is cast in the mold of preheating；Glass is moved into rapidly and is had warmed up to 420
DEG C Muffle furnace in, keep the temperature 10 hours, then room temperature be down to 10 DEG C/h of rate, take out glass sample after completely cooling.
To the glass, test result is as follows:
Sample after annealing is processed into sheet glass and the polishing of 20 × 10 × 1.0mm, tests its infrared penetrates and compose, in 980nm
Laser diode-pumped lower its fluorescence spectrum of test of wavelength.
Embodiment 3#~5#:
Composition is as 3 in table 1#To 5#Shown, specific preparation process is as follows:
According in table 13#The molar percentage of glass composition, calculates the weight respectively formed accordingly, weighs each raw material and mix
Uniformly；Mixture is put into corundum crucible and is melted in 1200~1250 DEG C of Elema electric furnace, temperature near 1100~
1150 DEG C, homogenizing is 15 minutes cooling, and glass metal is cast in the mold of preheating；Glass is moved into rapidly and is had warmed up to 420
DEG C Muffle furnace in, keep the temperature 10 hours, then room temperature be down to 10 DEG C/h of rate, take out glass sample after completely cooling.
To the glass, test result is as follows:
Sample after annealing is processed into sheet glass and the polishing of 20 × 10 × 1.0mm, tests its infrared penetrates and compose, in 980nm
Laser diode-pumped lower its fluorescence spectrum of test of wavelength.
Embodiment 6#:
Composition is as 6 in table 1#It is shown, specific preparation process such as embodiment 1#。
To the glass, test result is as follows:
Sample after annealing is processed into sheet glass and the polishing of 20 × 10 × 1.0mm, tests its infrared penetrates and compose, in 488nm
Its phonon energy is tested in laser pump (ing), and result is as shown in figure 3, show that its maximum phonon energy is 410cm-1。
Above-described embodiment test shows all there is embodiment 1#Infrared 2.7 mu m luminous erbium ion-doped germanium in obtained
Fig. 1 of gallium bismuthate glass and it is shown in Fig. 2 it is infrared through spectrum and 980nm wavelength it is laser diode-pumped under fluorescence light
The similar results of spectrum.Experiment shows that infrared 2.7 mu m luminous erbium ion-doped germanium gallium bismuthate glass is infrared by 2.7 in the present invention
Infrared transmittivity is high near μm, and phonon energy is low, excellent in physical and chemical performance, stability parameter T >=160 DEG C.In 980nm wave
It is long it is laser diode-pumped under can obtain infrared 2.7 μm of fluorescence in very strong, be suitable in infrared 2.7 μm of laser glasses with
The preparation and application of fiber optic materials.
Detailed description of the invention
Fig. 1 is embodiment 1#Infrared 2.7 mu m luminous erbium ion-doped germanium gallium bismuthate glass is infrared in obtained
Cross spectrum.
Fig. 2 is embodiment 1#Infrared 2.7 mu m luminous erbium ion-doped germanium gallium bismuthate glass in 980nm in obtained
Wavelength it is laser diode-pumped under fluorescence emission spectrum.
Fig. 3 is embodiment 6#The Raman spectrogram of obtained germanium gallium bismuthate glass.
Claims (3)
1. a kind of middle infrared band host material germanium gallium bismuthate glass, it is characterised in that its molar percentage composition are as follows:
Form mol%
Bi2O330~40,
GeO230~50,
Ga2O33~20,
Na2O25~16,
Er2O30~1.
2. germanium gallium bismuthate glass according to claim 1, it is characterised in that the glass phonon energy is low, thermostabilization
Property it is good, infrared transmittivity is high.
3. the preparation method of germanium gallium bismuthate glass according to claim 1, including the following steps:
1) the glass composition and its molar percentage are selected, the weight of corresponding each glass composition is calculated, accurately weighs
Each raw material is uniformly mixed and forms mixture；
2) mixture is put into corundum crucible and is melted in 1200~1250 DEG C of Elema electric furnace, fusing time be 15~
20 minutes；
3) fusion temperature is reduced to 1100~1150 DEG C, and homogenizing is 10~15 minutes cooling, and glass metal is cast in the mold of preheating
In；
4) glass is moved into rapidly and is had warmed up to lower than glass transformation temperature (Tg) in 10 DEG C of Muffle furnace, heat preservation 8~12 is small
When, then room temperature is down to 10 DEG C/h of rate, glass sample is taken out after cooling completely.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810307477.2A CN110357422A (en) | 2018-04-09 | 2018-04-09 | Middle infrared band luminous host material-germanium gallium bismuthate glass |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810307477.2A CN110357422A (en) | 2018-04-09 | 2018-04-09 | Middle infrared band luminous host material-germanium gallium bismuthate glass |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN110357422A true CN110357422A (en) | 2019-10-22 |
Family
ID=68213463
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810307477.2A Pending CN110357422A (en) | 2018-04-09 | 2018-04-09 | Middle infrared band luminous host material-germanium gallium bismuthate glass |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN110357422A (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112551884A (en) * | 2021-01-06 | 2021-03-26 | 长春理工大学 | Bismuthate glass optical fiber and preparation method thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1558943A (en) * | 2001-09-27 | 2004-12-29 | �����������˲�ҵ�����ۺ��о��� | Cleaning agent, antibacterial material, environment clarifying material, functional adsorbent |
| JP2007038213A (en) * | 2005-06-28 | 2007-02-15 | Sumitomo Chemical Co Ltd | Peroxide decomposing catalyst |
| US20080132399A1 (en) * | 2006-11-30 | 2008-06-05 | Bruce Gardiner Aitken | Phosphotellurite-containing glasses, process for making same and articles comprising same |
| CN103030274A (en) * | 2013-01-17 | 2013-04-10 | 中国科学院上海光学精密机械研究所 | Intermediate infrared 2.7 mum luminous erbium ion-doped gallium germanium bismuthate glass |
-
2018
- 2018-04-09 CN CN201810307477.2A patent/CN110357422A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1558943A (en) * | 2001-09-27 | 2004-12-29 | �����������˲�ҵ�����ۺ��о��� | Cleaning agent, antibacterial material, environment clarifying material, functional adsorbent |
| JP2007038213A (en) * | 2005-06-28 | 2007-02-15 | Sumitomo Chemical Co Ltd | Peroxide decomposing catalyst |
| US20080132399A1 (en) * | 2006-11-30 | 2008-06-05 | Bruce Gardiner Aitken | Phosphotellurite-containing glasses, process for making same and articles comprising same |
| CN103030274A (en) * | 2013-01-17 | 2013-04-10 | 中国科学院上海光学精密机械研究所 | Intermediate infrared 2.7 mum luminous erbium ion-doped gallium germanium bismuthate glass |
Non-Patent Citations (1)
| Title |
|---|
| 王国清等: "《无机化学》", 31 August 2015, 中国医药科技出版社 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112551884A (en) * | 2021-01-06 | 2021-03-26 | 长春理工大学 | Bismuthate glass optical fiber and preparation method thereof |
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Application publication date: 20191022 |