CN103073180A - Bismuth-doped silicon boron aluminate optical glass and preparation method thereof - Google Patents
Bismuth-doped silicon boron aluminate optical glass and preparation method thereof Download PDFInfo
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- CN103073180A CN103073180A CN2013100169231A CN201310016923A CN103073180A CN 103073180 A CN103073180 A CN 103073180A CN 2013100169231 A CN2013100169231 A CN 2013100169231A CN 201310016923 A CN201310016923 A CN 201310016923A CN 103073180 A CN103073180 A CN 103073180A
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- bismuth
- optical glass
- doped silicon
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- optical
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- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000005304 optical glass Substances 0.000 title abstract description 10
- -1 silicon boron aluminate Chemical class 0.000 title abstract 3
- 239000007788 liquid Substances 0.000 claims abstract description 15
- 150000001875 compounds Chemical class 0.000 claims description 15
- OJMOMXZKOWKUTA-UHFFFAOYSA-N aluminum;borate Chemical compound [Al+3].[O-]B([O-])[O-] OJMOMXZKOWKUTA-UHFFFAOYSA-N 0.000 claims description 14
- 239000002994 raw material Substances 0.000 claims description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 13
- 229910052710 silicon Inorganic materials 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 13
- 229910004298 SiO 2 Inorganic materials 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- 238000010792 warming Methods 0.000 claims description 7
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract description 9
- 238000000137 annealing Methods 0.000 abstract description 7
- 230000003287 optical effect Effects 0.000 abstract description 6
- 230000005284 excitation Effects 0.000 abstract description 4
- 238000002844 melting Methods 0.000 abstract description 3
- 230000008018 melting Effects 0.000 abstract description 3
- 238000004891 communication Methods 0.000 abstract description 2
- 239000000377 silicon dioxide Substances 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 abstract 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract 1
- 229910052681 coesite Inorganic materials 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 229910052593 corundum Inorganic materials 0.000 abstract 1
- 229910052906 cristobalite Inorganic materials 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 229910052682 stishovite Inorganic materials 0.000 abstract 1
- 229910052905 tridymite Inorganic materials 0.000 abstract 1
- 229910001845 yogo sapphire Inorganic materials 0.000 abstract 1
- 239000011521 glass Substances 0.000 description 10
- 229910052797 bismuth Inorganic materials 0.000 description 7
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 229910001451 bismuth ion Inorganic materials 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000013307 optical fiber Substances 0.000 description 4
- 230000003321 amplification Effects 0.000 description 3
- 238000003199 nucleic acid amplification method Methods 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- CWCCJSTUDNHIKB-UHFFFAOYSA-N $l^{2}-bismuthanylidenegermanium Chemical compound [Bi]=[Ge] CWCCJSTUDNHIKB-UHFFFAOYSA-N 0.000 description 1
- OTZGYUUQQRXJMY-UHFFFAOYSA-N $l^{2}-bismuthanylidenesilicon Chemical compound [Bi]=[Si] OTZGYUUQQRXJMY-UHFFFAOYSA-N 0.000 description 1
- 241000931526 Acer campestre Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- OBNDGIHQAIXEAO-UHFFFAOYSA-N [O].[Si] Chemical compound [O].[Si] OBNDGIHQAIXEAO-UHFFFAOYSA-N 0.000 description 1
- 150000001621 bismuth Chemical class 0.000 description 1
- LFTVQMXNFSJCFX-UHFFFAOYSA-N bismuth ytterbium Chemical compound [Yb].[Bi] LFTVQMXNFSJCFX-UHFFFAOYSA-N 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 230000028327 secretion Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
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- Glass Compositions (AREA)
Abstract
The invention provides bismuth-doped silicon boron aluminate optical glass and a preparation method thereof. The optical glass comprises the following components by mole percent: 20-40% of SiO2, 0-20% of B2O3, 0-20% of Al2O3, 0-30% of RO1, 0-30% of R2O1 and 0.1-5% of Bi2O3. The preparation method comprises the following steps: heating the components to 1100-1400 DEG C, insulating for 45-120 min, and melting the components into liquid; and annealing for 1-12 h at the temperature of 350-600 DEG C, and cooling to be room temperature at a speed of 1 DEG C/min to obtain the bismuth-doped silicon boron aluminate optical glass. The optical glass can emit near-infrared band fluorescent light, is higher in luminous intensity, long in fluorescent lifetime and wide in gain bandwidth, and is suitable for serving as a gain medium to be applied to optical amplifiers and/or lasers. Except that the melting temperature of the optical glass is remarkably reduced relative to quartz glass, the mechanical performance of the optical glass is higher, and the optical glass is provided with the optical performance of ultra wide band capable of covering the whole communication waveband under the excitation action of laser with continuous wavelength of 400-1000 nm.
Description
Technical field
The present invention relates to a kind of silicon aluminium borate opticglass of mixing bismuth and preparation method thereof, belong to the opticglass technical field.
Background technology
On March 4th, 1998, the quiet patent (special permission discloses flat 11-29334) that waits the people to apply for being entitled as " mixing secret silica glass, optical fiber and image intensifer manufacture method " of the liana of Mitsubishi Cable Ind Ltd.They utilize the zeolite of bismuth exchange as dispersion medium, and comprehensive sol-gel method and high-temperature melting method have prepared under the air and mixed the secret ion Bi of pentavalent
5+Silica glass, draw out corresponding optical fiber, realized the light amplification at 1.3 μ m places under the 800nm pumping.The photoluminescence peak of this glass is positioned near the 1130nm, and maximum fluorescence halfwidth is 250nm, and maximum fluorescence lifetime is 650 μ s, and stimulated emission cross section is approximately 1.0 * 10
-20Cm
2. on February 22 calendar year 2001, liana is quiet to wait the people to apply for again being entitled as " optical fiber and image intensifer " (the open 2002-252397 of special permission), and its basic glass consists of: A1
2O
3-SiO
2-Bi
2O
3, under the 1750oC air, found, draw out corresponding optical fiber, realized the light amplification at 1.3 μ m places under the 0.8 μ m pumping.Calendar year 2001, Fujimoto and Nakatsuka be at Jpn. J. App. Phys., and 40, preparation pentavalent bismuth ion Bi under air reported in (2001) L279 one literary composition
5+The A1 that mixes
2O
3-SiO
2Glass has reported that its near infrared light under 800nm laser excitation amplifies the realization gain.The Qiu Jianrong of Zhejiang University etc. has applied for a series of being entitled as " nano bismuth cluster doped silicon dioxide base optical glass and preparation method thereof ", " bismuth ion doped crystal that is used for tunable laser and broad band amplifier ", " mixing the preparation method of bismuth germanium base optical glass bismuth blended high silicon oxygen near-infrared super-broadband emission glass ", (patent publication No. 200510024483.X continuously, 200510023597.2,200410054217.7) about the patent of bismuth doped-glass as photosensitive enlarging material.They realize near infrared ultra-wideband-light amplification by the 808nm semiconductor laser as pump light source in above-mentioned patent, so that the selection of pump light source is single, be unfavorable for the selection of the different optical maser wavelengths of material, for " Ytterbium-bismuth co-doped phosphate base opticglass and preparation method thereof ", patent publication No. 200710044174.8, this glass should only can be at 405nm, 532nm, obtain stronger near infrared ultra broadband fluorescence under these four kinds of different wave length laser pumpings of 808nm and 980nm, so that material has selectivity for laser wavelength, limited to the use range of bismuth ion doping near infrared material.
Summary of the invention
The objective of the invention is to select single shortcoming in order to overcome above-mentioned bismuth dopant material pump light source, a kind of bismuth silicon aluminium borate opticglass and preparation method thereof of mixing is provided, this bismuth doped-glass has the optical property of the ultra broadband that can cover 1000～1700nm wave band under the laser excitation of 450～1000nm continuous wavelength, be expected at ultra broadband optics amplifier, superpower laser, the technical fields such as tunable laser are applied.
The present invention realizes by following technical proposal: a kind of bismuth-doped silicon aluminium borate opticglass is comprised of the component of following molar percentage:
SiO
2 20～40mol%、
B
2O
3 0～20mol%、
Al
2O
3 0～20mol%、
RO 10～30mol%、
R
2O 10～30mol%、
Bi
2O
3 0.1～5mol%；
Wherein, RO be among MgO, CaO, SrO, the BaO any one or several, R
2O is Li
2O, Na
2O, K
2Among the O one or several.
Another object of the present invention is to provide a kind of preparation method of bismuth-doped silicon aluminium borate opticglass, following each step of process:
(1) get the raw materials ready by the component of following molar percentage, remix is even:
SiO
2 20～40mol%、
B
2O
3 0～20mol%、
Al
2O
3 0～20mol%、
RO/RCO
3 10～30mol%、
R
2O/R
2CO
3 10～30mol%、
Bi
2O
3 0.1～5mol%；
Wherein, RO/RCO
3Being the carbonate of oxide compound and this oxide compound, is MgO, MgCO
3, CaO, CaCO
3, SrO, SrCO
3, BaO, BaCO
3In any one or several; R
2O/R
2CO
3Being the carbonate of oxide compound and this oxide compound, is Li
2O, Li
2CO
3, Na
2O, Na
2CO
3, K
2O, K
2CO
3In any one or several;
(2) compound with step (1) gained is warming up to 1100～1400 ℃, is incubated 45～120 minutes, makes raw materials melt become liquid;
(3) with the liquid of step (2) gained in annealing furnace 350～600 ℃ carried out anneal 1～12 hour, again with the speed cool to room temperature of 1 ℃/min, namely obtain bismuth-doped silicon aluminium borate opticglass.
The present invention compares with the silica glass method that bismuth ion is mixed in preparation, has following outstanding advantage:
This glass can be sent out near-infrared band fluorescence, has stronger luminous intensity, long fluorescence lifetime, and wide gain bandwidth is suitable as gain media and is applied to optical amplifier and/or laser apparatus.This glass except its melt temperature with respect to the obvious reduction of silica glass, the mechanical property of glass is higher, and has the optical property of the ultra broadband that can cover whole communication band under the laser excitation of 400～1000nm continuous wavelength.Be expected at ultra broadband optics amplifier, superpower laser, the technical fields such as tunable laser are applied.
Embodiment
Further illustrate content of the present invention below in conjunction with embodiment, but these examples do not limit protection scope of the present invention.
Embodiment 1
(1) get the raw materials ready by the component of following molar percentage, remix is even:
SiO
2 30mol%、
B
2O
3 15mol%、
Al
2O
3 2mol%、
CaO 10mol%、
BaO 20mol%、
Na
2O 20mol%、
Bi
2O
3 3mol%；
(2) compound with step (1) gained is warming up to 1200 ℃, is incubated 60 minutes, makes raw materials melt become liquid;
(3) with the liquid of step (2) gained in annealing furnace 450 ℃ carried out anneal 6 hours, again with the speed cool to room temperature of 1 ℃/min, namely obtain bismuth-doped silicon aluminium borate opticglass 30Si
2O – 15B
2O
3-2Al
2O
3-10CaO – 20Na
2O-20BaO-3Bi
2O
3
Embodiment 2
(1) get the raw materials ready by the component of following molar percentage, remix is even:
SiO
2 40mol%、
B
2O
3 20mol%、
MgCO
3 10mol%、
Li
2O 15mol%
K
2CO
3 14.9mol%
Bi
2O
3 0.1mol%；
(2) compound with step (1) gained is warming up to 1100 ℃, is incubated 120 minutes, makes raw materials melt become liquid;
(3) with the liquid of step (2) gained in annealing furnace 600 ℃ carried out anneal 1 hour, again with the speed cool to room temperature of 1 ℃/min, namely obtain bismuth-doped silicon aluminium borate opticglass 40Si
2O – 20B
2O
3-10MgO – 15Li
2O-14.9K
2O-0.1Bi
2O
3
Embodiment 3
(1) get the raw materials ready by the component of following molar percentage, remix is even:
SiO
2 20mol%、
Al
2O
3 20mol%、
MgO 15mol%、
SrCO
3 10mol%、
Li
2CO
3 30mol%、
Bi
2O
3 5mol%；
(2) compound with step (1) gained is warming up to 1400 ℃, is incubated 45 minutes, makes raw materials melt become liquid;
(3) with the liquid of step (2) gained in annealing furnace 350 ℃ carried out anneal 12 hours, again with the speed cool to room temperature of 1 ℃/min, namely obtain bismuth-doped silicon aluminium borate opticglass 20Si
2O – 20 Al
2O
3-15MgO-10SrO – 30Li
2O-5Bi
2O
3
Embodiment 4
(1) get the raw materials ready by the component of following molar percentage, remix is even:
SiO
2 30mol%、
B
2O
3 20mol%、
Al
2O
3 10mol%、
CaCO
3 29.2mol%、
Na
2CO
3 5mol%、
K
2O 5mol%、
Bi
2O
3 0.8mol%；
(2) compound with step (1) gained is warming up to 1350 ℃, is incubated 90 minutes, makes raw materials melt become liquid;
(3) with the liquid of step (2) gained in annealing furnace 500 ℃ carried out anneal 10 hours, again with the speed cool to room temperature of 1 ℃/min, namely obtain bismuth-doped silicon aluminium borate opticglass 30Si
2O – 20B
2O
3– 10Al
2O
3-29.2CaO-5Na
2O – 5K
2O-0.8Bi
2O
3
Embodiment 5
(1) get the raw materials ready by the component of following molar percentage, remix is even:
SiO
2 28mol%、
B
2O
3 15mol%、
Al
2O
3 15mol%、
SrO 10mol%、
BaCO
3 10mol%
Na
2O 10mol%
Li
2O 10mol%、
Bi
2O
3 2mol%；
(2) compound with step (1) gained is warming up to 1150 ℃, is incubated 100 minutes, makes raw materials melt become liquid;
(3) with the liquid of step (2) gained in annealing furnace 350 ℃ carried out anneal 11 hours, again with the speed cool to room temperature of 1 ℃/min, namely obtain bismuth-doped silicon aluminium borate opticglass 28Si
2O – 15B
2O
3– 15Al
2O
3-10SrO-10BaO-10Na
2O – 10Li
2O-2Bi
2O
3
Claims (2)
1. bismuth-doped silicon aluminium borate opticglass is characterized in that being comprised of the component of following molar percentage:
SiO
2 20～40mol%、
B
2O
3 0～20mol%、
Al
2O
3 0～20mol%、
RO 10～30mol%、
R
2O 10～30mol%、
Bi
2O
3 0.1～5mol%；
Wherein, RO be among MgO, CaO, SrO, the BaO any one or several, R
2O is Li
2O, Na
2O, K
2Among the O one or several.
2. the preparation method of a bismuth-doped silicon aluminium borate opticglass is characterized in that through following each step:
(1) get the raw materials ready by the component of following molar percentage, remix is even:
SiO
2 20～40mol%、
B
2O
3 0～20mol%、
Al
2O
3 0～20mol%、
RO/RCO
3 10～30mol%、
R
2O/R
2CO
3 10～30mol%、
Bi
2O
3 0.1～5mol%；
Wherein, RO/RCO
3Being the carbonate of oxide compound and this oxide compound, is MgO, MgCO
3, CaO, CaCO
3, SrO, SrCO
3, BaO, BaCO
3In any one or several; R
2O/R
2CO
3Being the carbonate of oxide compound and this oxide compound, is Li
2O, Li
2CO
3, Na
2O, Na
2CO
3, K
2O, K
2CO
3In any one or several;
(2) compound with step (1) gained is warming up to 1100～1400 ℃, is incubated 45～120 minutes, makes raw materials melt become liquid;
(3) liquid with step (2) gained carried out anneal 1～12 hour at 350～600 ℃, again with the speed cool to room temperature of 1 ℃/min, namely obtained bismuth-doped silicon aluminium borate opticglass.
Priority Applications (1)
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|---|---|---|---|
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013100169231A CN103073180A (en) | 2013-01-17 | 2013-01-17 | Bismuth-doped silicon boron aluminate optical glass and preparation method thereof |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103073180A true CN103073180A (en) | 2013-05-01 |
Family
ID=48149904
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
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|---|---|
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811800A (en) * | 2015-11-28 | 2017-06-09 | 中国科学院新疆理化技术研究所 | Lithium aluminosilicate nonlinear optical crystal and its production and use |
| CN108640504A (en) * | 2018-05-30 | 2018-10-12 | 华南理工大学 | A kind of glass and preparation method thereof of simulated solar optical illumination |
| CN109265160A (en) * | 2018-09-12 | 2019-01-25 | 桂林理工大学 | A kind of oxygen ion conductor material and preparation method of aluminium borate melilite structure |
| CN110752283A (en) * | 2019-10-12 | 2020-02-04 | 华南理工大学 | Broadband near-infrared LED device |
| CN113508097A (en) * | 2019-01-18 | 2021-10-15 | 康宁股份有限公司 | Low dielectric loss glass for electronic devices |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546405A (en) * | 2003-12-16 | 2004-11-17 | 中国科学院长春应用化学研究所 | Process for preparing rare-earth green long-lasting luminescent glass |
| CN102730970A (en) * | 2012-06-27 | 2012-10-17 | 华南理工大学 | Red silicate glass and preparation method thereof |
-
2013
- 2013-01-17 CN CN2013100169231A patent/CN103073180A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1546405A (en) * | 2003-12-16 | 2004-11-17 | 中国科学院长春应用化学研究所 | Process for preparing rare-earth green long-lasting luminescent glass |
| CN102730970A (en) * | 2012-06-27 | 2012-10-17 | 华南理工大学 | Red silicate glass and preparation method thereof |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106811800A (en) * | 2015-11-28 | 2017-06-09 | 中国科学院新疆理化技术研究所 | Lithium aluminosilicate nonlinear optical crystal and its production and use |
| CN106811800B (en) * | 2015-11-28 | 2019-06-04 | 中国科学院新疆理化技术研究所 | Lithium aluminosilicate nonlinear optical crystal and its preparation method and application |
| CN108640504A (en) * | 2018-05-30 | 2018-10-12 | 华南理工大学 | A kind of glass and preparation method thereof of simulated solar optical illumination |
| CN109265160A (en) * | 2018-09-12 | 2019-01-25 | 桂林理工大学 | A kind of oxygen ion conductor material and preparation method of aluminium borate melilite structure |
| CN113508097A (en) * | 2019-01-18 | 2021-10-15 | 康宁股份有限公司 | Low dielectric loss glass for electronic devices |
| CN113508097B (en) * | 2019-01-18 | 2022-08-09 | 康宁股份有限公司 | Low dielectric loss glass for electronic devices |
| US11629090B2 (en) | 2019-01-18 | 2023-04-18 | Corning Incorporated | Low dielectric loss glasses for electronic devices |
| CN110752283A (en) * | 2019-10-12 | 2020-02-04 | 华南理工大学 | Broadband near-infrared LED device |
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Application publication date: 20130501 |