CN1587139A - rare earth doped tungsten tellurate glass and preparation method thereof - Google Patents
rare earth doped tungsten tellurate glass and preparation method thereof Download PDFInfo
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- CN1587139A CN1587139A CN 200410053439 CN200410053439A CN1587139A CN 1587139 A CN1587139 A CN 1587139A CN 200410053439 CN200410053439 CN 200410053439 CN 200410053439 A CN200410053439 A CN 200410053439A CN 1587139 A CN1587139 A CN 1587139A
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- China
- Prior art keywords
- glass
- rare earth
- doped tungsten
- tellurate
- tellurate glass
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- 239000011521 glass Substances 0.000 title claims abstract description 50
- XHGGEBRKUWZHEK-UHFFFAOYSA-L tellurate Chemical compound [O-][Te]([O-])(=O)=O XHGGEBRKUWZHEK-UHFFFAOYSA-L 0.000 title claims abstract description 29
- WFKWXMTUELFFGS-UHFFFAOYSA-N tungsten Chemical compound [W] WFKWXMTUELFFGS-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910052721 tungsten Inorganic materials 0.000 title claims abstract description 20
- 239000010937 tungsten Substances 0.000 title claims abstract description 20
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 11
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 150000002910 rare earth metals Chemical class 0.000 title abstract description 5
- 239000000203 mixture Substances 0.000 claims abstract description 8
- 229910052691 Erbium Inorganic materials 0.000 claims abstract description 6
- 229910052788 barium Inorganic materials 0.000 claims abstract description 3
- 229910052790 beryllium Inorganic materials 0.000 claims abstract description 3
- 229910052791 calcium Inorganic materials 0.000 claims abstract description 3
- 229910052745 lead Inorganic materials 0.000 claims abstract description 3
- 229910052749 magnesium Inorganic materials 0.000 claims abstract description 3
- 229910052751 metal Inorganic materials 0.000 claims abstract description 3
- 239000002184 metal Substances 0.000 claims abstract description 3
- 229910052712 strontium Inorganic materials 0.000 claims abstract description 3
- 229910052725 zinc Inorganic materials 0.000 claims abstract description 3
- 238000002844 melting Methods 0.000 claims description 4
- 230000008018 melting Effects 0.000 claims description 4
- 238000005352 clarification Methods 0.000 claims description 3
- 229910052593 corundum Inorganic materials 0.000 claims description 3
- 239000010431 corundum Substances 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000007704 transition Effects 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 239000000156 glass melt Substances 0.000 claims description 2
- 239000000463 material Substances 0.000 abstract description 5
- 239000000758 substrate Substances 0.000 abstract description 4
- 238000000034 method Methods 0.000 abstract description 2
- 229910003069 TeO2 Inorganic materials 0.000 abstract 1
- 230000009477 glass transition Effects 0.000 abstract 1
- 238000007500 overflow downdraw method Methods 0.000 abstract 1
- 229910001404 rare earth metal oxide Inorganic materials 0.000 abstract 1
- LAJZODKXOMJMPK-UHFFFAOYSA-N tellurium dioxide Chemical compound O=[Te]=O LAJZODKXOMJMPK-UHFFFAOYSA-N 0.000 abstract 1
- 230000009466 transformation Effects 0.000 description 6
- 239000000835 fiber Substances 0.000 description 5
- 239000013307 optical fiber Substances 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000004615 ingredient Substances 0.000 description 3
- 238000005086 pumping Methods 0.000 description 3
- 238000001237 Raman spectrum Methods 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004891 communication Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000002189 fluorescence spectrum Methods 0.000 description 2
- 230000004927 fusion Effects 0.000 description 2
- 101100296543 Caenorhabditis elegans pbo-4 gene Proteins 0.000 description 1
- HMDDXIMCDZRSNE-UHFFFAOYSA-N [C].[Si] Chemical compound [C].[Si] HMDDXIMCDZRSNE-UHFFFAOYSA-N 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 230000003321 amplification Effects 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005266 casting Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004031 devitrification Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 238000000265 homogenisation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- SYHGEUNFJIGTRX-UHFFFAOYSA-N methylenedioxypyrovalerone Chemical compound C=1C=C2OCOC2=CC=1C(=O)C(CCC)N1CCCC1 SYHGEUNFJIGTRX-UHFFFAOYSA-N 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 238000003199 nucleic acid amplification method Methods 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000005365 phosphate glass Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005368 silicate glass Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000003685 thermal hair damage Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
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- Glass Compositions (AREA)
Abstract
The invention discloses a rare earth doped tungsten tellurate glass for a broadband amplifier and a preparation method thereof, wherein the rare earth doped tungsten tellurate glass comprises the following components in percentage by mole: TeO2：65－94.5；WO3：5－30；MO：0－20；Re2O3: 0.5-2, wherein M is a divalent metal element, M ═ Be, Mg, Ca, Sr, Ba, Pb, Zn; re is a rare earth element, specifically Er or Er/Yb codoped, and can also be extended to other rare earth elements. A series of glasses were prepared by the conventional fusion method according to the above composition ranges and certain process requirements. The glass has higher glass transition temperature, wider fluorescence full width at half maximum and higher phonon energy. Is a good substrate material of a broadband amplifier.
Description
Technical field
The present invention relates to the tungsten tellurate glass, rear-earth-doped tungsten tellurate glass that particularly a kind of phonon energy height, glass transformation temperature height and bandwidth are wide and preparation method thereof.
Background technology
Rare-earth doped optical fibre amplifier is that the gain that utilizes the rear-earth-doped material in the optical fiber to cause realizes light amplification.The most interested rare-earth doped optical fibre of opticfiber communication cable amplifies the composition of the rear-earth-doped tungsten tellurate glass of the present invention:
Ingredient m ol%
TeO
2 65-94.5
WO
3 5-30
MO 0-20
Re
2O
3 0.5-2
Wherein M is a divalent metal element, M=Be, Mg, Ca, Sr, Ba, Pb, Zn;
Re is a rare earth element, is specially Er or Er/Yb mixes altogether, also can expand to other rare earth elements.
Device is that operation wavelength is the erbium-doped fiber amplifier of 1550nm.In recent years, along with develop rapidly, the fiber optic transmission system long haul of computer network and data transport service are growing to message capacity and system extension, be badly in need of having at communication window that bandwidth is wide, the fiber amplifier of flat gain to be to satisfy the service requirements of present wavelength-division multiplex system.The conventional used optical fiber of erbium-doped fiber amplifier is the silica fibre of er-doped, and its flat gain district is narrower and gain fluctuation is bigger.Tellurate glass is considered to improve the substrate material of wdm system transmission capacity owing to its fluorescence halfwidth (FWHM) with bigger emission cross section and broad, thereby causes people's extensive concern.
Compare Er with silica glass
3+Ion has bigger solvability in tellurate glass, thereby may realize high-concentration dopant and serious agglomeration does not take place.Yet tellurate glass is as mixing Er
3+Substrate material exist weak point: the lower (770cm of its phonon energy
-1) last conversion takes place easily and can not adopt the laser diode LD of 980nm to carry out pumping; In addition, the transition temperature of tellurate glass is lower, approximately has only 290 ℃, causes the thermal damage of glass when pumping light power is strong easily.Therefore, needing to seek a kind of phonon energy height, glass transformation temperature height, is very necessary with the wide glass of Time Bandwidth.
Summary of the invention
The present invention be directed to the low and low deficiency of glass transformation temperature of existing tellurate glass phonon energy, a kind of rear-earth-doped tungsten tellurate glass and preparation method thereof is provided, this glass has phonon energy height, glass transformation temperature height and the wide characteristics of bandwidth.
Technical solution of the present invention is as follows:
The preparation method of the rear-earth-doped tungsten tellurate glass of the present invention adopts traditional melt casting method, comprise the following steps: according to above-mentioned composition, the compositing formula of selected glass, take by weighing certain frit, stir, put into corundum crucible then, place the globars electric furnace to found, glass melting temperature is controlled at 750～800 ℃, being cooled to 650 ℃～700 ℃ after the homogenizing clarification comes out of the stove, after glass melt being poured on the mould of prior preheating, put it into fast in the retort furnace that has been warming up to its transition temperature (Tg), be incubated after 2 hours, be annealed to about 275 ℃ with 10 ℃/hour speed, and then after being annealed to 50 ℃ with 20 ℃/hour speed, close retort furnace, naturally cool to room temperature.
The experiment proved that, compare that er-doped tungsten tellurate glass of the present invention has the fluorescence halfwidth of broad with erbium-doped tellurate glass; 290 ℃ of glass transformation temperatures that are higher than erbium-doped tellurate glass; Phonon energy 930cm
-1,, can adopt 980nmLD to carry out pumping and upward conversion of difficult generation greater than the phonon energy of erbium-doped tellurate glass.Therefore er-doped tungsten tellurate glass can be used as a kind of good broadband amplifier substrate material.
Description of drawings
Fig. 1 is the fluorescence spectrum of er-doped tungsten tellurate glass of the present invention.
Fig. 2 is the Raman spectrum of unadulterated tungsten tellurate glass.
Embodiment
Table 1 has provided the glass ingredient of 7 specific embodiments of tungsten tellurate glass of the present invention.Described composition is molar percentage.In order to obtain the opticglass of good uniformity, no bubble and striped, need strict melting technology and envrionment conditions.Below in conjunction with specific embodiment the present invention is further elaborated.
Table 1 tungsten tellurate glass is formed (mol ratio)
Original composition 1# 2# 3# 4# 5# 6# 7#
TeO
2 65 70 75 80 85 90 94.5
WO
3 30 8 6 15 10 5 5
BeO 4 — — — — — —
MgO — 20 — — — — —
CaO — — 18 — — — —
SrO — — — 3 — — —
BaO — — — — 4.5 — —
PbO — — — — — 4 —
ZnO — — — — — — 0
Er
2O
3 1 2 1 2 0.5 1 0.5
Er
2O
3Also can be Er
2O
3/ Yb
2O
3Mix altogether.
The preparation process of 1: the 1# component of embodiment:
Step 1: accurately take by weighing raw material by above-mentioned prescription, mix;
Step 2: compound is put into corundum crucible, place 800 ℃ silicon carbon rod electric furnace fusion;
Step 3: behind the glass melting, under oxygen atmosphere, stir;
Step 4: stop the ventilation, clarification and homogenization, then glass is cooled to 700 ℃ after, pour in the mould of preheating;
Step 5: fast glass is put into the retort furnace that is warming up to 375 ℃, be incubated after 2 hours, be annealed to about 275 ℃, and then after being annealed to 50 ℃ with 20 ℃/hour speed, close retort furnace, be cooled to room temperature with 10 ℃/hour speed.
Preparation technologies of all the other each group are close with first group, and temperature of fusion and annealing temperature are definite according to glass ingredient.It is 395 ℃ that experiment records glass transformation temperature Tg, does not have the crystallization peak, illustrates that the devitrification resistance of glass can better be suitable for the drawing of large size making and optical fiber.Fig. 1 is the fluorescence spectrum of er-doped tungsten tellurate glass, Er as can be seen
3+Fluorescence halfwidth (FWHM) be 67nm, greater than Er in phosphate glass and the silicate glass
3+The fluorescence halfwidth, satisfy the requirement of amplifying as the broadband.Fig. 2 is the Raman spectrum of unadulterated tungsten tellurate glass, and the phonon energy of tungsten tellurate glass is 930cm as we know from the figure
-1, this value can reduce and go up conversion greater than the phonon energy of tellurate glass.
Claims (2)
1, a kind of rear-earth-doped tungsten tellurate glass is characterized in that its composition:
Form content mol%
TeO
2 65-94.5
WO
3 5-30
MO 0-20
Re
2O
3 0.5-2
Wherein M is a divalent metal element, M=Be, Mg, Ca, Sr, Ba, Pb, Zn;
Re is a rare earth element, is specially Er or Er/Yb mixes altogether, also can expand to other rare earth elements.
2, the preparation method of rear-earth-doped tungsten tellurate glass according to claim 1 is characterized in that comprising the following steps being:
Compositing formula according to the selected glass of claim 1, take by weighing certain frit, stir, put into corundum crucible then, place the globars electric furnace to found, glass melting temperature is controlled at 750～800 ℃, being cooled to 650 ℃～700 ℃ after the homogenizing clarification comes out of the stove, after glass melt being poured on the mould of prior preheating, put it into fast in the retort furnace that has been warming up to its transition temperature, be incubated after 2 hours, be annealed to about 275 ℃ with 10 ℃/hour speed, and then after being annealed to 50 ℃ with 20 ℃/hour speed, close retort furnace, naturally cool to room temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410053439 CN1587139A (en) | 2004-08-04 | 2004-08-04 | rare earth doped tungsten tellurate glass and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410053439 CN1587139A (en) | 2004-08-04 | 2004-08-04 | rare earth doped tungsten tellurate glass and preparation method thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1587139A true CN1587139A (en) | 2005-03-02 |
Family
ID=34602855
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|---|---|---|---|
| CN 200410053439 Pending CN1587139A (en) | 2004-08-04 | 2004-08-04 | rare earth doped tungsten tellurate glass and preparation method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058516A (en) * | 2013-01-17 | 2013-04-24 | 中国科学院上海光学精密机械研究所 | High-concentration erbium ion doped tellurium tungstate glass capable of emitting light at mid-infrared 2.7 microns |
| CN105957803A (en) * | 2016-06-13 | 2016-09-21 | 四川洪芯微科技有限公司 | Passivation method of semiconductor device and semiconductor device |
| CN107235640A (en) * | 2017-06-29 | 2017-10-10 | 佛山科学技术学院 | A kind of Nd3+/Ho3+It is co-doped with realizing tellurate optical fiber of 2.0 μm of laser and preparation method thereof |
-
2004
- 2004-08-04 CN CN 200410053439 patent/CN1587139A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103058516A (en) * | 2013-01-17 | 2013-04-24 | 中国科学院上海光学精密机械研究所 | High-concentration erbium ion doped tellurium tungstate glass capable of emitting light at mid-infrared 2.7 microns |
| CN105957803A (en) * | 2016-06-13 | 2016-09-21 | 四川洪芯微科技有限公司 | Passivation method of semiconductor device and semiconductor device |
| CN107235640A (en) * | 2017-06-29 | 2017-10-10 | 佛山科学技术学院 | A kind of Nd3+/Ho3+It is co-doped with realizing tellurate optical fiber of 2.0 μm of laser and preparation method thereof |
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