CN103058516A - High-concentration erbium ion doped tellurium tungstate glass capable of emitting light at mid-infrared 2.7 microns - Google Patents
High-concentration erbium ion doped tellurium tungstate glass capable of emitting light at mid-infrared 2.7 microns Download PDFInfo
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- CN103058516A CN103058516A CN2013100175196A CN201310017519A CN103058516A CN 103058516 A CN103058516 A CN 103058516A CN 2013100175196 A CN2013100175196 A CN 2013100175196A CN 201310017519 A CN201310017519 A CN 201310017519A CN 103058516 A CN103058516 A CN 103058516A
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Abstract
The invention discloses a high-concentration erbium ion doped tellurium tungstate glass capable of emitting light at mid-infrared 2.7 microns. The glass comprises the following components by molar percent: 58-70% of TeO2, 15-25% of WO3, 0-15% of La2O3, 0-15% of LaF3 and 2-4% of Er2O3. The glass is prepared by adopting an electric furnace melting method of a corundum crucible and a silicon carbide rod. The glass is high in doping concentration of erbium ion, high in infrared transmittance near to the mid-infrared 2.7 microns and good in physicochemical properties; and the stability parameter delta T is not less than 180 DEG C. Strong mid-infrared 2.7 microns fluorescence is obtained under pumping of a laser diode with a wavelength of 980 nm; and the glass is suitable for preparation and application of erbium ion doped special glass and optical fiber materials capable of emitting light at mid-infrared 2.7 microns.
Description
Technical field
The present invention relates to glass, particularly a kind of high density erbium ion-doped in infrared 2.7 mu m luminous tellurium tungstate glasses.
Background technology
Erbium ion 2.7 μ m Laser outputs at first obtain by erbium ion-doped crystal.In recent years, the solid statelaser for erbium ion-doped 2.7 μ m output has caused investigator's concern because of its important application in medical surgery, remote sensing, biotechnology and military field.1967 in the LiYF4 crystal reported first pulse of 3 μ m and continuous laser output.1988, the Pollack reported first erbium ion-doped ZBLAN fluoride fiber because Er
3+:
4I
11/2→
4I
13/2Transition obtains centre wavelength at 2.78 μ m, and the output energy is the Laser output of 75J.2008, Zhu etc. obtained the output of watt level laser in the ZBLAN fluoride fiber, and investigators obtain nearly 10 watts and obtain 24 watts Laser output under the liquid cooling condition in succession afterwards.But because the crystal large size is difficult to prepare, doping concentration of rare earth ion is little and the thermostability of ZBLAN glass and chemical stability are relatively poor, their application in 3 μ m outputs have been limited.
Heavy metal oxide glass such as bismuth germanate glass, tellurate glass, bismuthate glass, has lower phonon energy, and rare earth ion solubleness is high simultaneously, and specific refractory power is high, and transition temperature is higher, and has preferably infrared transmission performance.These character provide guarantee for heavy metal oxide glass as infrared 2.7 mu m luminous realizations in the erbium ion.The tellurium tungstate glass has the feature of above-mentioned heavy metal oxide glass, and has realized the Laser output of 2 μ m, but both at home and abroad at present to realize the erbium ion list mix in research not all reports also of infrared 2.7 mu m luminous tellurium tungstate glasses.
Summary of the invention
The technical problem to be solved in the present invention be to provide a kind of high density erbium ion-doped in infrared 2.7 mu m luminous tellurium tungstate glasses, this glass has good thermostability, infrared transmission performance preferably, 980nm wavelength laser diode-pumped lower can obtain very strong in infrared 2.7 μ m fluorescence.
The concrete technical solution of the present invention is as follows:
Infrared 2.7 mu m luminous tellurium tungstate glasses during a kind of high density is erbium ion-doped, its characteristics are that the molar percentage of this glass consists of:
Form mol%
TeO
2 58～70，
WO
3 15～25，
La
2O
3 0～15，
LaF
3 0～15，
Er
2O
3 2～4。
The preparation method of infrared 2.7 mu m luminous tellurium tungstate glasses comprised the following steps: during above-mentioned high density was erbium ion-doped
1. selected described glass forms and molar percentage, calculates the weight that corresponding each glass forms, and accurately takes by weighing each raw material, mixes the formation compound;
2. compound is put into corundum crucible and melted in 1200～1250 ℃ globars electric furnace, fusing time is 15～20 minutes;
3. after material to be mixed melts fully, clarified 10～15 minutes, glass metal is cast in the mould of preheating;
4. glass is moved into rapidly be warming up to and is lower than glass transformation temperature (T
g) in 10 ℃ the retort furnace, be incubated 8～12 hours, be down to room temperature with 10 ℃/hour speed again, take out glass sample fully after the cooling.
Technique effect of the present invention is as follows:
Infrared 2.7 mu m luminous tellurium tungstate glasses during high density of the present invention is erbium ion-doped, by introducing the rare earth ion erbium ion in the tellurium tungstate glass, can obtain in very strong infrared 2.7 mu m luminous, glass Rare Earth Ion doping content is high, in near the infrared 2.7 μ m infrared transmittivity high, excellent in physical and chemical performance, stability parameter Δ T 〉=180 ℃.Can obtain 2.7 very strong μ m fluorescent emission at the laser diode-pumped lower of 980nm wavelength, preparation and the application of infrared 2.7 μ m laser glasses and fiber optic materials in being applicable to.
Description of drawings
Fig. 1 is embodiment 1
#The differential thermal curve of infrared 2.7 mu m luminous tellurium tungstate glasses during the high density that obtains is erbium ion-doped.
Fig. 2 is embodiment 1
#The infrared spectrum that sees through of infrared 2.7 mu m luminous tellurium tungstate glasses during the high density that obtains is erbium ion-doped.
Fig. 3 is embodiment 1
#The fluorescence spectrum under 980nm wavelength laser diode-pumped of infrared 2.7 mu m luminous tellurium tungstate glasses during the high density that obtains is erbium ion-doped.
Fig. 4 is embodiment 1
#To 3
#The fluorescence spectrum comparison diagram under the erbium ion-doped concentration conditions of laser diode-pumped lower difference of 980nm wavelength of infrared 2.7 mu m luminous tellurium tungstate glasses during the high density that obtains is erbium ion-doped.
Embodiment
The glass ingredient of 9 of infrared 2.7 mu m luminous tellurium tungstate glasses specific embodiments was as shown in table 1 during high density of the present invention was erbium ion-doped:
Table 1: the glass formula of concrete 9 embodiment
Embodiment 1
#:
Form as in the table 11
#Shown in, concrete preparation process is as follows:
According in the table 11
#The molar percentage that glass forms calculates corresponding each weight that forms, and takes by weighing each raw material and mixes; Compound is put into corundum crucible melt in 1200 ℃ globars electric furnace, material to be mixed melts rear clarification 15 minutes fully, glass metal is cast in the mould of preheating; Glass is moved into rapidly in the retort furnace that has been warming up to 420 ℃, is incubated 10 hours, be down to room temperature with 10 ℃/hour speed again, take out glass sample fully after the cooling.
Test result to this glass is as follows:
Get a little sample after the annealing, wear into fine powdered with agate mortar, carry out the differential thermal analysis test.The differential thermal curve of the erbium ion-doped tellurium tungstate glass of infrared 2.7 mu m luminous high densitys as shown in Figure 1 among the present invention.
Sample after the annealing is processed into sheet glass and the polishing of 20 * 10 * 1.0mm, tests its infrared spectrum that sees through, at its fluorescence spectrum of laser diode-pumped lower test of 980nm wavelength.The infrared of infrared 2.7 mu m luminous tellurium tungstate glasses saw through spectrum as shown in Figure 2 during high density of the present invention was erbium ion-doped.The fluorescence spectrum under 980nm wavelength laser diode-pumped of infrared 2.7 mu m luminous tellurium tungstate glasses as shown in Figure 3 during high density of the present invention was erbium ion-doped.Experiment shows, glass transparent, without crystallization, near the infrared 2.7 μ m infrared transmittivity high, excellent in physical and chemical performance, stability parameter Δ T 〉=180 ℃.980nm wavelength laser diode-pumped lower can obtain very strong in infrared 2.7 μ m fluorescence.
Embodiment 2
#:
Form as in the table 12
#Shown in, concrete preparation process is as follows:
According in the table 12
#The molar percentage that glass forms calculates corresponding each weight that forms, and takes by weighing each raw material and mixes; Compound is put into corundum crucible melt in 1200 ℃ globars electric furnace, material to be mixed melts rear clarification 15 minutes fully, glass metal is cast in the mould of preheating; Glass is moved into rapidly in the retort furnace that has been warming up to 420 ℃, is incubated 10 hours, be down to room temperature with 10 ℃/hour speed again, take out glass sample fully after the cooling.
Test result to this glass is as follows:
Get a little sample after the annealing, wear into fine powdered with agate mortar, carry out the differential thermal analysis test.
Sample after the annealing is processed into sheet glass and the polishing of 20 * 10 * 1.0mm, tests its infrared spectrum that sees through, at its fluorescence spectrum of laser diode-pumped lower test of 980nm wavelength.
Embodiment 3
#:
Form as in the table 13
#Shown in, concrete preparation process is as follows:
According in the table 13
#The molar percentage that glass forms calculates corresponding each weight that forms, and takes by weighing each raw material and mixes; Compound is put into corundum crucible melt in 1200 ℃ globars electric furnace, material to be mixed melts rear clarification 15 minutes fully, glass metal is cast in the mould of preheating; Glass is moved into rapidly in the retort furnace that has been warming up to 420 ℃, is incubated 10 hours, be down to room temperature with 10 ℃/hour speed again, take out glass sample fully after the cooling.
Test result to this glass is as follows:
Get a little sample after the annealing, wear into fine powdered with agate mortar, carry out the differential thermal analysis test.
Sample after the annealing is processed into sheet glass and the polishing of 20 * 10 * 1.0mm, tests its infrared spectrum that sees through, at its fluorescence spectrum of laser diode-pumped lower test of 980nm wavelength.
Above-described embodiment test shows, all have high density that embodiment 1 obtains erbium ion-doped in Fig. 1, Fig. 2, differential thermal curve shown in Figure 3, the infrared similar results that sees through the laser diode-pumped lower fluorescence spectrum of spectrum and 980nm wavelength of infrared 2.7 mu m luminous tellurium tungstate glasses.The embodiment of the invention 1
#To 3
#The fluorescence spectrum comparison diagram under the erbium ion-doped concentration conditions of laser diode-pumped lower difference of 980nm wavelength of infrared 2.7 mu m luminous tellurium tungstate glasses as shown in Figure 4 during the high density that obtains was erbium ion-doped.Experiment show high density of the present invention erbium ion-doped in infrared 2.7 mu m luminous tellurium tungstate glasses, near the infrared 2.7 μ m infrared transmittivity high, excellent in physical and chemical performance, stability parameter Δ T 〉=180 ℃.980nm wavelength laser diode-pumped lower can obtain very strong in infrared 2.7 μ m fluorescent emission, under the erbium ion-doped condition of high density without fluorescent quenching, preparation and the application of infrared 2.7 μ m laser glasses and fiber optic materials in being applicable to.
Embodiment 4
#To 9
#:
Form as in the table 14
#To 9
#Shown in, concrete preparation process such as embodiment 1
#
Test result to this glass is as follows:
Get a little sample after the annealing, wear into fine powdered with agate mortar, carry out the differential thermal analysis test.
Sample after the annealing is processed into sheet glass and the polishing of 20 * 10 * 1.0mm, tests its infrared spectrum that sees through, at its fluorescence spectrum of laser diode-pumped lower test of 980nm wavelength.
Above-described embodiment test shows, all have high density that embodiment 1 obtains erbium ion-doped in Fig. 1, Fig. 2 of infrared 2.7 mu m luminous tellurium tungstate glasses and differential thermal curve shown in Figure 3, the infrared similar results that sees through the laser diode-pumped lower fluorescence spectrum of spectrum and 980nm wavelength.The experiment show high density of the present invention erbium ion-doped in infrared 2.7 mu m luminous tellurium tungstate glasses, Heat stability is good (stability parameter Δ T 〉=160 ℃), in near the infrared 2.7 μ m infrared transmittivity high, excellent in physical and chemical performance, erbium ion-doped concentration is high, in infrared 2.7 mu m luminous strong, be applicable to as in infrared 2.7 μ m laser host materials.
Claims (2)
- A high density erbium ion-doped in infrared 2.7 mu m luminous tellurium tungstate glasses, it is characterized in that its molar percentage consists of:Form mol%TeO 2 58～70，WO 3 15～25，La 2O 3 0～15，LaF 3 0～15，Er 2O 3 2～4。
- High density according to claim 1 erbium ion-doped in infrared 2.7 mu m luminous tellurium tungstate glasses, it is characterized in that infrared 2.7 μ m fluorescence during erbium ion can obtain in the described glass under the 980nm pump light excites.And when erbium ion-doped concentration reached 3mol%, fluorescent quenching can not occur in infrared 2.7 μ m fluorescence in the erbium ion.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108690605A (en) * | 2018-06-28 | 2018-10-23 | 河南大学 | A kind of stannous methide functionalization and include polyacid mixing constructing block erbium insertion tellurium tungstate material and the preparation method and application thereof |
| CN108751697A (en) * | 2018-08-20 | 2018-11-06 | 长春理工大学 | A kind of high concentration rare earth doping tellurium tungsten lanthanum glass and preparation method thereof |
| CN109369007A (en) * | 2018-11-16 | 2019-02-22 | 华南理工大学 | 2.7 mu m luminous high-concentration dopant tellurium gallium zinc laser glasses of one kind and preparation method thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02217334A (en) * | 1989-02-15 | 1990-08-30 | Toshiba Glass Co Ltd | Filter glass for cutting near infrared ray |
| CN1587139A (en) * | 2004-08-04 | 2005-03-02 | 中国科学院上海光学精密机械研究所 | Rare-earth blended tungstotellurate glass and its preparing method |
-
2013
- 2013-01-17 CN CN2013100175196A patent/CN103058516A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02217334A (en) * | 1989-02-15 | 1990-08-30 | Toshiba Glass Co Ltd | Filter glass for cutting near infrared ray |
| CN1587139A (en) * | 2004-08-04 | 2005-03-02 | 中国科学院上海光学精密机械研究所 | Rare-earth blended tungstotellurate glass and its preparing method |
Non-Patent Citations (2)
| Title |
|---|
| GUOYING ZHAO等: "Efficient 2.7-μm emission in Er3+-doped bismuth germinate glass pumped by 980-nm laser diode", 《CHINESE OPTICS LETTERS》 * |
| 肖凯等: "Er3+掺杂钡镓锗玻璃上转换荧光淬灭机理研究", 《稀有技术材料与工程》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108690605A (en) * | 2018-06-28 | 2018-10-23 | 河南大学 | A kind of stannous methide functionalization and include polyacid mixing constructing block erbium insertion tellurium tungstate material and the preparation method and application thereof |
| CN108690605B (en) * | 2018-06-28 | 2020-10-02 | 河南大学 | Dimethyl tin functionalized tellurium tungstate material embedded with polyacid mixed building block erbium, and preparation method and application thereof |
| CN108751697A (en) * | 2018-08-20 | 2018-11-06 | 长春理工大学 | A kind of high concentration rare earth doping tellurium tungsten lanthanum glass and preparation method thereof |
| CN109369007A (en) * | 2018-11-16 | 2019-02-22 | 华南理工大学 | 2.7 mu m luminous high-concentration dopant tellurium gallium zinc laser glasses of one kind and preparation method thereof |
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Application publication date: 20130424 |