CN114455845B - Er 3+ /Yb 3+ /Nd 3+ Codoped near-infrared ultra-wideband emission tellurate optical fiber glass and preparation method thereof - Google Patents
Er 3+ /Yb 3+ /Nd 3+ Codoped near-infrared ultra-wideband emission tellurate optical fiber glass and preparation method thereof Download PDFInfo
- Publication number
- CN114455845B CN114455845B CN202210060392.5A CN202210060392A CN114455845B CN 114455845 B CN114455845 B CN 114455845B CN 202210060392 A CN202210060392 A CN 202210060392A CN 114455845 B CN114455845 B CN 114455845B
- Authority
- CN
- China
- Prior art keywords
- optical fiber
- glass
- fiber glass
- tellurate
- 20mol
- 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.)
- Active
Links
Images
Classifications
-
- 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
- C03C13/00—Fibre or filament compositions
- C03C13/04—Fibre optics, e.g. core and clad fibre compositions
- C03C13/048—Silica-free oxide glass compositions
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
-
- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/02—Manufacture of glass fibres or filaments by drawing or extruding, e.g. direct drawing of molten glass from nozzles; Cooling fins therefor
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Materials Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Optics & Photonics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Glass Compositions (AREA)
- Lasers (AREA)
Abstract
The invention provides an Er 3+ /Yb 3+ /Nd 3+ The co-doped near-infrared ultra-wideband emission tellurate optical fiber glass and the preparation method thereof solve the problem of Er in the prior art 3+ The single tellurate doped optical fiber glass has the technical problems of poor thermal stability, low luminous intensity and narrow bandwidth, and Er is added according to the mol percentage 3+ /Yb 3+ /Nd 3+ The co-doped near-infrared ultra-wideband emission tellurate optical fiber glass comprises the following raw materials: TeO 2 :46.3~47mol%;WO 3 :20mol%;ZnO:20mol%;Na 2 O:5mol%;Ta 2 O 5 :5mol%;Er 2 O 3 :0.5~1mol%;Yb 2 O 3 :2.1~2.5mol%;Nd 2 O 3 : 0.11-0.4 mol%, the invention also discloses Er 3+ /Yb 3+ /Nd 3+ The preparation method of the co-doped near-infrared ultra-wideband emission tellurate optical fiber glass can be widely applied to the field of optical fiber communication materials.
Description
Technical Field
The invention belongs to the field of optical fiber communication materials, and particularly relates to Er 3+ /Yb 3+ /Nd 3+ Co-doped near-infrared ultra-wideband emission tellurate optical fiber glass and a preparation method thereof.
Background
In recent years, with the rapid development of optical communication systems and high-speed transmission systems, it is required to expand the gain bandwidth of an optical fiber amplifier in a Wavelength Division Multiplexing (WDM) system, and thus it has been a hot spot of research to obtain a wider and more efficient gain bandwidth. Erbium-doped fiber amplifiers (EDFAs), Er being one of the key components for optical communication in WDM network systems 3+ The ion-doped tellurate optical fiber glass plays an important role in the development of the EDFA. However, currently Er 3+ The single tellurate doped optical fiber glass has the problems of poor thermal stability, low luminous intensity and narrow bandwidth, can not meet the requirement of communication development, and greatly limits the application of the single tellurate doped optical fiber glass in the field of erbium-doped optical fiber amplifiers.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention provides Er 3+ /Yb 3+ /Nd 3+ The co-doped near-infrared ultra-wideband emission tellurate optical fiber glass and the preparation method thereof improve the thermal stability and near-infrared luminous intensity of the tellurate optical fiber glass and obtain wider and more efficient gain bandwidth.
To solve the above technical problems, the present invention provides an Er 3+ /Yb 3+ /Nd 3+ The co-doped near-infrared ultra-wideband emission tellurate optical fiber glass comprises the following raw materials in percentage by mole:
TeO 2 :46.3~47mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 O:5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :0.5~1mol%;
Yb 2 O 3 :2.1~2.5mol%;
Nd 2 O 3 :0.11~0.4mol%。
preferably, the raw materials comprise the following components in percentage by mole:
TeO 2 :46.39mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 O:5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :1mol%;
Yb 2 O 3 :2.5mol%;
Nd 2 O 3 :0.11mol%。
preferably, the raw materials comprise the following components in percentage by mole:
TeO 2 :46.3mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 O:5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :1mol%;
Yb 2 O 3 :2.5mol%;
Nd 2 O 3 :0.2mol%。
preferably, Na 2 O is Na 2 CO 3 Is incorporated in the form of, i.e. Na 2 O is formed from an equimolar amount of Na 2 CO 3 Instead. Na (Na) 2 O mainly adds Na + Due to Na 2 O is poor in stability in air, so Na is used 2 CO 3 Decomposition at high temperature can produce Na 2 The reaction of O can also be carried out by adding Na + The function of (1).
Er of any one of the above 3+ /Yb 3+ /Nd 3+ The method for co-doping the near-infrared ultra-wideband emission tellurate optical fiber glass comprises the following steps:
(1) weighing the raw materials according to the mol percentage for later use;
(2) putting the raw material obtained in the step (1) into an agate mortar for uniform grinding;
(3) putting the raw materials uniformly ground in the step (2) into a corundum crucible, and putting the corundum crucible into a tubular furnace to heat for 40 minutes at 920-950 ℃ to obtain molten glass liquid; taking out the corundum crucible from the tubular furnace, stirring the molten glass liquid in the corundum crucible for 2 minutes while the corundum crucible is hot, and continuously placing the corundum crucible in the tubular furnace at the temperature of 920-950 ℃ for melting for 20 minutes to obtain molten glass;
(4) pouring the molten glass obtained in the step (3) on a graphite mold which is preheated to 370-400 ℃ for quenching to obtain sheet glass;
preferably, the sheet glass obtained in the step (4) is annealed in a muffle furnace at 370-400 ℃, and after the annealing is completed, the graphite mold filled with tellurate optical fiber glass is taken out from the muffle furnace to obtain the tellurate optical fiber glass sheet.
Preferably, the annealing treatment process of step (5) is as follows: and (3) preserving the heat for 3 hours in a muffle furnace at 370-400 ℃, and then cooling to 50 ℃ at the speed of 15 ℃/h.
Preferably, the tellurate optical fiber glass sheet obtained in the step (5) is thinned until the thickness of the glass sheet is 2mm, and then surface polishing treatment is carried out until the glass sheet is transparent, so that the tellurate optical fiber glass with two polished surfaces is finally obtained.
Preferably, the purity of each raw material is 99.99% by mass.
The invention has the beneficial effects that:
(1) the tellurate glass obtained by the invention has high density, high glass transition temperature and thermal stability parameter delta T far larger than 100 ℃, and can meet the requirements of tellurate optical fiber drawing.
(2) Introduction of small amount of Ta 2 O 5 Improve the glassThermal stability and near infrared luminous intensity of the glass.
(3) Er under the pumping of laser diode with wavelength of 808nm 3+ /Yb 3+ /Nd 3+ The glass can generate an ultra-wideband near-infrared emission spectrum covering from an optical communication O waveband to a U waveband under the combined action.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present application, the drawings needed to be used in the embodiments or the prior art descriptions will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art to obtain other drawings based on these drawings without inventive exercise.
FIG. 1 is a DSC curve of the tellurate glass of example 1, comparative experiment 1;
FIG. 2 is a fluorescence spectrum of the tellurite glass of example 1 and example 2 pumped at a wavelength of 808 nm;
FIG. 3 is a fluorescence spectrum of the tellurite glass of examples 3 and 4 pumped at a wavelength of 808 nm;
FIG. 4 is a graph showing fluorescence spectra of the tellurite glasses of example 1, comparative experiment 1 and comparative experiment 2 pumped at a wavelength of 808 nm.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present application clearer, the present application is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the present application and are not intended to limit the present application. The raw materials and the apparatus used are, unless otherwise specified, conventional commercially available products.
Example 1
The invention provides a method for preparing Er 3+ /Yb 3+ /Nd 3+ The method for co-doping the near-infrared ultra-wideband emission tellurate optical fiber glass comprises the following steps:
(1) weighing the following raw materials according to the following mol percentage, wherein the purity of each raw material is 99.99%;
TeO 2 :46.39mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 CO 3 :5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :1mol%;
Yb 2 O 3 :2.5mol%;
Nd 2 O 3 :0.11mol%。
(2) and (2) putting the raw material obtained in the step (1) into an agate mortar for uniformly grinding.
(3) Putting the raw materials uniformly ground in the step (2) into a corundum crucible, and putting the corundum crucible into a tubular furnace to heat for 40 minutes at 920 ℃ to obtain molten glass liquid; and taking the corundum crucible out of the tubular furnace, stirring the glass liquid in the corundum crucible for 2 minutes while the corundum crucible is hot, and continuously placing the corundum crucible in the tubular furnace at 920 ℃ for melting for 20 minutes to obtain the glass melt.
(4) Pouring the molten glass obtained in the step (3) on a graphite mold which is preheated to 380 ℃ for quenching to obtain sheet glass;
(5) preserving the temperature of the glass sheet obtained in the step (4) in a muffle furnace at 380 ℃ for 3 hours, cooling to 50 ℃ at the speed of 15 ℃/h for annealing, and taking out a graphite mold filled with tellurate optical fiber glass from the muffle furnace to obtain the tellurate optical fiber glass sheet;
(6) and (5) thinning the tellurate optical fiber glass sheet obtained in the step (5) until the thickness of the glass sheet is 2mm, and then performing surface polishing treatment until the glass sheet is transparent to finally obtain the tellurate optical fiber glass with two polished surfaces.
The glass sample finally obtained in example 1 was ground to 200 mesh in a small amount and subjected to a differential thermal analysis test, and the results are shown in FIG. 1. The fluorescence spectrum obtained by testing under the pump of a laser diode with the wavelength of 808nm is shown in FIG. 2.
Example 2
The invention provides a method for preparing Er 3+ /Yb 3+ /Nd 3+ The method for co-doping the near-infrared ultra-wideband emission tellurate optical fiber glass comprises the following steps:
(1) weighing the following raw materials according to the following mol percentage, wherein the purity of each raw material is 99.99%;
TeO 2 :46.3mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 CO 3 :5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :1mol%;
Yb 2 O 3 :2.5mol%;
Nd 2 O 3 :0.2mol%;
(2) and (2) putting the raw material obtained in the step (1) into an agate mortar for uniformly grinding.
(3) Putting the raw materials uniformly ground in the step (2) into a corundum crucible, and putting the corundum crucible into a tubular furnace to heat for 40 minutes at 920 ℃ to obtain molten glass liquid; and taking the corundum crucible out of the tubular furnace, stirring the glass liquid in the corundum crucible for 2 minutes while the corundum crucible is hot, and continuously placing the corundum crucible in the tubular furnace at 920 ℃ for melting for 20 minutes to obtain the glass melt.
(4) Pouring the molten glass obtained in the step (3) on a graphite mold which is preheated to 390 ℃ for quenching to obtain sheet glass;
(5) preserving the temperature of the sheet glass obtained in the step (4) in a muffle furnace at 390 ℃ for 3 hours, then cooling to 50 ℃ at the speed of 15 ℃/h for annealing treatment, and taking out a graphite mold filled with tellurate optical fiber glass from the muffle furnace to obtain tellurate optical fiber glass sheets;
(6) and (5) thinning the tellurate optical fiber glass sheet obtained in the step (5) until the thickness of the glass sheet is 2mm, and then performing surface polishing treatment until the glass sheet is transparent to finally obtain the tellurate optical fiber glass with two polished surfaces.
The fluorescence spectrum of the glass sample finally obtained in example 2 was measured under the pump of a laser diode with a wavelength of 808nm and is shown in FIG. 2.
Example 3
The invention provides a method for preparing Er 3+ /Yb 3+ /Nd 3+ The method for co-doping the near-infrared ultra-wideband emission tellurate optical fiber glass comprises the following steps:
(1) weighing the following raw materials according to the following mol percentage, wherein the purity of each raw material is 99.99%;
TeO 2 :46.8mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 CO 3 :5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :0.5mol%;
Yb 2 O 3 :2.4mol%;
Nd 2 O 3 :0.3mol%;
(2) and (2) putting the raw material obtained in the step (1) into an agate mortar for uniformly grinding.
(3) Putting the raw materials uniformly ground in the step (2) into a corundum crucible, and putting the corundum crucible into a tubular furnace to heat for 40 minutes at 950 ℃ to obtain molten glass liquid; and taking the corundum crucible out of the tubular furnace, stirring the glass liquid in the corundum crucible for 2 minutes while the corundum crucible is hot, and continuously placing the corundum crucible in the tubular furnace at 950 ℃ for melting for 20 minutes to obtain the glass melt.
(4) Pouring the molten glass obtained in the step (3) on a graphite mold which is preheated to 400 ℃ for quenching to obtain sheet glass;
(5) preserving the temperature of the sheet glass obtained in the step (4) in a muffle furnace at 400 ℃ for 3 hours, cooling to 50 ℃ at a speed of 15 ℃/h for annealing, and taking out a graphite mold filled with tellurate optical fiber glass from the muffle furnace to obtain tellurate optical fiber glass sheets;
(6) and (5) thinning the tellurate optical fiber glass sheet obtained in the step (5) until the thickness of the glass sheet is 2mm, and then performing surface polishing treatment until the glass sheet is transparent to finally obtain the tellurate optical fiber glass with two polished surfaces.
The fluorescence spectrum of the glass sample finally obtained in example 3 was measured under the pump of a laser diode with a wavelength of 808nm and is shown in FIG. 3.
Example 4
The invention provides a method for preparing Er 3+ /Yb 3+ /Nd 3+ The method for co-doping the near-infrared ultra-wideband emission tellurate optical fiber glass comprises the following steps:
(1) weighing the following raw materials according to the following mol percentage, wherein the purity of each raw material is 99.99%;
TeO 2 :47mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 CO 3 :5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :0.5mol%;
Yb 2 O 3 :2.1mol%;
Nd 2 O 3 :0.4mol%;
(2) and (2) putting the raw material obtained in the step (1) into an agate mortar for uniformly grinding.
(3) Putting the raw materials uniformly ground in the step (2) into a corundum crucible, and putting the corundum crucible into a tubular furnace to heat for 40 minutes at 950 ℃ to obtain molten glass liquid; and taking the corundum crucible out of the tubular furnace, stirring the glass liquid in the corundum crucible for 2 minutes while the corundum crucible is hot, and continuously placing the corundum crucible in the tubular furnace at 950 ℃ for melting for 20 minutes to obtain the glass melt.
(4) Pouring the molten glass obtained in the step (3) on a graphite mold with the pre-heating temperature of 370 ℃ for quenching to obtain sheet glass;
(5) preserving the temperature of the sheet glass obtained in the step (4) in a muffle furnace at 370 ℃ for 3 hours, cooling to 50 ℃ at a speed of 15 ℃/h for annealing, and taking out a graphite mold filled with tellurate optical fiber glass from the muffle furnace to obtain tellurate optical fiber glass sheets;
(6) and (5) thinning the tellurate optical fiber glass sheet obtained in the step (5) until the thickness of the glass sheet is 2mm, and then performing surface polishing treatment until the glass sheet is transparent to finally obtain the tellurate optical fiber glass with two polished surfaces.
The final glass sample obtained in example 4 was tested under the pump of a laser diode with a wavelength of 808nm to obtain a fluorescence spectrum as shown in FIG. 3.
To better illustrate Ta 2 O 5 The thermal stability and near infrared luminous intensity of tellurate optical fiber glass are improved without introducing Ta 2 O 5 The obtained rare earth doped tellurate optical fiber glass is subjected to a comparative experiment.
Comparative experiment 1: without introduction of Ta 2 O 5 The rare earth doped tellurate optical fiber glass comprises the following components in percentage by mol:
TeO 2 :51.39mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 CO 3 :5mol%;
Er 2 O 3 :1mol%;
Yb 2 O 3 :2.5mol%;
Nd 2 O 3 :0.11mol%;
the procedure is as in example 1 and will not be repeated here.
A small amount of the glass sample obtained in comparative experiment 1 was ground to 200 mesh for differential thermal analysis, and the results are shown in FIG. 1. The fluorescence spectrum obtained by testing under the pump of a laser diode with the wavelength of 808nm is shown in FIG. 4.
For better explanation of Er 3+ /Yb 3+ /Nd 3+ Co-doped and single-doped Er 3+ Compared with the obtained near infrared luminescence with higher intensity and wider wavelength range, the rare earth doped tellurate optical fiber glass is changed into the rare earth doped tellurate optical fiber glass only doped with Er 3+ The obtained rare earth doped tellurate optical fiber glass is subjected to a comparative experiment.
Comparative experiment 2: single doped Er 3+ The rare earth doped tellurate optical fiber glass comprises the following components in percentage by mol:
TeO 2 :49mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 CO 3 :5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :1mol%;
the procedure is as in example 1 and will not be repeated here.
The glass sample obtained in experiment 2 was compared and tested under the pump of a laser diode with wavelength of 808nm to obtain a fluorescence spectrum as shown in FIG. 4.
As shown in FIG. 1, the glass transition temperature T in example 1 g 397 ℃ and glass crystallization onset temperature T x 539 ℃ and a thermal stability parameter Δ T ═ T (T) x -T g ) 142 ℃. Glass transition temperature T in comparative experiment 1 g 366 ℃ and the glass crystallization onset temperature T x At 483 deg.C, the thermal stability parameter Δ T ═ T (T) x -T g ) 117 ℃. Experiments show that: ta 2 O 5 The introduction of (A) significantly increases the glass transition temperature T g And thermal stability, making the glass more resistant to thermal shock. The prepared tellurate optical fiber glass can meet the requirement of optical fiber drawing experiment (delta T)>100℃)。
As shown in FIG. 2 and FIG. 3, the fluorescence experiment results show that Er is pumped by a laser diode with the wavelength of 808nm 3+ /Yb 3+ /Nd 3+ The fluorescence spectrum band of the co-doped tellurate optical fiber glass is 850-1700 nm. The spectrum has four luminescence centers, located around 876nm, 1000nm, 1332nm and 1530nm, respectively.
As can be seen from FIG. 4, Ta 2 O 5 The luminous intensity of the band of 876nm, 1000nm and 1530nm is improved, and the improvement of the band of 1530nm is most obvious. And single doped Er 3+ In contrast, Yb 3+ /Nd 3+ After addition, Yb 3+ By means of energy transmissionEnhanced Er 3+ Absorption efficiency of pump light, and Yb 3+ Can absorb part of Nd 3+ Energy transfer of (2) to Er 3+ 。Nd 3+ Absorbing the energy of the excitation light source can produce new emission peaks around 900 and 1300 nm. Thus Er 3+ /Yb 3+ /Nd 3+ The combined action enables the fluorescence spectrum to emit light in two wave bands of 850-920 nm and 1300-1400 nm, the light-emitting wavelength covers the optical communication O wave band to the U wave band, and the light-emitting intensity is obviously enhanced.
The invention provides an Er 3+ /Yb 3+ /Nd 3+ The tellurate glass prepared by the method has high transition temperature, the thermal stability performance parameter delta T is far more than 100 ℃, and the requirement of tellurate optical fiber drawing can be met; introduction of small amount of Ta 2 O 5 The thermal stability and the near-infrared luminous intensity of the glass are improved; er under the pumping of laser diode with wavelength of 808nm 3+ /Yb 3+ /Nd 3+ The glass can generate an ultra-wideband near-infrared emission spectrum covering from an optical communication O waveband to a U waveband under the combined action. It has great application prospect in the aspect of optical amplifiers.
The above description is only exemplary of the present application and should not be taken as limiting the present application, as any modification, equivalent replacement, or improvement made within the spirit and principle of the present application should be included in the protection scope of the present application.
Claims (6)
1. Er 3+ /Yb 3+ /Nd 3+ The co-doped near-infrared ultra-wideband emission tellurate optical fiber glass is characterized by comprising the following raw materials in percentage by mole:
TeO 2 :46.3~47mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 O:5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :0.5~1mol%;
Yb 2 O 3 :2.1~2.5mol%;
Nd 2 O 3 :0.11~0.4mol%。
2. an Er according to claim 1 3+ /Yb 3+ /Nd 3+ The co-doped near-infrared ultra-wideband emission tellurate optical fiber glass is characterized by comprising the following raw materials in percentage by mole:
TeO 2 :46.39mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 O:5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :1mol%;
Yb 2 O 3 :2.5mol%;
Nd 2 O 3 :0.11mol%。
3. an Er according to claim 1 3+ /Yb 3+ /Nd 3+ The co-doped near-infrared ultra-wideband emission tellurate optical fiber glass is characterized by comprising the following raw materials in percentage by mole:
TeO 2 :46.3mol%;
WO 3 :20mol%;
ZnO:20mol%;
Na 2 O:5mol%;
Ta 2 O 5 :5mol%;
Er 2 O 3 :1mol%;
Yb 2 O 3 :2.5mol%;
Nd 2 O 3 :0.2mol%。
4. an Er according to any one of claims 1-3 3+ /Yb 3+ /Nd 3+ Co-doped near-infrared ultra-wideband emission tellurateOptical fiber glass characterized in that said Na 2 O is Na 2 CO 3 Is incorporated in the form of (1).
5. Preparation of an Er according to any one of claims 1 to 4 3+ /Yb 3+ /Nd 3+ The method for co-doping the near-infrared ultra-wideband emission tellurate optical fiber glass is characterized by comprising the following steps of:
(1) weighing the raw materials according to the mol percentage for later use;
(2) putting the raw material obtained in the step (1) into an agate mortar for uniform grinding;
(3) putting the raw materials uniformly ground in the step (2) into a corundum crucible, and putting the corundum crucible into a tubular furnace to heat for 40 minutes at 920-950 ℃ to obtain molten glass liquid; taking out the corundum crucible from the tubular furnace, stirring the molten glass liquid in the corundum crucible for 2 minutes while the corundum crucible is hot, and continuously placing the corundum crucible in the tubular furnace at the temperature of 920-950 ℃ for melting for 20 minutes to obtain molten glass;
(4) pouring the molten glass obtained in the step (3) on a graphite mold with the well-preheated temperature of 370-400 ℃ for quenching to obtain sheet glass;
(5) annealing the sheet glass obtained in the step (4) in a muffle furnace at 370-400 ℃, and taking out the graphite mold filled with tellurate optical fiber glass from the muffle furnace after the annealing is completed to obtain tellurate optical fiber glass sheets;
the annealing treatment process of the step (5) comprises the following steps: preserving heat for 3 hours in a muffle furnace at 370-400 ℃, and then cooling to 50 ℃ at the speed of 15 ℃/h;
and (5) thinning the tellurate optical fiber glass sheet obtained in the step (5) until the thickness of the glass sheet is 2mm, and then performing surface polishing treatment until the glass sheet is transparent to finally obtain the tellurate optical fiber glass with two polished surfaces.
6. The method of claim 5, wherein each of the raw materials has a purity of 99.99% by mass.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210060392.5A CN114455845B (en) | 2022-01-19 | 2022-01-19 | Er 3+ /Yb 3+ /Nd 3+ Codoped near-infrared ultra-wideband emission tellurate optical fiber glass and preparation method thereof |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN202210060392.5A CN114455845B (en) | 2022-01-19 | 2022-01-19 | Er 3+ /Yb 3+ /Nd 3+ Codoped near-infrared ultra-wideband emission tellurate optical fiber glass and preparation method thereof |
Publications (2)
Publication Number | Publication Date |
---|---|
CN114455845A CN114455845A (en) | 2022-05-10 |
CN114455845B true CN114455845B (en) | 2022-08-02 |
Family
ID=81409571
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
---|---|---|---|
CN202210060392.5A Active CN114455845B (en) | 2022-01-19 | 2022-01-19 | Er 3+ /Yb 3+ /Nd 3+ Codoped near-infrared ultra-wideband emission tellurate optical fiber glass and preparation method thereof |
Country Status (1)
Country | Link |
---|---|
CN (1) | CN114455845B (en) |
Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1378523A (en) * | 1999-10-12 | 2002-11-06 | 康宁股份有限公司 | Tellurite glasses and optical components |
CN1587138A (en) * | 2004-07-13 | 2005-03-02 | 中国科学院上海光学精密机械研究所 | Yb3+ blended tellurate glass and its preparing method |
KR20070002941A (en) * | 2005-06-30 | 2007-01-05 | 한국전자통신연구원 | Tellurite glass composite, optical waveguide and optical amplifier using the same |
KR20130119048A (en) * | 2012-04-23 | 2013-10-31 | 광주과학기술원 | Optical glass for gain medium with high fluorescence efficiency and optical fiber using the optical glass |
CN112429965A (en) * | 2020-11-11 | 2021-03-02 | 中国科学院上海硅酸盐研究所 | Near-infrared light-emitting heavy metal oxide glass material with ultra-wide processing temperature range |
CN112897878A (en) * | 2021-02-06 | 2021-06-04 | 威海长和光导科技有限公司 | Near-infrared band ultra-wideband emission Bi-Er-Tm co-doped tellurate optical fiber glass and preparation method thereof |
-
2022
- 2022-01-19 CN CN202210060392.5A patent/CN114455845B/en active Active
Patent Citations (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN1378523A (en) * | 1999-10-12 | 2002-11-06 | 康宁股份有限公司 | Tellurite glasses and optical components |
CN1587138A (en) * | 2004-07-13 | 2005-03-02 | 中国科学院上海光学精密机械研究所 | Yb3+ blended tellurate glass and its preparing method |
KR20070002941A (en) * | 2005-06-30 | 2007-01-05 | 한국전자통신연구원 | Tellurite glass composite, optical waveguide and optical amplifier using the same |
KR20130119048A (en) * | 2012-04-23 | 2013-10-31 | 광주과학기술원 | Optical glass for gain medium with high fluorescence efficiency and optical fiber using the optical glass |
CN112429965A (en) * | 2020-11-11 | 2021-03-02 | 中国科学院上海硅酸盐研究所 | Near-infrared light-emitting heavy metal oxide glass material with ultra-wide processing temperature range |
CN112897878A (en) * | 2021-02-06 | 2021-06-04 | 威海长和光导科技有限公司 | Near-infrared band ultra-wideband emission Bi-Er-Tm co-doped tellurate optical fiber glass and preparation method thereof |
Non-Patent Citations (1)
Title |
---|
Improvement of ultra-broadband near-infrared emission in Nd3+-Er3+-Pr3+ tri-doped tellurite glasses;Hou Guangning et al.;《Optical Materials》;20201029;第111卷;第1-6页 * |
Also Published As
Publication number | Publication date |
---|---|
CN114455845A (en) | 2022-05-10 |
Similar Documents
Publication | Publication Date | Title |
---|---|---|
Stevenson et al. | Fluoride materials for optical applications: Single crystals, ceramics, glasses, and glass–ceramics | |
CN102659313B (en) | Near-infrared broadband luminescence erbium and thulium-co-doped bismuthate laser glass and preparation method thereof | |
CN111377609B (en) | Preparation method of transparent glass with mid-infrared 3.9 mu m luminescence characteristic at room temperature | |
CN100513339C (en) | Rare earth doped gallium germanium bismuth lead luminous glass material and its preparation method and uses | |
CN112010557A (en) | Transparent glass with middle infrared 3.5 mu m luminescence characteristic and preparation method thereof | |
CN103011593A (en) | Erbium neodymium ion co-doped tellurium fluoride glass for emitting 2.7 microns of intermediate infrared light | |
CN104230167A (en) | Quantum dot doped glass and preparation method thereof | |
CN113816604B (en) | Fluoride laser glass with high erbium doping and low hydroxyl content of 3.5 microns and preparation method thereof | |
CN110510875B (en) | Method for improving 2-micron waveband fluorescence emission of rare earth ion doped germanate glass | |
CN114455845B (en) | Er 3+ /Yb 3+ /Nd 3+ Codoped near-infrared ultra-wideband emission tellurate optical fiber glass and preparation method thereof | |
CN105271727B (en) | Infraluminescence fluorine zirconium zinc-base glass and preparation method thereof in Er ions | |
CN117023984A (en) | Erbium-doped tellurate glass and preparation method and application thereof | |
CN109437562B (en) | 2-micron ultra-wideband tunable rare earth-doped laser glass capable of emitting light to separate out quantum dots and preparation method thereof | |
CN116253512B (en) | Germanate glass capable of inhibiting darkening of gamma ray irradiation and preparation method thereof | |
CN106495470A (en) | Neodymium ytterbium codope quartz laser glass and preparation method thereof | |
CN112897878B (en) | Near-infrared band ultra-wideband emission Bi-Er-Tm co-doped tellurate optical fiber glass and preparation method thereof | |
Qiu et al. | Broadband near-infrared luminescence in bismuth borate glasses | |
CN112851129B (en) | Near-infrared band broadband emission rare earth doped bismuthate optical fiber glass and preparation method thereof | |
CN103359939A (en) | Green-light-emitting tellurate glass and preparation method thereof | |
CN110304831B (en) | Dy-Ag co-doped silicate anti-sputtering plate glass and preparation method thereof | |
CN109369007B (en) | 2.7-micron luminous high-concentration tellurium-gallium-zinc-doped laser glass and preparation method thereof | |
CN113754279A (en) | High erbium-doped mid-infrared 3.5-micron laser glass and preparation method thereof | |
CN107162413A (en) | A kind of fluorotellurite glass and preparation method thereof | |
CN112876069A (en) | Ho3+/Eu3+Co-doped fluorine indium glass capable of generating 3.9 mu m mid-infrared band fluorescence | |
CN112110649A (en) | Tellurium bismuthate mid-infrared 2.7 micron luminescent glass and preparation method thereof |
Legal Events
Date | Code | Title | Description |
---|---|---|---|
PB01 | Publication | ||
PB01 | Publication | ||
SE01 | Entry into force of request for substantive examination | ||
SE01 | Entry into force of request for substantive examination | ||
GR01 | Patent grant | ||
GR01 | Patent grant |