Disclosure of Invention
The invention provides near-infrared band ultra-wideband emission Bi-Er-Tm co-doped tellurate optical fiber glass and a preparation method thereof, aiming at the technical problems in the prior art.
In order to solve the technical problem, the invention provides near-infrared band ultra-wideband emission Bi-Er-Tm co-doped tellurate optical fiber glass which comprises the following raw materials in percentage by mole: 74-75 mol% of TeO214 to 15 mol% of ZnO, 4.5 to 5 mol% of Na2O, 4.5-5 mol% of WO30.5 to 2 mol% of Bi2O30.1 to 0.5 mol% of Er2O30.4 to 0.6 mol% Tm2O3。
Preferably, the raw materials comprise the following components in percentage by mole: 74 mol% TeO214 mol% of ZnO, 5 mol% of Na2O, 5 mol% of WO 31 mol% of Bi2O30.5 mol% Er2O3Tm of 0.5 mol%2O3。
Preferably, the raw materials comprise the following components in percentage by mole: 75 mol% of TeO214.7 mol% ZnO, 4.6 mol% Na2O, 4.6 mol% of WO30.5 mol% of Bi2O30.1 mol% Er2O3Tm of 0.5 mol%2O3。
Preferably, Na2O is Na2CO3Is incorporated in the form of, i.e. Na2O is formed from an equimolar amount of Na2CO3Instead. Na (Na)2O mainly adds Na+Due to Na2O is poor in stability in air, so Na is used2CO3Decomposition at high temperature can produce Na2The reaction of O can also be carried out by adding Na+The function of (1).
A method for preparing any one of the above near-infrared band ultra-wideband emission Bi-Er-Tm co-doped tellurate optical fiber glass comprises the following steps:
(1) weighing the raw materials according to the mol percentage for later use;
(2) fully and uniformly mixing the raw materials weighed in the step (1), and heating and melting to obtain a glass solution;
(3) quenching and forming the glass solution obtained in the step (2) to obtain a glass sheet;
(4) and (4) annealing the glass sheet obtained in the step (3) to obtain tellurate optical fiber glass.
Preferably, step (2): fully grinding the weighed raw materials in the step (1), uniformly mixing, pouring into a corundum crucible, and placing in a high-temperature furnace at 880-920 ℃ for melting for 1h to obtain a glass solution. The grinding tool can be an agate mortar; the high temperature furnace can be a silicon carbide rod electric furnace.
Preferably, step (3): and taking the corundum crucible filled with the glass solution out of the high-temperature furnace, and carrying out quenching forming on a preheated graphite mold to obtain the glass sheet.
Preferably, step (4): and (3) putting the graphite mold poured with the glass solution into a muffle furnace at 300-320 ℃ for annealing, and obtaining the tellurate optical fiber glass after the annealing is finished.
Preferably, the annealing process is as follows: and transferring the graphite mold with the glass liquid to a muffle furnace heated to 300-320 ℃, preserving heat for 2h, and then cooling to room temperature at the speed of 8-10 ℃/h.
Preferably, step (4): and taking out the graphite mold filled with the tellurate optical fiber glass from the muffle furnace, and carrying out double-sided polishing treatment on the tellurate optical fiber glass.
Preferably, the temperature of the graphite mold preheated in the step (3) is 300 ℃;
preferably, the raw material has a purity of 99.99% by mass.
The invention has the beneficial effects that: the invention provides near-infrared band ultra-wideband emission Bi-Er-Tm co-doped tellurate optical fiber glass and a preparation method thereof, the preparation process is simple, the cost is low, the physical and chemical properties are excellent, the performance is stable, and Bi is introduced into the tellurate optical fiber glass+Ion, Er3+Ion and Tm3+The Bi-Er-Tm co-doped tellurate optical fiber glass covers five wave bands of O (1260-The half-height width of fluorescence of glass (FWHM-50 nm) and Er/Tm co-doped multi-component glass (FWHM-200 nm) greatly improves the communication capacity of a wavelength division multiplexing system, and has good application value in an optical communication system.
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.
Example 1
The invention provides near-infrared ultra-wideband luminescent Bi-Er-Tm co-doped tellurate optical fiber glass, which comprises the following steps:
(1) weighing the following raw materials in percentage by mole: 74 mol% TeO214 mol% of ZnO, 5 mol% of Na2CO35 mol% of WO 31 mol% of Bi2O30.5 mol% Er2O3Tm of 0.5 mol%2O3And is ready for use; wherein, the purity of each raw material is required to be 99.99 percent by mass.
(2) Fully grinding the weighed raw materials in the step (1), uniformly mixing, pouring into a corundum crucible, and placing in a high-temperature furnace at 900 ℃ for melting for 1h to obtain a glass solution.
(3) Taking out the corundum crucible filled with the glass solution from the high-temperature furnace, and carrying out quenching forming on a preheated graphite mold to obtain a glass sheet; wherein the temperature of the graphite mold heated in advance is 300 ℃.
(4) Putting the graphite mold poured with the glass solution into a muffle furnace for annealing, wherein the annealing process comprises the following steps: and transferring the graphite mold with the glass liquid poured into the graphite mold into a muffle furnace heated to 300 ℃, preserving heat for 2h, then cooling to room temperature at the speed of 10 ℃/h, and obtaining the tellurate optical fiber glass after annealing.
(5) And taking out the graphite mold filled with the tellurate optical fiber glass from the muffle furnace, and carrying out double-sided polishing treatment on the tellurate optical fiber glass to obtain the tellurate optical fiber glass with polished two sides of 1.5cm multiplied by 1.5 mm.
Example 2
The invention provides near-infrared ultra-wideband luminescent Bi-Er-Tm co-doped tellurate optical fiber glass, which comprises the following steps:
(1) weighing the following raw materials in percentage by mole: 75 mol% of TeO214.7 mol% ZnO, 4.6 mol% Na2CO34.6 mol% of WO30.5 mol% of Bi2O30.1 mol% Er2O3Tm of 0.5 mol%2O3And is ready for use; wherein, the purity of each raw material is required to be 99.99 percent by mass.
(2) Fully grinding the weighed raw materials in the step (1), uniformly mixing, pouring into a corundum crucible, and placing in a high-temperature furnace at 900 ℃ for melting for 1h to obtain a glass solution.
(3) Taking out the corundum crucible filled with the glass solution from the high-temperature furnace, and carrying out quenching forming on a preheated graphite mold to obtain a glass sheet; wherein the temperature of the graphite mold heated in advance is 300 ℃.
(4) Putting the graphite mold poured with the glass solution into a muffle furnace for annealing, wherein the annealing process comprises the following steps: and transferring the graphite mold with the glass liquid poured into the graphite mold into a muffle furnace heated to 300 ℃, preserving heat for 2h, then cooling to room temperature at the speed of 10 ℃/h, and obtaining the tellurate optical fiber glass after annealing.
(5) And taking out the graphite mold filled with the tellurate optical fiber glass from the muffle furnace, and carrying out double-sided polishing treatment on the tellurate optical fiber glass to obtain the tellurate optical fiber glass with polished two sides of 1.5cm multiplied by 1.5 mm.
Example 3
The invention provides near-infrared ultra-wideband luminescent Bi-Er-Tm co-doped tellurate optical fiber glass, which comprises the following steps:
(1) weighing the following raw materials in percentage by mole: 74 mol% TeO215 mol% of ZnO, 4.5 mol% of Na2CO34.5 mol% of WO31.5 mol% of Bi2O30.1 mol% Er2O3Tm of 0.4 mol%2O3And is ready for use; wherein, the purity of each raw material is required to be 99.99 percent by mass.
(2) Fully grinding the weighed raw materials in the step (1), uniformly mixing, pouring into a corundum crucible, and placing in a high-temperature furnace at 880 ℃ for melting for 1h to obtain a glass solution.
(3) Taking out the corundum crucible filled with the glass solution from the high-temperature furnace, and carrying out quenching forming on a preheated graphite mold to obtain a glass sheet; wherein the temperature of the graphite mold heated in advance is 300 ℃.
(4) Putting the graphite mold poured with the glass solution into a muffle furnace for annealing, wherein the annealing process comprises the following steps: and transferring the graphite mold with the glass liquid poured into the graphite mold into a muffle furnace heated to 310 ℃, preserving heat for 2h, then cooling to room temperature at the speed of 8 ℃/h, and obtaining the tellurate optical fiber glass after annealing.
(5) And taking out the graphite mold filled with the tellurate optical fiber glass from the muffle furnace, and carrying out double-sided polishing treatment on the tellurate optical fiber glass to obtain the tellurate optical fiber glass with polished two sides of 1.5cm multiplied by 1.5 mm.
Example 4
The invention provides near-infrared ultra-wideband luminescent Bi-Er-Tm co-doped tellurate optical fiber glass, which comprises the following steps:
(1) weighing the following raw materials in percentage by mole: 74.2 mol% TeO214 mol% of ZnO, 4.5 mol% of Na2CO34.5 mol% of WO 32 mol% of Bi2O30.20 mol% Er2O3Tm of 0.6 mol%2O3And is ready for use; wherein, the purity of each raw material is required to be 99.99 percent by mass.
(2) Fully grinding the weighed raw materials in the step (1), uniformly mixing, pouring into a corundum crucible, and placing in a high-temperature furnace at 920 ℃ for melting for 1h to obtain a glass solution.
(3) Taking out the corundum crucible filled with the glass solution from the high-temperature furnace, and carrying out quenching forming on a preheated graphite mold to obtain a glass sheet; wherein the temperature of the graphite mold heated in advance is 300 ℃.
(4) Putting the graphite mold poured with the glass solution into a muffle furnace for annealing, wherein the annealing process comprises the following steps: and transferring the graphite mold with the glass liquid poured into the graphite mold into a muffle furnace heated to 320 ℃, preserving heat for 2h, then cooling to room temperature at the speed of 9 ℃/h, and obtaining the tellurate optical fiber glass after annealing.
(5) And taking out the graphite mold filled with the tellurate optical fiber glass from the muffle furnace, and carrying out double-sided polishing treatment on the tellurate optical fiber glass to obtain the tellurate optical fiber glass with polished two sides of 1.5cm multiplied by 1.5 mm.
The tellurate optical fiber glasses prepared in the above embodiments 1 to 4 are respectively subjected to performance tests, and fluorescence emission spectra of near-infrared bands are obtained by testing under the excitation of pump light with wavelength of 808 nm.
As shown in FIGS. 1 and 2, the glass of example 1 was tested to obtain a fluorescence spectrum having a gain spectrum ranging from about 1000 to 2100nm and a spectrum having three luminescence centers of Bi at 1290nm+Emission Peak, Er at 1530nm3+Ion emission Peak, Tm of 1800nm3+An emission peak, the full width at half maximum (FWHM) of the tellurate optical fiber glass reaches 695nm, the full width at half maximum of the tellurate optical fiber glass in test example 2 is 690nm, and the telluric acid in test example 3The full width at half maximum of the fluorescence of the salt optical fiber glass is 708nm, the full width at half maximum of the fluorescence of the tellurate optical fiber glass in the test example 4 is 680nm, covers five wave bands of O (1260-.
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.