CN1308255C - Manufacturing method of erbium doped high silicon oxygen infrared luminous glass - Google Patents
Manufacturing method of erbium doped high silicon oxygen infrared luminous glass Download PDFInfo
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- CN1308255C CN1308255C CNB2005100310225A CN200510031022A CN1308255C CN 1308255 C CN1308255 C CN 1308255C CN B2005100310225 A CNB2005100310225 A CN B2005100310225A CN 200510031022 A CN200510031022 A CN 200510031022A CN 1308255 C CN1308255 C CN 1308255C
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Abstract
The present invention relates to a method for making erbium doped high-silica infrared luminescent glass, which comprises the following steps that firstly, high-silica porous glass is selected, and the content of SiO2 in the glass is from 95 to 98 wt%; secondly, solution which comprises erbium ions is prepared, and the concentration range of the erbium ions is from 0.02 to 0.42mol/l; thirdly, the high-silica porous glass is immersed in the solution which comprises the erbium ions, so that the solution which comprises the erbium ions is immersed in the high-silica porous glass to form the high-silica porous glass which comprises the erbium ions; finally, by drying, the high-silica porous glass which comprises the erbium ions is placed in a high temperature furnace for solid-phase sintering at the temperature of 1050 to 1200 DEG C. The glass manufactured by the method of the present invention can produce infrared red light nearby the frequency range of 1.53 micrometer and can produce laser of 1.54 micrometer in a laser cavity.
Description
Technical field
The present invention relates to fluorescent glass, particularly a kind of manufacture method of erbium doped high silicon oxygen infrared luminous glass.
Background technology
Er-doped ionic oxide formation thing glass can be used as the operation material of active parts such as fiber amplifier and flat optical waveguide amplifier, and 1.54 microns optical maser wavelength of er doped silica glasses can be absorbed by water, be suitable for range finder of doing paired eye-safe etc., because these application prospects are arranged, people have studied the characteristics of luminescence of erbium ion in silicate, phosphoric acid acid, boric acid acid, germanate and silica glass widely, and quartz optical fiber amplifier (EDFA) has become requisite Primary Component in the present opticfiber communication cable.But, in above-mentioned multiple glass system, have only er-doped ion quartz glass optical fibre to obtain practical application at present, its reason be the optical loss of er-doped ion silica glass far below other oxide glass, and satisfactory stability is arranged.But the er-doped silica glass exists some shortcomings: the one, and erbium ion concentration is not high; This is because erbium ion easy spontaneous formation in silica glass is trooped, thereby produces the concentration delustring.Lower concentration will make that the gain of unit length of optical fiber is little, is unfavorable for the development of device miniaturization.The 2nd, the luminous bandwidth of erbium ion in silica glass is narrower, for the expansion of amplifying bandwidth has brought difficulty.Therefore, although the er-doped quartz glass optical fibre has obtained application in opticfiber communication cable, but, if can discover a kind of suitable substrate material or preparation method, not only make the fundamental characteristics of silica glass be maintained, simultaneously, the higher erbium ion-doped concentration and the bandwidth of an emission of broad are arranged again, if like this, can remedy the deficiency of present er-doped silica glass undoubtedly, important practical value is arranged.
Summary of the invention
The object of the present invention is to provide a kind of manufacture method of erbium doped high silicon oxygen infrared luminous glass,, in laserresonator, produce 1.54 microns laser to obtain near producing infraluminescence 1.53 microns the frequency band.
Technical solution of the present invention is as follows:
A kind of manufacture method of erbium doped high silicon oxygen infrared luminous glass is characterized in that this method comprises the following steps:
1. choose high silica porous glass, SiO in this glass
2Content be 95～98wt%, the aperture of aperture is 1.0～10 nanometers, the volume that aperture accounts for glass is 23～28%;
2. preparation contains the solution of erbium ion, and the concentration range of erbium ion is 0.02～0.42 mol;
3. described high silica porous glass is immersed in the described solution that contains erbium ion,, forms the high silica porous glass that contains erbium ion so that the described solution that contains erbium ion immerses in this high silica porous glass;
4. through super-dry, this high silica porous glass that contains erbium ion is put into High Temperature Furnaces Heating Apparatus, solid state sintering under 1050-1200 ℃ of temperature: from 5 ℃ of the temperature rise rate≤per minutes of room temperature to 400 ℃, from 400 ℃ to 900 ℃ temperature rise rates is 10 ℃ of per minutes, from 5 ℃ of temperature rise rate≤per minutes of 950 ℃ to 1050-1200 ℃, more than 30 minutes, be cooled to room temperature 1050-1200 ℃ of insulation then.
The described solution that contains erbium ion, it is molten altogether wherein also to contain ytterbium ion/aluminum ion, and the concentration range of described ytterbium ion is 0.27～0.71 mol, and described aluminum ions concentration range is 0.11～0.53 mol.
The described solvent that contains the solution of erbium ion is water, acid, alcohol or acetone.
Described acid is nitric acid, hydrochloric acid or sulfuric acid.
Described high silica porous glass is to adopt the sintered glass that divides the phase method preparation with borosilicate glass, this glass SiO
2Content be 95～98wt% (weight percent) since preparation process in acid treatment can not moltenly fully remove other composition, so the also residual B that 1～3wt% is arranged in the glass
2O
3With 1～2wt%Al
2O
3The aperture of this sintered glass is 1.0～10 nanometers, and it is 23～28% that aperture accounts for the glass volume.
Through super-dry, the described high silica porous glass that contains erbium ion is put into High Temperature Furnaces Heating Apparatus, with 1050～1200 ℃ of high temperature sinterings 0.5～2 hour, sintered glass becomes the transparent infrared luminous glass of atresia.The luminescent properties that continues high temperature sintering glass no longer changes.After polishing, erbium ion-doped vagcor is under the 808nm laser pumping, and the vagcor that erbium and ytterbium ion are mixed altogether can produce infraluminescence near 1.53 microns frequency band under the laser pumping of 980nm; Mix aluminum ion simultaneously altogether and can obviously strengthen near 1.53 microns frequency bands luminous intensity.This glass can further be processed into optical fiber and planar optical waveguide, can produce 1.54 microns laser in laserresonator.
Described erbium ion solution is that Erbium trinitrate or Erbium trioxide, Erbium trichloride, acetate erbium etc. can be dissolved fully by water, acid (comprising salpeter solution, hydrochloric acid soln, sulphuric acid soln), ethanol and acetone soln, and the material that high temperature can decompose and form the erbium ion oxide compound down fully dissolves in the above-mentioned solution, be prepared into water, the acid solution of er-doped solion, comprise salpeter solution, hydrochloric acid soln, sulphuric acid soln, ethanolic soln and acetone soln.
In order to improve the luminescent properties of erbium ion,, can also introduce ytterbium Yb simultaneously introducing erbium ion simultaneously with solution method
3+With aluminum ion Al
3+The weight percent that these ionic account for behind glass sintering in the glass is about 0.1～4.0wt%, both can introduce simultaneously, also can introduce respectively, introduce erbium, ytterbium and aluminum ions upper bound condition and be behind the glass sintering not devitrification, introduce that the content of silicon-dioxide surpassed 91% during glass was formed behind these ions.Ytterbium ion and aluminum ions introducing and erbium ion are same, and nitrate compound, muriate or the acetic acid compound of ytterbium and aluminium dissolved in the aqueous solution, acid solution, ethanolic soln and the acetone soln that is prepared into them in water, acid (comprising salpeter solution, hydrochloric acid soln, sulphuric acid soln), ethanol and the acetone soln.Introduce after erbium ion and ytterbium and the aluminum ion, will be mixed with these ionic high silica porous glass and put into High Temperature Furnaces Heating Apparatus, through 1050-1200 ℃ high temperature solid-phase sintering, eliminating micropore becomes closely knit transparent vagcor.In the sintering process, ℃ to heat up at a slow speed from room temperature to 400, the speed of per minute below 5 ℃, avoiding the cracking of sintered glass, from heating up at a slow speed to 1050-1200 ℃ about 950 ℃, the speed of per minute below 5 ℃ is to avoid glass deformation.After arriving sintering temperature (1050-1200 ℃), be incubated 0.5～2 hour, sintered glass becomes nonporous glass, therefore, continues high temperature sintering glass luminescent properties and no longer changes.
Experiment shows: the vagcor that er-doped behind the sintering and erbium, aluminium and ytterbium ion are mixed altogether is through after polishing, under the laser pumping of 808nm or 980nm, can near 1.53 microns frequency band, produce infraluminescence, in laserresonator, can produce 1.54 microns laser.
Description of drawings
Fig. 1 is that the erbium doped high silicon oxygen glass that utilizes the inventive method to make is the luminescent spectrum under the laser excitation of 808nm at wavelength
Fig. 2 is that the erbium doped high silicon oxygen glass that utilizes the inventive method to make is the luminescent spectrum under the laser excitation of 980nm at wavelength
Fig. 3 is that the erbium doped high silicon oxygen glass that utilizes the inventive method to make is the luminescent spectrum under the laser excitation of 980nm at wavelength
Embodiment
The invention will be further described below in conjunction with embodiment.
Embodiment 1
The Er of 1.0g will be equivalent to after decomposing
2O
3The analytically pure Er (NO of 2.32g
3)
35H
2O puts into 25 milliliters deionized water solution, after the dissolving, is made into Er fully
3+Ionic concn is the solution of 0.21 mol, is 5 * 5 * 3mm, SiO with size again
2Content be that the sintered glass of 97wt% is put into this solution and soaked more than 10 minutes; Afterwards, the high silica porous glass that is mixed with erbium ion is put into High Temperature Furnaces Heating Apparatus, through 1150 ℃ solid state sintering, eliminating micropore becomes the closely knit transparent Er that mixes in air or oxygen
2O
3Concentration is about 1.0% vagcor.In sintering process, with the speed of per minute below 5 ℃, after being raised to 400 ℃ from room temperature, speed with 10 ℃ of per minutes is raised to 950 ℃ of front and back, then, be raised to 1150 ℃ and after the insulation of this temperature is more than 30 minutes with the speed of per minute below 5 ℃ from this temperature, turn off the power supply of High Temperature Furnaces Heating Apparatus, allow the glass furnace cooling.This glass can send the infraluminescence that is centered close to 1530nm under the laser excitation of 808nm.Curve among Fig. 1 (1) is exactly the luminescent spectrum curve of this glass.
The Er of 0.1g will be equivalent to after decomposing
2O
3The analytically pure Er (NO of 0.23g
3)
35H
2O puts into 25 milliliters ethanolic soln, after the dissolving, is made into Er fully
3+Ionic concn is the solution of 0.02 mol, is 5 * 5 * 3mm, SiO with size again
2Content be that the sintered glass of 98wt% is put into this solution and soaked more than 10 minutes; Afterwards, should put into High Temperature Furnaces Heating Apparatus by high silica micropore glass, through the solid state sinterings of 1200 ℃ of degree temperature, eliminating micropore becomes the closely knit transparent Er that mixes in air or oxygen
2O
3Concentration is about 0.1% vagcor.In sintering process, with the speed of per minute below 5 ℃, after being raised to 400 ℃ from room temperature, speed with 10 ℃ of per minutes is raised to 950 ℃ of front and back, then, be raised to 1200 ℃ and after the insulation of this temperature is more than 30 minutes with the speed of per minute below 5 ℃ from this temperature, turn off the power supply of High Temperature Furnaces Heating Apparatus, allow the glass furnace cooling.This glass can send the infraluminescence that is centered close to 1530nm under the laser excitation of 808nm.
Embodiment 3
The Er of 1.0g will be equivalent to after decomposing
2O
3The analytically pure Er (NO of 2.32g
3)
35H
2Analytically pure Al (the NO of O and 5.0g
3)
39H
2O puts into 1 normal hydrochloric acid soln of 25 milliliters, after the dissolving, is made into Er fully
3+Ionic concn is 0.21 mol, Al
3+Ionic concn is the solution of 0.53 mol, is 5 * 5 * 3mm, SiO with size again
2Content be that the sintered glass of 97wt% is put into this solution and soaked more than 10 minutes; Afterwards, will be mixed with the high silica micropore glass of these ionic and put into High Temperature Furnaces Heating Apparatus, through the solid state sintering of 1120 ℃ of degree temperature, eliminating micropore becomes closely knit transparent vagcor in air or oxygen.In sintering process, with the speed of per minute below 5 ℃, be raised to 400 ℃ from room temperature after, be raised to 950 ℃ with the speed of 10 ℃ of per minutes.Then, be raised to 1120 ℃ and after 1120 ℃ of insulations are more than 30 minutes from 950 ℃, turn off the power supply of High Temperature Furnaces Heating Apparatus, allow the glass furnace cooling with the speed of per minute below 5 ℃.This glass can send the infraluminescence that is centered close to 1530nm under the laser excitation of 808nm.Curve 2 among Fig. 1 is exactly the luminescent spectrum curve of this glass.
Embodiment 4
The Er of 1.0g will be equivalent to after decomposing
2O
3The analytically pure Er (NO of 2.32g
3)
35H
2The Yb that is equivalent to 1.35g after O and the decomposition
2O
3The analytically pure Yb (NO of 3.2g
3)
36H
2O puts into 1 normal salpeter solution of 25 milliliters, after the dissolving, is made into Er fully
3+Ionic concn is 0.21 mol, Yb
3+Ionic concn is the solution of 0.27 mol, is 5 * 5 * 3mm, SiO with size again
2Content be that the sintered glass of 97wt% is put into this solution and soaked more than 10 minutes; Afterwards, will be mixed with the high silica micropore glass of these ionic and put into High Temperature Furnaces Heating Apparatus, through the solid state sintering of 1100 ℃ of degree temperature, eliminating micropore becomes closely knit transparent vagcor in air or oxygen.In sintering process, with the speed of per minute below 5 ℃, be raised to 400 ℃ from room temperature after, be raised to 950 ℃ with the speed of 10 ℃ of per minutes.Then, be raised to 1100 ℃ and after 1100 ℃ of insulations are more than 30 minutes from 950 ℃, turn off the power supply of High Temperature Furnaces Heating Apparatus, allow the glass furnace cooling with the speed of per minute below 5 ℃.This glass can send the infraluminescence that is centered close to 1530nm under the laser excitation of 980nm.Curve 2 among Fig. 2 is exactly the luminescent spectrum curve of this glass.
Embodiment 5
The Er of 1.0g will be equivalent to after decomposing
2O
3The analytically pure Er (NO of 2.32g
3)
35H
2The Yb that is equivalent to 1.35g after O and the decomposition
2O
3The analytically pure Yb (NO of 3.2g
3)
36H
2Analytically pure Al (the NO of O and 5.0g
3)
39H
2O puts into 1 normal sulphuric acid soln of 25 milliliters, after the dissolving, is made into Er fully
3+Ionic concn is 0.21 mol, Yb
3+Ionic concn is 0.27 mol, Al
3+Ionic concn is the solution of 0.53 mol, is 5 * 5 * 3mm, SiO with size again
2Content be that the sintered glass of 96wt% is put into this solution and soaked more than 10 minutes; Afterwards, will be mixed with the high silica micropore glass of these ionic and put into High Temperature Furnaces Heating Apparatus, through the solid state sintering of 1080 ℃ of degree temperature, eliminating micropore becomes closely knit transparent vagcor in air or oxygen.In sintering process, with the speed of per minute below 5 ℃, be raised to 400 ℃ from room temperature after, be raised to 950 ℃ with the speed of 10 ℃ of per minutes.Then, be raised to 1080 ℃ and after 1080 ℃ of insulations are more than 30 minutes from 950 ℃, turn off the power supply of High Temperature Furnaces Heating Apparatus, allow the glass furnace cooling with the speed of per minute below 5 ℃.This glass can send the infraluminescence that is centered close to 1530nm under the laser excitation of 980nm.Curve 2 among Fig. 3 is exactly the luminescent spectrum curve of this glass.
Embodiment 6
The Er of 2.0g will be equivalent to after decomposing
2O
3The analytically pure Er (NO of 4.64g
3)
35H
2The Yb that is equivalent to 2.0g after O and the decomposition
2O
3The analytically pure Yb (NO of 4.74g
3)
36H
2Analytically pure Al (the NO of O and 2.5g
3)
39H
2O puts into 1 normal hydrochloric acid soln of 25 milliliters, after the dissolving, is made into Er fully
3+Ionic concn is 0.42 mol, Yb
3+Ionic concn is 0.4 mol, Al
3+Ionic concn is the solution of 0.28 mol, is 5 * 5 * 3mm, SiO with size again
2Content be that the sintered glass of 96wt% is put into this solution and soaked more than 10 minutes; Afterwards, will be mixed with the high silica micropore glass of these ionic and put into High Temperature Furnaces Heating Apparatus, through the solid state sintering of 1070 ℃ of degree temperature, eliminating micropore becomes closely knit transparent vagcor in air or oxygen.In sintering process, with the speed of per minute below 5 ℃, be raised to 400 ℃ from room temperature after, be raised to 950 ℃ with the speed of 10 ℃ of per minutes from room temperature.Then, be raised to 1070 ℃ and after 1070 ℃ of insulations are more than 30 minutes from 950 ℃, turn off the power supply of High Temperature Furnaces Heating Apparatus, allow the glass furnace cooling with the speed of per minute below 5 ℃.This glass can send the infraluminescence that is centered close to 1530nm under the laser excitation of 980nm.
Embodiment 7
The Er of 0.5g will be equivalent to after decomposing
2O
3The analytically pure Er (NO of 1.2g
3)
35H
2The Yb that is equivalent to 3.5g after O and the decomposition
2O
3The analytically pure Yb (NO of 8.3g
3)
36H
2Analytically pure Al (the NO of O and 1.0g
3)
39H
2O puts into 25 milliliters the ethanol and the solution of acetone, after the dissolving, is made into Er fully
3+Ionic concn is 0.11 mol, Yb
3+Ionic concn is 0.71 mol, Al
3+Ionic concn is the solution of 0.11 mol, is 5 * 5 * 3mm, SiO with size again
2Content be that the sintered glass of 95wt% is put into this solution and soaked more than 10 minutes; Afterwards, will be mixed with the high silica micropore glass of these ionic and put into High Temperature Furnaces Heating Apparatus, through the solid state sintering of 1050 ℃ of temperature, eliminating micropore becomes closely knit transparent vagcor in air or oxygen.In sintering process, with the speed of per minute below 5 ℃, be raised to 400 ℃ from room temperature after, be raised to 950 ℃ with the speed of 10 ℃ of per minutes.Then, be raised to 1050 ℃ and after 1050 ℃ of insulations are more than 30 minutes from 950 ℃, turn off the power supply of High Temperature Furnaces Heating Apparatus, allow the glass furnace cooling with the speed of per minute below 5 ℃.This glass can send the infraluminescence that is centered close to 1530nm under the laser excitation of 980nm.
As seen from the figure, curve 1 among Fig. 1 is that vagcor that embodiment 1 only is mixed with erbium ion is the luminescent spectrum under the laser excitation of 808nm at wavelength, curve 2 is that vagcor that embodiment 3 erbiums and aluminum ion are mixed altogether is the luminescent spectrum under the laser excitation of 808nm at wavelength, after mixing aluminum ion altogether, luminous intensity increases about about 1 times.Curve 1 among Fig. 2 is same spectrum with the curve 1 among Fig. 1, curve 2 among Fig. 2 is that vagcor that embodiment 4 erbiums and ytterbium ion are mixed altogether is the luminescent spectrum under the laser excitation of 980nm at wavelength, under the laser excitation of same power, more than the luminous intensity that erbium and ytterbium ion are mixed glass has altogether increased about 12 times.In addition, the luminescent spectrum halfwidth of the vagcor that er-doped ionic vagcor and erbium and aluminum ion are mixed altogether is about 30nm, and the halfwidth of the luminescent spectrum of the vagcor that erbium and ytterbium ion are mixed altogether is about 74nm, has increased more than 1 times.Curve 1 among Fig. 3 is same curves with the curve 2 among Fig. 2, curve 2 among Fig. 3 is that embodiment 5 erbiums, ytterbium and three kinds of ions of aluminium are mixed the luminescent spectrum under the laser excitation that glass is 980nm at wavelength altogether, after mixing aluminum ion altogether, luminous intensity has increased about about 1 times again, and the halfwidth of its luminescent spectrum remains on about 70nm.This erbium ion-doped vagcor infrared luminous glass is improved to common er-doped, ytterbium and three kinds of ions of aluminium from single er-doped, and under the laser excitation of same power, its luminous intensity has increased about 25%.
Claims (4)
1, a kind of manufacture method of erbium doped high silicon oxygen infrared luminous glass is characterized in that this method comprises the following steps:
1. choose high silica porous glass, SiO in this glass
2Content be 95～98wt%, the aperture of aperture is 1.0～10 nanometers, the volume that aperture accounts for glass is 23～28%;
2. preparation contains the solution of erbium ion, and its concentration range is 0.02～0.42 mol;
3. described high silica porous glass is immersed in the described solution that contains erbium ion,, forms the high silica porous glass that contains erbium ion so that the described solution that contains erbium ion immerses in this high silica porous glass;
4. through super-dry, this high silica porous glass that contains erbium ion is put into High Temperature Furnaces Heating Apparatus, solid state sintering under 1050～1200 ℃ of temperature: from 5 ℃ of the temperature rise rate≤per minutes of room temperature to 400 ℃, from 400 ℃ to 900 ℃ temperature rise rates is 10 ℃ of per minutes, from 5 ℃ of temperature rise rate≤per minutes of 950 ℃ to 1050～1200 ℃, more than 30 minutes, be cooled to room temperature 1050～1200 ℃ of insulations then.
2, the manufacture method of erbium doped high silicon oxygen infrared luminous glass according to claim 1, it is characterized in that the described solution that contains erbium ion, it is molten altogether wherein also to contain ytterbium ion or aluminum ion or ytterbium ion and aluminum ion, the concentration range of described ytterbium ion is 0.27～0.71 mol, and described aluminum ions concentration range is 0.11～0.53 mol.
3, the manufacture method of erbium doped high silicon oxygen infrared luminous glass according to claim 2 is characterized in that the described solvent that contains the solution of erbium ion is water, acid, alcohol or acetone.
4, the manufacture method of erbium doped high silicon oxygen infrared luminous glass according to claim 3 is characterized in that described acid is nitric acid, hydrochloric acid or sulfuric acid.
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| CN102030479B (en) * | 2009-09-24 | 2014-04-09 | 海洋王照明科技股份有限公司 | Copper nanoparticle-doped porous glass and preparation method thereof |
| CN102030480B (en) * | 2009-09-24 | 2014-04-09 | 海洋王照明科技股份有限公司 | Porous glass doped with nickel nano particle and preparation method thereof |
| CN102030481B (en) * | 2009-09-24 | 2013-09-11 | 海洋王照明科技股份有限公司 | Cobalt nanoparticle-doped cellular glass and preparation method thereof |
| EP2594537A4 (en) * | 2010-07-14 | 2015-10-28 | Oceans King Lighting Science | Rare earth ions doped alkali metal silicate luminescent glass and the preparation method thereof |
| CN107162441B (en) * | 2017-04-28 | 2019-06-18 | 华中科技大学 | A kind of glass and preparation method thereof of doped ITO nanoparticle |
| CN107082571B (en) * | 2017-04-28 | 2019-06-18 | 华中科技大学 | A kind of up-conversion luminescent glass and its preparation method and application of doped ITO nanoparticle |
| CN113934079B (en) * | 2021-09-30 | 2023-04-07 | 华中科技大学 | Optical waveguide amplifier and preparation method thereof |
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| CN1618760A (en) * | 2004-11-05 | 2005-05-25 | 中国科学院上海光学精密机械研究所 | Preparation method of neodymium doped high silica blue light glass |
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