CN1944297A - Method for producing neodymium-ytterbium co-blended high silicon-oxygen laser glass - Google Patents
Method for producing neodymium-ytterbium co-blended high silicon-oxygen laser glass Download PDFInfo
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- CN1944297A CN1944297A CNA2006101174557A CN200610117455A CN1944297A CN 1944297 A CN1944297 A CN 1944297A CN A2006101174557 A CNA2006101174557 A CN A2006101174557A CN 200610117455 A CN200610117455 A CN 200610117455A CN 1944297 A CN1944297 A CN 1944297A
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- 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
- C03C3/00—Glass compositions
- C03C3/04—Glass compositions containing silica
- C03C3/06—Glass compositions containing silica with more than 90% silica by weight, e.g. quartz
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- 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
- C03C4/00—Compositions for glass with special properties
- C03C4/0071—Compositions for glass with special properties for laserable glass
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Abstract
The process of making Nd-Yb co-blended high silica laser glass includes the following steps: preparing porous glass; compounding mixed Nd-Yb ion solution; soaking the porous glass inside the mixed Nd-Yb ion solution for over 30 min; drying the porous glass in air at 200-800 deg.C; and sintering at 1100-1200 deg.C in a high temperature furnace to eliminate pores and to form dense transparent Nd-Yb co-blended high silica laser glass. Thus made Nd-Yb co-blended high silica laser glass has excellent physical performance, and can emit 950-1100 nm wide band light under the pump of 808 nm laser and realize xenon lamp pumped laser output.
Description
Technical field
The present invention relates to laser glass, particularly a kind of manufacture method of neodymium-ytterbium co-blended high silicon-oxygen laser glass.
Background technology
Developing rapidly to developing new laser medium material of laser diode-pumped solid statelaser provides an opportunity.The rare earth neodymium ytterbium ion is mixed glass altogether has potential to use, and promises to be a kind of new laser medium material.The neodymium ytterbium is mixed glass altogether under the 808nm diode-end-pumped, Nd
3+Produce in the ion
4I
9/2→
4F
5/2,
2H
9/2Absorb, radiationless transition is to Nd then
3+Ionic
4F
3/2Energy level, Nd
3+ 4F
3/2Energy levels is a little more than Yb
3+ 2F
5/2Energy levels, and can make it that energy takes place to shift, the neodymium ytterbium is mixed glass altogether and just can be produced from 950 to 1100nm broad-band illumination like this, can produce infrared laser in laserresonator.And the neodymium ytterbium mixes glass altogether and might realize xenon flash lamp pumping, widens the application of ytterbium ion, and is also significant at some special dimensions such as national defense and military.
Though multicomponent glass such as silicate or phosphoric acid salt can be realized high rare earth ion doped, their thermal expansivity is big, is difficult to realize the output of high frequency laser.Therefore, low-expansion coefficient and the silica glass of good optical performance and excellent chemical stability waited in expectation for a long time substrate material and laserable material as a kind of rare earth and transition metal light emitting ionic are arranged.But because rare earth ion is in quartz glass high temperature fusion preparation process, easy spontaneous formation cluster causes concentration quenching, and rare earth ion is difficult to higher doping in silica glass.Although in the practical application of mixing the rare earth silica fibre, by increasing the low absorption problem that fiber lengths can remedy the rare earth ion lower concentration, the gain of optical fiber unit length is little, is unfavorable for miniaturization of devices.For the inhibition concentration cancellation, both at home and abroad the researchist has attempted a lot of methods, comprises methods such as chemical vapor deposition (CVD) and sol-gel, but all fails obviously to strengthen their luminous intensity.A kind of appropriate preparation method if can develop, not only make the fundamental characteristics of silica glass be protected, and have higher ion doping concentration, this glass just might become a kind of new quartzy laser glass material again.Vagcor is formed near silica glass, has the good characteristic of silica glass.
Summary of the invention
The manufacture method that the purpose of this invention is to provide a kind of neodymium-ytterbium co-blended high silicon-oxygen laser glass, the neodymium ytterbium that has good physical with acquisition is mixed vagcor altogether, 950 to 1100nm broad-band illumination under the 808nm laser pumping, and realize the output of xenon flash lamp pumping laser.
The concrete technical solution of the present invention is as follows:
A kind of manufacture method of neodymium-ytterbium co-blended high silicon-oxygen laser glass is characterized in that this method comprises the following steps:
2. prepare sintered glass, this sintered glass composed as follows:
Ingredient w t%
SiO
2 ≥94.0
B
2O
3 1.0～3.0
Al
2O
3 1.0～3.0
The aperture of this sintered glass is 1.0～10 nanometers, and aperture accounts for 25～40% of glass volume;
2. prepare neodymium ion and ytterbium ion mixing solutions; With neodymium nitrate, Neodymium trichloride or neodymium acetate, with the mixing solutions that is made into neodymium ion and ytterbium ion in the water-soluble in proportion solution of ytterbium nitrate, Ytterbium trichloride or ytterbium acetate or acid solution or the ethanolic soln, institute's compounding closes that neodymium ion concentration is 0.1～1mol/L in the solution, ytterbium ion concentration is 0.1～1mol/L, and the ratio of ytterbium ion and the molar content of neodymium ion in solution is in 0.1～10 scope;
3. adopt infusion method, described sintered glass is immersed in described neodymium ion and the ytterbium ion mixing solutions more than the 30min, neodymium ion and ytterbium ion are introduced in the sintered glass;
The sintered glass that 4. will be mixed with neodymium, ytterbium ion is dry under 200～800 ℃ in air;
5. the sintered glass that will be mixed with neodymium, ytterbium ion is put into High Temperature Furnaces Heating Apparatus, and through 1100～1200 ℃ solid state sintering, eliminating micropore becomes closely knit transparent neodymium-ytterbium co-blended high silicon-oxygen laser glass in air or oxygen;
Described acid solution can be salpeter solution, or hydrochloric acid soln, or sulphuric acid soln.
Described by soaking when in sintered glass, introducing neodymium, ytterbium ion, also introduce Al
3-Ion.
Technique effect of the present invention is:
The present invention adopts physical method that neodymium, ytterbium ion are dispersed in the porous borosilicate glass, does not need high-temperature fusion in the making processes, thereby effectively suppresses the spontaneous cluster of rare earth ion, strengthens luminous intensity.
The present invention sinters the high silica laser glass that the neodymium ytterbium is mixed altogether or neodymium ytterbium aluminium is mixed altogether into, our experiments show that, under the 808nm laser pumping, produce the infrared broad-band illumination from 950nm to 1100nm, in laserresonator, produce the purpose of near-infrared laser through the laser pumping of 808nm.
The present invention helps realizing laser output by adding the luminescent properties that aluminum ion can further improve this neodymium-ytterbium co-blended high silicon-oxygen laser glass simultaneously.
Compare with phosphate laser glass with silicate, the high silica laser glass that neodymium ytterbium aluminium of the present invention is mixed altogether is because the coefficient of expansion is little, thermal shock resistance is superior, the laser damage threshold height is suitable as the laser medium material of the micro-slice laser of laser diode-pumped and superpower, high repetition frequency, compact construction.
Description of drawings
Fig. 1 is the vagcor fluorescence spectrum contrast that embodiment 1 and neodymium ion list are mixed.
Fig. 2 mixes the contrast of vagcor luminescent spectrum for embodiment 5 (alumina doped) altogether with the neodymium ytterbium of alumina doped not.
Embodiment
The present invention is further illustrated by the following examples, but should not limit protection scope of the present invention with this.
Embodiment 1
With 0.88g analytical pure Nd (NO
3)
36H
2O and 0.94g analytical pure Yb (NO
3)
36H
2O is dissolved in the deionized water fully, is made into the 0.1mol/L Nd of 20ml
3+With 0.1mol/L Yb
3+The ionic mixing solutions.Be 5 * 5 * 3mm with size again, SiO
2Content is put into mixing solutions above the sintered glass of 94wt% and is soaked 30min; After sintered glass takes out from solution, thorough drying in 200 ℃ of air.The sintered glass that will contain neodymium, ytterbium ion is put into High Temperature Furnaces Heating Apparatus afterwards, and through 1100 ℃ solid state sintering, the elimination micropore becomes closely knit transparent neodymium ytterbium and mixes vagcor altogether in air or oxygen atmosphere.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1100 ℃ of the heat-up rates of 5 ℃/min, at 1100 ℃ of insulation 45min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Neodymium ion and ytterbium ion account for the 0.43wt% and the 0.52wt% of vagcor weight percent behind the sintering respectively, and the ratio of ytterbium neodymium ion molar content is Yb
3+: Nd
3+=1.Sample produces the infrared broad-band illumination (accompanying drawing 1) of 950nm to 1100nm through precise polished back under the 808nm laser pumping, produce laser in laserresonator under the laser pumping of 808nm.
Embodiment 2
With 8.75g analytical pure Nd (NO
3)
36H
2O and 2.82g analytical pure Yb (NO
3)
36H
2O is dissolved in rare nitric acid of 1mol/L fully, is made into the 1mol/L Nd of 20ml
3+With 0.3mol/L Yb
3+The ionic mixing solutions.Be 5 * 5 * 3mm with size again, SiO
2Content is put into mixing solutions above the sintered glass of 94wt% and is soaked 45min; After sintered glass takes out from solution, thorough drying in 300 ℃ of air.The sintered glass that will contain neodymium, ytterbium ion is put into High Temperature Furnaces Heating Apparatus afterwards, and through 1150 ℃ solid state sintering, the elimination micropore becomes closely knit transparent neodymium ytterbium and mixes vagcor altogether in air or oxygen atmosphere.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1150 ℃ of the heat-up rates of 5 ℃/min, at 1150 ℃ of insulation 30min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Neodymium ion and ytterbium ion account for the 4.30wt% and the 1.56wt% of vagcor weight percent behind the sintering respectively, and the ratio of ytterbium neodymium ion molar content is Yb
3+: Nd
3+=3: 10.Sample produces the infrared broad-band illumination of 950nm to 1100nm through precise polished back under the 808nm laser pumping, the laser pumping through 808nm in laserresonator produces laser.
With 0.88g analytical pure Nd (NO
3)
36H
2O and 9.40g analytical pure Yb (NO
3)
36H
2O is dissolved in the deionized water fully, is made into the 0.1mol/L Nd of 20ml
3+With 1mol/L Yb
3+The ionic mixing solutions.Be 5 * 5 * 3mm with size again, SiO
2Content is put into mixing solutions above the sintered glass of 94wt% and is soaked 30min; After sintered glass takes out from solution, thorough drying in 400 ℃ of air.The sintered glass that will contain neodymium, ytterbium ion is put into High Temperature Furnaces Heating Apparatus afterwards, and through 1200 ℃ solid state sintering, the elimination micropore becomes closely knit transparent neodymium ytterbium and mixes vagcor altogether in air or oxygen atmosphere.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1200 ℃ of the heat-up rates of 5 ℃/min, at 1200 ℃ of insulation 50min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Neodymium ion and ytterbium ion account for the 0.43wt% and the 5.19wt% of vagcor weight percent behind the sintering respectively, and ytterbium neodymium ion molar percentage is Yb
3+: Nb
3+=10.Sample produces the infrared broad-band illumination of 950nm to 1100nm through precise polished back under the 808nm laser pumping, produce laser in laserresonator under the laser pumping of 808nm.
Embodiment 4
With 8.75g analytical pure Nd (NO
3)
36H
2O, 1.87g analytical pure Yb (NO
3)
36H
2O and 30.20g analytical pure Al (NO
3)
39H
2O is dissolved in rare nitric acid of 1mol/L fully, is made into the 1mol/L Nd of 20ml
3+, 0.2mol/L Yb
3+With 2mol/L Al
3+The ionic mixing solutions.Be 5 * 5 * 3mm with size again, SiO
2Content is put into mixing solutions above the sintered glass of 94wt% and is soaked 60min; After sintered glass takes out, be warmed up to thorough drying in 800 ℃ of air at a slow speed from solution.The sintered glass that will contain neodymium, ytterbium ion is put into High Temperature Furnaces Heating Apparatus afterwards, and through 1180 ℃ solid state sintering, the elimination micropore becomes closely knit transparent neodymium ytterbium and mixes vagcor altogether in air or oxygen atmosphere.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1180 ℃ of the heat-up rates of 5 ℃/min, at 1180 ℃ of insulation 45min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Neodymium ion and ytterbium ion account for the 0.86wt% and the 1.04wt% of vagcor weight percent behind the sintering respectively, and aluminium composition accounts for the 1.62wt% of vagcor weight percent behind the sintering.The ratio of the aluminum ions molar content of ytterbium neodymium is Yb in the glass
3+: Nd
3+: Al
3+=1: 5: 10.Sample produces the infrared broad-band illumination of 950nm to 1100nm through precise polished back under the 808nm laser pumping, produce laser in laserresonator under the laser pumping of 808nm.
Embodiment 5
With 3.50g analytical pure Nd (NO
3)
36H
2O, 9.35g analytical pure Yb (NO
3)
36H
2O and 5.98g analytical pure Al (NO
3)
39H
2O is dissolved in the deionized water fully, is made into the 0.4mol/L Nd of 20ml
3+, 0.5mol/L Yb
3+With 0.8mol/L Al
3+The ionic mixing solutions.Be 5 * 5 * 3mm with size again, SiO
2Content is put into mixing solutions above the sintered glass of 94wt% and is soaked 120min; After sintered glass takes out from solution, thorough drying in 300 ℃ of air.The sintered glass that will contain neodymium, ytterbium ion is put into High Temperature Furnaces Heating Apparatus afterwards, and through 1200 ℃ solid state sintering, the elimination micropore becomes closely knit transparent neodymium ytterbium and mixes vagcor altogether in air or oxygen atmosphere.In sintering process, be raised to 900 ℃ with the heat-up rate of 10 ℃/min from room temperature, with from 900 to 1200 ℃ of the heat-up rates of 5 ℃/min, at 1200 ℃ of insulation 60min, glass is with the High Temperature Furnaces Heating Apparatus cool to room temperature afterwards then.Neodymium ion and ytterbium ion account for the 1.72wt% and the 5.20wt% of vagcor weight percent behind the sintering respectively, and aluminium composition accounts for the 0.32wt% of vagcor weight percent behind the sintering.The ratio of the aluminum ions molar content of ytterbium neodymium is Yb in the glass
3+: Nb
3+: Al
3+=5: 2: 4.Sample produces the infrared broad-band illumination of 950nm to 1100nm through precise polished back under the 808nm laser pumping, produce laser in laserresonator under the laser pumping of 808nm.And mixing of aluminum oxide significantly improved the luminous intensity that the neodymium ytterbium is mixed vagcor altogether, sees also Fig. 2.
Claims (3)
1, a kind of manufacture method of neodymium-ytterbium co-blended high silicon-oxygen laser glass is characterized in that this method comprises the following steps:
1. prepare sintered glass, this sintered glass composed as follows:
Ingredient w t%
SiO
2 ≥94.0
B
2O
3 1.0～3.0
Al
2O
3 1.0～3.0
The aperture of this sintered glass is 1.0～10 nanometers, and aperture accounts for 25～40% of glass volume;
2. prepare neodymium ion and ytterbium ion mixing solutions; With neodymium nitrate, Neodymium trichloride or neodymium acetate, with the mixing solutions that is made into neodymium ion and ytterbium ion in the water-soluble in proportion solution of ytterbium nitrate, Ytterbium trichloride or ytterbium acetate or acid solution or the ethanolic soln, institute's compounding closes that neodymium ion concentration is 0.1～1mol/L in the solution, ytterbium ion concentration is 0.1～1mol/L, and the ratio of ytterbium ion and the molar content of neodymium ion in solution is in 0.1～10 scope;
3. adopt infusion method, described sintered glass is immersed in described neodymium ion and the ytterbium ion mixing solutions more than the 30min, neodymium ion and ytterbium ion are introduced in the sintered glass;
The sintered glass that 4. will be mixed with neodymium, ytterbium ion is dry under 200～800 ℃ in air;
5. the sintered glass that will be mixed with neodymium, ytterbium ion is put into High Temperature Furnaces Heating Apparatus, and through 1100～1200 ℃ solid state sintering, eliminating micropore becomes closely knit transparent neodymium-ytterbium co-blended high silicon-oxygen laser glass in air or oxygen.
2, the manufacture method of neodymium-ytterbium co-blended high silicon-oxygen laser glass according to claim 1 is characterized in that described acid solution can be salpeter solution, or hydrochloric acid soln, or sulphuric acid soln.
3, the manufacture method of neodymium-ytterbium co-blended high silicon-oxygen laser glass according to claim 1 is characterized in that describedly by soaking when introducing neodymium, ytterbium ion in sintered glass, also introduces aluminum ion.
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|---|---|---|---|
| CNA2006101174557A CN1944297A (en) | 2006-10-24 | 2006-10-24 | Method for producing neodymium-ytterbium co-blended high silicon-oxygen laser glass |
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|---|---|---|---|
| CNA2006101174557A CN1944297A (en) | 2006-10-24 | 2006-10-24 | Method for producing neodymium-ytterbium co-blended high silicon-oxygen laser glass |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215093B (en) * | 2007-12-26 | 2010-06-09 | 中国科学院上海光学精密机械研究所 | Method for manufacturing integrated colorful luminous vycor glass |
| CN101928111B (en) * | 2009-06-26 | 2012-04-25 | 海洋王照明科技股份有限公司 | Luminescent glass, making method and application thereof |
| CN101931033B (en) * | 2009-06-26 | 2012-06-27 | 海洋王照明科技股份有限公司 | White light diode and manufacturing method thereof |
| CN102002357B (en) * | 2009-09-02 | 2013-08-07 | 海洋王照明科技股份有限公司 | Luminescent glass component and manufacturing method thereof |
| CN101962533B (en) * | 2009-07-23 | 2013-10-16 | 海洋王照明科技股份有限公司 | Organic-inorganic compound fluorescent powder, manufacturing method and application |
| CN104059635A (en) * | 2013-03-21 | 2014-09-24 | 海洋王照明科技股份有限公司 | Neodymium and ytterbium double doping alkali fluoborate up-conversion luminescent material, preparation method and application thereof |
| CN104099090A (en) * | 2013-04-09 | 2014-10-15 | 海洋王照明科技股份有限公司 | Dysprosium-doped alkali fluosilicic acid glass up-conversion luminescent material, and preparation method and application thereof |
| CN106430920A (en) * | 2016-09-07 | 2017-02-22 | 中国建筑材料科学研究总院 | Method for preparing quartz glass and quartz glass |
| CN106495470A (en) * | 2016-10-17 | 2017-03-15 | 中国科学院上海光学精密机械研究所 | Neodymium ytterbium codope quartz laser glass and preparation method thereof |
| CN107591670A (en) * | 2017-09-27 | 2018-01-16 | 中国科学院理化技术研究所 | A kind of double-doped crystal laser production method and device |
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2006
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|---|---|---|---|---|
| CN101215093B (en) * | 2007-12-26 | 2010-06-09 | 中国科学院上海光学精密机械研究所 | Method for manufacturing integrated colorful luminous vycor glass |
| CN101928111B (en) * | 2009-06-26 | 2012-04-25 | 海洋王照明科技股份有限公司 | Luminescent glass, making method and application thereof |
| CN101931033B (en) * | 2009-06-26 | 2012-06-27 | 海洋王照明科技股份有限公司 | White light diode and manufacturing method thereof |
| CN101962533B (en) * | 2009-07-23 | 2013-10-16 | 海洋王照明科技股份有限公司 | Organic-inorganic compound fluorescent powder, manufacturing method and application |
| CN102002357B (en) * | 2009-09-02 | 2013-08-07 | 海洋王照明科技股份有限公司 | Luminescent glass component and manufacturing method thereof |
| CN104059635A (en) * | 2013-03-21 | 2014-09-24 | 海洋王照明科技股份有限公司 | Neodymium and ytterbium double doping alkali fluoborate up-conversion luminescent material, preparation method and application thereof |
| CN104099090A (en) * | 2013-04-09 | 2014-10-15 | 海洋王照明科技股份有限公司 | Dysprosium-doped alkali fluosilicic acid glass up-conversion luminescent material, and preparation method and application thereof |
| CN106430920A (en) * | 2016-09-07 | 2017-02-22 | 中国建筑材料科学研究总院 | Method for preparing quartz glass and quartz glass |
| CN106430920B (en) * | 2016-09-07 | 2019-08-13 | 中国建筑材料科学研究总院 | The preparation method and quartz glass of quartz glass |
| CN106495470A (en) * | 2016-10-17 | 2017-03-15 | 中国科学院上海光学精密机械研究所 | Neodymium ytterbium codope quartz laser glass and preparation method thereof |
| CN107591670A (en) * | 2017-09-27 | 2018-01-16 | 中国科学院理化技术研究所 | A kind of double-doped crystal laser production method and device |
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Open date: 20070411 |