CN101328614A - Yb and Er double doping plumbous tungstate crystal conversion material and preparation thereof - Google Patents
Yb and Er double doping plumbous tungstate crystal conversion material and preparation thereof Download PDFInfo
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- CN101328614A CN101328614A CNA2008100647849A CN200810064784A CN101328614A CN 101328614 A CN101328614 A CN 101328614A CN A2008100647849 A CNA2008100647849 A CN A2008100647849A CN 200810064784 A CN200810064784 A CN 200810064784A CN 101328614 A CN101328614 A CN 101328614A
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- tungstate crystal
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Abstract
The invention relates to a transition material on a Yb and Er dual-doped lead tungstate crystal and a preparation method thereof, relating to the transition material on the lead tungstate crystal and a preparation method thereof. The method solves the problem of low luminous intensity of a transition material on an Er-doped lead tungstate crystal prepared by the prior art. The transition material on the Yb and Er dual-doped lead tungstate crystal is prepared by WO3, PbO, Er2O3 and Yb2O3. The method comprises the following steps: firstly, required compositions are weighed; secondly, sintering is performed; and thirdly, the crystal is grown by adoption of the crystal pulling method, and then the transition material on the Yb and Er dua-doped lead tungstate crystal is obtained. The method dopes element ytterbium (Yb) in the transition material on the Er-doped lead tungstate crystal, and improves the luminous strength on a green wave band of the Er-doped lead tungstate crystal by three times on the basis of preserving the prior superior performance of the Er-doped lead tungstate crystal.
Description
Technical field
The present invention relates to a kind of crystal of lead tungstate up-conversion and preparation method thereof.
Background technology
More and more to the performance study of Er dopant material in recent years, comprise on infrared-visible light and changing, the optics of Er and electrical properties research, add the progress and the development of laser diode, make Er doping and luminous research obtain unprecedented attention, constantly seek suitable matrix, carry out the doping experiment of Er.Crystal of lead tungstate not only satisfies Er and mixes and luminous condition, and because its optical clarity is good, optical density(OD) is big, irradiation hardness is strong, physico-chemical property is stable, the thermal conductivity advantage of higher, more help the miniaturization of upconversion laser, therefore more and more be subjected to people's attention, but the luminous intensity of Er lead tungstate-doped crystal up-conversion is low, causes that up-conversion luminescence efficient is not high to have had a strong impact on practical application.
Summary of the invention
The present invention seeks to the low problem of luminous intensity, and a kind of Yb and Er double doping plumbous tungstate crystal conversion material and preparation method thereof are provided for the Er lead tungstate-doped crystal up-conversion that solves prior art for preparing.
Yb of the present invention and Er double doping plumbous tungstate crystal conversion material are by WO
3, PbO, Er
2O
3And Yb
2O
3Make; WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.1～3mol%, Yb
2O
3Doping content be 0.1～3mol%.
The method for preparing Yb and Er double doping plumbous tungstate crystal conversion material realizes according to the following steps: one, take by weighing WO
3, PbO, Er
2O
3And Yb
2O
3, WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.1～3mol%, Yb
2O
3Doping content be 0.1～3mol%; Two, with the WO that takes by weighing
3, PbO, Er
2O
3And Yb
2O
3Put into platinum crucible after mixing, place then environment sintering 1～3h of 1000～1100 ℃, be cooled to room temperature; Three, adopt Czochralski grown crystal: through seeding, necking down, shouldering, receipts shoulder, isodiametric growth, pull and cycle of annealing, namely get Yb and Er double doping plumbous tungstate crystal conversion material; Seeding program in the step 3 wherein: will be warming up to fusing through the polycrystal material of oversintering, and keep fusion temperature 30min, and slowly reduce then temperature, and stop cooling, seed crystal continued growth under this temperature to seed crystal molten change in melt.
The present invention is doped element ytterbium (Yb) in Er lead tungstate-doped crystal up-conversion, and Yb energy level gap is about 10
4Cm
-1Wide coverage, can be excited by 980nm LD, its introducing can cause the bigger enhancing of the rare earth ion up-conversion luminescence of mixing altogether by transmission ofenergy, on the basis that keeps the original premium properties of Er lead tungstate-doped crystal, improved nearly three times of the green light band luminous intensity of Er lead tungstate-doped crystal.
Description of drawings
Fig. 1 is the luminous intensity curve spectrogram of gained Yb and Er double doping plumbous tungstate crystal conversion material and existing Er lead tungstate-doped crystal up-conversion in the embodiment 15, wherein a is the luminous intensity curve of Yb and Er double doping plumbous tungstate crystal conversion material, and b is the luminous intensity curve of Er lead tungstate-doped crystal up-conversion.
Embodiment
The specific embodiment one: present embodiment Yb and Er double doping plumbous tungstate crystal conversion material are by WO
3, PbO, Er
2O
3And Yb
2O
3Make; WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.1～3mol%, Yb
2O
3Doping content be 0.1～3mol%.
The specific embodiment two: present embodiment and the specific embodiment one are different is that Yb and Er double doping plumbous tungstate crystal conversion material are by WO
3, PbO, Er
2O
3And Yb
2O
3Make; WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.5mol%, Yb
2O
3Doping content be 0.5mol%.Other is identical with embodiment one.
The specific embodiment three: that present embodiment is different from the specific embodiment one or two is WO
3, PbO, Er
2O
3And Yb
2O
3Quality purity all be higher than 99.99%.Other is identical with embodiment one or two.
The specific embodiment four: the method that present embodiment prepares Yb and Er double doping plumbous tungstate crystal conversion material realizes according to the following steps: one, take by weighing WO
3, PbO, Er
2O
3And Yb
2O
3, WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.1～3mol%, Yb
2O
3Doping content be 0.1～3mol%; Two, with the WO that takes by weighing
3, PbO, Er
2O
3And Yb
2O
3Put into platinum crucible after mixing, place then environment sintering 1～3h of 1000～1100 ℃, be cooled to room temperature; Three, adopt Czochralski grown crystal: through seeding, necking down, shouldering, receipts shoulder, isodiametric growth, pull and cycle of annealing, namely get Yb and Er double doping plumbous tungstate crystal conversion material; Seeding program in the step 3 wherein: will be warming up to fusing through the polycrystal material of oversintering, and keep fusion temperature 30min, and slowly reduce then temperature, and stop cooling, seed crystal continued growth under this temperature to seed crystal molten change in melt.
The present embodiment crystal pulls after annealing can eliminate or reduce the structural stress that crystalline thermal stresses and doping bring.
The specific embodiment five: what present embodiment and the specific embodiment four were different is to take by weighing WO in the step 1
3, PbO, Er
2O
3And Yb
2O
3, WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.5mol%, Yb
2O
3Doping content be 0.5mol%.Other step and parameter are identical with embodiment four.
Embodiment six: what present embodiment and embodiment four were different is to place 1050 ℃ environment sintering 2h in the step 2, is cooled to room temperature.Other step and parameter are identical with embodiment four.
Embodiment seven: present embodiment and embodiment four are different be in the step 3 in the seeding program seed crystal do not change continued growth 2mm under the temperature molten.Other step and parameter are identical with embodiment four.
Embodiment eight: what present embodiment and embodiment four were different is the crystal pulling growth speed of protecting rotating speed and the 2～4mm/h of 30～45r/min in seeding in the step 3, shouldering, receipts shoulder and the isodiametric growth program; Crystal keeps the speed of rotation of 30～45r/min in cycle of annealing.Other step and parameter are identical with embodiment four.
Embodiment nine: present embodiment and embodiment four are different is that in the necking down program diameter of seed crystal to be contracted in the step 3 carefully be 3～4mm.Other step and parameter are identical with embodiment four.
Present embodiment can be eliminated the optical defect of seed crystal itself, and drops to the probability that the dislocation defects of seed crystal itself is introduced grown crystal minimum.
Embodiment ten: present embodiment and embodiment four are different be in the step 3 in the isometrical growth procedure temperature with the growth that heats up of the speed of 2 ℃/h.Other step and parameter are identical with embodiment four.
Embodiment 11: what present embodiment and embodiment four were different is to lift axial-temperature gradient in the step 3: be to be 15～25 ℃/cm under 40～50 ℃/cm, the liquid level on the liquid level, lifting radial symmetry gradient is 4～6 ℃/cm.Other step and parameter are identical with embodiment four.
Embodiment 12: present embodiment and embodiment four are different be in the step 3 with the speed annealing of 40～60 ℃/h, reduce temperature to room temperature.Other step and parameter are identical with embodiment four.
Embodiment 13: present embodiment and embodiment four are different be in the step 3 in the isometrical growth procedure temperature rise with the speed of 2 ℃/h.Other step and parameter are identical with embodiment four.
Embodiment 14: present embodiment and embodiment four are different is to pull in the step 3 immediately crystal to be lifted out liquid level after stopping in the program lifting.Other step and parameter are identical with embodiment four.
The specific embodiment 15: the method that present embodiment prepares Yb and Er double doping plumbous tungstate crystal conversion material realizes according to the following steps: one, take by weighing WO
3, PbO, Er
2O
3And Yb
2O
3, WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.5mol%, Yb
2O
3Doping content be 0.5mol%; Two, with the WO that takes by weighing
3, PbO, Er
2O
3And Yb
2O
3Put into platinum crucible after mixing, place then 1050 ℃ environment sintering 2h, be cooled to room temperature; Three, adopt Czochralski grown crystal: through seeding, necking down, shouldering, receipts shoulder, isodiametric growth, pull and cycle of annealing, namely get Yb and Er double doping plumbous tungstate crystal conversion material; Seeding program in the step 3 wherein: will be warming up to fusing through the polycrystal material of oversintering, and keep fusion temperature 30min, and slowly reduce then temperature, and stop cooling, seed crystal continued growth under this temperature to seed crystal molten change in melt.
Gained Yb and Er double doping plumbous tungstate crystal conversion material are tested after the surface finish of C face directional cutting and optical quality level in the present embodiment, by finding out among Fig. 1, Yb and Er double doping plumbous tungstate crystal conversion material improve nearly three times in the luminous intensity of the luminous strength ratio Er at 550nm green light band place lead tungstate-doped crystal up-conversion.
Claims (10)
1, Yb and Er double doping plumbous tungstate crystal conversion material is characterized in that Yb and Er double doping plumbous tungstate crystal conversion material are by WO
3, PbO, Er
2O
3And Yb
2O
3Make; WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.1～3mol%, Yb
2O
3Doping content be 0.1～3mol%.
2, Yb according to claim 1 and Er double doping plumbous tungstate crystal conversion material is characterized in that Yb and Er double doping plumbous tungstate crystal conversion material are by WO
3, PbO, Er
2O
3And Yb
2O
3Make; WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.5mol%, Yb
2O
3Doping content be 0.5mol%.
3, Yb according to claim 1 and 2 and Er double doping plumbous tungstate crystal conversion material is characterized in that WO
3, PbO, Er
2O
3And Yb
2O
3Quality purity all be higher than 99.99%.
4, the method for preparation Yb as claimed in claim 1 and Er double doping plumbous tungstate crystal conversion material is characterized in that the method for preparing Yb and Er double doping plumbous tungstate crystal conversion material realizes according to the following steps: one, take by weighing WO
3, PbO, Er
2O
3And Yb
2O
3, WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.1～3mol%, Yb
2O
3Doping content be 0.1～3mol%; Two, with the WO that takes by weighing
3, PbO, Er
2O
3And Yb
2O
3Put into platinum crucible after mixing, place then environment sintering 1～3h of 1000～1100 ℃, be cooled to room temperature; Three, adopt Czochralski grown crystal: through seeding, necking down, shouldering, receipts shoulder, isodiametric growth, pull and cycle of annealing, namely get Yb and Er double doping plumbous tungstate crystal conversion material.
5, the method for preparing Yb and Er double doping plumbous tungstate crystal conversion material according to claim 4 is characterized in that taking by weighing in the step 1 WO
3, PbO, Er
2O
3And Yb
2O
3, WO wherein
3With the mol ratio of PbO be 1: 1, Er
2O
3Doping content be 0.5mol%, Yb
2O
3Doping content be 0.5mol%.
6, the method for preparing Yb and Er double doping plumbous tungstate crystal conversion material according to claim 4 is characterized in that placing 1050 ℃ environment sintering 2h in the step 2, is cooled to room temperature.
7, the method for preparing Yb and Er double doping plumbous tungstate crystal conversion material according to claim 4 is characterized in that in the step 3 in the seeding program that seed crystal do not change continued growth 2mm under the temperature molten.
8, the method for preparing Yb and Er double doping plumbous tungstate crystal conversion material according to claim 4 is characterized in that the crystal pulling growth speed of protecting rotating speed and the 2～4mm/h of 30～45r/min in seeding in the step 3, shouldering, receipts shoulder and the isodiametric growth program; Crystal keeps the speed of rotation of 30～45r/min in cycle of annealing.
9, the method for preparing Yb and Er double doping plumbous tungstate crystal conversion material according to claim 4, it is characterized in that lifting axial-temperature gradient in the step 3: be to be 15～25 ℃/cm under 40～50 ℃/cm, the liquid level on the liquid level, lifting radial symmetry gradient is 4～6 ℃/cm.
10, the method for preparing Yb and Er double doping plumbous tungstate crystal conversion material according to claim 4 is characterized in that in the step 3 that temperature in the isometrical growth procedure is with the growth that heats up of the speed of 2 ℃/h.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100647849A CN101328614A (en) | 2008-06-20 | 2008-06-20 | Yb and Er double doping plumbous tungstate crystal conversion material and preparation thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100647849A CN101328614A (en) | 2008-06-20 | 2008-06-20 | Yb and Er double doping plumbous tungstate crystal conversion material and preparation thereof |
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|---|---|
| CN101328614A true CN101328614A (en) | 2008-12-24 |
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935879A (en) * | 2010-09-07 | 2011-01-05 | 中国科学院上海硅酸盐研究所 | Ytterbium/bismuth dual-doped lead tungstate crystal and preparation method thereof |
| CN102071023A (en) * | 2010-12-03 | 2011-05-25 | 陕西师范大学 | Silver gadolinium tungstate up-conversion material and preparation method thereof |
| CN110694611A (en) * | 2019-10-15 | 2020-01-17 | 大连工业大学 | Rare earth modified nRe-MxWO3FyParticles and method for producing same |
-
2008
- 2008-06-20 CN CNA2008100647849A patent/CN101328614A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101935879A (en) * | 2010-09-07 | 2011-01-05 | 中国科学院上海硅酸盐研究所 | Ytterbium/bismuth dual-doped lead tungstate crystal and preparation method thereof |
| CN101935879B (en) * | 2010-09-07 | 2012-05-30 | 中国科学院上海硅酸盐研究所 | Ytterbium/bismuth dual-doped lead tungstate crystal and preparation method thereof |
| CN102071023A (en) * | 2010-12-03 | 2011-05-25 | 陕西师范大学 | Silver gadolinium tungstate up-conversion material and preparation method thereof |
| CN102071023B (en) * | 2010-12-03 | 2013-06-12 | 陕西师范大学 | Silver gadolinium tungstate up-conversion material and preparation method thereof |
| CN110694611A (en) * | 2019-10-15 | 2020-01-17 | 大连工业大学 | Rare earth modified nRe-MxWO3FyParticles and method for producing same |
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Open date: 20081224 |