CN102051684A - Method for growing thulium-holmium co-doped yttrium calcium aluminate laser crystal - Google Patents
Method for growing thulium-holmium co-doped yttrium calcium aluminate laser crystal Download PDFInfo
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- CN102051684A CN102051684A CN 201110008857 CN201110008857A CN102051684A CN 102051684 A CN102051684 A CN 102051684A CN 201110008857 CN201110008857 CN 201110008857 CN 201110008857 A CN201110008857 A CN 201110008857A CN 102051684 A CN102051684 A CN 102051684A
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- 239000013078 crystal Substances 0.000 title claims abstract description 91
- 238000000034 method Methods 0.000 title claims abstract description 14
- DFENVCUUBABVIU-UHFFFAOYSA-N [Ca].[Y] Chemical compound [Ca].[Y] DFENVCUUBABVIU-UHFFFAOYSA-N 0.000 title claims abstract description 11
- WQNUBQUNDDGZTB-UHFFFAOYSA-N [Ho].[Tm] Chemical compound [Ho].[Tm] WQNUBQUNDDGZTB-UHFFFAOYSA-N 0.000 title claims abstract description 11
- 239000000463 material Substances 0.000 claims description 27
- 239000002994 raw material Substances 0.000 claims description 17
- 229910052741 iridium Inorganic materials 0.000 claims description 11
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims description 11
- 238000005245 sintering Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 230000006698 induction Effects 0.000 claims description 4
- 238000005086 pumping Methods 0.000 claims description 4
- 230000000630 rising effect Effects 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 2
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 2
- 238000012856 packing Methods 0.000 claims description 2
- 238000003746 solid phase reaction Methods 0.000 claims description 2
- 238000010671 solid-state reaction Methods 0.000 claims description 2
- 238000007664 blowing Methods 0.000 claims 1
- 230000007547 defect Effects 0.000 abstract description 3
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 3
- -1 Rare earth ions Chemical class 0.000 abstract description 2
- 238000002474 experimental method Methods 0.000 abstract description 2
- 239000011159 matrix material Substances 0.000 abstract description 2
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 239000011521 glass Substances 0.000 description 6
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 238000010257 thawing Methods 0.000 description 6
- 238000010792 warming Methods 0.000 description 6
- 238000005336 cracking Methods 0.000 description 5
- 238000000862 absorption spectrum Methods 0.000 description 3
- 229910052689 Holmium Inorganic materials 0.000 description 2
- 229910052775 Thulium Inorganic materials 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- 241001216449 Crystallophyes Species 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000003776 cleavage reaction Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 230000007017 scission Effects 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 238000009331 sowing Methods 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
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Abstract
A method for growing thulium-holmium co-doped yttrium calcium aluminate laser crystal directly on CaYAlO4Simultaneous doping of Tm in a crystalline matrix3+，Ho3+Rare earth ions are grown into high-quality Tm/Ho CaYAlO by a pulling method4Experiments show that the method is feasible, and the grown crystal is complete and has no crack and no macroscopic defect and can be used as a laser medium.
Description
Technical field
The present invention relates to laser crystals, particularly a kind of thulium holmium is mixed the yttrium-calcium aluminate laser crystals altogether and (is designated hereinafter simply as Tm/Ho:CaYAlO
4) growth method.
Background technology
Laser diode-pumped solid laser has compact construction, good beam quality, and the energy advantages of higher, it is widely used in industry, fields such as national defence.Because Ho
3+ 5I
7→
5I
8Energy level transition is mixed Ho
3+Solid laser has unique advantage at 2 mu m waveband lasers.But mix Ho at present
3+Laser crystals does not also have suitable laser diode pumping source, usually adopts Tm
3+The pumping of ion laser resonance realizes laser output.
As a kind of easier method is exactly directly with Tm
3+, Ho
3+Mix altogether in a certain crystal substrate, the transmission ofenergy between its particle is finished in same matrix inside, thereby simplify laser structure, realize the purpose of high-efficient operation.2010, reported first such as A.A.Lagatsky Tm, Ho mixes the femtosecond output of laser crystals altogether, exports average laser power at 2055nm place and reaches 130mW (referring to Optics Letters, 35 (2010), 172).CaYAlO
4Have perovskite structure, rare earth element Tm, Ho are in C in lattice
4vSymmetric position.CaYAlO
4The crystallophy excellent performance is the unordered laser host of a kind of ideal, codope Tm/Ho:CaYAlO
4Crystal yet there are no report.
Summary of the invention
The purpose of this invention is to provide the growth method that a kind of thulium holmium is mixed the yttrium-calcium aluminate laser crystals altogether, directly at CaYAlO
4Tm simultaneously mixes in the crystal substrate
3+, Ho
3+Rare earth ion adopts Czochralski grown to prepare high-quality Tm/Ho:CaYAlO
4Laser crystals.
Technical solution of the present invention is as follows:
A kind of thulium holmium is mixed the growth method of yttrium-calcium aluminate laser crystals altogether, and its characteristics are to comprise the following steps:
1. adopt Frequency Induction Heating Czochralski grown Tm/Ho:CaYAlO
4Crystal, heating element are iridium crucible, and this crystalline raw material takes by weighing according to the mol ratio of following reaction formula:
2CaCO
3+(1-x-y)Y
2O
3+xHo
2O
3+yTm
2O
3+Al
2O
3＝2CaY
(1-x-y)Ho
xTm
yAlO
4+2CO
2
Wherein the span of x and y is: 0＜x≤0.008,0＜y≤0.12;
2. described raw material is ground be mixed even after, under hydropress, be compacted into piece, and in retort furnace 1200 ℃ of sintering 10 hours, solid state reaction takes place, the piece material that sinters pack into the iridium crucible and the pulling growth single crystal growing furnace of packing into;
3. described single crystal growing furnace pumping high vacuum charges into nitrogen atmosphere then, 1810 ℃ of growth temperatures, crystal pull rate 1-2mm/h, speed of rotation 10-20rpm;
4. seed crystal is goed deep into melt, through the crystal necking down, shouldering, isodiametric growth, the ending stage, crystal is pulled from melt, slowly reduce the interior temperature of czochralski furnace then to room temperature;
5. open stay-warm case, in the pulling growth single crystal growing furnace, take out the seed crystal frame, take out crystal, obtain the thulium holmium and mix the yttrium-calcium aluminate laser crystals altogether.
Described crystal raw material rises to 1810 ℃ in described pulling growth single crystal growing furnace after, temperature to 1820 in the continuation rising stove～1900 ℃, and kept 0.5～1 hour, allow the liquation body fully melt mixing.
Described seed crystal composition is CaYAlO
4, or Tm/Ho:CaYAlO
4, seed crystal end face direction is [100], [101], or [001].
The Czochralski grown Tm/Ho:CaYAlO that the present invention is used
4The device of laser crystals is common Frequency Induction Heating single crystal growing furnace.Total system comprises iridium crucible, vacuum apparatus, parts such as Medium frequency induction generator power and temperature control.
Experiment shows that method of the present invention is feasible, and the crystal perfection of growth does not have cracking, and no macroscopic defects can be used as in laser medium.When using [100] direction seed crystal, have well (001) crystal face embodiment at plane of crystal, further specify this kind method and prepare Tm/Ho:CaYAlO
4The feasibility of laser crystals.
Description of drawings
Fig. 1 is the CaY of one embodiment of the invention
0.935Ho
0.005Tm
0.06AlO
4Crystalline polarization absorption spectrum
Embodiment
The invention will be further described below in conjunction with embodiment and accompanying drawing, but should not limit protection scope of the present invention with this.
Embodiment 1:
Get x=0.005 in the proportioning raw materials of this embodiment, y=0.06.With CaCO
3, Y
2O
3, Ho
2O
3, Tm
2O
3, Al
2O
3High pure raw material (content is all greater than 99.999%), by 2: 0.935: 0.005: stoichiometric ratio took by weighing in 0.06: 1.After mechanically mixing is even, on swager, be pressed into block material with the synthetic glass mould.With the material that presses 1200 ℃ of sintering 10 hours in retort furnace.Then the refrigerative material is put into iridium crucible, reinstall czochralski furnace.After vacuumizing in the stove, charge into nitrogen again.Be warming up to 1850 ℃, allow after the abundant thawing mixing of material, after 1 hour, be cooled to 1810 ℃, put down [100] direction CaYAlO
4Seed crystal, beginning growing crystal, crystal pulling rate 1.2mm/h, speed of rotation 10rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal.Crystal perfection does not have cracking, is the plano-convex interface during crystal growth as can be seen from the afterbody pattern.
With above-mentioned CaY
0.935Ho
0.005Tm
0.06AlO
4The monocrystalline orientation cuts out 11 * 10 * 1mm
3Thin slice.After the lamina of light optical polishing, adopt Lambda 900 spectrophotometers to test polarized absorption spectrum under its room temperature.Fig. 1 is present embodiment CaY
0.935Ho
0.005Tm
0.06AlO
4The monocrystalline thin slice can be used for laser medium at the polarized absorption spectrum of 300～2200nm wave band.
Embodiment 2:
Get x=0.005 in the proportioning raw materials of present embodiment, y=0.10.With CaCO
3, Y
2O
3, Ho
2O
3, Tm
2O
3, Al
2O
3High pure raw material (content is all greater than 99.999%), by 2: 0.895: 0.005: stoichiometric ratio took by weighing in 0.10: 1.After mechanically mixing is even, on swager, be pressed into block material with the synthetic glass mould.With the material that presses 1200 ℃ of sintering 10 hours in retort furnace.Then the refrigerative material is put into iridium crucible, reinstall lifting furnace.After vacuumizing in the stove, charge into nitrogen again.Be warming up to 1840 ℃, allow after the abundant thawing mixing of material, after 1 hour, be cooled to 1810 ℃, put down [101] direction CaYAlO
4Seed crystal, the beginning growing crystal.Crystal pulling rate 1.0mm/h, speed of rotation 15rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal, crystal perfection does not have cracking.In the present embodiment, with the crystal that [101] direction seeded growth is come out, the surface does not embody cleavage surface.
Embodiment 3:
Get x=0.004 in the proportioning raw materials of present embodiment, y=0.08.With CaCO
3, Y
2O
3, Ho
2O
3, Tm
2O
3, Al
2O
3High pure raw material (content is all greater than 99.999%), by 2: 0.916: 0.004: stoichiometric ratio took by weighing in 0.08: 1.After mechanically mixing is even, on swager, be pressed into block material with the synthetic glass mould.With the material that presses 1200 ℃ of sintering 10 hours in retort furnace.Then the refrigerative material is put into iridium crucible, reinstall lifting furnace.After vacuumizing in the stove, charge into nitrogen again.Be warming up to 1820 ℃, allow after the abundant thawing mixing of material, after 0.5 hour, be cooled to 1810 ℃.Seed crystal adopts [100] direction Tm/Ho:CaYAlO
4Seed crystal, the beginning growing crystal.Crystal pulling rate 1.3mm/h, speed of rotation 20rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal.Crystal perfection does not have cracking, is the plano-convex interface when afterbody shows crystal growth as can be seen from afterbody, and well embodies (001) crystal face.Soaking time is short slightly after changing material in the present embodiment, but compares with above-mentioned embodiment in the stage of sowing, and does not observe obvious difference.
Embodiment 4:
Get x=0.004 in the proportioning raw materials of present embodiment, y=0.12.With CaCO
3, Y
2O
3, Ho
2O
3, Tm
2O
3, Al
2O
3High pure raw material (content is all greater than 99.999%), by 2: 0.876: 0.004: stoichiometric ratio took by weighing in 0.12: 1.After mechanically mixing is even, on swager, be pressed into block material with the synthetic glass mould.With the material that presses 1200 ℃ of sintering 10 hours in retort furnace.Then the refrigerative material is put into iridium crucible, reinstall lifting furnace.After vacuumizing in the stove, charge into nitrogen again.Be warming up to 1840 ℃, allow after the abundant thawing mixing of material, after 1 hour, be cooled to 1810 ℃.Put down [001] direction Tm/Ho:CaYAlO
4Seed crystal, the beginning growing crystal.Crystal pulling rate 1.5mm/h, speed of rotation 20rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal, crystal mass is good.
Embodiment 5:
Get x=0.006 in the proportioning raw materials of present embodiment, y=0.10.With CaCO
3, Y
2O
3, Ho
2O
3, Tm
2O
3, Al
2O
3High pure raw material (content is all greater than 99.999%), by 2: 0.894: 0.006: stoichiometric ratio took by weighing in 0.10: 1.After mechanically mixing is even, on swager, be pressed into block material with the synthetic glass mould.With the material that presses 1200 ℃ of sintering 10 hours in retort furnace.Then the refrigerative material is put into iridium crucible, reinstall lifting furnace.After vacuumizing in the stove, charge into nitrogen again.Be warming up to 1840 ℃, allow after the abundant thawing mixing of material, after 1 hour, be cooled to 1810 ℃, put down [101] CaYAlO
4Seed crystal, the beginning growing crystal.Crystal pulling rate 1.5mm/h, speed of rotation 20rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal.
Embodiment 6:
Get x=0.008 in the proportioning raw materials of present embodiment, y=0.08.With CaCO
3, Y
2O
3, Ho
2O
3, Tm
2O
3, Al
2O
3High pure raw material (content is all greater than 99.999%), by 2: 0.912: 0.008: stoichiometric ratio took by weighing in 0.08: 1.After mechanically mixing is even, on swager, be pressed into block material with the synthetic glass mould.With the material that presses 1200 ℃ of sintering 10 hours in retort furnace.Then the refrigerative material is put into iridium crucible, reinstall lifting furnace.After vacuumizing in the stove, charge into nitrogen again.Be warming up to 1840 ℃, allow after the abundant thawing mixing of material, after 1 hour, be cooled to 1810 ℃, put down [001] CaYAlO
4Seed crystal, the beginning growing crystal.Crystal pulling rate 1.5mm/h, speed of rotation 15rpm.Behind the growing crystal, slowly reduce to room temperature, take out crystal, crystal does not have cracking, no macroscopic defects.
Claims (3)
1. the growth method that the thulium holmium is mixed the yttrium-calcium aluminate laser crystals altogether is characterized in that comprising the following steps:
1. adopt Frequency Induction Heating Czochralski grown Tm/Ho:CaYAlO
4Crystal, heating element are iridium crucible, and this crystalline raw material takes by weighing according to the mol ratio of following reaction formula:
2CaCO
3+(1-x-y)Y
2O
3+xHo
2O
3+yTm
2O
3+Al
2O
3＝2CaY
(1-x-y)Ho
xTm
yAlO
4+2CO
2
Wherein the span of x and y is: 0＜x≤0.008,0＜y≤0.12;
2. described raw material is ground be mixed even after, under hydropress, be compacted into piece, and in retort furnace 1200 ℃ of sintering 10 hours, solid state reaction takes place, the piece material that sinters pack into the iridium crucible and the czochralski furnace of packing into;
3. described single crystal growing furnace pumping high vacuum charges into nitrogen atmosphere then, 1810 ℃ of growth temperatures, crystal pull rate 1-2mm/h, speed of rotation 10-20rpm;
4. seed crystal is goed deep into melt, through the crystal necking down, shouldering, isodiametric growth, the ending stage, crystal is pulled from melt, slowly reduce the interior temperature of lifting furnace then to room temperature;
5. stay-warm case is opened in blowing out, takes out the seed crystal frame in the pulling growth single crystal growing furnace, takes out crystal, obtains the thulium holmium and mixes the yttrium-calcium aluminate laser crystals altogether.
2. thulium holmium according to claim 1 is mixed the growth method of yttrium-calcium aluminate laser crystals altogether, after it is characterized in that in lifting furnace, rising to 1810 ℃, and temperature to 1820 in the continuation rising stove～1900 ℃, and kept 0.5～1 hour, allow the liquation body fully melt mixing.
3. thulium holmium according to claim 1 is mixed the growth method of yttrium-calcium aluminate laser crystals altogether, it is characterized in that described seed crystal composition is CaYAlO
4, or Tm/Ho:CaYAlO
4, seed crystal end face direction is [100], [101], or [001].
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109338460A (en) * | 2018-09-30 | 2019-02-15 | 中国科学院合肥物质科学研究院 | A method of control garnet crystal nucleus growth |
| CN111041557A (en) * | 2019-06-04 | 2020-04-21 | 中国科学院上海光学精密机械研究所 | Thulium-holmium double-doped lutetium oxide laser crystal and growth method and application thereof |
| CN115491765A (en) * | 2022-10-27 | 2022-12-20 | 江苏师范大学 | Thulium-doped calcium yttrium aluminate single crystal fiber with waveband of 2 microns and preparation method thereof |
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|---|---|---|---|---|
| CN101529672A (en) * | 2006-10-24 | 2009-09-09 | 皇家飞利浦电子股份有限公司 | Optically pumped solid-state laser with co-doped gain medium |
| CN101701355A (en) * | 2009-11-25 | 2010-05-05 | 中国科学院上海光学精密机械研究所 | Pulling growth method of neodymium-doped calcium yttrium aluminate laser crystal |
-
2011
- 2011-01-14 CN CN 201110008857 patent/CN102051684A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101529672A (en) * | 2006-10-24 | 2009-09-09 | 皇家飞利浦电子股份有限公司 | Optically pumped solid-state laser with co-doped gain medium |
| CN101701355A (en) * | 2009-11-25 | 2010-05-05 | 中国科学院上海光学精密机械研究所 | Pulling growth method of neodymium-doped calcium yttrium aluminate laser crystal |
Non-Patent Citations (3)
| Title |
|---|
| 《Journal of Crystal growth》 20001031 Wanyan Wang,etc Study of single-crystal growth of Tm3+:CaYAlO4 by the floating-zone method 56-60 1-3 第219卷, 第1-2期 * |
| 《Journal of Crystal Growth》 20100731 Dong zhen Li,etc Crystal growth and spectroscopic properties of Yb:CaYAlO4 single crystal 2117-2121 1-3 第312卷, 第14期 * |
| 《Optical materials》 19941031 J.Andrew Hutchinson,etc Spectroscopic evaluation of CaYAlO4 doped with trivalent Er,Tm,Yb and Ho for eyesafe laser applications 287-306 1-3 第3卷, 第4期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109338460A (en) * | 2018-09-30 | 2019-02-15 | 中国科学院合肥物质科学研究院 | A method of control garnet crystal nucleus growth |
| CN111041557A (en) * | 2019-06-04 | 2020-04-21 | 中国科学院上海光学精密机械研究所 | Thulium-holmium double-doped lutetium oxide laser crystal and growth method and application thereof |
| CN115491765A (en) * | 2022-10-27 | 2022-12-20 | 江苏师范大学 | Thulium-doped calcium yttrium aluminate single crystal fiber with waveband of 2 microns and preparation method thereof |
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Application publication date: 20110511 |