CN1233882C - Yb-YAG laser crystal growth method - Google Patents
Yb-YAG laser crystal growth method Download PDFInfo
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- CN1233882C CN1233882C CN 03116348 CN03116348A CN1233882C CN 1233882 C CN1233882 C CN 1233882C CN 03116348 CN03116348 CN 03116348 CN 03116348 A CN03116348 A CN 03116348A CN 1233882 C CN1233882 C CN 1233882C
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- 238000002109 crystal growth method Methods 0.000 title 1
- 239000013078 crystal Substances 0.000 claims abstract description 63
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 24
- 238000000034 method Methods 0.000 claims abstract description 22
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000001301 oxygen Substances 0.000 claims abstract description 16
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 16
- 229910052741 iridium Inorganic materials 0.000 claims abstract description 12
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 claims abstract description 12
- 230000006698 induction Effects 0.000 claims abstract description 10
- 239000002994 raw material Substances 0.000 claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 238000005303 weighing Methods 0.000 claims abstract description 3
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 8
- 229910052757 nitrogen Inorganic materials 0.000 abstract description 8
- 238000001816 cooling Methods 0.000 abstract 1
- 238000007599 discharging Methods 0.000 abstract 1
- 239000000463 material Substances 0.000 abstract 1
- 238000002844 melting Methods 0.000 abstract 1
- 230000008018 melting Effects 0.000 abstract 1
- 229910019655 synthetic inorganic crystalline material Inorganic materials 0.000 description 40
- 238000010521 absorption reaction Methods 0.000 description 9
- 239000000155 melt Substances 0.000 description 6
- 150000002500 ions Chemical class 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 2
- JNDMLEXHDPKVFC-UHFFFAOYSA-N aluminum;oxygen(2-);yttrium(3+) Chemical compound [O-2].[O-2].[O-2].[Al+3].[Y+3] JNDMLEXHDPKVFC-UHFFFAOYSA-N 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000002939 deleterious effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 229910019901 yttrium aluminum garnet Inorganic materials 0.000 description 1
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Abstract
A Yb: YAG laser crystal growing method, the device used is an induction heating pulling type single crystal furnace, the steps include: weighing raw materials according to the ratio of Yb to YAG, uniformly mixing, placing in an iridium crucible, and charging; slowly vacuumizing, inflating and heating the single crystal furnace; growing a crystal by using a lower seed crystal; slowly cooling to room temperature after the crystal growth is finished, and discharging; the method is characterized in that: the specific process of slowly vacuumizing, inflating and heating the single crystal furnace comprises the following steps: slowly vacuumizing the single crystal furnace to 8 x 10-3And (3) MP, pure nitrogen is filled, the temperature is raised after the pressure reaches 0.12MP, the pressure in the furnace is observed when the temperature reaches 1500 ℃, 1-5% of oxygen is filled according to the pressure in the furnace, and then the melting material is raised.
Description
Technical field:
The present invention relates to yb yag laser crystal (hereinafter to be referred as Yb:YAG), particularly a kind of growth method of Yb:YAG laser crystals.
Background technology:
YAG crystalline mineral name is a yttrium aluminum garnet, and molecular formula is Y
3Al
5O
12, belonging to isometric system, spacer is Oh (10)-Ia3d, in the Yb:YAG crystal, Yb
3+Ion can replace and is positioned at the Y that the dodecahedron center has eight-coordinate in the lattice
3+The ion case.Y
3+Ion and Yb
3+The effective ionic radius of ion in the dodecahedron lattice is close, is respectively: R
Yb 3+=0.985 , R
Y 3+=1.019 .
General with Czochralski grown Yb:YAG crystal, it is blue that the crystal that obtains is.This is because there is Yb
2+With the Re-F colour center, (consult document J.Appl.Phys.83 (1998): 3825).Owing to contain Yb in the crystal
2+, lattice is distorted, lattice imperfection is rolled up, and to Yb
3+Level structure cause disadvantageous effect.Caused 370nm and 625nm place to have the formation of absorption bands and Re-F colour center.Yb
2+With the existence of Re-F colour center be deleterious for the intrinsic spectrum property of Yb:YAG, the Yb that has not only reduced at 900-1050nm
3+The emissive porwer of intrinsic absorption and 1028-1060nm, and shortened Yb
3+Fluorescence lifetime in the YAG crystal.
Summary of the invention:
The growth method that the purpose of this invention is to provide a kind of Yb:YAG laser crystals is to improve the quality of Yb:YAG laser crystals.
Technical solution of the present invention is as follows:
A kind of growth method of Yb:YAG laser crystals, used device are induction heating pull-type single crystal growing furnace, and its step comprises: according to Yb:YAG ratio raw materials weighing and mix, place iridium crucible, shove charge; Single crystal growing furnace slowly vacuumizes, inflates and heats up; Following seeded growth crystal; Crystal growth finishes and slowly is cooled to room temperature, comes out of the stove; It is characterized in that:
The detailed process that described single crystal growing furnace slowly vacuumizes, inflates and heats up comprises: single crystal growing furnace slowly is evacuated to 8 * 10
-3MP charges into pure nitrogen gas, begins to the 0.12MP pressure to heat up, and observes the pressure in the stove during to 1500 ℃, charges into 1～5% oxygen and then intensification melt again according to the pressure in the stove.
The key here is to adopt the method for two steps inflation, is based on iridium crucible and can plays strong reaction with oxygen in the high temperature section below 1500 ℃, surpasses this thermotonus and then can reduce widely.It is colourless after the crystal of gas replenishment process growth is come out of the stove like this.
Through the Yb:YAG crystal of top process growth with common nitrogen in the Yb:YAG crystal Medium frequency induction Czochralski grown Yb:YAG laser crystals comparison of growing.The former disappears at the absorption bands at 370nm and 625nm place, and lattice imperfection has reduced a lot, at the Yb of 900-1050nm
3+Intrinsic absorbs and the emissive porwer of 1028-1060nm all improves greatly, and fluorescence lifetime has also improved a lot.
We analyze this is owing in our technical process, Yb
2+Can fully contact with oxygen, thereby can make wherein Yb
2+Fully react with oxygen and be oxidized to Yb
3+, oxygen enters and makes the oxygen vacancy defect obviously reduce in the lattice simultaneously.
Advantage of the present invention: adopt two step inflation processes to avoid valuable iridium crucible and play strong reaction, reduced the strong problem of oxidation of iridium crucible that direct introducing oxygen is caused in high temperature section below 1500 ℃ and oxygen; Also avoided simultaneously in the crystal annealing process because crystal is block, thereby made Yb wherein
2+Be difficult to be transformed into fully Yb
3+Problem.
Description of drawings:
Fig. 1 is used to grow Yb:YAG crystal unit synoptic diagram
Embodiment
The invention will be further described to enumerate several embodiment below.
Embodiment 1:
With Yb:YAG raw material mixing proportionally, place iridium crucible, shove charge.Slowly be evacuated to 8 * 10
-3MP charges into pure nitrogen gas, begins to the 0.12MP pressure to heat up, and observes the pressure in the stove during to 1500 ℃, charges into 1% oxygen again according to the pressure in the stove, the melt that heats up then, and following seed crystal is grown.Growth conditions is pulling rate 1～2mm/hr, and rotating speed 5～20rpm reduces to room temperature gradually after growth finishes and comes out of the stove.
Through the Yb:YAG crystal of top process growth with common nitrogen in the Yb:YAG crystal Medium frequency induction Czochralski grown Yb:YAG laser crystals comparison of growing.The former disappears at the absorption bands at 370nm and 625nm place, and lattice imperfection has reduced a lot, at the Yb of 900-1050nm
3+Intrinsic absorbs and the emissive porwer of 1028-1060nm all improves greatly, and fluorescence lifetime has also improved a lot.
Embodiment 2:
With Yb:YAG raw material mixing proportionally, place iridium crucible, shove charge.Slowly be evacuated to 8 * 10
-3MP charges into pure nitrogen gas, begins to the 0.12MP pressure to heat up, and observes the pressure in the stove during to 1500 ℃, charges into 1.5% oxygen again according to the pressure in the stove, the melt that heats up then, and following seed crystal is grown.Growth conditions is pulling rate 1～2mm/hr, and rotating speed 5～20rpm reduces to room temperature gradually after growth finishes and comes out of the stove.
Through the Yb:YAG crystal of top process growth with common nitrogen in the Yb:YAG crystal Medium frequency induction Czochralski grown Yb:YAG laser crystals comparison of growing.The former disappears at the absorption bands at 370nm and 625nm place, and lattice imperfection has reduced a lot, at the Yb of 900-1050nm
3+Intrinsic absorbs and the emissive porwer of 1028-1060nm all improves greatly, and fluorescence lifetime has also improved a lot.
Embodiment 3:
With Yb:YAG raw material mixing proportionally, place iridium crucible, shove charge.Slowly be evacuated to 8 * 10
-3MP charges into pure nitrogen gas, begins to the 0.12MP pressure to heat up, and observes the pressure in the stove during to 1500 ℃, charges into 2% oxygen again according to the pressure in the stove, the melt that heats up then, and following seed crystal is grown.Growth conditions is pulling rate 1～2mm/hr, and rotating speed 5～20rpm reduces to room temperature gradually after growth finishes and comes out of the stove.
Through the Yb:YAG crystal of top process growth with common nitrogen in the Yb:YAG crystal Medium frequency induction Czochralski grown Yb:YAG laser crystals comparison of growing.The former disappears at the absorption bands at 370nm and 625nm place, and lattice imperfection has reduced a lot, at the Yb of 900-1050nm
3+Intrinsic absorbs and the emissive porwer of 1028-1060nm all improves greatly, and fluorescence lifetime has also improved a lot.
Embodiment 4:
With Yb:YAG raw material mixing proportionally, place iridium crucible, shove charge.Slowly be evacuated to 8 * 10
-3MP charges into pure nitrogen gas, begins to the 0.12MP pressure to heat up, and observes the pressure in the stove during to 1500 ℃, charges into 3% oxygen again according to the pressure in the stove, the melt that heats up then, and following seed crystal is grown.Growth conditions is pulling rate 1～2mm/hr, and rotating speed 5～20rpm reduces to room temperature gradually after growth finishes and comes out of the stove.
Through the Yb:YAG crystal of top process growth with common nitrogen in the Yb:YAG crystal Medium frequency induction Czochralski grown Yb:YAG laser crystals comparison of growing.The former disappears at the absorption bands at 370nm and 625nm place, and lattice imperfection has reduced a lot, at the Yb of 900-1050nm
3+Intrinsic absorbs and the emissive porwer of 1028-1060nm all improves greatly, and fluorescence lifetime has also improved a lot.
Embodiment 5:
With Yb:YAG raw material mixing proportionally, place iridium crucible, shove charge.Slowly be evacuated to 8 * 10
-3MP charges into pure nitrogen gas, begins to the 0.12MP pressure to heat up, and observes the pressure in the stove during to 1500 ℃, charges into 3.5% oxygen again according to the pressure in the stove, the melt that heats up then, and following seed crystal is grown.Growth conditions is pulling rate 1～2mm/hr, and rotating speed 5～20rpm reduces to room temperature gradually after growth finishes and comes out of the stove.
Through the Yb:YAG crystal of top process growth with common nitrogen in the Yb:YAG crystal Medium frequency induction Czochralski grown Yb:YAG laser crystals comparison of growing.The former disappears at the absorption bands at 370nm and 625nm place, and lattice imperfection has reduced a lot, at the Yb of 900-1050nm
3+Intrinsic absorbs and the emissive porwer of 1028-1060nm all improves greatly, and fluorescence lifetime has also improved a lot.
Embodiment 6:
With Yb:YAG raw material mixing proportionally, place iridium crucible, shove charge.Slowly be evacuated to 8 * 10
-3MP charges into pure nitrogen gas, begins to the 0.12MP pressure to heat up, and observes the pressure in the stove during to 1500 ℃, charges into 5% oxygen again according to the pressure in the stove, the melt that heats up then, and following seed crystal is grown.Growth conditions is pulling rate 1～2mm/hr, and rotating speed 5～20rpm reduces to room temperature gradually after growth finishes and comes out of the stove.
Through the Yb:YAG crystal of top process growth with common nitrogen in the Yb:YAG crystal Medium frequency induction Czochralski grown Yb:YAG laser crystals comparison of growing.The former disappears at the absorption bands at 370nm and 625nm place, and lattice imperfection has reduced a lot, at the Yb of 900-1050nm
3+Intrinsic absorbs and the emissive porwer of 1028-1060nm all improves greatly, and fluorescence lifetime has also improved a lot.
Claims (1)
1, a kind of Yb: the growth method of YAG laser crystals, used device are induction heating pull-type single crystal growing furnace, and its step comprises: according to Yb: YAG ratio raw materials weighing also mixes, and places iridium crucible, shove charge; Single crystal growing furnace slowly vacuumizes, inflates and heats up; Following seeded growth crystal; Crystal growth finishes and slowly is cooled to room temperature, comes out of the stove; It is characterized in that:
The detailed process that described single crystal growing furnace slowly vacuumizes, inflates and heats up comprises: single crystal growing furnace slowly is evacuated to 8 * 10
-3MP charges into pure nitrogen gas, begins to the 0.12MP pressure to heat up, and observes the pressure in the stove during to 1500 ℃, charges into 1～5% oxygen and then intensification melt again according to the pressure in the stove.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116348 CN1233882C (en) | 2003-04-11 | 2003-04-11 | Yb-YAG laser crystal growth method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03116348 CN1233882C (en) | 2003-04-11 | 2003-04-11 | Yb-YAG laser crystal growth method |
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| Publication Number | Publication Date |
|---|---|
| CN1442517A CN1442517A (en) | 2003-09-17 |
| CN1233882C true CN1233882C (en) | 2005-12-28 |
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|---|---|---|---|
| CN 03116348 Expired - Fee Related CN1233882C (en) | 2003-04-11 | 2003-04-11 | Yb-YAG laser crystal growth method |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104357899B (en) * | 2014-11-21 | 2017-03-29 | 中国电子科技集团公司第二十六研究所 | Large scale Yb YAG laser crystal kyropoulos preparation method |
| CN110067025A (en) * | 2018-01-20 | 2019-07-30 | 河北胤丞光电科技有限公司 | A kind of preparation method of the YAG crystal of high-output power |
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2003
- 2003-04-11 CN CN 03116348 patent/CN1233882C/en not_active Expired - Fee Related
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| Publication number | Publication date |
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| CN1442517A (en) | 2003-09-17 |
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Granted publication date: 20051228 Termination date: 20120411 |