CN1837419B - Ytterbium doped Y0.8LaCa4O(BO3)3 laser crystal, its preparation method and use - Google Patents
Ytterbium doped Y0.8LaCa4O(BO3)3 laser crystal, its preparation method and use Download PDFInfo
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- CN1837419B CN1837419B CN2005100639957A CN200510063995A CN1837419B CN 1837419 B CN1837419 B CN 1837419B CN 2005100639957 A CN2005100639957 A CN 2005100639957A CN 200510063995 A CN200510063995 A CN 200510063995A CN 1837419 B CN1837419 B CN 1837419B
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Abstract
This invention provides a laser crystal adulterated with ytterbium boracic acid lanthanum oxygen calcium illinium lanthanum and its method for preparation and usage, which relates to an artificial crystal field, in particular to A laser crystal adulterated with ytterbium boracic acid lanthanum oxygen calcium illinium lanthanum and its method for preparation and usage. Using lifting and pulling method, at about 1500 degrees, with crystal rotary rate of 5-20 revolutions per minuten and pulling rate of 0.5-2 millimeter of hour, producing Yb3+:Ca3La2(BO3)4 crystal of top-quality and bigger size. The crystal is a new laser crystal, and can produce laser output of about 1 mum wavelength. The solid-state laser produced from the crystal can be used in many fields such as spectroscopy, biomedicine and military affairs.
Description
Technical field
The present invention relates to artificial lens and growth field thereof, especially relate to a kind of laser crystal material as the operation material in the solid laser.
Background technology
Laser crystals is the operation material of solid statelaser, and it is meant with the crystal to be matrix, and the luminescence center absorptive pumping luminous energy through separation also is translated into the luminescent material of laser output.Solid laser working substance is made up of substrate material and active ions, and its various physics and chemical property are mainly by the substrate material decision, and its spectral response curve and fluorescence lifetime etc. are then determined by the level structure of active ions.From nineteen sixty, succeeded in developing since the synthetic ruby pulsed laser, up to now, found hundreds of laser crystalss, but because of a variety of causes, the laser crystals that can really obtain practical application has only ten to plant.
At present, most widely used laser crystals is yttrium aluminum garnet (YAG) crystal of Nd ion doped, and it has various preferably physics and chemical property, and is easy to grow high optical quality, large-sized gem-quality crystal.But it is narrow that it exists spectral line of absorption, is unwell to the shortcoming of carrying out pumping with LD, and the LD pumping will be the developing direction of laser pumping source from now on.
All actively seek various physics, chemical property and superior both at home and abroad at present, and be easy to the high-quality laser crystal material that grows high optical quality, large size and be suitable for the LD pumping.Ytterbium ion is the simplest ion of level structure, and it absorbs bandwidth and effectively is coupled with InGaAs LD pumping source, is fit to very much the LD pumping.Than neodymium ion, ytterbium ion has many good qualities, and as not having excited state absorption and last conversion, has high fluorescence lifetime and light conversion efficiency or the like.Therefore, ytterbium ion becomes the choosing of the hot topic of laser crystals active ions in recent years.
Summary of the invention
The object of the invention just is to develop a kind of new laser crystals Yb
3+: Y
0.8La
0.2Ca
4O (BO
3)
3, can directly use photoflash lamp and LD pumping, laser crystal material with higher conversion efficiency.
Yb
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystal belongs to oblique system, has Cm spacer structure.Wherein ytterbium ion is as dopant ion; Replace the crystallographic site of yttrium and lanthanum ion, the doping content of ytterbium is between 1at.%～20at.%, and fluorescence lifetime (τ) is 1.5～3.0ms; Its fluorescence lifetime is the function of ytterbium ion concentration, can mix the ytterbium ion of different concns according to different needs.Experimental result shows the laser of its exportable 1 μ m wavelength around, can be used as laser crystals.Yb
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystal is a kind of compound of congruent melting, adopts Czochralski grown to go out, and presses reaction formula: 4CaCO
3+ 0.4Y
2O
3+ 0.1La
2O
3+ 3H
3BO
3=Y
0.8La
0.2Ca
4O (BO
3)
3+ 3CO
2+ 4.5H
2The ratio of O is claimed appearance, mixing, compressing tablet, and Yb
2O
3Then pressing desired concn adds.Raw materials usedly be:
| The medicine name | Purity | Producer |
| Yb 2O 3 | 99.999％ | Changchun Applied Chemistry Research Inst., Chinese Academy of Sciences |
| Y 2O 3 | 99.999％ | Changchun Applied Chemistry Research Inst., Chinese Academy of Sciences |
| La 2O 3 | 99.999％ | Changchun Applied Chemistry Research Inst., Chinese Academy of Sciences |
| CaCO 3 | 99.99％ | Shanghai the May 4th chemical reagent factory |
| H 3BO 3 | 99.99％ | Shanghai chemical reagents corporation of Chinese Medicine group |
Its main growth conditions is following: growth be in the iridium crucible, rare gas element is (like N
2, Ar etc.) carry out under the atmosphere, the parameter of crystal growth is about 1500 ℃ of growth temperatures, pulling speed is 0.5～2.0 millimeter/hour, 5～20 rev/mins of crystal rotating speeds have grown high-quality Yb
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystal.
With the Yb that grows
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystal has carried out the collection of diffraction data on four-circle diffractometer, structural analysis shows that it belongs to oblique system, and spacer is Cm, and unit cell parameters does
β=101.22 °,
, density 3.39g/cm
3Adopting oil-immersion method to record its specific refractory power is 1.71.
With the Yb that grows
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystal carries out the analytical test of absorption spectrum, fluorescence spectrum and fluorescence lifetime etc., and the result shows: the ytterbium ion doping content is the Yb of 10.0at.%
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystalline master absorption peak is at 977nm, and its peak width at half is 2nm, and the absorption jump cross section is 1.37 * 10
-20Cm
2, be suitable for adopting the InGaAs semiconductor laser to carry out pumping, help the absorption of laser crystals to pump light, improve pumping efficiency; The emission band that a non-constant width is arranged at the 900nm-1150nm place, wherein the emission transition cross section of emission peak 1033nm is 9.76 * 10
-21Cm
2, fluorescence lifetime is 2.69ms, the crystal that fluorescence lifetime is long can accumulate more particle at last energy level, has increased energy storage, helps the raising of device output rating and output energy.Therefore, Yb
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystal can obtain bigger output, is a kind of high conversion efficiency, low cost, high optical quality and actual application prospect is arranged and the laser crystals of use value.
Yb
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystal can grow superior in quality crystal easily with crystal pulling method; Fast growth, the crystal quality is hard, has good heat-conducting; Good optical characteristics is arranged; Be easy to obtain laser output with flash lamp pumping and LD pumping, laser output wavelength is about 1 μ m, and this crystal can be used as a kind of laser crystals preferably.
Embodiment
Embodiment 1: the Czochralski grown doping content is 10.0at.%Yb
3+Yb
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Laser crystals.
Will be by the load weighted CaCO of proportion speed
3, Y
2O
3, La
2O
3, H
3BO
3, Yb
2O
3Mixed grinding is even, behind the compressing tablet, puts into φ 60 * 40mm
3Platinum alloy crucible in, in retort furnace in 800 ℃ of solid state reactions 12 hours; After the taking-up, grind compressing tablet again and be warming up to 1200 ℃ of reactions 24 hours again.Synthetic good above sample is put into the iridium crucible, adopt crystal pulling method, at N
2In the atmosphere, growth temperature is that 1505 ℃, crystal rotating speed are 12 rev/mins, and pulling rate is under 1 millimeter/hour the situation, to have grown and be of a size of 20 * 16 * 15mm
3High-quality Yb
3+Content is the Yb of 10.0at.%
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystal.
Embodiment 2: the Czochralski grown doping content is 15.0at.%Yb
3+Yb
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Laser crystals.
Will be by the load weighted CaCO of proportion speed
3, Y
2O
3, La
2O
3, H
3BO
3, Yb
2O
3Mixed grinding is even, behind the compressing tablet, puts into φ 60 * 40mm
3Platinum alloy crucible in, in retort furnace in 800 ℃ of solid state reactions 12 hours; After the taking-up, grind compressing tablet again and be warming up to 1200 ℃ of reactions 24 hours again.Synthetic good above sample is put into the iridium crucible, adopt crystal pulling method, at N
2In the atmosphere, growth temperature is that 1500 ℃, crystal rotating speed are 10 rev/mins, and pulling rate is under 1 millimeter/hour the situation, to have grown and be of a size of 25 * 22 * 15mm
3High-quality Yb
3+Content is the Yb of 15.0at.%
3+: Y
0.8La
0.2Ca
4O (BO
3)
3Crystal.
Claims (3)
1. blended ytterbium boric acid oxygen calcium yttrium lanthanum laser crystals, it is characterized in that: this crystalline molecular formula is Yb
3+: Y
0.8La
0.2Ca
4O (BO
3)
3, Yb
3+Ion replaces Y in the crystal as dopant ion
3+And La
3+The ionic crystallographic site, its doping content belongs to oblique system between 1at.-20at.%, and spacer is Cm, and unit cell parameters does
β=101.22 °,
Density 3.39g/cm
3, specific refractory power 1.71.
2. the preparation method of the laser crystals of a claim 1 is characterized in that: this crystal by adopting Czochralski grown, and with Y
2O
3, La
2O
3, CaCO
3, H
3BO
3And Yb
2O
3Be raw material, press reaction formula: 4CaCO
3+ 0.4Y
2O
3+ 0.1La
2O
3+ 3H
3BO
3==Y
0.8La
0.2Ca
4O (BO
3)
3+ 3CO
2+ 4.5H
2The ratio of O is claimed appearance, mixing, compressing tablet, and Yb
2O
3Then press desired concn and add, in the iridium crucible, pulling growth goes out crystal under the inert gas atmosphere, and the parameter of crystal growth is about 1500 ℃ of growth temperatures, and pulling speed is 0.5～2.0 millimeter/hour, and the crystal rotating speed is 5～20 rev/mins.
3. the purposes of the laser crystals of a claim 1, it is characterized in that: this crystal is used for solid statelaser as working-laser material, uses flash lamp pumping and LD pumping, excites the laser that produces 1 μ m wavelength around to export.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005100639957A CN1837419B (en) | 2005-03-25 | 2005-03-25 | Ytterbium doped Y0.8LaCa4O(BO3)3 laser crystal, its preparation method and use |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2005100639957A CN1837419B (en) | 2005-03-25 | 2005-03-25 | Ytterbium doped Y0.8LaCa4O(BO3)3 laser crystal, its preparation method and use |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1837419A CN1837419A (en) | 2006-09-27 |
| CN1837419B true CN1837419B (en) | 2012-05-30 |
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|---|---|---|---|
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102965730A (en) * | 2011-09-01 | 2013-03-13 | 中国科学院福建物质结构研究所 | Novel ytterbium-activating-gadolinium calcium borate ultrafast laser crystal |
| CN110528075A (en) * | 2019-10-17 | 2019-12-03 | 中国工程物理研究院化工材料研究所 | A kind of blended ytterbium boric acid calcium lanthanum yttrium mixed crystal laser crystal and its preparation method and application |
| CN110607558A (en) * | 2019-10-17 | 2019-12-24 | 中国工程物理研究院化工材料研究所 | Ytterbium-doped calcium borate gadolinium yttrium mixed crystal laser crystal and preparation method and application thereof |
| CN110863244A (en) * | 2019-11-28 | 2020-03-06 | 中国工程物理研究院化工材料研究所 | Ytterbium-doped strontium borate lanthanum yttrium mixed crystal laser crystal and preparation method and application thereof |
-
2005
- 2005-03-25 CN CN2005100639957A patent/CN1837419B/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| D. Xue et al..Structural analysis of nonlinearities of Ca4ReO(BO3)3 (Re=La,Nd,Sm,Gd,Er,Y).《Applied Physics A》.1999,第68卷57-61. * |
| 孟宪林 等.Yb··YCOB晶体制备及其光谱与激光二极管抽运激光特性.《光学学报》.2000,第20卷(第3期),419-422. * |
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