CN101212122A - Ytterbium doped gadolinium lanthanum calcium oxoborate laser crystal, producing method, and purpose - Google Patents
Ytterbium doped gadolinium lanthanum calcium oxoborate laser crystal, producing method, and purpose Download PDFInfo
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- CN101212122A CN101212122A CNA2006101353843A CN200610135384A CN101212122A CN 101212122 A CN101212122 A CN 101212122A CN A2006101353843 A CNA2006101353843 A CN A2006101353843A CN 200610135384 A CN200610135384 A CN 200610135384A CN 101212122 A CN101212122 A CN 101212122A
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- boric acid
- gadolinium lanthanum
- acid oxygen
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Abstract
The invention discloses a method for preparing and using laser crystal mixed with the ytterbium doped gadolinium lanthanum calcium oxyborate, which relate to the field of the intraocular lens. At a temperature of about 1470 DEG C, the invention, at a crystal rotation speed of 5 to 20 rotations per minute and a pulling rate of 0.5 to 2mm per hour, produce the crystal of Yb<3+>:Gd<1-X>La<X>Ca<4>O(BO3)3 of high quality and larger dimension though a czochralski method. The crystal is a novel laser crystal, which can generate a laser output with a wavelength of about 1 Mum. The crystal also has the frequency-doubled effect and can get blue-green laser output through a self-frequency-doubling or self-mixing nonlinear optical method. A solid laser made from the crystal can be applied in the fields such as spectroscopy, biomedicine, military science and etc.
Description
Technical field
Blended ytterbium boric acid oxygen calcium gadolinium lanthanum laser crystal and its production and use, it relates to artificial lens and field of crystal growth in the technical field of optoelectronic functional materials, especially relates to a kind of laser crystal material as the operation material in the solid-state laser.
Background technology
Laser crystal is the operation material of solid state laser, and it is meant with the crystal to be matrix, by discrete luminescence center absorptive pumping light energy and be translated into the luminescent material of laser output.Solid laser working substance is made up of host material and active ions, and its various physics and chemical property are mainly by the host material decision, and its spectral characteristic and fluorescence lifetime etc. are then determined by the level structure of active ions.From nineteen sixty, succeeded in developing since the synthetic ruby pulse laser, up to now, found hundreds of laser crystals, but because of a variety of causes, the laser crystal that can really obtain practical application has only ten to plant.
At present, most widely used laser crystal is yttrium-aluminium-garnet (YAG) crystal of mixing ytterbium ion, 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 absorption line, 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 mechanical performance excellence both at home and abroad at present, and be easy to the high-quality laser crystal material that grows high optical quality, large scale 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 crystal active ions in recent years.
Boracic acid oxygen calcium gadolinium (GdCOB) crystal is a kind of novel non-linearity crystalline material that grows up the nineties in last century.The GdCOB crystal can realize that the secondary frequency multiplication of laser and three frequencys multiplication are had very wide transmission wave band, stable physical and chemical performance and favorable mechanical processing characteristics.And the gadolinium ion in this crystal can be activated ion such as neodymium, ytterbium replaces, and becomes from frequency multiplication, perhaps the self-mixing laser crystal.Studies show that the Gd ion can partly be replaced by other rare earth ions, form displaced type solid solution, improve the physical property and the optical property of crystal.
Summary of the invention
Purpose of the present invention just is to develop a kind of new laser crystal Yb
3+: Gd
1-XLa
XCa
4O (BO
3)
3X＜0.5 (is abbreviated as Yb
3+: GLCOB), can directly use photoflash lamp and LD pumping, laser crystal material with better laser activity and higher conversion efficiency.This crystal is that forming with GdCOB is the solid solution of base with the part gadolinium ion among the alternative GdCOB of lanthanum ion.Yb
3+: the GLCOB crystal belongs to monoclinic system, has Cm space group structure.Wherein ytterbium ion is as dopant ion, replaces the lattice position of gadolinium and lanthanum ion, and the doping content of ytterbium is between 1at%～20at%.
Yb
3+: the GLCOB crystal is a kind of compound of congruent melting, can adopt Czochralski grown.Yb in molar ratio
yGd
1-x-yLa
xCa
4O (BO
3) ratio claim sample, mixing, compressing tablet, carry out solid phase synthesis then.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 |
| Gd 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 as follows: growth be in the iridium crucible, inert gas is (as N
2, Ar etc.) carry out under the atmosphere, the parameter of crystal growth is about 1500 ℃ of growth temperatures, hoisting velocity is 0.5～2.0 millimeter/hour, 5～20 rev/mins of crystal rotating speeds.
With the Yb that grows
3+: the GLCOB crystal, carried out orientation, determined its refractive index main shaft.Carried out polarization absorption spectrum, fluorescence spectrum then, the analytical test of fluorescence lifetime and physico-chemical property etc., the result shows: Yb
3+: physico-chemical property such as GLCOB crystal thermodynamics character and hardness and GdCOB crystal are basic identical.But its spectrum property has had significant raising.For example, when X=0.27, the absorptive transition cross section of its main absworption peak 977nm is 1.1 * 10
-20Cm
2, be very suitable for adopting the InGaAs semiconductor laser to carry out pumping, help the absorption of laser crystal 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 1032nm is 0.8 * 10
-21Cm
2Its Clock Multiplier Factor is 3.1 times of KDP.Compare Yb
3+: GdCOB, its emission transition cross section improves a lot.This is very beneficial for improving Yb
3+: the laser activity of GLCOB crystal.
Yb
3+: the GLCOB crystal can grow superior in quality crystal easily with czochralski method, fast growth, hardness of crystals is moderate, 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, perhaps by obtaining blue green light from frequency multiplication.Therefore, this crystal can be used as a kind of laser crystal preferably or laser self frequency-doubling crystal.
Embodiment
Realize that experiment optimal way of the present invention is as follows:
Embodiment 1: the Czochralski grown doping content is 10.0at.%Yb
3+Yb
3+: Gd
0.78La
0.12Ca
4O (BO
3)
3Laser crystal.
Will be by the load weighted CaCO of proportion speed
3, Gd
2O
3, La
2O
3, H
3BO
3, Yb
2O
3Mixed grinding is even, behind the compressing tablet, puts into φ 40 * 60mm
3Platinum alloy crucible in, in Muffle furnace in 900 ℃ of solid phase 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 czochralski method, at N
2In the atmosphere, growth temperature is about 1475 ℃, the crystal rotating speed is 12 rev/mins, pulling rate be the 0.5-2 millimeter/hour situation under, grown and be of a size of φ 21 * 26mm
3High-quality Yb
3+Content is the Yb of 10.0at.%
3+: Gd
0.78La
0.12Ca
4O (BO
3)
3Crystal.
Embodiment 2: the Czochralski grown doping content is 10.0at.%Yb
3+Yb
3+: Gd
0.63La
0.27Ca
4O (BO
3)
3Laser crystal.
Will be by the load weighted CaCO of proportion speed
3, Gd
2O
3, La
2O
3, H
3BO
3, Yb
2O
3Mixed grinding is even, behind the compressing tablet, puts into φ 40 * 60mm
3Platinum alloy crucible in, in Muffle furnace in 900 ℃ of solid phase 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 czochralski method, at N
2In the atmosphere, growth temperature is about 1460 ℃, the crystal rotating speed is 10 rev/mins, pulling rate be the 0.5-1.5 millimeter/hour situation under, grown and be of a size of φ 19 * 25mm
3High-quality Yb
3+Content is the Yb of 10.0at.%
3+: Gd
0.63La
0.27Ca
4O (BO
3)
3Crystal.
Claims (5)
1. blended ytterbium boric acid oxygen calcium gadolinium lanthanum laser crystal, it is characterized in that: the molecular formula of this crystal is Yb
3+: Gd
1-XLa
xCa
4O (BO
3)
3, wherein X is less than 0.5.This crystal belongs to monoclinic system, and space group is Cm.
2. blended ytterbium boric acid oxygen calcium gadolinium lanthanum laser crystal as claimed in claim 1 is characterized in that: in this crystal, and Yb
3+Ion replaces Gd in the crystal as dopant ion
3+And La
3+The lattice position of ion, its doping content is between 1at.-20at.%.
3. the preparation method of the blended ytterbium boric acid oxygen calcium gadolinium lanthanum laser crystal of a claim 1 is characterized in that: this crystal by adopting Czochralski grown, and with Gd
2O
3, La
2O
3, CaCO
3, H
3BO
3And Yb
2O
3Be raw material, in molar ratio Yb
yGd
1-x-yLa
xCa
4O (BO
3)
3Ratio claim sample, mixing, compressing tablet, solid phase synthesis.In the iraurite crucible, pulling growth goes out crystal under the inert gas atmosphere, and the parameter of crystal growth is about 1470 ℃ of growth temperatures, and hoisting velocity is 0.5～2.0 millimeter/hour, and the crystal rotating speed is 5～20 rev/mins.
4. the purposes of the blended ytterbium boric acid oxygen calcium gadolinium lanthanum laser crystal of a claim 1, it is characterized in that: this crystal is used for solid state laser as working-laser material, use photoflash lamp or laser diode as pumping source, excite the laser output that produces 1 μ m wavelength around.
5. the purposes of the blended ytterbium boric acid oxygen calcium gadolinium lanthanum laser crystal of a claim 1, it is characterized in that: this crystal is used for solid state laser as working-laser material, use photoflash lamp or laser diode as pumping source, obtain the output of blue-green laser by non-linear optical means from frequency multiplication or self-mixing.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101353843A CN101212122A (en) | 2006-12-27 | 2006-12-27 | Ytterbium doped gadolinium lanthanum calcium oxoborate laser crystal, producing method, and purpose |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2006101353843A CN101212122A (en) | 2006-12-27 | 2006-12-27 | Ytterbium doped gadolinium lanthanum calcium oxoborate laser crystal, producing method, and purpose |
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| Publication Number | Publication Date |
|---|---|
| CN101212122A true CN101212122A (en) | 2008-07-02 |
Family
ID=39611879
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|---|---|---|---|
| CNA2006101353843A Pending CN101212122A (en) | 2006-12-27 | 2006-12-27 | Ytterbium doped gadolinium lanthanum calcium oxoborate laser crystal, producing method, and purpose |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676443B (en) * | 2008-09-16 | 2013-04-17 | 中国科学院福建物质结构研究所 | Neodymium-doped cesium lanthanum tungstate laser crystal and preparation method and application thereof |
| CN110541197A (en) * | 2019-10-17 | 2019-12-06 | 中国工程物理研究院化工材料研究所 | Ytterbium-doped calcium-gadolinium-lanthanum borate mixed crystal laser crystal and preparation method and application thereof |
| 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 |
| CN110725003A (en) * | 2019-11-28 | 2020-01-24 | 中国工程物理研究院化工材料研究所 | Ytterbium-doped strontium gadolinium lanthanum borate laser crystal and preparation method and application thereof |
| CN112421370A (en) * | 2019-08-22 | 2021-02-26 | 山东大学 | Self-frequency-doubling full-solid-state laser based on quasi-two-level laser radiation |
| CN113067245A (en) * | 2021-03-18 | 2021-07-02 | 江西理工大学 | Terbium activated borate crystal and 544nm or 586nm band laser |
-
2006
- 2006-12-27 CN CNA2006101353843A patent/CN101212122A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676443B (en) * | 2008-09-16 | 2013-04-17 | 中国科学院福建物质结构研究所 | Neodymium-doped cesium lanthanum tungstate laser crystal and preparation method and application thereof |
| CN112421370A (en) * | 2019-08-22 | 2021-02-26 | 山东大学 | Self-frequency-doubling full-solid-state laser based on quasi-two-level laser radiation |
| CN110541197A (en) * | 2019-10-17 | 2019-12-06 | 中国工程物理研究院化工材料研究所 | Ytterbium-doped calcium-gadolinium-lanthanum borate mixed crystal laser crystal and preparation method and application thereof |
| 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 |
| CN110725003A (en) * | 2019-11-28 | 2020-01-24 | 中国工程物理研究院化工材料研究所 | Ytterbium-doped strontium gadolinium lanthanum borate laser crystal and preparation method and application thereof |
| CN113067245A (en) * | 2021-03-18 | 2021-07-02 | 江西理工大学 | Terbium activated borate crystal and 544nm or 586nm band laser |
| CN113067245B (en) * | 2021-03-18 | 2022-05-31 | 江西理工大学 | Terbium activated borate crystal and 544nm or 586nm band laser |
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Open date: 20080702 |