CN101037796A - Neodymium boracic acid oxygen calcium gadolinium lanthanum doped laser crystal and preparation method and usage thereof - Google Patents
Neodymium boracic acid oxygen calcium gadolinium lanthanum doped laser crystal and preparation method and usage thereof Download PDFInfo
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- CN101037796A CN101037796A CN 200610067570 CN200610067570A CN101037796A CN 101037796 A CN101037796 A CN 101037796A CN 200610067570 CN200610067570 CN 200610067570 CN 200610067570 A CN200610067570 A CN 200610067570A CN 101037796 A CN101037796 A CN 101037796A
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Abstract
A neodymium-intermingled calcium-gadolinium-lanthanum borate laser crystal and its preparing method and its use, relate to artificial lens field. Nd3+:GdXLa1-xCa4O(BO3)3 crystal having high quality and bigger size is produced by the pulling method (Czochralski method) at 1480 DEG C, at the crystal rotational speed of 5-20 turns/minute, under the drawing speed of 0.5-2 mm/hour. The crystal belongs to monoclinic system and Cm space group. The crystal is a novel laser crystal and can produce the laser output of 1060 nm wavelength. The crystal has also frequency-doubled effect, accordingly the blue-green laser output can be produced by itself-frequency-doubled and itself-frequency-mixed non-linear optical means. The solid laser produced by the crystal can be used in the a plurality of fieldes such as spectroscopy, biomedicine, military affairs, ect.
Description
Technical field
The present invention relates to artificial lens and field of crystal growth in the technical field of optoelectronic functional materials.
Background technology
Laser crystals is the operation material of solid statelaser, and it is meant with the crystal to be matrix, by discrete luminescence center absorptive pumping luminous energy and be 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 aluminmiu 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 seeking various physics, chemical property and mechanical property excellence both at home and abroad at present, and be easy to grow high optical quality, large-sized high-quality laser crystal material, and this crystal to be suitable for the LD pumping.Self-frequency doubling laser crystal is the focus of studying in the crystallography always, because its set laser crystal and non-linear optic crystal function are, helps the output of short wavelength laser.
Summary of the invention
Purpose of the present invention just is to develop a kind of new self-frequency doubling laser crystal material neodymium-doped oxygen calcium gadolinium lanthanum Nd that can directly use photoflash lamp and LD pumping with higher conversion efficiency
3+: Gd
1-xLa
xCa
4O (BO
3)
3(x＜0.5) is by obtaining the output of blue-greenish colour laser from means such as frequency multiplication or self-mixings.
Nd
3+: Gd
xLa
1-xCa
4O (BO
3)
3Crystal belongs to oblique system, has C
mThe spacer structure.Wherein neodymium ion is as dopant ion, replace the crystallographic site of gadolinium and lanthanum ion, the doping content of neodymium is between 0.05at%～10at%, and fluorescence lifetime (τ) is 50～120 μ s, its fluorescence lifetime is the function of neodymium ion concentration, can mix the chromium ion of different concns according to different needs
Nd
3+: Gd
1-xLa
xCa
4O (BO
3)
3Crystal is a kind of compound of congruent melting, can adopt Czochralski grown, presses chemical equation: (1-x) Gd
2O
3+ xLa
2O
3+ 8CaCO
3+ 6H
3BO
3==2Gd
1-xLa
xCa
4O (BO
3)
3+ 8CO
2↑+9H
2O ↑ ratio claim sample, mixing, compressing tablet, and Nd
2O
3Then press desired concn and add, raw materials usedly be:
| The medicine name | Purity | Producer |
| Nd 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, rare gas element is (as N
2, Ar etc.) carry out under the atmosphere, the parameter of crystal growth is about 1480 ℃ of growth temperatures, pulling speed is 0.5～2.0 millimeter/hour, the crystal rotating speed is 5～20 rev/mins, has grown high-quality Nd
3+: Gd
1-xLa
xCa
4O (BO
3)
3Crystal.
With the Nd that grows
3+: Gd
1-xLa
xCa
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 C
m, how many its cell parameters mixes with lanthanum ion and changes, for example when x=0.16, and a=8.086 , b=15.988 , c=3.566 , β=101.17 °, V=452
3, density 3.72g/cm
3When x=0.33, a=8.114 , b=16.001 , c=3.577 , β=101.52 °, V=455
3, density 3.68g/cm
3
With the Nd that grows
3+: Gd
1-xLa
xCa
4O (BO
3)
3Crystal has carried out orientation, has determined its specific refractory power main shaft.Carried out the analytical test of polarization absorption spectrum, fluorescence spectrum and fluorescence lifetime etc. then, the result shows: Nd
3+: Gd
1-xLa
xCa
4O (BO
3)
3Crystalline master absorption peak is at 812nm, and main emission peak is at 1064nm.What and slight change its peak width at half height, absorption jump cross section, emission transition cross section mix with lanthanum ion.For example: when x=0.33, in the E//Z direction, the peak width at half height of 812nm place absorption peak is 20nm, and the absorption jump cross section is 1.55 * 10
-20Cm
2, be very suitable for adopting the AsGaAl semiconductor laser to carry out pumping in the bigger peak width at half height in 812nm place, help the absorption of laser crystals to pump light, improve pumping efficiency.Its peak width at half height at the 1064nm place (FWHM) is 15nm, and fluorescence lifetime is 93 μ s, because the long crystal of fluorescence lifetime can accumulate more particle at last energy level, has increased energy storage, helps the raising of device output rating and output energy.Therefore, Nd
3+: Gd
1-xLa
xCa
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.
Neodymium-doped oxygen calcium gadolinium lanthanum Nd
3+: Gd
1-xLa
xCa
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 1060nm, and this crystal can be used as a kind of laser crystals preferably.
Embodiment
Embodiment 1: the Czochralski grown doping content is 3.0at.%Nd
3+Nd
3+: Gd
0.84La
0.16Ca
4O (BO
3)
3Laser crystals.
Will be by the load weighted Gd of proportion speed
2O
3, La
2O
3, CaCO
3, H
3BO
3And Nd
2O
3Mixed grinding is even, behind the compressing tablet, puts into φ 60 * 40mm
3Platinum alloy crucible in, in retort furnace,, be warming up to 1200 ℃ of reactions 24 hours again in 1000 ℃ of solid state reactions 12 hours.Synthetic good above sample is put into lifting furnace, adopt crystal pulling method, at N
2In the atmosphere, growth temperature is about 1470 ℃, and the crystal rotating speed is 5-20 rev/min, pulling rate be the 0.5-2 millimeter/hour situation under, grown and be of a size of 30 * 25 * 18mm
3High-quality Nd
3+Content is the Nd of 3.0at.%
3+: Gd
0.84La
0.16Ca
4O (BO
3)
3Crystal.
Embodiment 2: the Czochralski grown doping content is 3.0at.%Nd
3+Nd
3+: Gd
0.67La
0.33Ca
4O (BO
3)
3Laser crystals.
Will be by the load weighted Gd of proportion speed
2O
3, La
2O
3, CaCO
3, H
3BO
3And Nd
2O
3Mixed grinding is even, behind the compressing tablet, puts into φ 60 * 40mm
3Platinum alloy crucible in, in retort furnace,, be warming up to 1200 ℃ of reactions 24 hours again in 1000 ℃ of solid state reactions 10 hours.Synthetic good above sample is put into lifting furnace, adopt crystal pulling method, at N
2In the atmosphere, growth temperature is about 1460 ℃, and the crystal rotating speed is 5-20 rev/min, pulling rate be the 0.5-2 millimeter/hour situation under, grown and be of a size of 32 * 23 * 23mm
3High-quality Nd
3+Content is the Nd of 3.0at.%
3+: Gd
0.67La
0.33Ca
4O (BO
3)
3Crystal.
Claims (4)
1. neodymium boracic acid oxygen calcium gadolinium lanthanum doped laser crystal, it is characterized in that: this crystalline molecular formula is Nd
3+: Gd
1-XLa
xCa
4O (BO
3)
3(x＜0.5), Nd
3+Ion doping concentration belongs to oblique system between 0.05at-10at%, spacer is C
m, how many its cell parameters mixes with lanthanum ion and changes, when x=0.16, and a=8.086 , b=15.988 , c=3.566 , β=101.17 °, V=452
3, density 3.72g/cm
3When x=0.33, a=8.114 , b=16.001 , c=3.577 , β=101.52 °, V=455
3, density 3.68g/cm
3
2. the preparation method of the neodymium boracic acid oxygen calcium gadolinium lanthanum doped laser crystal of a claim 1 is characterized in that: this crystal by adopting Czochralski grown.
3. the preparation method of laser crystals as claimed in claim 2, it is characterized in that: this crystal pulling method is with Gd
2O
3, La
2O
3, CaCO
3, H
3BO
3And Nd
2O
3Be raw material, under the inert gas atmosphere, the parameter of crystal growth is about 1480 ℃ of growth temperatures, and pulling speed is 0.5～2.0 millimeter/hour, and the crystal rotating speed is 5～20 rev/mins.
4. the purposes of the neodymium boracic acid oxygen calcium gadolinium lanthanum doped laser crystal of a claim 1, it is characterized in that: this crystal is used for solid statelaser as working-laser material.
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|---|---|---|---|
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|---|---|---|---|
| CN 200610067570 CN101037796A (en) | 2006-03-17 | 2006-03-17 | Neodymium boracic acid oxygen calcium gadolinium lanthanum doped laser crystal and preparation method and usage thereof |
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676445B (en) * | 2008-09-16 | 2012-08-22 | 中国科学院福建物质结构研究所 | Neodymium-doped gadolinium barium lithium tungstate laser crystal and preparation method and application thereof |
| 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 |
| CN109516677A (en) * | 2018-10-31 | 2019-03-26 | 成都鑫扬锦睿合成材料有限公司 | A kind of synthetic cut stone cylinder moulding process |
| 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 |
-
2006
- 2006-03-17 CN CN 200610067570 patent/CN101037796A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676445B (en) * | 2008-09-16 | 2012-08-22 | 中国科学院福建物质结构研究所 | Neodymium-doped gadolinium barium lithium tungstate laser crystal and preparation method and application thereof |
| 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 |
| CN109516677A (en) * | 2018-10-31 | 2019-03-26 | 成都鑫扬锦睿合成材料有限公司 | A kind of synthetic cut stone cylinder moulding process |
| 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 |
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Open date: 20070919 |