CN102936751A - Neodymium-doped sodium lutetium molybdate laser crystal and preparation method thereof - Google Patents
Neodymium-doped sodium lutetium molybdate laser crystal and preparation method thereof Download PDFInfo
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- CN102936751A CN102936751A CN 201210407773 CN201210407773A CN102936751A CN 102936751 A CN102936751 A CN 102936751A CN 201210407773 CN201210407773 CN 201210407773 CN 201210407773 A CN201210407773 A CN 201210407773A CN 102936751 A CN102936751 A CN 102936751A
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- neodymium
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- absorption
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Abstract
The invention provides a neodymium-doped sodium lutetium molybdate laser crystal and a preparation method thereof. The crystal belongs to a tetragonal crystal system, wherein a space group is represented below. Lattice parameters of the crystal are that: a=5.1624 angstrom, c=11.2397 angstrom, V=299.5422 angstrom<3>, Z=2, and Dc=5.741g/cm3. The crystal can be grown by using a flux method. According to the invention, 60-80at% Na2Mo2O7 is adopted as a flux, a temperature reducing speed is 0.5-1.5 DEG C/day, and a rotation speed is 5-30rpm, such that high-quality large-size Nd<3+>:NaLu(MoO4)2 crystals are grown. The absorption spectrum of the crystal shows a relatively large absorption cross-section at 817nm, an absorption half-peak width reaches 16nm, and an emission cross-section is 12.31*10<-20>cm<2>. The crystal can be developed into a novel laser crystal, and can be practically applied.
Description
Technical field
The present invention relates to technical field of optoelectronic functional materials, especially relate to a kind of laser crystal material of solid laser operation material of suitable AlGaAs diode laser pumped.
Background technology
From nineteen sixty the U.S. plum graceful (T. H. Maiman) in the laboratory, invented in the world the First laser apparatus with artificial ruby crystal since, all solid state laser has obtained development at full speed.And 1961 first at CaF
2: Sm
3+The Laser output of realizing in the crystal has been opened and has been studied energetically trivalent rare earth ions as the prelude of the active ions solid-state laser crystal of stimulated emission.To twentieth century the mid-80, fast development along with semiconductor diode, the diode laser (LD) that utilizes its excellent properties to develop substitutes traditional photoflash lamp as novel pumping source and also is incorporated into widely in the laser apparatus as pumping source, thereby greatly improved the output efficiency of laser apparatus, promoted the develop rapidly of laser technology.The LD pump laser refers to utilize laser diode to come the exciting laser crystal as pumping source, produces laser generation.The advantage of this novel pumping source is:
[1] LD has much higher spectrum and spatial brightness, high photoelectric transformation efficiency, long life-span and output radiation has greater flexibility in time waveform.
[2] oneself warp of the emission wavelength of LD is infrared from purple extends at present, and as the AlGaAs of pumping source, the emission peak of AlGaIn and InGaAs laser diode is in respectively 797 ~ 810 nm, 670 ~ 690 nm and 900 ~ 1100 nm, and these scopes have covered Nd
3+Etc. the main absorption band of multiple trivalent rare earth ions, assimilated efficiency is higher, has avoided too much thermal losses.
[3] the LD pumping source is much smaller with respect to the flash lamp pumping source to the dimensional requirement of laser crystals, has relaxed the requirement of crystal growth size, relatively more easily obtains to be used for the dielectric crystal of development laser apparatus.And, the heat energy of the high energy storage when undersized crystal medium can reduce pumping and consequent laser crystals inherence, thus the thermal load of laser apparatus reduced.
At present, the LD pumping source has become the most frequently used topmost pumping source in the laser apparatus development.In order to take full advantage of and bring into play the advantage of LD pumping source, the high-quality laser crystals that just needs acquisition to be complementary with it.Major requirement is:
[1] laser crystals will have wider absorption band.This is that it is 0.2 ~ 0.3 nm/ that wavelength varies with temperature rate because the peak width at half height of LD is 2 ~ 3 nm
oC so wider absorption band not only is conducive to laser crystals to the pumping Optical Absorption, and has reduced the temperature controlled requirement to device.
[2] long fluorescence lifetime (τ).The crystal that fluorescence lifetime is long can accumulate more particle at upper energy level, has increased energy storage capacity, is conducive to the raising of device output rating or energy.
[3] large emission transition cross section (σ).Because pulse and continuous laser threshold value are inversely proportional to σ and σ τ respectively.So large σ is more conducive to realize laser generation.
In current laser crystals field, research is neodymium ion doped laser crystals the most widely, and near the absorption band of this ion 808nm can be complementary with the emission wavelength of AlGaAs.At present, best, that be widely used in laser apparatus is Nd
3+: the YAG crystal, its over-all properties is better, but also has some shortcomings, for example absorbs peak width at half height very narrow, and growth is relatively difficult.The shortcomings such as common neodymium ion doped borate crystal has physical and chemical performance preferably mostly, is difficult to growing large-size high-quality monocrystalline but but exist, and quantum yield is low.Two molybdate laser crystals of neodymium-doped are more widely class laser crystalss of Recent study.This type of crystalline structure is simple, cost of material is cheap, majority is easier to growth, and quality is better, and near the absorption 808nm is stronger, have larger absorption crosssection and emission cross section, and, because the randomness of ion in the part crystal has increased the absorption peak width at half height greatly, thereby be conducive to the absorption to AlGaAs diode laser emission wavelength, reduced the requirement to pumping source stability.So this compounds is for seeking the Nd that more has premium properties
3+The laser crystals of ion doping provides explores the space widely.
Summary of the invention
Purpose of the present invention just is to develop a kind of new laser crystals, and it has wide absorption band, and larger absorption emission cross section is suitable for adopting the LD pumping, has preferably various over-all propertieies, can realize the Laser output of better quality.
Molybdic acid lutetium sodium (NaLu (MoO
4)
2) belong to tetragonal system, have
The spacer structure is a kind of good laser host material.Neodymium ion can mix in the lattice as the laser active ion, replaces the crystallographic site of lutetium ion, and its doping content is between 0.5at% ~ 3at%.The room temperature fluorescence life-span (τ) of this doped crystal is 130 ~ 230 μ s, and its fluorescence lifetime and Concentration of Neodymium Ion in Czochralski have direct relation, can mix according to different needs the neodymium ion of different concns.Experimental result shows that near its absorption peak width at half height 817nm reaches 16nm, and much larger than the neodymium ion doped laser crystals of commercially producing, its absorption crosssection surpasses 11 * 10
-20Cm
2, this is also much larger than general crystal.
Technical scheme of the present invention is as follows:
Concrete chemical equation:
Na
2CO
3+Lu
2O
3+4MoO
3=2NaLu(MoO
4)
2+CO
2
Na
2CO
3+2MoO
3=Na
2Mo
2O
7+CO
2
Used material purity and producer:
| The medicine name | Purity | Producer |
| Lu 2O 3 | 99.99% | Solution on Chemical Reagents in Shanghai company of Chinese Medicine group |
| Na 2CO 3 | 99.9% | Solution on Chemical Reagents in Shanghai company of Chinese Medicine group |
| MoO 3 | 99.99% | Solution on Chemical Reagents in Shanghai company of Chinese Medicine group |
| Nd 2O 3 | 99.99% | Solution on Chemical Reagents in Shanghai company of Chinese Medicine group |
By experiment, we have found case of flux methods growth neodymium-doped molybdic acid lutetium sodium [Nd
3+: NaLu (MoO
4)
2] the comparatively ideal fusing assistant of crystal: Na
2Mo
2O
7And a small amount of additive: NaF, and explore best growth conditions, grown high-quality Nd
3+: NaLu (MoO
4)
2Crystal (seeing embodiment 1 and 2).Case of flux methods growth neodymium-doped molybdic acid lutetium sodium crystal, its main growth conditions is as follows: used fusing assistant is Na
2Mo
2O
7, the concentration of fusing assistant is added a small amount of NaF in addition as additive between 60 ~ 80at%, and consumption is at 1at-5at%, and growth temperature is between 850 ~ 950 ℃, and rate of temperature fall is 0.5 ~ 1.5 ℃/day, the crystal rotating speed is 5 ~ 30rpm.
With the Nd that grows
3+: NaLu (MoO
4)
2Crystal has carried out the collection of diffraction data at four-circle diffractometer, structural analysis shows, it belongs to tetragonal system,
Spacer, concrete unit cell parameters: a=5.1624, c=11.2397, V=299.5422
3, Z=2, D
c=5.741 g/cm
3
To the Nd that grows
3+: NaLu (MoO
4)
2Crystal carries out the analytical test of absorption spectrum, fluorescence spectrum and fluorescence lifetime etc.Absorption spectrum under the room temperature of this crystal, as seen eight obvious absorption bands are arranged between 400 ~ 1000nm, its highest peak is at the 596nm place, time strong absorption band that peak center is in 817nm and allow the people interested most, it just in time is in the transmitted wave strong point of AlGaAs, can well mate, it absorbs peak width at half height and reaches 16nm, and wider absorption peak and larger absorption crosssection are conducive to crystal to the pumping Optical Absorption.Nd for 2.19at%
3+: NaLu (MoO
4)
2Crystal, the absorption crosssection at 817nm place has reached 11.48 * 10
-20Cm
2, the fluorescence spectrum under its room temperature presents very strong fluorescent emission near 1064nm, and its peak width at half height is 14nm, and emission cross section is 12.31 * 10
-20Cm
2, fluorescence lifetime is 126.7 μ s.
Neodymium-doped molybdic acid lutetium sodium crystal [Nd of the present invention
3+: NaLu (MoO
4)
2], can enough flux methods grow quickly superior in quality crystal, growth technique is easy, raw material is easy to get, satisfactory mechanical property, and have good optical characteristics, can directly use the plurality of advantages such as LD pumping, this crystal can be used as a kind of preferably laser crystals.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but should not limit protection scope of the present invention with this.
Embodiment 1: with Na
2Mo
2O
7For the fluxing agent growth doping content is 0.5at.% Nd
3+Nd
3+: NaLu (MoO
4)
2Laser crystals.
Adopt flux method, in φ 60 * 50mm platinum alloy crucible, the mol ratio of growth raw material and solubility promoter is: NaLu (MoO
4)
2: Na
2Mo
2O
7=2:3 (mol ratio) mixes the Nd of 0.5at%
3+Ion, and the NaF that adds about 1at% in order to reduce viscosity, improves environment of crystal growth as additive.Crystal growth temperature is 915 → 865 ℃, and with 1 ℃/day rate of temperature fall, 10 rev/mins crystal rotating speed has grown and has been of a size of 25 * 18 * 9mm
3High-quality Nd
3+: NaLu (MoO
4)
2Crystal.The analysis showed that Nd in the crystal through ICP (plasma emission spectrum)
3+Ion content is 0.54 at%.
Embodiment 2: with Na
2Mo
2O
7For the fluxing agent growth doping content is 2.0at.% Nd
3+Nd
3+: NaLu (MoO
4)
2Laser crystals.
Adopt flux method, in φ 60 * 50mm platinum alloy crucible, the mol ratio of growth raw material and solubility promoter is: NaLu (MoO
4)
2: Na
2Mo
2O
7=1:4 (mol ratio) mixes the Nd of 2.0at%
3+Ion, and the NaF that adds about 2at% to reduce viscosity, improves environment of crystal growth as additive.Crystal growth temperature is 895 → 855 ℃, and with 1.5 ℃/day rate of temperature fall, 20 rev/mins crystal rotating speed has grown and has been of a size of 23 * 20 * 11mm
3High-quality Nd
3+: NaLu (MoO
4)
2Crystal.The analysis showed that Nd in the crystal through ICP (plasma emission spectrum)
3+Ion content is 2.19 at%.
Claims (3)
1. neodymium-doped molybdic acid lutetium sodium laser crystals, it is characterized in that: the molecular formula of this crystal is Nd
3+: NaLu (MoO
4)
2, belong to tetragonal system, have
Spacer structure, unit cell parameters are a=5.1624, and c=11.2397, V=299.5422
3, Z=2, D
c=5.741 g/cm
3
2. neodymium-doped molybdic acid lutetium sodium laser crystals as claimed in claim 1 is characterized in that: as the Nd of dopant ion
3+Its valence state of ion is+3 valencys, replaces the crystallographic site of lutetium ion, and its doping content is between 0.5at% ~ 3at%.
3. the preparation method of a neodymium-doped molybdic acid lutetium sodium laser crystals claimed in claim 1 is characterized in that: this crystal by adopting flux method growth, used fusing assistant is Na
2Mo
2O
7, concentration is between 60at ~ 80at%, and growth temperature is between 850 ~ 950 ℃, and rate of temperature fall is 0.5 ~ 1.5 ℃/day, and the crystal rotating speed is 5 ~ 30rpm.
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|---|---|---|---|
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|---|---|
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Family
ID=47695672
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103898609A (en) * | 2014-04-01 | 2014-07-02 | 中国科学院福建物质结构研究所 | Tunable laser crystal chrome-doped sodium magnesium molybdate and preparation method thereof |
| CN105463570A (en) * | 2015-12-24 | 2016-04-06 | 淮南师范学院 | Multifunctional caesium lanthanum molybdate crystal as well as preparation method and application thereof |
| CN113249790A (en) * | 2021-05-26 | 2021-08-13 | 曲阜师范大学 | Neodymium activated ion doped Na5Lu (MoO4)4 crystal and preparation method and application thereof |
-
2012
- 2012-10-22 CN CN 201210407773 patent/CN102936751A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103898609A (en) * | 2014-04-01 | 2014-07-02 | 中国科学院福建物质结构研究所 | Tunable laser crystal chrome-doped sodium magnesium molybdate and preparation method thereof |
| CN105463570A (en) * | 2015-12-24 | 2016-04-06 | 淮南师范学院 | Multifunctional caesium lanthanum molybdate crystal as well as preparation method and application thereof |
| CN113249790A (en) * | 2021-05-26 | 2021-08-13 | 曲阜师范大学 | Neodymium activated ion doped Na5Lu (MoO4)4 crystal and preparation method and application thereof |
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