CN103820858A - Er- or Ho-activated ABC3O7 type intermediate infrared ultrafast laser crystal - Google Patents
Er- or Ho-activated ABC3O7 type intermediate infrared ultrafast laser crystal Download PDFInfo
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- CN103820858A CN103820858A CN201410071392.0A CN201410071392A CN103820858A CN 103820858 A CN103820858 A CN 103820858A CN 201410071392 A CN201410071392 A CN 201410071392A CN 103820858 A CN103820858 A CN 103820858A
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Abstract
The invention aims to disclose an Er- or Ho-activated ABC3O7 melilite structured intermediate infrared ultrafast laser crystal. In allusion to the problems of complicated devices and poor beam quality existing in the prior art, the invention brings forward LD-pumped Er<3+>, Ho<3+> activated ABC3O7 melilite structured crystal. 2.5-3 micron wave band of intermediate infrared mode locked ultrafast laser is directly realized. Chemical formula of the crystal is ErxAB1-xC3O7 or HoyAB1-yC3O7(A is at least one of Ca, Sr and Ba; B is at least one of Y, La and Gd; and C is at least one of Ga and Al), wherein dosage concentration x of Er<3+> is 0.01-0.5; dosage concentration y of Ho<3+> is 0.01-0.3; and Er<3+> and Ho<3+> both replace B<3+> (namely Y<3+>, La<3+> and Gd<3+>) in the crystal.
Description
Technical field
The present invention relates to field of laser crystal materials.
Background technology
2.5～3.0 mu m wavebands are positioned at " molecular fingerprint district ", are transmission windows of atmosphere, and this wave band of laser has stronger penetration power to haze, flue dust etc., and the gas molecule scattering that transmission is subject in sea level is little.The detector of infrared guidance guided missile and infraed early warning system is all to this wave band sensitivity, ultrafast mid-infrared laser can provide very high peak power to be enough to damage these sensitive detection parts in moment, and the ultrafast mid-infrared laser therefore with high-peak power has a lot of potential application in military confrontation.Aspect civilian, because water exists strong absorption to the light of wavelength 2.5～3.0 μ m, the uptake factor (α=13000cm of water
-1) be respectively 2.1 μ m (α=50cm
-1) or 1.064 μ m (α=l cm
-1) 2 or 4 orders of magnitude, and the thermodiffusion of ablation threshold and surrounding tissue and uptake factor are inversely proportional to, this strong absorption makes Laser emission be absorbed (d=1/ α) with the very shallow degree of depth, and therefore this wave band ultrafast laser is very effective in ophthalmology, dentistry and endoscope microsurgery.In addition, 2.5～3.0 μ m ultrafast lasers also have important application at aspects such as remote sensing, environment detection, optical soliton communication, meticulous mechanical workouts, still study narrow can gap semiconductor and superlattice Multiple Quantum Well interband transient state optical transition process, semi-conductor in optical excitation kinetics and molecule and intermolecular energy transfer conciliate the important means of the dynamics problems such as phase phenomenon.
At present, the method that realizes in the world ultra-short mid-infrared optical laser pulse mainly contains four kinds:
(1) parametric oscillation method (OPO).The efficiency of conversion of parametric oscillation method is higher, but single pulse energy is lower; The optical parametric oscillation of accurate phase matched has higher non-linear conversion efficiency, can make those crystal that cannot realize phase matched under usual conditions and logical optical band realize frequency transformation, is applicable to the frequency transformation continuously and under miniaturization.
(2) difference frequency produces method.The method is usually used in producing the tunable ir radiation of high spectral resolution, particularly produces the main method of far red light.Conventional crystal is mainly AgGaS
2, AgGaSe
2, the semiconductor type crystal such as GaAs, this crystal-like effective light transmission wide ranges, and nonlinear factor is larger, transparency range is wide, shortcoming is that damage threshold is low.At present, adopt the method for difference frequency can realize the mid-infrared laser of output rating hundred milliwatts, pulsewidth tens fs.
(3) parameter amplifying method (OPA).Utilize high gain that parameter amplifies gain saturatiuon point amplifies can obtain superpower femtosecond in infrared output, it is the main method of generation superpower femtosecond mid-infrared laser pulse that the optical parameter that at present super continuous spectrums injects is amplified.Conventional crystal is mainly to have the very MgO:LiNbO of high damage threshold
3with KTP and isomrophous crystal etc. thereof.Domestic, professor Qian Liejia of Shanghai Communications University is successfully by tunable within the scope of 2.0～4.5 μ m the middle infrared femtosecond laser of 100fs.
(4) directly output.Utilize Er
3+, Ho
3+or Cr
2+optical fiber or near the transmitting of crystal 2.5～3.0 μ m of doping, take suitable pumping source, locked mode element and mode-locking technique etc., directly realizes this wave band ultrafast laser.The method device concision and compact, beam quality is high, can produce the ultra-short pulse laser of diffraction limit and the Fu Shi conversion limit, can overcome the shortcomings such as the high complexity that above-mentioned other three kinds of methods use materials and devices system, expensive, poor beam quality and low signal-to-noise ratio, it is another optimal technical scheme that realizes 2.5～3.0 mu m waveband ultrafast laser outputs, also being one of the most effective technological approaches, is the study hotspot in all-solid state laser field in the world at present.All the time, people concentrate on first three methods the sight of ultrafast laser, and have ignored this more wide research space of direct output.
Er
3+ion
4i
11/2→
4i
13/2and Ho
3+ion
5i
6→
5i
7transition can produce the ultrafast laser of 2.5～3.0 μ m middle-infrared bands.Er
3+, Ho
3+doped crystal is the core gain medium of all solid state ultrafast mode locked laser of 2.5～3.0 mu m waveband, is one of important factor affecting ultrafast laser Laser output.In general, in order to realize 2.5～3.0 μ m ultra-short pulse lasers, substrate material at least should meet following some conditions: 1. phonon energy is low, multi-phonon relaxation and radiationless transition probability reduce like this, contribute to improve lasing efficiency, so the conventional host crystal of near-infrared band is as all too high in phonon energies such as borate, tungstate, vanadate, be difficult to realize the mid-infrared laser of superpower, ultrashort pulsewidth, can select gallate that phonon energy is lower, sulphur system, fluorine halide etc.2. select the crystal of part disordered structure.They absorb after mixing rare earth luminous ion, the obvious broadening of fluorescence emission spectrum, the width of laser crystals fluorescence emission spectrum is larger, the width of the laser pulse that it can be realized is narrower, is outstanding ultra-short pulse laser gain material so have the crystal of disordered structure feature.3. active ions Er
3+, Ho
3+after mixing, there is outstanding spectrum property: for example large in 2.5～3.0 mu m waveband fluorescent emission cross sections, fluorescence branching ratios are high, upper laser level
4i
11/2life-span is long to realize population inversion etc.4. there is good physical and chemical performance, easily growth obtains, crystal optics quality is good etc.In having realized recently, the Cr:ZnS of infrared femtosecond Laser output and Cr:ZnSe crystal have the problems such as bad mechanical strength, growth conditions harshness, doping content be inhomogeneous, and sulphur system, fluorine halide etc. face the difficult problem that growth is difficult equally, seriously hindered further develop with practical application may.
Therefore, we will select Er
3+, Ho
3+the ABC activating
3o
7(A is Ca, Sr, at least one in Ba; B is Y, La, at least one in Gd; C is Ga, at least one in Al) serial crystal is as the ultrafast laser gain media of middle-infrared band, mainly for following reason:
The first, ABC
3o
7serial crystal, as a kind of laser host material of excellence, is one of preferred material producing superpower, short pulse mid-infrared laser.
ABC
3o
7crystal extended familys belong to tetragonal system, spacer
there is melilite structure.This system has physical and chemical performance good (nonhygroscopic, be insoluble to soda acid), the high (SrGdGa of thermal conductivity
3o
7: 11Wm
-1k
-1), large, the low (SrLaGa of phonon energy of physical strength
3o
7: 560cm
-1) etc. advantage, 1500～1650 ℃ of left and right of fusing point, congruent melting, can adopt crystal pulling method to be easier to obtain large size high-quality monocrystalline.These features make crystal not only meet the general requirement of 2.5～3.0 mu m waveband ultrafast lasers, and have high light injury threshold and laser quantum efficiency.And, ABC
3o
7serial crystal has certain disordered structure feature, and this is that the crystal such as business-like YAG, YSGG, YAP are not available.With SrGdGa
3o
7crystal is example, and this molecule is by stratiform GaO
4 5-tetrahedron forms, Sr between layers
2+, Gd
3+ion is with 1:1 ratio, mirror symmetry being distributed on respective lattices point position.Due to the difference of its valence state, particle radii and crystal property, cause the disordered structure of crystals, make dopant ion Nd
3+replace Gd
3+after ion, in host crystal, form the activation center of many configurations, cause its Absorption and emission spectra to obtain inhomogeneous broadening, similarly at Er:SrLaGa
3o
7the phenomenon of also found on crystal～2.7 mu m waveband fluorescence spectrum broadenings, like this, will be conducive to the generation of mode-locked laser on the one hand, also will cause on the other hand Er
3+the splitting of quasi-three-level system laser lower level increases, thereby overcomes by Er
3+the upper conversion existing in system and backward energy transmit the shortcomings such as the caused high laser threshold of homenergic loss and low laser effect, can reduce widely laser threshold and improve Laser output effect.
The second, Er
3+the ABC activating
3o
7serial crystal can become 2.5～3.0 outstanding μ m ultrafast laser gain medias.
Nd
3+the ABC of doping
3o
7crystal has caused that as femtosecond laser gain media people study interest, for example Nd:SrGdGa widely
3o
7crystal has been realized the output of self-locking mode pulse laser, and output rating 400mW repeats power 80GHz, and pulse width is 616fs, is current Nd
3+the short pulse width [Optics Letters, 37 (4), pp461-463,2012] that doped crystal self-locking mode laser is realized, 2013 years A.Agnesi etc. adopt passive mode-locking technology at Nd:BaLaGa
3o
7on crystal, realize wideband adjustable femtosecond pulse, in the time that output wavelength is 1060nm, pulsewidth is 316fs, and in the time that pulsewidth is ps magnitude output wavelength at tunable [the Advanced Solid-State Lasers Congress Technical Digest of 1072～1090nm
aTu3A.32,2013], simultaneously at Nd:SrLaGa
3o
7crystal is realized femtosecond laser output, and in the time of 1061nm, pulsewidth is 378fs, and in the time of 1071nm, pulsewidth is 534fs[Advanced Solid-State Lasers Congress Technical Digest
aM1A.7,2013].Above result of study shows: the ABC with disordered structure feature
3o
7crystal family is the ultrafast laser crystal that over-all properties is given prominence to very much, with existing YAG YAP YSGG compared with GGG crystal, their fusing point is lower, be easier to adopt crystal pulling method to obtain large size gem-quality crystal, and compare with GGG crystal with for example YSGG of other gallate, it also has, and an outstanding advantage---crystalline structure is unordered, thereby causes Ho
3+, Er
3+the ABC activating
3o
7the remarkable broadening of spectrum of crystal, is very beneficial for realizing middle-infrared band ultrafast laser.Nd in this serial crystal
3+the research of doping is many, Er
3+, Ho
3+doping report is few, and there is no at present Er
3+, Ho
3+the ABC activating
3o
7crystal is as the research report of 2.5～3.0 mu m waveband ultrafast laser crystal.
Summary of the invention
The object of the invention is to disclose the ABC of the novel erbium of a class, holmium activation
3o
7infrared ultrafast laser crystals in melilite structure.The present invention is directed to the problems such as the device existing in prior art is numerous and diverse, beam quality is not high, provide LD pumping one class Er
3+, Ho
3+the ABC activating
3o
7the crystal of melilite structure is infrared locked mode ultrafast laser in directly realizing, and the chemical formula of crystal is Er
xaB
1-xc
3o
7or Ho
yaB
1-yc
3o
7(A is Ca, Sr, at least one in Ba; B is Y, La, at least one in Gd; C is Ga, at least one in Al), wherein Er
3+doped parameterx=0.01～0.5, Ho
3+doping content y=0.01～0.3, Er
3+and Ho
3+all replace the B in crystal
3+(be Y
3+, La
3+, Gd
3+).
Embodiment:
Er
xaB
1-xc
3o
7or Ho
yaB
1-yc
3o
7growth preparation and the spectrum property of crystal
The crystal pulling instrument used of growing is the intermediate frequency lifting furnace of DJL-400, and intermediate frequency power supply model is KGPF25-0.3-2.5.Adopt the thermopair of Pt/Pt-Rh and the Ou Lubiao temperature control that model is 815EPC.The crucible adopting is the iridium crucible of Ф 55mm × 30mm, and raw material used is the SrCO of 4N level
3, Gd
2o
3, Ga
2o
3, Er
2o
3, Ho
2o
3deng.According to following chemical equation preparation raw material:
2ACO
3+(1-x)B
2O
3+xEr
2O
3+3C
2O
3→2AB
(1－x)Er
xC
3O
7+CO
2↑
2ACO
3+ (1-y) B
2o
3+ yHo
2o
3+ 3C
2o
3→ 2AB
(1-y)ho
yc
3o
7+ CO
2↑ wherein, A is Ca, Sr, at least one in Ba; B is Y, La, at least one in Gd; C is Ga, at least one in Al, Er
3+doped parameterx=0.01～0.5, Ho
3+doping content y=0.01～0.3, Er
3+and Ho
3+all replace the B in crystal
3+(be Y
3+, La
3+, Gd
3+).Raw material is mixed, be pressed into sheet, put platinum crucible into, insert in ordinary sinter stove, be slowly warmed up to 1080 ℃ with 150 ℃/h, keep 48h, repeat this process, then put into high temperature sintering furnace constant temperature sintering 72h at 1200 ℃, take out polycrystal, until X-ray powder diffraction conforms to completely with standard card.
Raw material is packed in the iridium crucible of Ф 55mm × 30mm, for fear of the oxidation of iridium crucible, first extract the air in stove out, make the air pressure in stove reach negative 0.01MPa, being filled with high pure nitrogen makes air pressure reach 0.04MPa again, then be warmed up to than the temperature of high 50 ℃ of fusing point, constant temperature 1 hour, makes raw material fusing completely.In process of growth, the rate of pulling of seed rod is 1.3～1.5mm/h, and rate of temperature fall is 2～10 ℃/h, and the slewing rate of seed rod is 12～20r.p.m., after growth finishes, crystal is lifted to liquid level, is down to room temperature with the speed of 10～30 ℃/h, obtains size and is greater than
transparent crystals.
Claims (2)
1. a class Er
3+or Ho
3+the ABC activating
3o
7the crystal of configuration, is characterized in that: described crystal belongs to melilite structure, and molecular formula is Er
xaB
1-xc
3o
7or Ho
yaB
1-yc
3o
7, wherein, A is Ca, Sr, and at least one in Ba, B is Y, La, at least one in Gd, C is Ga, at least one in Al; Er
3+doped parameterx=0.01～0.5, Ho
3+doping content y=0.01～0.3, Er
3+and Ho
3+all replace the B in crystal.
2. the purposes of crystal described in claim 1, directly realizes the infrared locked mode ultrafast laser output of 2.5～3 mu m waveband for semiconductor laser pumping.
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Cited By (4)
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| CN105821478A (en) * | 2016-05-31 | 2016-08-03 | 山东省科学院新材料研究所 | Thulium and holmium codoping gallium acid barium and lanthanum laser crystal, manufacturing method and application of crystal |
| CN105887200A (en) * | 2016-05-31 | 2016-08-24 | 山东省科学院新材料研究所 | Thulium-holmium-codoped strontium lanthanum gallate laser crystal, preparation method and application of crystal |
| CN107419334A (en) * | 2017-08-10 | 2017-12-01 | 中国科学院福建物质结构研究所 | A kind of crystalline material, its preparation method and the application as laser crystal |
| CN108823633A (en) * | 2018-06-27 | 2018-11-16 | 中国科学院福建物质结构研究所 | A kind of crystal optical fibre material |
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| CN107419334A (en) * | 2017-08-10 | 2017-12-01 | 中国科学院福建物质结构研究所 | A kind of crystalline material, its preparation method and the application as laser crystal |
| CN108823633A (en) * | 2018-06-27 | 2018-11-16 | 中国科学院福建物质结构研究所 | A kind of crystal optical fibre material |
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