CN103397385B - Mix ytterbium lutetium GGG laser crystal and preparation method thereof and application - Google Patents
Mix ytterbium lutetium GGG laser crystal and preparation method thereof and application Download PDFInfo
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Abstract
The invention provides one and mix ytterbium lutetium GGG laser crystal and preparation method thereof and application.The molecular formula of this crystal is (Yb
ylu
xgd
1-x-y)
3ga
5o
12, 0 & lt; X & lt; 1,0.01≤y≤0.5, and x+y≤1; Yb
3+as active ions, under laser diode (LD) or other laser pumpings, continuous and pulse laser output near 1 μm can be realized.The present invention adopts this crystal of melt Czochralski grown Yb:(Lu
xgd
1-x)
3ga
5o
12.The present invention mixes part Lu at the Dodecahedral sites of Yb:GGG crystal
3+obtain Yb:LGGG crystal.This crystal growth interface is stablized, and crystal mass is high, can be used as the application of laser crystals producing continuous laser output, Q-switch laser, mode-locked laser.
Description
Technical field
The present invention relates to a kind of novel laser crystal and growth thereof and apply, particularly mixing ytterbium lutetium GGG laser crystal (Yb:LGGG), growth method and application, belong to crystal and device arts.
Technical background
Laser is one of 20th century greatest invention, the excellent specific properties such as it has, and coherency is good, good directionality, brightness height.Since nineteen sixty, first ruby laser was born, laser technology presents fast-developing trend in miniaturization, superpower, spike pulse etc., and be widely used in the fields such as industry, military affairs, medical treatment, communication, start the brand-new situation of optical field, facilitate the development of photoelectron technology.
Current laser apparatus is of a great variety, by operation material classification, can be divided into gas, solid, dyestuff and semiconductor laser etc.Wherein Solid State Laser technology is as irreplaceable sophisticated technologies of key areas such as current information, industry, national defence, gets more and more people's extensive concerning.Working-laser material is core and the basis of Solid State Laser technical development, and therefore efficient laserable material has meaning as milestone for the development of Solid State Laser.
Yb-Gd-Ga doped garnet crystal (Yb:GGG) is a kind of laserable material having potential using value: on the one hand, active ions Yb
3+there is a lot of excellent specific property: 1. level structure is simple, only has two electronic state (ground state
2f
7/2and excited state
2f
5/2), there is not excited state absorption and upper conversion, light conversion efficiency is high; 2. pumping wavelength and laser emission wavelength close, quantum yield can up to 90% in theory; 3. under relatively high doping content, also there will not be concentration quenching; 4. fluorescence lifetime is long, is conducive to energy storage.On the other hand, gadolinium gallium garnet has the advantages such as good mechanical property, thermal conductivity is high, hardness is large, physicochemical property are stable, realizes large size, coreless crystal growth by crystal pulling method, is the preferred substrate material that high power laser light exports.Therefore, people have carried out extensive research to the calorifics of Yb-Gd-Ga doped garnet crystal, spectroscopy and laser performance.Found by deep research, Yb
3+ionic radius be less than Gd
3+, therefore, its effective segregation coefficient in crystal is greater than 1, and this can cause Yb
3+concentration in crystal reduces from top to bottom gradually.Especially, when the crystal of growing large-size, the usage quantity of raw material will be very large, and the concentration gradient problem at this moment in crystal will be more outstanding.Yb in crystal
3+that adulterates is uneven, and by causing, the optical homogeneity of crystal is poor, directly affects the beam quality of laser.In addition, segregation coefficient much larger than 1 time, can give crystal growth also bring series of problems, such as: constitutional supercooling problem, growth interface instability problem etc.
Summary of the invention
For prior art Problems existing, the invention provides one and mix ytterbium lutetium GGG laser crystal and preparation method thereof and application.This mixes ytterbium lutetium substitute GGG crystal can realize high-efficiency and continuous and pulse laser output.
Technical scheme of the present invention is as follows:
One mixes ytterbium lutetium GGG laser crystal, and the molecular formula of this crystal is (Yb
ylu
xgd
1-x-y)
3ga
5o
12, 0<x<1,0.01≤y≤0.5, and x+y≤1.
This crystal belongs to isometric system, and spacer is O
h(10)-Ia3d.Wherein, Yb
3+and Lu
3+all the Gd replacing crystal Dodecahedral sites
3+.
Mix ytterbium lutetium GGG laser crystal, chemical formula is Yb:(Lu
xgd
1-x)
3ga
5o
12, wherein, Yb
3+doping content be 1-50at.%.Yb
3+as active ions, under laser diode (LD) or other laser pumpings, continuous and pulse laser output near 1 μm can be realized.
Preferred according to the present invention, molecular formula (Yb
ylu
xgd
1-x-y)
3ga
5o
12in, x=0.05-0.25, y=0.05-0.45; Preferred further, x=0.05, y=0.05-0.15.
Mix a preparation method for ytterbium lutetium substitute GGG crystal, adopt melt Czochralski grown, step is as follows:
(1) polycrystal synthesis
By molecular formula (Yb
ylu
xgd
1-x-y)
3ga
5o
12stoichiometric ratio, takes raw material Yb
2o
3, Lu
2o
3, Gd
2o
3and Ga
2o
3, and make Ga more on this basis
2o
3excessive 1-3wt.%, with the Ga stoichiometrically calculated
2o
3quality meter;
Solid sintering technology or liquid phase method synthesis is adopted to mix the polycrystal of ytterbium lutetium gadolinium gallium garnet.
(2) crystal growth
Obtained polycrystal is loaded in Iridium Crucible, load lifting furnace, vacuumize, fill protection gas; Intensification makes polycrystal melt, and after melt fully mixes, lower seed crystal, starts growing crystal; Pull rate: 0.5-5mm/ hour, rotating speed: 5-60 rev/min; When crystal growth is to desired size, carry de-crystal, cool to room temperature with the speed of 10-60 DEG C/h, come out of the stove; Crystal after coming out of the stove is annealed in atmosphere, and annealing temperature is 1200-1500 DEG C.
Preparation method of the present invention, considers to there is Ga especially in crystal growing process
2o
3volatilization Sum decomposition, step (1) prepare burden time make its excessive 1-3wt.%, preferably, Ga
2o
3excessive 2wt.%, with the Ga stoichiometrically calculated
2o
3quality is radix meter.
Preparation in accordance with the present invention, filling protection gas in step (2) is argon gas or nitrogen.
Preparation in accordance with the present invention, described in step (2), seed crystal is Nd:GGG crystal.Nd:GGG is writing a Chinese character in simplified form of Nd-Gd-Ga garnet, is the existing crystal in this area.
Preparation in accordance with the present invention, preferably, in step (2) during growing crystal, pull rate: 1-3mm/ hour, rotating speed 20-25 rev/min.
The raw material Yb that the present invention uses
2o
3, Lu
2o
3, Gd
2o
3and Ga
2o
3, purity is 99.99%.
Preferred according to the present invention, the polycrystal that ytterbium lutetium gadolinium gallium garnet is mixed in solid sintering technology synthesis described in step (1) is: fully mixed by the raw material prepared, then, raw material is pressed into cylindrical block, put into corundum crucible, at 1200-1500 DEG C, calcine 25-35 hour with sintering oven, can obtain and mix ytterbium lutetium gadolinium gallium garnet polycrystal.
Preferred according to the present invention, the polycrystal that ytterbium lutetium gadolinium gallium garnet is mixed in the liquid phase method synthesis described in step (1) is: the raw material prepared and concentrated nitric acid are reacted, obtain Yb (NO
3)
3, Lu (NO
3)
3, Gd (NO
3)
3with Ga (NO
3)
3nitrate mixed solution, then regulates mixing solutions pH value to 4-5 with ammoniacal liquor, then adds ammonium bicarbonate soln and precipitate, and by the precipitation of gained through repeatedly centrifugal, oven dry, finally carries out compressing tablet, calcining, obtains the polycrystal mixing ytterbium lutetium gadolinium gallium garnet.
Above-described concentrated nitric acid is concentration massfraction well known in the art is 65-68%; Ammoniacal liquor is pH adjusting agent, and concentration is not limit, and the massfraction of conventional commercial is the ammoniacal liquor of 25-28%.Bicarbonate of ammonia, commercially available technical grade, is mixed with the solution that concentration is 2-2.6mol/L.
Ytterbium lutetium substitute GGG crystal of mixing of the present invention is when using as laser crystal material, needs to process the crystal of growth, uses after polishing; Crystal two ends polishing or be coated with deielectric-coating further again, the logical light face of crystal is circular or square.
Mix the application of ytterbium lutetium substitute GGG crystal as laser crystal material, comprise following any one:
Mix ytterbium lutetium substitute GGG crystal as the application producing the laser crystals that continuous laser exports;
Mix ytterbium lutetium substitute GGG crystal as the application producing Q-switch laser material;
Mix ytterbium lutetium substitute GGG crystal as the application producing mode-locked laser material.
Preferred according to the present invention:
1, ytterbium lutetium substitute GGG crystal of mixing of the present invention is for continuous laser device, mixes ytterbium lutetium substitute GGG crystal as laser crystals, adopts laser diode (LD) or other laser pumpings, realizes continuous laser near 1025nm and exports.
2, ytterbium lutetium substitute GGG crystal is mixed for Q-switch laser device, mix ytterbium lutetium substitute GGG crystal as laser crystals and Q switched element, comprise electric-optically Q-switched element, acousto-optic Q modulation element or saturated absorbing body, be placed in laser cavity, adopt laser diode (LD) or other laser pumpings, realize Q-switch laser near 1025nm and export.
3, ytterbium lutetium substitute GGG crystal is mixed as the application realizing mode-locked laser output services material.
The present invention mixes part Lu at the Dodecahedral sites of Yb-Gd-Ga doped garnet (Yb:GGG) crystal
3+ytterbium lutetium substitute GGG crystal (Yb:LGGG) is mixed in acquisition.This crystal not only with Yb-Gd-Ga doped garnet isostructural, be a kind of working-laser material of excellent property, but also possess following superiority: 1. Lu
3+introducing make crystalline structure become more complicated and unordered, and Gd
3+and Lu
3+at Yb
3+around stochastic distribution can cause active ions ligand field uneven, and these factors can bring the spectrum inhomogeneous broadening of crystal, are conducive to the running of ultrafast laser; 2. the less Lu of dopant ion radius is passed through
3+can make to mix Yb in ytterbium lutetium substitute GGG crystal
3+effective segregation coefficient trend ideal value 1, solve the problems such as constitutional supercooling, growth interface be unstable, be conducive to crystal mass and improve.3. mixing ytterbium lutetium substitute GGG crystal is a kind of new pattern laser material, does not also mix the relevant report of ytterbium lutetium substitute GGG crystal as laser crystals both at home and abroad at present.
The present invention adopts Czochralski grown to mix ytterbium lutetium substitute GGG crystal, and simple to operate, growth cycle is short; The crystal of preparation have can highly doped (without concentration quenching), upper level lifetime long, absorb and the advantage such as emission spectrum bandwidth, quantum yield are high, calorifics and spectrum property excellence, and planar interface coreless crystal growth can be realized; Large size crucible is used to prepare large size single crystal; The crystal obtained conveniently can be processed into Laser Devices and realize efficient Laser output; The raw material that present method uses all can obtain in market.
Accompanying drawing explanation
Fig. 1 be embodiment 1 prepare the XRD(mixing ytterbium lutetium gadolinium gallium garnet polycrystal powder on) and gadolinium gallium garnet standard diffraction compose (under) contrast.
Fig. 2 is that nearly planar interface prepared by embodiment 1 mixes ytterbium lutetium substitute GGG crystal photo.
Fig. 3 is the laser aid test schematic diagram that embodiment 5 and embodiment 6 use.In figure, 1, semiconductor laser, 2, fiber coupling system, 3, focusing system, 4, concave mirror, 5, mix ytterbium lutetium substitute GGG crystal, 6, saturated absorbing body V
3+: YAG crystal, 7, output coupling mirror.
Fig. 4 is the continuous laser curve of output in embodiment 5.
Fig. 5 is Automatic Diameter Control (ADC) system and device schematic diagram that prior art is weighed.In figure, 21, lifting rod, 22, seed crystal, 23, the crystal of growth, 24, polycrystal melt, 25, Iridium Crucible, 26, quartz sleeve, 27, oxidation zircon sand, 28, radio-frequency coil, 29, zirconium white felt, 30, zirconium white sleeve, 31, support, 32, zircon sand is oxidized, 33, pedestal, 34, automatic control system, 35, DSP intermediate frequency power supply.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, but be not limited thereto.
Embodiment 1:x=0.05, y=0.05, mixing ytterbium lutetium substitute GGG crystal chemical formula is Yb
0.15lu
0.15gd
2.7ga
5o
12
Mix ytterbium lutetium substitute GGG crystal preparation method as follows:
(1) solid sintering technology is adopted to carry out the synthesis of polycrystal
Initial feed is Yb
2o
3, Lu
2o
3, Gd
2o
3and Ga
2o
3, purity is 99.99%.Chemical equation is as follows:
0.15Yb
2O
3+0.15Lu
2O
3+2.7Gd
2O
3+5Ga
2O
3＝2Yb
0.15Lu
0.15Gd
2.7Ga
5O
12
According to Yb
0.15lu
0.15gd
2.7ga
5o
12stoichiometric ratio takes corresponding raw material Yb
2o
3, Lu
2o
3, Gd
2o
3and Ga
2o
3, consider to there is Ga in crystal growing process
2o
3volatilization Sum decomposition, prepare burden time make Ga
2o
3excessive 2wt.% is (with the Ga stoichiometrically calculated
2o
3quality meter).Then put into mixer fully to mix, mixing time is 48 hours.After batch mixing, with hydropress, raw material is pressed into cylindrical block, put into corundum crucible, sintering oven is adopted to calcine 30 hours at 1300 DEG C, can obtain and mix ytterbium lutetium gadolinium gallium garnet polycrystal, as shown in Figure 1, in figure, each peak and gadolinium gallium garnet standard diffraction collection of illustrative plates coincide good its powder X-ray RD, show that synthesized is high-purityly mix ytterbium lutetium gadolinium gallium garnet polycrystal.
(2) melt Czochralski grown is adopted to mix ytterbium lutetium substitute GGG crystal
In whole crystal growing process, be full of argon gas in burner hearth as shielding gas, prevent Iridium Crucible to be oxidized.The detailed process of crystal growth comprises: the ytterbium lutetium gadolinium gallium garnet polycrystal of mixing sintered is placed in clean Iridium Crucible, crucible size is Φ 60mm × 35mm, Frequency Induction Heating material, and under overheated about 20 DEG C conditions constant temperature 20-60min, melt is fully mixed, and reduces the crystallite existed in melt.Subsequently slowly under enter Nd:GGG seed crystal, regulate temperature of sowing and make the micro-molten receipts footpath of seed crystal, when seed crystal diameter receive thin to 2-3mm time, enter Automatic Diameter Control program and carry out the stages such as shouldering, isometrical, ending.Pulling rate in process of growth and rotating speed be respectively 1 milli m/h and 20-25 rev/min.Crystal growth to about 53mm(height) time carry de-crystal, be then slowly down to room temperature by 50-55 DEG C/h of speed, come out of the stove.
Automatic Diameter Control of more than weighing (ADC) system is prior art, and device schematic diagram as shown in Figure 5.
After crystal growth terminates, carrying out high temperature air ambient anneal to mixing ytterbium lutetium substitute GGG crystal, to eliminate the Lacking oxygen that thermal stresses in crystal and anaerobic environment cause, improving crystal mass.Concrete cycle of annealing is: being warmed up to 1400 DEG C of constant temperature 15 hours by growing the ytterbium lutetium substitute GGG crystal of mixing obtained, then slowly dropping to room temperature.Fig. 2 grows the photo that the nearly planar interface obtained mixes ytterbium lutetium substitute GGG crystal, and crystalline size is Φ 26mm × 30mm, and profile is complete, without cracking.
Embodiment 2:x=0.05, y=0.15, mixing ytterbium lutetium substitute GGG crystal chemical formula is Yb
0.45lu
0.15gd
2.4ga
5o
12
According to Yb
0.45lu
0.15gd
2.4ga
5o
12stoichiometric ratio takes corresponding raw material Yb
2o
3, Lu
2o
3, Gd
2o
3and Ga
2o
3, and make Ga
2o
3excessive 3wt.% is (with the Ga stoichiometrically calculated
2o
3quality meter), then fully mix, mixing time is 50 hours.With hydropress, raw material is pressed into cylindrical block, puts into corundum crucible, adopt sintering oven to calcine 30 hours at 1350 DEG C, ytterbium lutetium gadolinium gallium garnet polycrystal must be mixed.
(2) crystal growth
As in embodiment 1 as described in step (2), difference is: in crystal growing process, pulling rate is down to: 0.5mm/ hour; Crystal growth is complete carry de-after, rate of temperature fall is 40 DEG C/h.
Embodiment 3:
As described in Example 1, difference is the synthesis adopting liquid phase method to carry out polycrystal
By raw material Yb
2o
3, Lu
2o
3, Gd
2o
3and Ga
2o
3with concentrated nitric acid (massfraction is about 65%) reaction, and the hydrochloric acid (massfraction is about 35%) adding raw material total mass 10% promotes reaction process, obtains Yb (NO
3)
3, Lu (NO
3)
3, Gd (NO
3)
3with Ga (NO
3)
3four kinds of nitrate mixed solutions, then regulate mixing solutions pH value to 4.5 with ammoniacal liquor, then slowly add 2molL
-1ammonium bicarbonate soln, until do not have bubble to produce in solution, now pH=7.By the precipitation of gained through centrifuge out, centrifugal again with distilled water wash subsequently, repeatable operation twice.Then precipitation loft drier is dried, calcine 10 hours at 800 DEG C after being pressed into thin slice with pressing machine, obtain the polycrystal mixing ytterbium lutetium gadolinium gallium garnet.
Embodiment 4:x=0.25, y=0.45, mixing ytterbium lutetium substitute GGG crystal chemical formula is Yb
1.35lu
0.75gd
0.9ga
5o
12
As described in Example 1, difference is: according to Yb
1.35lu
0.75gd
0.9ga
5o
12stoichiometric ratio takes corresponding raw material Yb
2o
3, Lu
2o
3, Gd
2o
3and Ga
2o
3, consider to there is Ga in crystal growing process
2o
3volatilization Sum decomposition, prepare burden time make Ga
2o
3excessive 2wt.% is (with the Ga stoichiometrically calculated
2o
3quality meter).
The ytterbium lutetium gadolinium gallium garnet polycrystal of mixing sintered is placed in Iridium Crucible, and heating makes polycrystal material, and overheated 20 DEG C of constant temperature 40min make melt fully mix, subsequently slowly under enter Nd:GGG seed crystal.Pulling rate in process of growth and rotating speed be respectively 1.5 milli m/h and 25-30 rev/min.Crystal growth carries de-crystal to during about 45mm, is then slowly down to room temperature by 30-40 DEG C/h of speed, comes out of the stove.
Embodiment 5:
Realize continuous laser near 1025nm with the Laser Devices of embodiment 1 laser crystals manufacture to export, laser testing device (during continuous laser running, needs to remove saturated absorbing body V in figure as shown in Figure 3
3+: YAG crystal 6), along light path successively by semiconductor laser 1, fiber coupling system 2, focusing system 3, concave mirror 4, mix ytterbium lutetium substitute GGG crystal 5, saturated absorbing body V
3+: YAG crystal 6, output coupling mirror 7 form.
Test sample Yb
0.15lu
0.15gd
2.7ga
5o
12crystal, is of a size of 4mm × 4mm × 5mm, and logical light face is plated film, and wrap with indium foil and be put in the aluminium block of water-cooled, the temperature of water coolant maintains 16 DEG C.The radius-of-curvature of concave mirror 4 is 100mm, front surface plates the deielectric-coating (940nm place light wave reflection rate is less than 0.5%) of anti-reflection 940nm, and high 942nm is thoroughly plated and the deielectric-coating of high anti-1010-1100nm (1010-1100nm place light wave reflection rate is greater than 99.8%) in rear surface; Plane mirror 7 is output coupling mirrors, is respectively 1% and 5% in the transmitance at 1010 ~ 1070nm place.Pumping source is semiconductor laser 1, its exportable Maximum pumping is 30W, the centre wavelength of launching is 942nm, spot radius and numerical aperture are respectively 400 μm and 0.22, by fiber coupling system 2 and focusing system 3, pump light is focused on and mixes in ytterbium lutetium substitute GGG crystal 5, then by saturated absorbing body V
3+: YAG crystal 6, output coupling mirror 7 Output of laser.Resistance dynamometer (Fieldmax II, Coherent) testing laser is adopted to export mean power.Laser cavity is long is optimized for 20mm, when outgoing mirror transmitance is 5%, realizes maximum continuous laser output rating 4.3W near 1025nm, as shown in Figure 4.
Embodiment 6: realize passively Q switched laser near 1025nm with the Laser Devices of the laser crystals manufacture of embodiment 2 and export.
The laser aid in embodiment 5 is adopted to carry out passively Q switched laser test.V
3+: YAG crystal is as saturated absorbing body, and its size and initial transmitance are respectively 3mm × 3mm × 2mm and 97%.Laser pulse signal is by Tyke oscilloscope TektronixDPL7104(bandwidth 1GHz, sample rate 5Gs/s) and photodetector (Newfocus, model 1611, lift velocity≤1ns) carry out record.Under pump light effect, passively Q switched laser near 1025nm can be realized and export.
Claims (6)
1. mix a preparation method for ytterbium lutetium substitute GGG crystal, described in mix ytterbium lutetium substitute GGG crystal molecular formula be (Yb
ylu
xgd
1-x-y)
3ga
5o
12, 0<x<1,0.01≤y≤0.5, and x+y≤1; Adopt melt Czochralski grown, step is as follows:
(1) polycrystal synthesis
By molecular formula (Yb
ylu
xgd
1-x-y)
3ga
5o
12stoichiometric ratio, takes raw material Yb
2o
3, Lu
2o
3, Gd
2o
3and Ga
2o
3, and make Ga more on this basis
2o
3excessive 1-3wt.%, with the Ga stoichiometrically calculated
2o
3quality meter; Solid sintering technology or liquid phase method synthesis is adopted to mix the polycrystal of ytterbium lutetium gadolinium gallium garnet;
(2) crystal growth
Obtained polycrystal is loaded in Iridium Crucible, load lifting furnace, vacuumize, fill protection gas argon gas or nitrogen; Intensification makes polycrystal melt, and after melt fully mixes, lower seed crystal, starts growing crystal; Pull rate: 0.5-5mm/ hour, rotating speed: 5-60 rev/min; When crystal growth is to desired size, carry de-crystal, cool to room temperature with the speed of 10-60 DEG C/h, come out of the stove; Crystal after coming out of the stove is annealed in atmosphere, and annealing temperature is 1200-1500 DEG C.
2. mix the preparation method of ytterbium lutetium substitute GGG crystal as claimed in claim 1, described in it is characterized in that, mix x=0.05-0.25, y=0.05-0.45 in the molecular formula of ytterbium lutetium substitute GGG crystal.
3. mix the preparation method of ytterbium lutetium substitute GGG crystal as claimed in claim 1, described in it is characterized in that, mix x=0.05, y=0.05-0.15 in the molecular formula of ytterbium lutetium substitute GGG crystal.
4. mix the preparation method of ytterbium lutetium substitute GGG crystal as claimed in claim 1, it is characterized in that Ga in step (1)
2o
3excessive 2wt.%.
5. mix the preparation method of ytterbium lutetium substitute GGG crystal as claimed in claim 1, it is characterized in that described in step (2), seed crystal is Nd:GGG crystal.
6. mix the preparation method of ytterbium lutetium substitute GGG crystal as claimed in claim 1, when it is characterized in that growing crystal in step (2), pull rate: 1-3mm/ hour, rotating speed 20-25 rev/min.
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| CN101654807A (en) * | 2009-09-18 | 2010-02-24 | 广州半导体材料研究所 | Tombarthite and ytterbium ion activation garnet scintillation crystal containing lutetium, yttrium and aluminum and preparation method thereof |
| CN101768779A (en) * | 2009-11-06 | 2010-07-07 | 中国科学院上海光学精密机械研究所 | Yb3+ or Nd3+ doped yttrium-lutetium-aluminum garnet laser crystal and growing method thereof |
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| EP3851562A4 (en) * | 2019-08-21 | 2022-02-09 | Meishan Boya Advanced Materials Co., Ltd. | Multi-component garnet-structured scintillation crystal growth method and equipment |
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