CN102181931A - Erbium-doped lutetium silicate laser crystal and preparation method thereof - Google Patents

Erbium-doped lutetium silicate laser crystal and preparation method thereof Download PDF

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CN102181931A
CN102181931A CN 201110071323 CN201110071323A CN102181931A CN 102181931 A CN102181931 A CN 102181931A CN 201110071323 CN201110071323 CN 201110071323 CN 201110071323 A CN201110071323 A CN 201110071323A CN 102181931 A CN102181931 A CN 102181931A
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crystal
sio
crucible
doped lutetium
laser crystal
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丁雨憧
赵广军
董勤
陈建玉
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Shanghai Institute of Optics and Fine Mechanics of CAS
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Abstract

The invention discloses an erbium-doped lutetium silicate laser crystal and a preparation method thereof. The molecular formula of the crystal is (ErxLu1-x)2SiO5, wherein the value range of the x is 0.005 to 0.01. The erbium-doped lutetium silicate laser crystal is grown by adopting a melt method. A commercial InP laser diode and an erbium optical fiber laser device can be used as pumping light sources in the erbium-doped lutetium silicate laser crystal; and the erbium-doped lutetium silicate laser crystal has high emission bandwidth and is favorable for realizing wide wavelength tuning.

Description

Er-doped lutetium oxyorthosilicate laser crystal and preparation method thereof
Technical field
The present invention relates to laser crystals, particularly a kind of er-doped lutetium oxyorthosilicate laser crystal and preparation method thereof, it is suitable for the InP diode and the erbium optical fiber laser carries out the resonance pumping.
Background technology
Erbium ion has abundant energy level, and emission wavelength has 9 transition passages from seeing near infrared.Wherein the Laser emission of 1.5 mu m wavebands corresponding to 4I 13/2→ 4I 15/2Energy level transition.The laser of this wavelength both can be used as the safe laser to human eye, can be used for optical-fibre communications again, so all significant to fields such as laser processing, communication and range findings.
At present, research er-doped laser crystals the most widely is er-doped ionic yttrium aluminum garnet (YAG) crystal, and it has better physical and chemical property, and is easy to grow high quality, large-sized gem-quality crystal.People such as J.W.Kim in 2008 adopt the two optical fiber laser pump Er:YA6 that mix of ytterbium erbium, have obtained the continuous laser output (W.A.Alarkson, Opt.Express 16 (2008) 5807 for D.Y.Shen, J.K.Sahu) of 60W at 1645nm.But it exists spectral line of absorption narrow, is not suitable for the shortcoming of laser diode (abbreviating LD as) pumping, 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 property excellence both at home and abroad at present, and be easy to the high-quality laser crystal material that grows high optical quality, large size and be suitable for the LD pumping.
Silicic acid lutetium crystal (Lu 2SiO 5) belong to oblique system, have two case features of low assymetric crystal structure, torsional deformation, for dopant ion provides stronger crystal field and ligand field, help the splitting of energy levels of dopant ion.Recent years, be mixed with Ho 3+, Yb 3+Lu Deng rare earth ion 2SiO 5Crystal is in the news, and has obtained effective continuous laser output or pulse laser output, but has not seen Er 3+Adulterated Lu 2SiO 5The relevant report of crystalline.
Summary of the invention
The purpose of invention is to provide a kind of er-doped lutetium oxyorthosilicate laser crystal and preparation method thereof, and this laser crystals is a kind ofly can adopt InP diode and the pumping of erbium optical fiber laser resonance, realizes the laserable material of 1.5 mu m waveband lasers running.
Technical solution of the present invention is as follows:
A kind of er-doped lutetium oxyorthosilicate laser crystal, its characteristics are that this crystalline molecular formula is:
(Er xLu 1-x) 2SiO 5, wherein the span of x is 0.005～0.01.
The preparation method of described er-doped lutetium oxyorthosilicate laser crystal, this method comprises the following steps:
1. initial feed adopts Er 2O 3, Lu 2O 3And SiO 2, after the value of selected x, according to the molecular formula (Er of er-doped lutetium oxyorthosilicate laser crystal xLu 1-x) 2SiO 5, x in molar ratio: (1-x): 1 prepares burden, accurately each raw material of weighing;
2. with the even back briquetting on hydropress of raw material thorough mixing, in the alumina crucible of packing into then, put sintering in the retort furnace into, be warming up to 1200 ℃ with 10 hours, be incubated after 10 hours again with being cooled to room temperature in 10 hours;
3. the piece material is taken out and put into crucible, adopt melt method for growing er-doped lutetium oxyorthosilicate laser crystal.
Described melting method is a crystal pulling method, and described crucible is an iridium crucible, and seed crystal is the Lu of b axle 2SiO 5Single crystal rod, crystal growth is in high-purity N 2Carry out in the atmosphere, adopt Frequency Induction Heating raw material to be melted fully to～2150 ℃, then by weight sensing control crystal growth size.Pull rate is 1～3mm/h, and speed of rotation is 15～30rpm.
Described melting method is a temperature gradient method, and described crucible is a molybdenum crucible, puts into b at the bottom of the crucible to Lu 2SiO 5Single crystal rod is as seed crystal, and crystal growth is in high-purity N 2Carry out in the atmosphere, persistently overheating with graphite resistance to 2150 ℃, and after keeping 0.5～2 hour, lower the temperature and growing crystal with the rate of temperature fall of 1～3 ℃/h.
(Er xLu 1-x) 2SiO 5Crystal, Er 3+Replace Lu 3+Case, under the effect of intensive crystal field, the absorption and the spectral line of emission can improve the lasing efficiency of diode pumping, and help wide wavelength tuning all than broad.At concentration of Er is 0.5% o'clock, and the emission cross section at the 1485nm place is 0.58 * 10 -20Cm 2, absorb bandwidth up to 13nm, be 7 times of Er:YAG crystal (1.9nm).
Characteristics of the present invention are to adopt melt method for growing to go out a kind of superior in quality er-doped lutetium oxyorthosilicate laser crystal, can adopt business-like InP laser diode as highly effective pump light source, and have big bandwidth of an emission, help wide wavelength tuning.
Description of drawings
Fig. 1 is (Er 0.005Lu 0.995) 2SiO 5Crystalline absorbs and spectrum;
Fig. 2 is (Er 0.005Lu 0.995) 2SiO 5The crystalline gain trace.
Embodiment
Below in conjunction with
The invention will be further described for embodiment and accompanying drawing, but should not limit transformation range of the present invention with this.
Embodiment 1.
With Er 2O 3, Lu 2O 3And SiO 2High pure raw material is according to the x=0.005 weighing.Mix back briquetting on hydropress, in the alumina crucible of packing into, put sintering in the retort furnace into, be warming up to 1200 ℃ with 10 hours, be incubated after 10 hours and be cooled to room temperature with 10 hours again, make it that solid state reaction take place, synthetic er-doped silicic acid lutetium (abbreviating Er:LSO as) polycrystalline; Polycrystalline piece material is put in the iridium crucible, adopts Czochralski grown Er:LSO monocrystalline, concrete steps are as follows:
1. polycrystalline piece material is put into iridium crucible, place in the lifting furnace, be evacuated to 1～10Pa after shove charge is intact, charge into high-purity N then 2Gas;
2. adopt the Frequency Induction Heating iridium crucible,, polycrystalline piece material is melted fully～2150 ℃ of left and right sides constant temperature 0.5～1 hour;
3. use b to silicic acid lutetium (Lu 2SiO 5) single crystal rod is as seed crystal, in the process of seed crystal down, notice that seed crystal drops to the contact liquid level gradually, whole process is observed seed crystal face and whether is in melting state, and suitably regulates temperature in the body of heater, and it is solid-state that seed crystal is in;
4. pulling rate is 1～3mm/h in the crystal growing process, and rotating speed is 15-30rpm.Pass through necking down successively, shouldering, isodiametric growth when crystal length reaches predetermined size, pulls crystal from melt again, and the speed with 20～30 ℃/h is cooled to room temperature then.
(Er with above-mentioned growth xLu 1-x) 2SiO 5Crystal, dicing behind the optical polish, is at room temperature tested its spectrum property, adopts Lambda 900 spectrophotometers test absorption spectrum.Adopt Fluorolog-3 fluorescence spectrophotometer test infra-red emission, it is the InGaAs laser diode of 980nm that pumping source adopts wavelength.Fig. 1 is (Er 0.005Lu 0.995) 2SiO 5Crystalline absorbs and emmission spectrum, and wherein the strong absorption band of 1450～1570nm wave band helps adopting InP diode and erbium optical fiber laser to carry out the resonance pumping.(Er 0.005Lu 0.995) 2SiO 5The emission cross section of crystal at the 1485nm place is 0.58 * 10 -20Cm 2, absorb bandwidth up to 13nm, be 7 times of Er:YAG crystal (1.9nm).Fig. 2 is (Er 0.005Lu 0.995) 2SiO 5The crystalline gain trace.As shown in the figure, Er:LSO crystalline gain trace presents smooth broad peak, along with population is sent out rate of rotation β and is increased to 0.9 from 0.7, in the gain cross section at 1596nm place from 0.113 * 10 -20Cm 2Increase to 0.161 * 10 -20Cm 2Because 1596nm place atmosphere does not absorb, so can realize laser generation at this wavelength.
Embodiment 2.
With Er 2O 3, Lu 2O 3And SiO 2High pure raw material is according to the x=0.008 weighing.Raw material forms polycrystalline piece material through mixing, compacting and sintering process; Polycrystalline piece material is put into iridium crucible, to adopt Czochralski grown crystal, seed crystal be b to Lu 2SiO 5Single crystal rod, crystal growth is in high-purity N 2Carry out in the atmosphere; Process of growth is with embodiment 1, and different is that pull rate is 1～3mm/h, and speed of rotation is 15～30rpm.
Embodiment 3.
With Er 2O 3, Lu 2O 3And SiO 2High pure raw material is according to the x=0.01 weighing.Raw material forms polycrystalline piece material through mixing, compacting and sintering process; Polycrystalline piece material is put into iridium crucible, adopt Czochralski grown crystal; Seed crystal be b to Lu 2SiO 5Single crystal rod, crystal growth is in high-purity N 2Carry out in the atmosphere.Process of growth is with embodiment 1, and different is that pull rate is 1～3mm/h, and speed of rotation is 15～30rpm.
Embodiment 4.
With Er 2O 3, Lu 2O 3And SiO 2High pure raw material is according to the x=0.005 weighing.Mix back briquetting on hydropress, in the alumina crucible of packing into, put sintering in the retort furnace into, be warming up to 1200 ℃ with 10 hours, be incubated after 10 hours and be cooled to room temperature with 10 hours again, make its generation solid state reaction, synthesize the Er:LSO polycrystalline.
Polycrystalline piece material is put into molybdenum crucible, adopt temperature gradient method growth Er:LSO monocrystalline; Put at crucible bottom seed slot place b to Lu 2SiO 5Single crystal rod is as seed crystal; Be evacuated to 1～10Pa after installing stove, charge into high-purity N then 2Gas; Adopt graphite resistance to be heated to～2150 ℃ of constant temperature 0.5～1 hour, polycrystalline piece material is melted fully, the speed with 1～3 ℃/h is cooled to room temperature then.
Embodiment 5.
With Er 2O 3, Lu 2O 3And SiO 2High pure raw material is according to the x=0.008 weighing.Raw material forms polycrystalline piece material through mixing, compacting and sintering process; Polycrystalline piece material is put into molybdenum crucible, adopt temperature gradient method growth Er:LSO monocrystalline; Crucible bottom be placed with b to Lu 2SiO 5Single crystal rod is in high-purity N 2Growing crystal in the atmosphere, process of growth are with embodiment 4, and different is that rate of temperature fall is 1～3 ℃/h.
Embodiment 6.
With Er 2O 3, Lu 2O 3And SiO 2High pure raw material is according to the x=0.01 weighing.Raw material forms polycrystalline piece material through mixing, compacting and sintering process; Polycrystalline piece material is put into molybdenum crucible, adopt temperature gradient method growth Er:LSO monocrystalline; Crucible bottom be placed with b to Lu 2SiO 5Single crystal rod is in high-purity N 2Growing crystal in the atmosphere, process of growth are with embodiment 4, and different is that rate of temperature fall is 1～3 ℃/h.
The spectrum test of the foregoing description has the result identical with embodiment 1, pardons me and repeats no more.

Claims (4)

1. er-doped lutetium oxyorthosilicate laser crystal is characterized in that this crystalline molecular formula is:
(Er xLu 1-x) 2SiO 5, wherein the span of x is 0.005～0.01.
2. the preparation method of the described er-doped lutetium oxyorthosilicate laser crystal of claim 1 is characterized in that this method comprises the following steps:
1. initial feed adopts Er 2O 3, Lu 2O 3And SiO 2, after the value of selected x, according to the molecular formula (Er of er-doped lutetium oxyorthosilicate laser crystal xLu 1-x) 2SiO 5, x in molar ratio: (1-x): 1 prepares burden, accurately each raw material of weighing;
2. with the even back briquetting on hydropress of raw material thorough mixing, in the alumina crucible of packing into then, put sintering in the retort furnace into, be warming up to 1200 ℃ with 10 hours, be incubated after 10 hours again with being cooled to room temperature in 10 hours;
3. the piece material is taken out and put into crucible, adopt melt method for growing er-doped lutetium oxyorthosilicate laser crystal.
3. the preparation method of er-doped lutetium oxyorthosilicate laser crystal according to claim 2 is characterized in that described melting method is a crystal pulling method, and described crucible is an iridium crucible, and seed crystal is the Lu of b axle 2SiO 5Single crystal rod, crystal growth is in high-purity N 2Carry out in the atmosphere, adopt Frequency Induction Heating raw material to be melted fully to～2150 ℃, then by weight sensing control crystal growth size.Pull rate is 1～3mm/h, and speed of rotation is 15～30rpm.
4. the preparation method of er-doped lutetium oxyorthosilicate laser crystal according to claim 2 is characterized in that described melting method is a temperature gradient method, and described crucible is a molybdenum crucible, puts into b at the bottom of the crucible to Lu 2SiO 5Single crystal rod is as seed crystal, and crystal growth is in high-purity N 2Carry out in the atmosphere, persistently overheating with graphite resistance to 2150 ℃, and after keeping 0.5～2 hour, lower the temperature and growing crystal with the rate of temperature fall of 1～3 ℃/h.
CN 201110071323 2011-03-23 2011-03-23 Erbium-doped lutetium silicate laser crystal and preparation method thereof Pending CN102181931A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101701359A (en) * 2009-11-25 2010-05-05 中国科学院上海光学精密机械研究所 Neodymium-doped lutetium oxyorthosilicate laser crystal and preparation method thereof
CN101709507A (en) * 2009-11-27 2010-05-19 中国科学院上海光学精密机械研究所 Neodymium-doped silicic acid yttrium gadolinium laser crystal and preparation method thereof
CN101717998A (en) * 2009-11-27 2010-06-02 中国科学院上海光学精密机械研究所 Neodymium-doped silicic acid yttrium lutecium laser crystal and preparation method thereof

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101701359A (en) * 2009-11-25 2010-05-05 中国科学院上海光学精密机械研究所 Neodymium-doped lutetium oxyorthosilicate laser crystal and preparation method thereof
CN101709507A (en) * 2009-11-27 2010-05-19 中国科学院上海光学精密机械研究所 Neodymium-doped silicic acid yttrium gadolinium laser crystal and preparation method thereof
CN101717998A (en) * 2009-11-27 2010-06-02 中国科学院上海光学精密机械研究所 Neodymium-doped silicic acid yttrium lutecium laser crystal and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
《Journal of Crystal Growth》 20100330 Yuchong Ding等 Crystal growth and spectroscopic properties of erbium doped Lu2SiO5 2103-2106 第312卷, *

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Application publication date: 20110914