CN102747423A - Cr<3+>:KMgSc(WO4)3 doped tunable laser crystal and method for preparing same - Google Patents

Cr<3+>:KMgSc(WO4)3 doped tunable laser crystal and method for preparing same Download PDF

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Publication number
CN102747423A
CN102747423A CN2012102493396A CN201210249339A CN102747423A CN 102747423 A CN102747423 A CN 102747423A CN 2012102493396 A CN2012102493396 A CN 2012102493396A CN 201210249339 A CN201210249339 A CN 201210249339A CN 102747423 A CN102747423 A CN 102747423A
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crystal
kmgsc
tunable laser
laser
ion
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王国建
王国富
林州斌
张莉珍
黄溢声
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Fujian Institute of Research on the Structure of Matter of CAS
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Fujian Institute of Research on the Structure of Matter of CAS
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Abstract

The invention provides a Cr<3+>:KMgSc(WO4)3 doped tunable laser crystal and a method for the crystal. The crystal belongs to the trigonal system and has the space group as descried in the description and the following cell parameters: a=9.493A, C=24.545A, V=1915.68A<3>, Z=6 and Dc=4.412g/cm<3>. The crystal can be grown by using flux growth method, wherein the 60-80at% K2W2O7 is used as flux, the temperature decreasing speed is 1-5 DEG C per day, and the rotating speed is 5-30rpm. The high-quality large-size Cr<3+>:KMgSc(WO4)3 crystal has the tunable range of 710-1300nm and is expected to become a novel tunable laser crystal for practical application.

Description

Mix chromium potassium wolframate magnesium scandium tunable laser crystal and preparation method thereof
Technical field
The present invention relates to technical field of optoelectronic functional materials, especially relate to a kind of laser crystal material as the operation material in the tunable solid laser apparatus.
Background technology
Tunable laser is meant a kind of like this effect: pump excitation is mixed the active ions in the Solid State Laser matrix; Make generation laser, adopt prism tuning method, F-P etalon tuning method, grating tuning method, color filter tuning method and distributed feed-back system tuning method etc. to obtain tunable laser output.
People such as L.F. Johnson adopted flash lamp pumping in 1963, were mixing Ni 2+MgF 2Realized first solid adjustable laser operation (L.F. Johnson R.E. Dietz & H.J. Guggenheim, J.Phys.Rev.Lett., 11 (1963) 318) in the crystal.A lot of tunable laser crystals have appearred subsequently, like Ti 3+: Al 2O 3, Cr 3+: Mg 2SiO 4, Cr 3+: LiSrAlF 6, Cr 3+: BeAl 2O 4Deng, but because a variety of causes, many tunable laser crystals are only limited to makes laboratory tool, can't push industrial application to.The tunable laser crystal maximum, that got into Application Areas of research at present is Cr 3+: BeAl 2O 4(alexandrite crystal), Ti 3+: Al 2O 3(titanium-doped sapphire) and Cr 3+: LiCaAlF 6, Cr 3+: LiSrAlF 6, but the defective that they also all exist some to be difficult to avoid makes their range of application be restricted.
Cr 3+: BeAl 2O 4(alexandrite crystal) crystalline main drawback is: tuning range is between 700 ~ 800nm, and emission cross section is little by (6 * 10 -21Cm 2), required pumping threshold is high, but also has shortcomings such as high damage rate and high thermal lensing effect, in addition because the BeO severe toxicity also brings very big difficulty to growth.
Ti 3+: Al 2O 3The crystalline main drawback is: Ti in this crystal 3+-Ti 4+The appearance of pair ion; Make at laser output wave band; Be that absorbing appears in near-infrared band, influenced its laser activity, and because its upper laser level life-span short (having only 3.2 μ s); Need also further limit its application with short-pulse laser, Q-switch laser, continuous wave laser or the flash lamp pumping that produces special short pulse.
Cr 3+: LiCaAlF 6, Cr 3+: LiSrAlF 6Plurality of advantages such as although crystal has the tuning range broad, emission cross section is big, and required pumping threshold is low.But also exist problems such as uptake factor is little, the lasing efficiency of LD pumping is low.Therefore, it is wideer to seek tunable range, and can directly use the tunable laser crystal material of photoflash lamp and LD pumping to become one of focus of present laser crystals research field.
Summary of the invention
The object of the invention just is to develop a kind of new tunable laser crystal, and it can directly use photoflash lamp and LD pumping, has the tunable range of broad.
Potassium wolframate magnesium scandium (KMgSc (WO 4) 3) be a kind of newfound compound, it belongs to trigonal system, has The spacer structure is a kind of good laser host material.Chromium ion can more easily mix in the lattice as the laser active ion, replaces the crystallographic site of scandium or mg ion, and its doping content is between 0.2at% ~ 5at%.The room temperature fluorescence life-span (τ) of this doped crystal is 10 ~ 30 μ s, and its fluorescence lifetime is the function of chromium ion concentration, can mix the chromium ion of different concns according to different needs.Experimental result shows that its tunable range between 710 ~ 1300nm, can be used as tunable laser crystal.
Technical scheme of the present invention is following:
Concrete reaction formula: K 2CO 3+ 2MgO+ Sc 2O 3+ 6WO 3=2KMgSc (WO 4) 3+ CO 2
K 2CO 3+?2WO 3?=?K 2W 2O 7+?CO 2
Used material purity and producer:
The medicine name Purity Producer
Sc 2O 3 99.999% Changchun Inst. of Applied Chemistry, Chinese Academy of Sciences
Cr 2O 3 99.95% Shanghai chemical reagents corporation of Chinese Medicine group
K 2CO 3 99.9% Shanghai chemical reagents corporation of Chinese Medicine group
WO 3 99.99% Shanghai chemical reagents corporation of Chinese Medicine group
MgO 99.9% Shanghai chemical reagents corporation of Chinese Medicine group
We have found the case of flux methods growth to mix chromium potassium wolframate magnesium scandium [Cr through experiment 3+: KMgSc (WO 4) 3] the comparatively ideal fusing assistant of crystalline: K 2W 2O 7, and best growth conditions, and grown high-quality crystal Cr 3+: KMgSc (WO 4) 3(seeing embodiment 1 and 2).Chromium potassium wolframate magnesium scandium crystal is mixed in the case of flux methods growth, and its main growth conditions is following: used fusing assistant is K 2W 2O 7, the concentration of fusing assistant is between 60 ~ 80at%, and growth temperature is between 750 ~ 850 ℃, and rate of temperature fall is 1 ~ 5 ℃/day, and the crystal rotating speed is 5 ~ 30rpm.
With the Cr that grows 3+: KMgSc (WO 4) 3Crystal has carried out the collection of diffraction data on four-circle diffractometer, structural analysis shows that it belongs to trigonal system, Spacer, concrete unit cell parameters: a=9.493, c=24.545, V=1915.68 3, Z=6, D c=4.412 g/cm 3
With the Cr that grows 3+: KMgSc (WO 4) 3Crystal carries out the analytical test of absorption spectrum, fluorescence spectrum and fluorescence lifetime etc.From Cr 3+: KMgSc (WO 4) 3Absorption spectrum under the crystalline room temperature; It is thus clear that two strong absorption bands are arranged between 400 ~ 600nm and 610 ~ 820nm; Its peak value is respectively 478nm and 689nm, and two absorption bandwidth all are about 150nm, can adopt photoflash lamp and LD to carry out pumping; The absorption peak of broad helps the absorption of crystal to pump light, has improved output rating.From Cr 3+: KMgSc (WO 4) 3Fluorescence spectrum under the crystalline room temperature, visible have very strong fluorescent emission at 880nm, and its peak width is 700 ~ 1300nm, and its peak width at half is 215nm, and emission cross section is 2.2 * 10 -20Cm 2, fluorescence lifetime is 26 μ s, can between 710 ~ 1300 nm, carry out tuning.
The chromium potassium wolframate magnesium scandium tunable laser crystal of mixing of the present invention; Have and enough flux methods to grow superior in quality crystal easily; Growth technique is stable, good heat-conducting, good optical characteristics; Raw material is easy to get, the tunable laser wide waveband, can directly use plurality of advantages such as photoflash lamp and LD pumping, and this crystal can be used as a kind of laser crystals preferably.
Embodiment
Below in conjunction with specific embodiment, the present invention is described further, but should limit protection scope of the present invention with this.
Embodiment 1: with K 2W 2O 7For the fluxing agent growth doping content is 1.0at.%Cr 3+Cr 3+: KMgSc (WO 4) 3Laser crystals.
Growth raw material is KMgSc (WO 4) 3: K 2W 2O 7=1:4 (mol ratio) mixes the Cr of 1.0at% 3+Ion.Adopt flux method, in φ 60 * 50mm platinum alloy crucible, growth temperature is between 820 ~ 750 ℃, and with 1 ℃/day rate of temperature fall, 5 rev/mins crystal rotating speed has grown and has been of a size of 25 * 25 * 10mm 3High-quality Cr 3+: KMgSc (WO 4) 3Crystal.Cr in ICP (plasma emission spectrum) analysis revealed crystal 3+Ion content is 0.5 at%.
Embodiment 2: with K 2W 2O 7For the fluxing agent growth doping content is 2.0at.%Cr 3+Cr 3+: KMgSc (WO 4) 3Laser crystals.
Growth raw material is KMgSc (WO 4) 3: K 2W 2O 7=2:3 (mol ratio) mixes the Cr of 2.0at% 3+Ion.Adopt flux method, in φ 60 * 50mm platinum alloy crucible, growth temperature is between 850 ~ 770 ℃, and with 3 ℃/day rate of temperature fall, 30 rev/mins crystal rotating speed has grown and has been of a size of 15 * 15 * 10mm 3High-quality Cr 3+: KMgSc (WO 4) 3Crystal.Cr in ICP (plasma emission spectrum) analysis revealed crystal 3+Ion content is 1.0 at%.

Claims (3)

1. mix chromium potassium wolframate magnesium scandium tunable laser crystal, it is characterized in that: this crystalline molecular formula is Cr 3+: KMgSc (WO 4) 3, belong to trigonal system, have Spacer structure, unit cell parameters are a=9.493, and c=24.545, V=1915.68 3, Z=6, D c=4.412 g/cm 3, can produce tunable laser.
2. laser crystals as claimed in claim 1 is characterized in that: its valence state of chromium ion as dopant ion is+3 valencys, replaces the crystallographic site of scandium or mg ion, and its doping content is between 0.2at% ~ 5at%.
3. the preparation method of the described laser crystals of claim 1 is characterized in that: this crystal by adopting flux method growth, used fusing assistant is K 2W 2O 7, concentration is between 60at ~ 80at%, and growth temperature is between 750 ~ 850 ℃, and rate of temperature fall is 1 ~ 5 ℃/day, and the crystal rotating speed is 5 ~ 30rpm.
CN2012102493396A 2012-07-19 2012-07-19 Cr<3+>:KMgSc(WO4)3 doped tunable laser crystal and method for preparing same Pending CN102747423A (en)

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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
JP2020512422A (en) * 2017-09-28 2020-04-23 ルミレッズ ホールディング ベーフェー Wavelength conversion material for light emitting devices

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CN103173862A (en) * 2013-03-06 2013-06-26 中国科学院福建物质结构研究所 Chromium-doped calcium magnesium silicate tunable laser crystal and preparation method thereof
CN103173862B (en) * 2013-03-06 2017-08-15 中国科学院福建物质结构研究所 Chromium-doped calcium magnesium silicate tunable laser crystal and preparation method thereof
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
JP2020512422A (en) * 2017-09-28 2020-04-23 ルミレッズ ホールディング ベーフェー Wavelength conversion material for light emitting devices
JP2021185596A (en) * 2017-09-28 2021-12-09 ルミレッズ ホールディング ベーフェー Wavelength converting material for light emitting device
JP7250851B2 (en) 2017-09-28 2023-04-03 ルミレッズ ホールディング ベーフェー Wavelength conversion materials for light emitting devices
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Application publication date: 20121024