CN1664178A - Tungstate laser crystal and its preparation method and use - Google Patents
Tungstate laser crystal and its preparation method and use Download PDFInfo
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- CN1664178A CN1664178A CN 200410007185 CN200410007185A CN1664178A CN 1664178 A CN1664178 A CN 1664178A CN 200410007185 CN200410007185 CN 200410007185 CN 200410007185 A CN200410007185 A CN 200410007185A CN 1664178 A CN1664178 A CN 1664178A
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Abstract
A sort of tungstic laser crystal, in addition to the method of making it and its usage, relates to the laser crystal material field. The molecular formula of the crystal is R2xM2(1-x)(WO4)3. The crystal has steady property, and don not slake in the air, and can grow by lengthening. Also the crystal can output a series of laser with different wave length in a certain range through the self-Laman effect.
Description
Technical field
The present invention relates to the laser crystals field, especially relate to a class tungstate crystal and a growing and preparing thereof that can be applicable to Solid State Laser.
Background technology
Solid statelaser has advantages such as device compactness, laser beam quality height, stable and reliable operation.Present solid statelaser adopts laser crystals as its operation material mostly.Laser crystals generally is made of host crystal and active ions (transition group or rare earth ion) two portions.Host crystal is one and disperses fixedly " support " of active ions that it makes the interaction of active ions unlikely too strong, has guaranteed the desired line spectrum characteristic of Laser emission on the one hand; On the other hand it in the active ions line shift, divide, widen, play an important role in energy shifts and Laser emission is indispensable radiation and the nonradiative process.At present, the more tungstate laser host crystal of research mainly contains KY (WO
4)
2, KGd (WO
4)
2, PbWO
4Deng.These crystal not only physical and chemical performance are stable, and preparation cost is cheap, and has stronger excited Raman effect, can will export Wavelength of Laser by the excited Raman effect of self and suitably move, and with the needs that are more suitable for using, thereby are subjected to paying close attention to widely.
Summary of the invention
The molecular formula of laser crystals of the present invention is R
2xM
2 (1-x)(WO
4)
3, wherein M is rare earth or trivalent transition metal, is the combination of a certain element in Ti, Cr, Y, Sc and the lanthanon or some elements, R
3+For the part of determining according to factors such as pumping source, laser cavity and application needs substitutes M in the crystal substrate
3+Certain rare earth of ion position or transition metal ion (R=Ti, Cr, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm, Yb etc.), generally be referred to as active ions, the value of x can change between 0 to 1 according to doping ionic species and laser operation needs.The molecular formula of such laser crystals also can be write as R
3+: M
2(WO
4)
3This crystalloid belongs to oblique system, and spacer is C2/c.This crystal deliquescence not in air.This crystalloid is except the characteristic spectral line that group of the lanthanides or transition metal bring, and is transparent at 350nm to 3000nm wave band.
Laser crystals provided by the invention can mix transition group or rare earth ion as sensitizing agent.
The present invention adopts following growing and preparing technology: take by weighing and meet R
2xM
2 (1-x)(WO
4)
3The rare earth of mol ratio or trivalent transition metal oxide M
2O
3, transition group or rare earth oxide R
2O
3With the WO about excessive 1.5mol%
3Place the agate mortar ground and mixed even together.With oil press with 2.5/cm
2Pressure be pressed into thin slice, be enclosed in the crystal growth temperature interval do not occur being out of shape, softening and with the crucible that the high temperature materials such as metal, alloy or oxide compound of crystal composition react with are made, place retort furnace 950 ℃ of sintering 24 hours.The crucible of then solid state reaction synthetic product being packed into places crystal pulling growth stove, and fusing heats up.The condition of growth is: about 1090 ℃ of temperature of fusion, exceeding 30 ℃ of left and right sides constant temperature of fusing point 3 hours, and slowly be cooled to above about 5 ℃ of fusing point, introduce seed crystal.Through introduce a fine variety, shouldering, isodiametric growth, pulling rate 0.5～1mm/h, rotating speed 15～20rpm, the solid-liquid interface temperature head is 10～30 ℃ longitudinally, process of growth is finished in annealing at last, obtains to satisfy the high optical quality single crystal of laser work needs.
R of the present invention
2xM
2 (1-x)(WO
4)
3Crystalloid has good optical, machinery and thermal conductivity, higher chemical stability, and stronger excited Raman effect, and can use Czochralski grown, preparation cost is lower.This crystalloid can be used as the working medium of solid statelaser, is exported Solid State Laser by photoflash lamp, semiconductor laser or other light sources pumping.Can also be by the Raman effect a series of different wavelength of laser of output in certain wavelength region of self.
Embodiment
Example 1: the Nd that takes by weighing 2.76g
2O
3, 86.33g La
2O
3WO with 192.85g
3, place the agate mortar ground and mixed even together these three kinds of raw materials, use oil press with 2.5/cm
2Pressure be pressed into thin slice, place retort furnace 950 ℃ of sintering 24 hours.φ 40 * 40mm then packs solid state reaction synthetic product into
3Platinum crucible, place crystal pulling growth stove, fusing heats up.The condition of growth is: about 1090 ℃ of temperature of fusion, exceeding 30 ℃ of left and right sides constant temperature of fusing point 3 hours, and slowly be cooled to above about 5 ℃ of fusing point, introduce seed crystal.Through introduce a fine variety, shouldering, isodiametric growth, pulling rate 0.5～1mm/h, rotating speed 15～20rpm, the solid-liquid interface temperature head is 10～30 ℃ longitudinally, process of growth is finished in annealing at last.Growth obtains size greater than φ 15 * 20mm
3High-quality transparent single crystal Nd
0.06La
1.94(WO
4)
3This crystal deliquescence not in air, its cell parameter is a=7.878 , b=11.839 , c=11.657 , α=γ=90 °, β=109.3 °, D=6.52g/cm
3The specific refractory power at this crystal 1060nm wavelength place is 1.96, and the emission cross section at 1058nm place is 1.12 * 10
-19Cm
2, fluorescence lifetime is 112 microseconds.
Example 2: the Er that takes by weighing 2.10g
2O
3, 87.22g La
2O
3WO with 192.80g
3, place the agate mortar ground and mixed even together these three kinds of raw materials, use oil press with 2.5/cm
2Pressure be pressed into thin slice, place retort furnace 950 ℃ of sintering 24 hours.φ 40 * 40mm then packs solid state reaction synthetic product into
3Platinum crucible, place crystal pulling growth stove, fusing heats up.The condition of growth is: about 1090 ℃ of temperature of fusion, exceeding 30 ℃ of left and right sides constant temperature of fusing point 3 hours, and slowly be cooled to above about 5 ℃ of fusing point, introduce seed crystal.Through introduce a fine variety, shouldering, isodiametric growth, pulling rate 0.5～1mm/h, rotating speed 15～20rpm, the solid-liquid interface temperature head is 10～30 ℃ longitudinally, process of growth is finished in annealing at last.Growth obtains size greater than φ 15 * 20mm
3High-quality transparent single crystal Er
0.04La
1.96(WO
4)
3The specific refractory power at this crystal 1550nm wavelength place is 1.94, and the emission cross section at 1535nm place is 4.14 * 10
-21Cm
2, fluorescence lifetime is 5.74 milliseconds.
Example 3: the Yb that takes by weighing 5.55g
2O
3, 87.23g La
2O
3WO with 199.0g
3, place the agate mortar ground and mixed even together these three kinds of raw materials, use oil press with 2.5/cm
2Pressure be pressed into thin slice, place retort furnace 950 ℃ of sintering 24 hours.φ 40 * 40mm then packs solid state reaction synthetic product into
3Platinum crucible, place crystal pulling growth stove, fusing heats up.The condition of growth is: about 1090 ℃ of temperature of fusion, exceeding 30 ℃ of left and right sides constant temperature of fusing point 3 hours, and slowly be cooled to above about 5 ℃ of fusing point, introduce seed crystal.Through introduce a fine variety, shouldering, isodiametric growth, pulling rate 0.5～1mm/h, rotating speed 15～20rpm, the solid-liquid interface temperature head is 10～30 ℃ longitudinally, process of growth is finished in annealing at last.Growth obtains size greater than φ 15 * 20mm
3High-quality transparent single crystal Yb
0.1La
1.9(WO
4)
3The peak value of this crystal absorption spectrum is 975nm, and absorption cross is 5.6 * 10
-21Cm
2, halfwidth is 40nm; Emission spectra peak is 1010nm, and emission cross section is 7.0 * 10
-21Cm
2, halfwidth is 51nm.
Claims (7)
1. tungstate laser crystal, it is characterized in that: this crystalline molecular formula is R
2xM
2 (1-x)(WO
4)
3, the value of x changes between 0 to 1, and wherein M is the combination of a certain element or some elements in Ti, Cr, Y or Sc or the lanthanon, R
3+Be Ti, Cr, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm or Yb.
2. laser crystals as claimed in claim 1 is characterized in that: this crystalline molecular formula is Nd
2xLa
2 (1-x)(WO
4)
3, the value of x changes between 0 to 1, and this crystalloid belongs to oblique system, and spacer is C2/c.
3. laser crystals as claimed in claim 2 is characterized in that: this crystalline molecular formula is Nd
0.06La
1.94(WO
4)
3, its cell parameter is a=7.878 , b=11.839 , c=11.657 , α=γ=90 °, β=109.3 °, D=6.52g/cm
3, the specific refractory power at this crystal 1060nm wavelength place is 1.96, the emission cross section at 1058nm place is 1.12 * 10
-19Cm
2, fluorescence lifetime is 112 microseconds.
4. laser crystals as claimed in claim 1 or 2 is characterized in that: this crystal at doping transition group or rare earth ion as sensitizing agent.
5. laser crystals as claimed in claim 1 or 2 is characterized in that: adopt the pumping source of semiconductor laser as this solid statelaser.
6. the preparation method of the laser crystals of a claim 2 is characterized in that: take by weighing and meet R
2xM
2 (1-x)(WO
4)
3The rare earth of mol ratio or trivalent transition metal oxide M
2O
3, transition group or rare earth oxide R
2O
3With the WO about excessive 1.5mol%
3Ground and mixed is even, and 1090 ℃ of temperature of fusion are exceeding 30 ℃ of constant temperature of fusing point 3 hours, slowly is cooled to above 5 ℃ of fusing point, through introduce a fine variety, shouldering, isodiametric growth, pulling rate 0.5～1mm/h, rotating speed 15～20rpm, the solid-liquid interface temperature head is 10～30 ℃ longitudinally.
7. the purposes of claim 1 or 2 laser crystals, it is characterized in that: this crystal is as the solid statelaser operation material.
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|---|---|---|---|
| CN 200410007185 CN1664178A (en) | 2004-03-02 | 2004-03-02 | Tungstate laser crystal and its preparation method and use |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410007185 CN1664178A (en) | 2004-03-02 | 2004-03-02 | Tungstate laser crystal and its preparation method and use |
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ID=35035479
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101928988A (en) * | 2009-06-26 | 2010-12-29 | 中国科学院福建物质结构研究所 | Erbium-doped lithium barium gadolinium tungstate laser crystal as well as preparation method and application thereof |
| CN101676443B (en) * | 2008-09-16 | 2013-04-17 | 中国科学院福建物质结构研究所 | Neodymium-doped cesium lanthanum tungstate laser crystal and preparation method and application thereof |
| CN103254898A (en) * | 2013-03-28 | 2013-08-21 | 中国科学院福建物质结构研究所 | Thulium and dysprosium co-doped sodium yttrium tungstate white luminescent material and its use |
| CN104671784A (en) * | 2015-02-03 | 2015-06-03 | 桂林理工大学 | Temperature stabilizing type high-quality factor microwave dielectric ceramic Nd2La2W3O15 and preparation method thereof |
| CN105586639A (en) * | 2016-02-29 | 2016-05-18 | 江南大学 | Preparation method of second-order nonlinear optical crystal material {[Tb(NMP)7][WS4Ag3I4]} |
-
2004
- 2004-03-02 CN CN 200410007185 patent/CN1664178A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101676443B (en) * | 2008-09-16 | 2013-04-17 | 中国科学院福建物质结构研究所 | Neodymium-doped cesium lanthanum tungstate laser crystal and preparation method and application thereof |
| CN101928988A (en) * | 2009-06-26 | 2010-12-29 | 中国科学院福建物质结构研究所 | Erbium-doped lithium barium gadolinium tungstate laser crystal as well as preparation method and application thereof |
| CN103254898A (en) * | 2013-03-28 | 2013-08-21 | 中国科学院福建物质结构研究所 | Thulium and dysprosium co-doped sodium yttrium tungstate white luminescent material and its use |
| CN104671784A (en) * | 2015-02-03 | 2015-06-03 | 桂林理工大学 | Temperature stabilizing type high-quality factor microwave dielectric ceramic Nd2La2W3O15 and preparation method thereof |
| CN104671784B (en) * | 2015-02-03 | 2016-11-30 | 桂林理工大学 | Temperature-stable high quality factor microwave dielectric ceramic Nd2la2w3o15and preparation method thereof |
| CN105586639A (en) * | 2016-02-29 | 2016-05-18 | 江南大学 | Preparation method of second-order nonlinear optical crystal material {[Tb(NMP)7][WS4Ag3I4]} |
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